Fly ash cleaning method
阅读说明:本技术 飞灰清洗方法 (Fly ash cleaning method ) 是由 陈磊 叶健欣 张燊华 张宇鹏 于 2020-12-28 设计创作,主要内容包括:本发明公开了一种飞灰清洗方法,包括如下步骤:a、将飞灰与酸性溶液混合,恒温搅拌,得到混合液;b、抽滤,保留滤渣;c、将滤渣经水清洗;d、将清洗后的滤渣与二价铁盐溶液混合,并恒温搅拌;e、抽滤,保留滤渣;f、将滤渣与水混合;g、搅拌抽滤,得到滤渣;h、重复步骤f至步骤g1次~3次。本发明提供的飞灰清洗方法,先通过酸洗,将飞灰进行预处理,然后抽滤得到滤渣,然后通过清水对滤渣进行清洗,得到酸处理后的飞灰滤渣,将滤渣与二价铁盐混合,通过二价铁盐将飞灰中的率离子夺取,然后通过清水清洗去除,通过该方法,最终可以将飞灰中的氯元素去除率高达99%。(The invention discloses a fly ash cleaning method, which comprises the following steps: a. mixing the fly ash with the acidic solution, and stirring at constant temperature to obtain a mixed solution; b. performing suction filtration, and keeping filter residue; c. washing the filter residue with water; d. mixing the cleaned filter residue with a ferrous salt solution, and stirring at constant temperature; e. performing suction filtration, and keeping filter residue; f. mixing the filter residue with water; g. stirring and filtering to obtain filter residue; h. repeating the steps f to g1 times to 3 times. The method for cleaning the fly ash comprises the steps of firstly carrying out acid washing, pretreating the fly ash, then carrying out suction filtration to obtain filter residue, then cleaning the filter residue through clear water to obtain the fly ash filter residue after acid treatment, mixing the filter residue with ferrous salt, capturing ions in the fly ash through the ferrous salt, and then cleaning and removing the ions through the clear water, wherein the removal rate of chlorine elements in the fly ash can be up to 99 percent finally.)
1. A fly ash cleaning method is characterized by comprising the following steps:
a. mixing the fly ash with the acidic solution, and stirring at constant temperature to obtain a mixed solution;
b. performing suction filtration, and keeping filter residue;
c. washing the filter residue with water;
d. mixing the cleaned filter residue with a ferrous salt solution, and stirring at constant temperature;
e. performing suction filtration, and keeping filter residue;
f. mixing the filter residue with water;
g. stirring and filtering to obtain filter residue;
h. repeating the steps f to g1 times to 3 times.
2. A fly ash washing method according to claim 1, wherein in step a, the acidic solution is hydrochloric acid or acetic acid.
3. A fly ash washing method according to claim 1, wherein in step d, the ferrous salt is ferrous oxalate, ferrous citrate or ferrous sulfide.
4. A fly ash washing method according to claim 1, wherein in step a, the mass ratio of the fly ash to the acidic solution is 1:7 to 1: 12.
5. A fly ash cleaning method according to claim 1, wherein the pH of the mixed liquid in step a is in the range of 7.1 to 7.8.
6. A fly ash washing method according to claim 1, wherein the fly ash is formed by incineration of domestic waste.
7. A fly ash washing method according to any one of claims 1 to 6, wherein steps b to c are repeated at least twice.
Technical Field
The invention relates to the field of environmental purification, in particular to a fly ash cleaning method.
Background
Prior art of
The components contained in the fly ash from refuse incineration are similar to those of fly ash, and can be used for producing cement instead of lime, and at the same time the temperature in the cement kiln can be up to 1500 deg.C, the heavy metals in the fly ash can be solidified in the cement production process, and the dioxin can be completely destroyed. The firing of cement by using fly ash in Japan has been industrialized, and China has also studied and tried. The main current symptoms are that the fly ash contains more chloride, and chloride ions in the raw materials of cement directly influence the calcination of a preheater and a kiln in the novel dry-process cement production, so that accidents such as ring formation, material blockage and the like are caused, and the normal operation of equipment and the quality of cement clinker are influenced. The chloride ion content of the raw materials must be controlled in the cement production process. In addition, the chlorine in the fly ash can also cause the formation of dioxin in the flue gas of the cement kiln; therefore, when the fly ash is used for producing building materials, reliable and effective measures must be adopted to remove chlorine in the fly ash; the pretreatment such as water washing is one of effective dechlorination methods, and international research is very active at present. However, the effect of water washing to remove chlorine and the optimum parameters are not clear, and we have conducted experimental studies on this.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides a method for cleaning fly ash.
