阅读说明：本技术 一种酸解浸取后钛液质量的分析方法 (Method for analyzing quality of titanium liquid after acidolysis leaching ) 是由 邓冰 于 2019-09-04 设计创作，主要内容包括：本发明涉及一种酸解浸取后钛液质量的分析方法,具体过程包括：取酸解浸取后的钛液,分别检测钛液中的二氧化钛含量A、稳定性B、硫酸含量C、残渣含量D以及钛铁矿中铁含量E；并根据二氧化钛含量A、稳定性B、硫酸含量C、残渣含量D以及钛铁矿中的铁含量E来计算酸解浸取后钛液综合质量Q；本发明提供的方法在传统钛液质量的分析中增加了残渣含量的测定,补充完善了酸解浸取后钛液的质量指标体系,并将生产该样品的原料钛铁矿的铁含量引入该分析方法的结果表示,使酸解浸取后钛液的质量表示更为全面,从而使酸解浸取后钛液的综合质量可以用单个的、可靠的指标进行监测和控制,在生产上具有重要意义。(The invention relates to a method for analyzing the quality of titanium liquid after acidolysis leaching, which comprises the following specific steps: taking titanium liquid after acidolysis leaching, and respectively detecting titanium dioxide content A, stability B, sulfuric acid content C, residue content D and iron content E in ilmenite in the titanium liquid; calculating the comprehensive quality Q of the titanium liquid after acidolysis leaching according to the titanium dioxide content A, the stability B, the sulfuric acid content C, the residue content D and the iron content E in the ilmenite; the method provided by the invention adds the residue content measurement in the traditional titanium liquid quality analysis, supplements and perfects the quality index system of the titanium liquid after acidolysis leaching, introduces the iron content of the ilmenite used as the raw material for producing the sample into the result representation of the analysis method, and enables the quality representation of the titanium liquid after acidolysis leaching to be more comprehensive, so that the comprehensive quality of the titanium liquid after acidolysis leaching can be monitored and controlled by a single and reliable index, and the method has important significance in production.)

1. The method for analyzing the quality of the titanium liquid after acidolysis leaching is characterized in that the method for analyzing the quality of the titanium liquid after acidolysis leaching comprises the following steps:

S1: detecting the content A of titanium dioxide in the titanium liquid;

S2: detecting the stability B of the titanium liquid;

S3: detecting the sulfuric acid content C in the titanium liquid;

s4: detecting the residue content D in the titanium liquid;

s5: detecting the iron content E of the ilmenite;

s6: the comprehensive quality Q of the titanium liquid after acidolysis leaching is calculated according to the following formula:

(ii) a Wherein R is a correction coefficient.

2. The method for analyzing the quality of the titanium solution after acidolysis leaching according to claim 1, wherein the step of detecting the content A of titanium dioxide in the titanium solution comprises the following steps:

S11: taking titanium liquid after acidolysis leaching, sucking 1-10 ml of titanium liquid sample into a conical flask, and adding 80-100 ml of mixed sulfur and salt acid and 2g of aluminum sheet;

s12: installing a cover funnel and plugging a rubber plug, adding a saturated solution of sodium bicarbonate into the cover funnel to 1/3 of the volume of a container, heating the mixture on an electric furnace with small fire until the reaction starts, then leaving a heat source, heating the mixture with fire after an aluminum sheet is dissolved completely, completely removing hydrogen in the solution, leaving the heat source when the solution is clarified, and cooling running water to room temperature;

S13: adding a saturated sodium bicarbonate solution in the cooling process, adding 2ml of an ammonium thiocyanate indicator, and immediately titrating with a ferric ammonium sulfate solution until the light red color is the end point; the titanium dioxide content a is expressed as:

(ii) a Wherein a is the concentration of the ammonium ferric sulfate standard solution; v is the volume of the ammonium ferric sulfate standard solution consumed; v1 is the volume as aspirated.

3. The method for analyzing the quality of the titanium solution after acidolysis leaching according to claim 1, wherein the step of detecting the stability B of the titanium solution specifically comprises the following steps:

taking titanium liquid after acidolysis leaching, sucking 1ml to 10ml of titanium liquid sample, placing the titanium liquid sample in a conical flask, and adding distilled water at 15 +/-1 ℃; adding N1ml, N2ml, N3ml, N4ml, N5ml, N6ml and N7ml … … Nn ml in sequence, shaking for 8-12 seconds after adding water each time, standing for 18-22 seconds until turbidity appears, and recording the number of milliliters of added distilled water; wherein, the stability B of the titanium liquid is represented as:。

4. the method for analyzing the quality of the titanium solution after acidolysis leaching according to claim 1, wherein the step of detecting the sulfuric acid content C in the titanium solution comprises the following steps:

Taking titanium liquid after acidolysis leaching, sucking 1ml to 10ml of titanium liquid sample into a conical flask, adding 10ml of distilled water and 25ml of ammonium chloride-barium chloride mixed solution, adding a methyl orange indicator, and titrating by using a sodium hydroxide standard solution until the upper layer solution is transparent orange yellow as a terminal point after the solution precipitation rapidly descends; the content C of the sulfuric acid in the titanium solution is represented as:

(ii) a Wherein b is the concentration of the sodium hydroxide standard solution, H is the volume of the sodium hydroxide standard solution consumed, and H1 is the volume of the sample taken up.

5. The method for analyzing the quality of titanium solution after acid hydrolysis leaching according to claim 4, further comprising detecting the F value of sulfuric acid, wherein the F value is expressed as:

(ii) a Wherein the content of the first and second substances,is the content of sulfuric acid in the sample,Is the titanium dioxide content of the sample.

6. the method for analyzing the quality of the titanium solution after acidolysis leaching according to claim 1, wherein the step of detecting the residue content D in the titanium solution comprises the following steps:

s41: connecting the detection devices, and detecting the air tightness of the detection devices;

s42: placing two pieces of wet phi 70mm quantitative filter paper in a Buchner funnel, flatly attaching the filter paper to the bottom of the funnel, opening a detection device, and keeping the vacuum degree in a filter flask below-0.04 Mpa;

s43: taking titanium liquid after complete acidolysis leaching, preserving heat at 60-70 ℃ to ensure that the titanium liquid does not separate out crystals, pouring the titanium liquid into a Buchner funnel for suction filtration, and after the titanium liquid is dried, using distilled water for suction washing for three to four times;

S44: and (3) transferring the filter paper and the residues into an evaporation dish, drying the evaporation dish in an oven preheated to 105 ℃ for 1 hour, taking out the evaporation dish, cooling and weighing to obtain the residue content D of the sample.

7. The method for analyzing the quality of the titanium solution after acidolysis leaching according to claim 1, wherein the step of detecting the iron content E of the ilmenite in the titanium solution specifically comprises the following steps:

S51: putting 0.200g of ilmenite sample into a ceramic crucible, adding 8-10 g of potassium pyrosulfate, covering the crucible cover, moving the crucible cover into a high-temperature furnace with the temperature of 400-500 ℃, placing the crucible cover for 9-11 min, heating the furnace to 700-750 ℃, melting for 13-15 min, taking out, and cooling to obtain a fusion cake;

s52: pouring the frit into a beaker, cleaning the crucible and a crucible cover with hot hydrochloric acid, adding 25ml of hydrochloric acid, diluting to about 70ml with water, and heating to completely dissolve the frit to obtain a test solution;

s53: heating the test solution in the S52 to bubbling, dropwise adding a stannous chloride solution until the yellow color of the solution disappears, dropwise adding 1-2 drops of the stannous chloride solution in excess, cooling the solution to room temperature with running water, adding 10ml of mercury dichloride saturated solution, shaking up, standing for 3-5 min, adding 18ml of sulfuric acid-phosphoric acid mixed acid and 3-5 drops of sodium diphenylamine sulfonate solution, and using a potassium dichromate standard solution until the solution is stable purple, namely the end point;

s54: analyzing and calculating the iron content E in the ilmenite in the titanium liquid; the iron content E of ilmenite in the titanium liquor is expressed as:

(ii) a Wherein k is the volume of the potassium dichromate standard titration solution consumed in the titration test solution;the volume of potassium dichromate standard titration solution consumed for the blank test; d is the molar concentration of the potassium dichromate standard titration solution;is the ilmenite sample mass.