The method comprises the following steps:
a. mixing the fly ash with the acidic solution, and stirring at constant temperature to obtain a mixed solution; b. performing suction filtration, and keeping filter residue; c. washing the filter residue with water; d. mixing the cleaned filter residue with a ferrous salt solution, and stirring at constant temperature; e. performing suction filtration, and keeping filter residue; f. mixing the filter residue with water; g. stirring and filtering to obtain filter residue; h. repeating the steps f to g1 times to 3 times.
Preferably, in step a, the acidic solution is hydrochloric acid or acetic acid.
Preferably, in step d, the ferrous salt is ferrous oxalate, ferrous citrate or ferrous sulfide.
Preferably, in the step a, the mass ratio of the fly ash to the acidic solution is 1: 7-1: 12.
Preferably, the pH range of the mixed solution in the step a is 7.1-7.8.
Preferably, the fly ash is formed by incineration of household waste.
Preferably, the steps b to c are repeated at least twice.
The method for cleaning the fly ash comprises the steps of firstly carrying out acid washing, pretreating the fly ash, then carrying out suction filtration to obtain filter residue, then cleaning the filter residue through clear water to obtain the fly ash filter residue after acid treatment, mixing the filter residue with ferrous salt, capturing ions in the fly ash through the ferrous salt, and then cleaning and removing the ions through the clear water, wherein the removal rate of chlorine elements in the fly ash can be up to 99 percent finally.
Detailed Description
A mass ratio of 60: 20, normal temperature, five times of water washing, 1.20g of ferrous sulfate
First water washing: 20.07g of fly ash is mixed with 60ml of water, and 1.20g of ferrous sulfate is added. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: (ii) 26.88g of fly ash was mixed with 60ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 24.36g of fly ash are mixed with 60ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 23.55g of fly ash were mixed with 60ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 1a mass ratio 60: 20, normal temperature, four times of water washing, 1.20g of ferrous sulfate
TABLE 1b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
1.50ms
563μs
Second washing with water
9.99ms
576μs
217μs
Third time of water washing
9.99ms
306μs
184μs
The fourth time of water washing
3.99ms
236μs
175μs
From this, the dechlorination rate was calculated (for example, ferrous sulfide)
Firstly: 20.07 × 11% ═ 2.2g, 2200 mg/kg;
and (3) finally: (9.99+9.99+9.99+3.99) × 1000 × 0.7 × 11% ═ 2230ppm
2230ppm-230ppm=2000ppm;
1ppm=1mg/l=1mg/kg;
(2000÷2200)×100%=90.9%。
Wherein, 0.7 is the conversion coefficient of the conductivity, 11 percent is the percentage of chlorine in the fly ash, and 230 is the chlorine content of the tap water.
The mass ratio of the two components is 100: 20, normal temperature, five times of water washing:
first water washing:
20.02g of fly ash are mixed with 100ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 22.75g of fly ash and 100ml of water are mixed. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 19.91g of fly ash are mixed with 100ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 17.68g of fly ash was mixed with 100ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: first 16.83g of fly ash are mixed with 100ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 2a mass ratio 100: 20, normal temperature, five times of water washing
TABLE 2b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
8.85ms
1.20ms
Second washing with water
9.99ms
1.93ms
395μs
Third time of water washing
9.38ms
720μs
257μs
The fourth time of water washing
8.17ms
655μs
243μs
Fifth washing with water
7.96ms
590μs
237μs
Three mass ratios of 140: 60, normal temperature and five times of water washing
First water washing: 60.04g of fly ash are mixed with 140ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: (ii) 87.15g of fly ash are mixed with 140ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 60.74g of fly ash was mixed with 140ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 72.04g of fly ash are mixed with 140ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 66.99g of fly ash are mixed with 140ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 3a mass ratio 140: 60, normal temperature and five times of water washing
TABLE 3b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
9.99ms
Second washing with water
9.99ms
9.99ms
2.09ms
Third time of water washing
9.99ms
5.28ms
745μs
The fourth time of water washing
9.99ms
1.65ms
332μs
Fifth washing with water
8.54ms
922μs
243μs
The mass ratio of the four components is 160: 40, washing with water at normal temperature for five times
First water washing: first, 40.03g of fly ash was mixed with 160ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 48.85g of fly ash are mixed with 160ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 42.47g of fly ash are mixed with 160ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 49.50g of fly ash are mixed with 160ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 46.90g of fly ash are mixed with 160ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 4a mass ratio 160: 40, washing with water at normal temperature for five times
TABLE 4b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
9.99ms
2.31ms
Second washing with water
9.99ms
3.73ms
393μs
Third time of water washing
9.99ms
1.59ms
475μs
The fourth time of water washing
9.99ms
1.18ms
409μs
Fifth washing with water
7.66ms
650μs
249μs
And the mass ratio of five is 180: 20, 50 ℃ and seven times of water washing (2)
First water washing: 20.12g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 26.63g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 18.97g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring.
Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously.
And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing:
14.50g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: first 16.25g of fly ash is mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And sixth water washing: first 16.30g of fly ash is mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And seventh water washing: 15.54g of fly ash and 180ml of water are mixed, stirred for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and the conductivity value and the pH value are measured after stirring is finished. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 5a mass ratio 180: 20, 50 ℃ and seven times of water washing (2)
TABLE 5b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
5.04ms
747μs
Second washing with water
9.99ms
980μs
273μs
Third time of water washing
6.69ms
542μs
218μs
The fourth time of water washing
6.74ms
438μs
213μs
Fifth washing with water
6.18ms
326μs
199μs
The sixth washing with water
5.85ms
348μs
200μs
The seventh time of water washing
5.49ms
382μs
200μs
The six mass ratios are 180: washing with water at 20, 50 deg.C for seven times, and microwave treating
First water washing: first 16.10g of fly ash was mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 10.82g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 18.20g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 17.23g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: first 16.85g of fly ash is mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And sixth water washing: 18.20g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And seventh water washing: 15.48g of fly ash are mixed with 180ml of water.
② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring.
Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled.
And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 6a mass ratio 180: washing with water at 20, 50 deg.C for seven times, and microwave treating
TABLE 6b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
5.07ms
778μs
Second washing with water
9.04ms
864μs
257μs
Third time of water washing
6.30ms
513μs
216μs
The fourth time of water washing
6.27ms
401μs
235μs
Fifth washing with water
5.95ms
439μs
218μs
The sixth washing with water
4.64ms
295μs
217μs
The seventh time of water washing
4.46ms
272μs
207μs
The mass ratio of the seven components is 180: washing with water at 20, 50 deg.C for seven times
First water washing: 20.06g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) second water washing: 20.20g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) washing for the third time: 19.81g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed solution is filtered, the filtrate is bottled, the filter residue is continuously washed with water, fourthly, the stock solution is diluted by 10 times and 100 times, and finally, the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times are measured.
Fourth water washing: 17.47g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Fifth water washing: first 16.90g of fly ash is mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity of the stock solution, the diluted stock solution and the diluted pH10 times and 100 times.