8. the method for analyzing the quality of the titanium solution after acidolysis leaching according to claim 7, wherein the ilmenite sample is weighed to 0.200g, to the accuracy of 0.0001 g; and/or the granularity of the ilmenite sample is not more than 90 mu m; and/or, the ilmenite sample needs to be dried for 2 hours at 105-110 ℃ in advance, placed in a dryer and cooled to room temperature; and/or detecting the iron content E of the ilmenite for not less than three times, and averaging.

9. the method for analyzing the quality of a titanium solution after acidolysis leaching according to claim 1, wherein the titanium solution sample is sampled after the acidolysis leaching operation and before the reduction operation; and/or detecting the content A, the stability B, the content C of sulfuric acid and the content D of residues in the titanium liquid by the same titanium liquid sample at the same time.

10. the method for analyzing the quality of titanium solution after acidolysis leaching according to claim 6, wherein the detection device comprises a discharge valve, a Buchner funnel, a filtration flask, a safety flask, a ball valve, a vacuum pressure reducing valve and a vacuum pump; the discharge valve is arranged on a discharge pipe at the bottom of the filter flask; the buchner funnel is arranged on the feed inlet of the filter flask; the filter flask is connected with the safety bottle through a first connecting pipe; the safety bottle is connected with the vacuum pump through a second connecting pipe; the ball valve and the vacuum reducing valve are arranged on the second connecting pipe in series.

Technical Field

The invention belongs to the technical field of titanium liquid quality analysis, and particularly relates to a method for analyzing the quality of titanium liquid subjected to acidolysis leaching.

background

the production of titanium dioxide by sulfuric acid method is that sulfuric acid reacts with ilmenite to produce black titanyl sulfate solution (hereinafter referred to as titanium solution), and through the processes of crystallization, hydrolysis, water washing, calcination and the like, high-purity white titanium dioxide powder (titanium dioxide) is finally produced.

the attached figure 1 shows the production process of titanium dioxide by a sulfuric acid method, and the acidolysis process is the first chemical reaction process in the production of titanium dioxide by a sulfuric acid method, and has the function of extracting titanium elements in titanium concentrate by sulfuric acid to convert the titanium elements into black titanyl sulfate solution (hereinafter referred to as black titanium solution) for the production of the subsequent process, and finally white titanium dioxide powder (titanium dioxide) is produced.

The acidolysis process shown in figure 2 is as follows:

Acid hydrolysis: fully and uniformly mixing the titanium concentrate and 93-98% concentrated sulfuric acid by compressed air, adding water or 23% dilute sulfuric acid, heating a mineral acid mixture to over 100 ℃ by using a large amount of dilution heat generated by the water in the waste acid and the concentrated sulfuric acid, carrying out violent exothermic main reaction, exceeding 180 ℃ within a few minutes, finishing the main reaction within 3-5 minutes, and gradually reducing the temperature;

curing: keeping the generated honeycomb solid phase object at 90-100 ℃ for curing for 2-3 hours;

leaching: adding a certain amount of water at a set speed, dissolving and leaching titanyl sulfate in the solid phase to form a black titanium solution, and keeping the leaching process at 68-73 ℃;

and fourthly, reduction: after leaching is finished, adding scrap iron or iron powder, reducing ferric iron in the black titanium liquid into ferrous iron, and keeping the temperature of the reduction process at 68-73 ℃;

sedimentation: and after reduction is finished, mixing the black titanium liquid and a flocculating agent in proportion, naturally settling particles for 2-4 hours, filtering supernatant liquid, and conveying the supernatant liquid to a post-process, wherein a solid-liquid mixture at the bottom is filtered by a filter press and then conveyed to the post-process.

the acidolysis process is one of the most important processes in titanium white production, and the quality of the titanyl sulfate solution produced in the process directly determines the quality of all products on the whole titanium white production line; once the acidolysis process has problems, the process accident is a serious process accident, and most commonly, all production raw materials are scrapped, so that huge irretrievable loss is caused. Therefore, in the titanium dioxide production by the sulfuric acid method, the titanium liquid after reduction is generally taken and detected after the reduction operation to monitor the quality of the titanium liquid produced in the acidolysis process, and the detected items comprise: titanium dioxide content, sulfuric acid content, stability. Wherein, the higher the content of the titanium dioxide is, the higher the acidolysis degree of the ilmenite is, and the higher the effective components in the titanium liquid are; the higher the sulfuric acid content (within a certain range) and the higher the stability, the less easily the titanium liquid is hydrolyzed at an early stage. However, the iron content, the residue content, which has a significant influence on the titanium dioxide production and the product quality, was not monitored. Titanium white production belongs to fine chemistry industry, and production control is very strict, and the iron content and the residue content in titanium liquid are indexes which need to be strictly controlled, but are not controlled in an acidolysis process, which is a defect in quality control of titanium white production by a sulfuric acid process.