And sixth water washing: 15.29g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And seventh water washing: 14.15g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, and filter residue and filtrate are respectively bottled. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Table 7a mass ratio 180: washing with water at 20, 50 deg.C for seven times
TABLE 7b
Stock solution DD
Diluting by 10 times
By a factor of 10
Diluting by 100 times
First washing with water
9.99ms
1.49ms
785μs
Second washing with water
9.99ms
1.10ms
270μs
Third time of water washing
7.86ms
607μs
227μs
The fourth time of water washing
7.83ms
606μs
226μs
Fifth washing with water
7.76ms
620μs
211μs
The sixth washing with water
6.83ms
459μs
222μs
The seventh time of water washing
5.83ms
425μs
221μs
Eight mass ratios of 180: washing with EDTA chitosan at 20, 50 deg.C for five times
First water washing: 20.03g of fly ash are mixed with 180ml of water. 3.18g of EDTA chitosan was added. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing:
24.16g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time:
22.21g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 21.53g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 20.64g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 8a mass ratio 180: washing with EDTA chitosan at 20, 50 deg.C for five times
TABLE 8b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
4.61ms
715μs
Second washing with water
8.35ms
900μs
252μs
Third time of water washing
6.09ms
552μs
203μs
The fourth time of water washing
5.30ms
427μs
196μs
Fifth washing with water
5.29ms
445μs
185μs
Nine mass ratios are 180: washing at 20, 50 deg.C for five times with water, pH 7.5
First water washing: 20.08g of fly ash are mixed with 180ml of water. The pH was adjusted to 7.5 by adding 9ml of glacial acetic acid solution. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 9.51g of fly ash are mixed with 180ml of water. The pH was adjusted to 7.5 by adding 0.5ml of glacial acetic acid solution. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 7.44g of fly ash are mixed with 180ml of water. The pH was adjusted to 7.5 by adding 0.5ml of glacial acetic acid solution. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 8.68g of fly ash are mixed with 180ml of water. The pH was adjusted to 7.5 by adding 0.5ml of glacial acetic acid solution. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 5.69g of fly ash was mixed with 180ml of water. Adding glacial acetic acid solution 0.5ml to adjust pH
7.5. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 9a mass ratio 180: washing at 20, 50 deg.C for five times with water, pH 7.5
TABLE 9b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
8.42ms
1.38ms
Second washing with water
6.28ms
1.03ms
313μs
Third time of water washing
2.41ms
504μs
241μs
The fourth time of water washing
3.71ms
679μs
261μs
Fifth washing with water
2.04ms
603μs
240μs
The mass ratio of ten is 180: washing at 20, 50 deg.C for five times with water, pH 7.7
First water washing: 20.07g of fly ash was mixed with 180ml of water. 10ml of 50% hydrochloric acid solution and 10ml of 80% hydrochloric acid solution were added to adjust the pH to 7.7. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 48.85g of fly ash are mixed with 180ml of water. 2.8ml of 80% hydrochloric acid solution was added to adjust the pH to 7.7. Secondly, stirring for 60 minutes at the normal temperature at the rotating speed of 433r/s, and measuring the conductivity value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the electric conductivity of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 42.47g of fly ash are mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 49.50g of fly ash are mixed with 180ml of water. Adding 1.5ml of 80% hydrochloric acid solution to adjust the pH value to 7.7, stirring at the rotating speed of 433r/s for 60 minutes at normal temperature, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 46.90g of fly ash are mixed with 180ml of water. 1.0ml of 80% hydrochloric acid solution was added to adjust the pH to 7.7. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 10a mass ratio 180: washing at 20, 50 deg.C for five times with water, pH 7.7
TABLE 10b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99s
9.99ms
1.51ms
Second washing with water
9.99ms
2.30ms
530μs
Third time of water washing
2.01ms
434μs
241μs
The fourth time of water washing
1.22ms
335μs
230μs
Fifth washing with water
809μs
226μs
281μs
Eleven mass ratios of 180: five times of water washing at 20 and 50 ℃, sodium dodecyl benzene sulfonate and betaine
First water washing: 20.14g of fly ash are mixed with 180ml of water. 3.02g of sodium dodecyl benzene sulfonate and 2.98g of betaine are added. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 27.43g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 30.34g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 25.59g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 28.12g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 50 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 11a mass ratio 180: five times of water washing at 20 and 50 ℃, sodium dodecyl benzene sulfonate and betaine
TABLE 11b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
4.81ms
754μs
Second washing with water
9.99ms
1.03ms
227μs
Third time of water washing
6.24ms
585μs
218μs
The fourth time of water washing
5.54ms
407μs
200μs
Fifth washing with water
5.22ms
403μs
201μs
The mass ratio of twelve is 180: 20, 80 ℃, seven times of water washing (2)
First water washing: 20.27g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 20.51g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 18.02g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the electric conductivity of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 20.40g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: first 16.25g of fly ash is mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And sixth water washing: first 16.07g of fly ash was mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And seventh water washing:
15.88g of fly ash is mixed with 180ml of water
② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring.
Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled.
And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 12a twelve mass ratio 180: 20, 80 ℃, seven times of water washing (2)
TABLE 12b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
4.98ms
710μs
Second washing with water
7.98ms
4.83ms
696μs
Third time of water washing
5.17ms
384μs
192μs
The fourth time of water washing
4.96ms
335μs
176μs
Fifth washing with water
4.70ms
296μs
179μs
The sixth washing with water
5.94ms
519μs
189μs
The seventh time of water washing
4.45ms
256μs
177μs
Thirteen mass ratios are 180: 20, 80 ℃, seven times of water washing (3)
First water washing: 20.27g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 19.46g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 18.82g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 17.25g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 18.26g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And sixth water washing: first 16.89g of fly ash was mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And seventh water washing:
15.64g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at the rotating speed of 433r/s and the temperature of 80 ℃, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled.
And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 13a mass ratio 180: 20, 80 ℃, seven times of water washing (3)
TABLE 13b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
7.12ms
936μs
Second washing with water
9.99ms
954μs
318μs
Third time of water washing
7.47ms
429μs
240μs
The fourth time of water washing
4.47ms
378μs
253μs
Fifth washing with water
6.46ms
477μs
241μs
The sixth washing with water
7.61ms
408μs
236μs
The seventh time of water washing
7.68ms
494μs
360μs
Fourteen mass ratios are 180: 20, normal temperature, five times of water washing, 2.99g of ferrous oxalate
First water washing: 20.07g of fly ash, 180.68g of water and 2.99g of ferrous oxalate are mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: (ii) mixing 30.07g of the first washing residue with 181.2g of water. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: (i) mixing 31.11g of the second water-washing residue with 180.6g of water. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 26.28g of third washing residue and 181.5g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 24.40g of the fourth washing residue and 180.5g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 14a mass ratio 180: 20, normal temperature, five times of water washing, 2.99g of ferrous oxalate
TABLE 14b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
3.15ms
727μs
Second washing with water
7.03ms
788μs
359μs
Third time of water washing
4.86ms
480μs
370μs
The fourth time of water washing
3.62ms
370μs
297μs
Fifth washing with water
3.05ms
387μs
287μs
Fifteen mass ratio is 180: 20, normal temperature, four times of water washing, 3.10g of chitosan containing molecular sieve
First water washing: 20.08g of fly ash are mixed with 180ml of water. 3.10g of chitosan containing a molecular sieve was added. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring.
Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 27.03g of fly ash was mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: firstly, 26.85g of fly ash is mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: firstly, 26.85g of fly ash is mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 15a mass ratio 180: 20, normal temperature, four times of water washing, 3.10g of chitosan containing molecular sieve
TABLE 15b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
5.00ms
700μs
Second washing with water
8.89ms
875μs
279μs
Third time of water washing
6.56ms
556μs
208μs
The fourth time of water washing
7.96ms
423μs
199μs
Sixteen mass ratios are 180: 20, washing with EDTA chitosan at normal temperature for five times
First water washing: 20.07g of fly ash was mixed with 180ml of water. 2.95g of EDTA chitosan was added. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: firstly, 26.88g of fly ash is mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 24.36g of fly ash are mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 23.55g of fly ash are mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 20.64g of fly ash are mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 16a mass ratio 180: 20, washing with EDTA chitosan at normal temperature for five times
TABLE 16b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
4.48ms
717μs
Second washing with water
8.83ms
916μs
244μs
Third time of water washing
6.58ms
624μs
202μs
The fourth time of water washing
5.95ms
528μs
186μs
Fifth washing with water
5.46ms
423μs
190μs
Seventeen mass ratio is 180: 20, normal temperature, five times of water washing, 3.655g of ferrous sulfide
First water washing: 20.00g of fly ash was mixed with 180.7g of water and 3.655g of ferrous sulfide. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: (ii) 28.56g of the first washing residue and 180.41g of water were mixed. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: (ii) mixing 26.12g of the second water-washing residue with 180.47g of water. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: (ii) mixing 24.18g of the third washing residue with 182.15g of water. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 23.19g of fourth water washing residue and 182.10g of water are mixed. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 17a mass ratio 180: 20, normal temperature, five times of water washing, 3.655g of ferrous sulfide
TABLE 17b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
3.53ms
563μs
Second washing with water
6.85ms
707μs
217μs
Third time of water washing
5.00ms
418μs
184μs
The fourth time of water washing
4.40ms
378μs
175μs
Fifth washing with water
3.72ms
289μs
171μs
Eighteen, the mass ratio is 180: 20, normal temperature, five times of water washing, 3.60g of ferrous sulfate.
First water washing: 20.05g of fly ash are mixed with 180ml of water. 3.60g of ferrous sulfate was added. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 36.70g of fly ash are mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 39.76g of fly ash was mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 39.23g of fly ash are mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 38.96g of fly ash are mixed with 180ml of water. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, and the filtrate and the filter residue are respectively bottled.
And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 18a mass ratio 180: 20, normal temperature, five times of water washing, 3.60g of ferrous sulfate
TABLE 18b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
4.30ms
703μs
Second washing with water
9.02ms
912μs
303μs
Third time of water washing
5.22ms
483μs
240μs
The fourth time of water washing
3.99ms
43176μs
232μs
Fifth washing with water
2.94ms
184μs
236μs
The nineteen mass ratios are 180: 20, normal temperature, five times of water washing, 3.04g of copper acetate
First water washing: 20.01g of fly ash was mixed with 183.8g of water and 3.06g of manganese chloride. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: (i) first washing residue 21.13g and 181.3g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: (ii) 23.24g of the second water-washing residue was mixed with 180.6g of water. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. ③ mixing
Filtering the solution, bottling the filtrate, and washing the filter residue with water. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: (i) mixing 21.80g of the third water-washing residue with 181.7g of water. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 22.24g of the fourth washing residue and 181.96g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 19a mass ratio 180: 20, normal temperature, five times of water washing, 3.04g of copper acetate
TABLE 19b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
5.35ms
901μs
Second washing with water
7.53ms
993μs
428μs
Third time of water washing
4.92ms
514μs
421μs
The fourth time of water washing
4.66ms
404μs
379μs
Fifth washing with water
4.18ms
491μs
403μs
Twenty mass ratios of 180: 20, room temperature, seven times of water washing
First water washing: 20.00g of fly ash was mixed with 180ml of water. ② stirring for 60 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) second water washing: 21.28g of fly ash is mixed with 180ml of water. ② stirring for 60 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) washing for the third time: 18.96g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Fourth water washing: 22.95g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Fifth water washing: 15.95g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And sixth water washing: 14.86g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And seventh water washing: 13.87g of fly ash are mixed with 180ml of water. ② stirring for 60 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 15 minutes. Thirdly, the mixed solution is filtered, filter residue and filtrate are respectively bottled, fourthly, the stock solution is diluted by 10 times and 100 times, and finally, the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times are measured.
Table 20a mass ratio 180: 20, room temperature, seven times of water washing
TABLE 20b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
1.49ms
785μs
Second washing with water
9.99ms
1.10ms
270μs
Third time of water washing
7.86ms
607μs
227μs
The fourth time of water washing
7.83ms
606μs
226μs
Fifth washing with water
7.76ms
620μs
211μs
The sixth washing with water
6.83ms
459μs
222μs
The seventh time of water washing
5.83ms
425μs
221μs
Twenty-one mass ratio 180: 20, room temperature, three times water washing (2)
First water washing: 20.30g of fly ash are mixed with 180ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) second water washing: 20.89g of fly ash was mixed with 180ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) washing for the third time: first 16.30g of fly ash is mixed with 180ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, and filter residue and filtrate are respectively bottled. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Table 21a mass ratio 180: 20, room temperature, three times water washing (2)
TABLE 21b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
6.02ms
872μs
Second washing with water
9.99ms
1.21ms
296μs
Third time of water washing
8.28ms
806μs
239μs
Twenty-two mass ratio 180: 20, room temperature, five water washes
First water washing: 20.04g of fly ash are mixed with 180ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) second water washing: 20.62g of fly ash are mixed with 180ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
And (3) washing for the third time: 19.91g of fly ash are mixed with 180ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Fourth water washing: 17.68g of fly ash are mixed with 180ml of water. ② stirring for 15 minutes at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value every 3 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Fifth water washing: first 16.83g of fly ash are mixed with 180ml of water. ② at room temperature at the rotating speed of 433r/s
The mixture was stirred for 15 minutes, and the conductivity value and pH were measured every 3 minutes. Thirdly, the mixed liquid is filtered, and filter residue and filtrate are respectively bottled. Fourthly, diluting the stock solution by 10 times and 100 times, and finally measuring the conductivity and the pH of the stock solution, the diluted 10 times and the diluted 100 times.
Table 22a mass ratio 180: 20, room temperature, five water washes
The twenty-three mass ratios are 180: washing with water at 20-room temperature for five times, and copper chloride 3.10g
First water washing: 20.00g of fly ash and 180.12g of water were mixed with 3.10g of copper chloride. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 23.10g of the first washing residue and 179.36g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: (ii) mixing 24.70g of the second water-washing residue with 181.1g of water. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 20.68g of the third water-washing residue and 180.5g of water were mixed.
② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 20.64g of the fourth washing residue and 180.14g of water are mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 23a mass ratio 180: washing with water at 20-room temperature for five times, and copper chloride 3.10g
TABLE 23b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
2.74ms
502μs
Second washing with water
3.32ms
404μs
174μs
Third time of water washing
1.54ms
208μs
150μs
The fourth time of water washing
1.21ms
167μs
143μs
Fifth washing with water
1.01ms
165μs
140μs
The twenty-four mass ratio is 180: washing with water at 20-room temperature for five times, cuprous chloride 3.00g
First water washing: 20.00g of fly ash was mixed with 180.5g of water and 3.00g of cuprous chloride. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: (ii) 28.45g of the first washing residue and 181.0g of water were mixed. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: (ii) 28.80g of the second water-washing residue was mixed with 181.0g of water. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 22.82g of the third water-washing residue and 187.5g of water were mixed. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 24.87g of fourth washing residue and 182.7g of water are mixed. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 24a mass ratio 180: washing with water at 20-room temperature for five times, cuprous chloride 3.00g
TABLE 24b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
2.83ms
513μs
Second washing with water
5.00ms
607μs
217μs
Third time of water washing
2.43ms
183μs
176μs
The fourth time of water washing
1.96ms
214μs
163μs
Fifth washing with water
1.79ms
186μs
160μs
Twenty-five mass ratio is 180: 20-Normal temperature, five times of water washing, 3.03g of ferrous citrate
First water washing: 20.10g of fly ash and 180.32g of water are mixed with 3.03g of ferrous citrate. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 36.78g of first water washing residue and 180.70g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: (ii) 29.27g of the second water-washing residue was mixed with 181.0g of water. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 25.31g of the third washing residue and 180.3g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 23.78g of the fourth washing residue and 180.8g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 25a mass ratio 180: 20-Normal temperature, five times of water washing, 3.03g of ferrous citrate
TABLE 25b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
3.94ms
714μs
Second washing with water
6.25ms
958μs
357μs
Third time of water washing
2.36ms
440μs
301μs
The fourth time of water washing
1.85ms
352μs
284μs
Fifth washing with water
2.14ms
347μs
282μs
Twenty-six mass ratios of 180: washing with water for five times at 20-normal temperature, and 3.434g of sodium phosphate
First water washing: 20.11g of fly ash and 180.4g of water were mixed with 3.434g of sodium phosphate. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: first washing residue 34.20g and 182.9g were mixed together. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 31.52g of the second water-washing residue and 180.9g of water were mixed. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 28.56g of the third water-washing residue was mixed with 181.21g of water. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 27.61g of the fourth water-washing residue and 180.51g of water were mixed. Secondly, stirring for 1 hour at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 30 minutes. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 26a mass ratio 180: washing with water for five times at 20-normal temperature, and 3.434g of sodium phosphate
TABLE 26b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
2.68ms
502μs
Second washing with water
6.48ms
664μs
218μs
Third time of water washing
4.19ms
408μs
173μs
The fourth time of water washing
3.46ms
277μs
169μs
Fifth washing with water
2.93ms
229μs
163μs
Twenty-seven mass ratio 180: 20-normal temperature, five times of water washing, 3.061g of manganese chloride
First water washing: 21.06g of fly ash was mixed with 180.68g of water and 3.04g of copper acetate. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously.
And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: 32.23g of the first washing residue and 180.60g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) washing for the third time: 29.94g of the second water-washing residue and 180.75g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fourth water washing: 27.94g of the third washing residue and 180.6g of water were mixed. ② stirring for 30min at room temperature at the rotating speed of 433r/s, and measuring the conductivity value and the PH value once after stirring for 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Fifth water washing: 25.52g of fourth water washing residue and 186.9g of water are mixed. ② at the rotating speed of
433r/s, stirring at room temperature for 30min, and measuring the conductivity value and the pH value once after stirring to 15 min. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the PH value of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
Table 27a mass ratio 180: 20-normal temperature, five times of water washing, 3.061g of manganese chloride
TABLE 27b
Stock solution DD
Diluting by 10 times
Diluting by 100 times
First washing with water
9.99ms
4.65ms
891μs
Second washing with water
7.76ms
915μs
373μs
Third time of water washing
4.00ms
505μs
374μs
The fourth time of water washing
2.86ms
357μs
333μs
Fifth washing with water
2.56ms
342μs
303μs
Aiming at the experimental tests, the dechlorination rate is comprehensively calculated, and the conditions corresponding to each experiment and the final dechlorination rate are as follows:
watch 28
As is clear from Table 28, the dechlorination rates of experiment 1, experiment 14, experiment 15, experiment 17, experiment 18 and experiment 19 were all high. The best dechlorination effect is ferrous sulfate and copper acetate, which reach 98%, and experiments 1, 14, 17 and 18 show that the contribution of ferrous ions to dechlorination is obviously higher.
In addition, it can be seen from the table that experiments 9 and 10 (compared to experiments 5 to 7) show an increase of about 20% in dechlorination rate after addition of hydrochloric acid and acetic acid.
Therefore, when the fly ash is dechlorinated and cleaned, the fly ash can be firstly pickled and then cleaned by adding ferrous ions, and therefore, the experimental verification is as follows: a. mixing fly ash and hydrochloric acid solution, and stirring at constant temperature to obtain a mixed solution; b. performing suction filtration, and keeping filter residue; c. Washing the filter residue with water;
d. mixing the cleaned filter residue with a ferrous salt solution, and stirring at constant temperature; e. performing suction filtration, and keeping filter residue; f. mixing the filter residue with water; g. Stirring and filtering to obtain filter residue; h. repeating the steps f to g1 times to 3 times. The specific operation is as follows: first water washing: 20.00g fly ash was mixed with 180ml water. The pH of the hydrochloric acid solution is adjusted to 7.2. Secondly, stirring for 60 minutes at normal temperature at the rotating speed of 433r/s, and measuring the conductivity value and the pH value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the conductivity and the pH of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times.
And (3) second water washing: the filter residue is mixed with 180ml of water for cleaning. Secondly, stirring for 60 minutes at the normal temperature at the rotating speed of 433r/s, and measuring the conductivity value after stirring. Thirdly, the mixed liquid is filtered, the filtrate is bottled, and the filter residue is washed by water continuously. And fourthly, diluting the filtrate by 10 times and 100 times, and finally measuring the electric conductivity of the filtrate, the liquid diluted by 10 times and the liquid diluted by 100 times. And (3) washing for the third time: the filter residue was mixed with 180ml of water, and 3.6g of ferrous sulfate was added. The rotation speed is 433r/s, stirring is carried out for 60 minutes at normal temperature, and the conductivity value and the pH value are measured after stirring is finished. Filtering the mixed solution, bottling the filtrate, and washing the filter residue with water. The filtrate was diluted 10-fold and 100-fold, and finally the conductivity and pH of the filtrate, the liquid after 10-fold and 100-fold dilution were measured. Fourth water washing: the filter residue was mixed with 180ml of water. Stirring at 433r/s at normal temperature for 60 min, and measuring conductivity and pH. And carrying out suction filtration on the mixed solution, bottling the filtrate, and continuously washing the filter residue with water. The filtrate was diluted 10-fold and 100-fold, and finally the conductivity and pH of the filtrate, the liquid after 10-fold and 100-fold dilution were measured. Fifth water washing: the filter residue was mixed with 180ml of water. Stirring at 433r/s at normal temperature for 60 min, and measuring conductivity and pH. Filtering the mixture, and bottling the filtrate and the residue respectively. The filtrate was diluted 10-fold and 100-fold, and finally the conductivity and pH of the filtrate, the liquid after 10-fold and 100-fold dilution were measured. The dechlorination rate of the 5 times of cleaning is calculated to reach 98.8 percent; after the second washing is repeated for 2 times, the third washing is carried out again to obtain the dechlorination rate of 99.2 percent; after repeating the fifth washing for 3 times, the dechlorination rate was 99.8%.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structures made by the present disclosure or directly or indirectly applied to other related technical fields are also included in the scope of the present invention.
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