In the traditional sulfate process titanium dioxide production, the iron content and the residue content in the titanium liquid are not monitored in the acidolysis process, and the following consideration should be given to the following reasons: after the acidolysis process, through settling and crystallization processes, most of iron elements in the titanium liquid are crystallized and separated out in the form of ferrous sulfate, most of residues are filtered, so that the titanium liquid is pure and transparent, only trace iron ions and residues exist in the titanium liquid at this time, the determination of the iron content and the residue amount in the crystallization process is more convenient, and the data is more stable. However, after many years of empirical conclusion of titanium dioxide production, it is necessary to introduce monitoring of the iron content and the residue content in the acidolysis step: the method can obtain relatively complete quality data of the titanium liquid at the first time after the feeding production, and is favorable for analyzing the use condition of various ilmenite and other production raw materials on the production line and the adaptability of the production line to the change of the production raw materials by combining the production quality control technology. According to production experience and statistical analysis, each quality index in the titanium liquid has certain correlation, and through the characteristic, a correlation model is established, so that the quality of the titanium liquid can be accurately controlled. The reason why the titanium liquid after the leaching operation is taken for analysis rather than the titanium liquid after the reduction operation is taken for analysis in common is that the titanium liquid obtained after the leaching operation is the initial liquid product obtained in the titanium white production, and the iron content in the titanium liquid after the reduction operation is changed because a certain amount of iron powder is added into the titanium liquid. After the leaching operation, the iron content in the ilmenite is unchanged, and the ilmenite is directly converted into iron ions in the titanium liquid through acidolysis reaction, under the condition of stable production state, the acidolysis rate of the ilmenite is basically stable, the iron content in the ilmenite can be completely substituted into the titanium liquid at the moment, and the quality model of the titanium liquid after acidolysis leaching is perfected.

Disclosure of Invention

the invention designs an analysis method for the quality of titanium liquid after acidolysis leaching, which solves the problem of accurate analysis of the quality of the titanium liquid after acidolysis leaching in the prior art.

In order to solve the technical problems, the invention adopts the following scheme:

A method for analyzing the quality of titanium liquid after acidolysis leaching is provided, which takes the titanium liquid after acidolysis leaching and comprises the following steps:

S1: detecting the content A of titanium dioxide in the titanium liquid;

S2: detecting the stability B of the titanium liquid;

S3: detecting the sulfuric acid content C in the titanium liquid;

s4: detecting the residue content D in the titanium liquid;

S5: detecting the iron content E of the ilmenite;

s6: the comprehensive quality Q of the titanium liquid after acidolysis leaching is calculated according to the following formula:

(ii) a Wherein R is a correction coefficient.

Further, the detection of the content A of the titanium dioxide in the titanium liquid specifically comprises the following steps:

s11: taking titanium liquid after acidolysis leaching, sucking 1-10 ml of titanium liquid sample into a conical flask, and adding 80-100 ml of mixed sulfur and salt acid and 2g of aluminum sheet;

S12: installing a cover funnel and plugging a rubber plug, adding a saturated solution of sodium bicarbonate into the cover funnel to 1/3 of the volume of a container, heating the mixture on an electric furnace with small fire until the reaction starts, then leaving a heat source, heating the mixture with fire after an aluminum sheet is dissolved completely, completely removing hydrogen in the solution, leaving the heat source when the solution is clarified, and cooling running water to room temperature;

s13: adding a saturated sodium bicarbonate solution in the cooling process, adding 2ml of an ammonium thiocyanate indicator, and immediately titrating with a ferric ammonium sulfate solution until the light red color is the end point; the titanium dioxide content a is expressed as:

(ii) a Wherein a is the concentration of the ammonium ferric sulfate standard solution; v is the volume of the ammonium ferric sulfate standard solution consumed; v1 is the volume as aspirated.

Further, the detection of the stability B of the titanium liquid specifically comprises the following steps:

taking titanium liquid after acidolysis leaching, sucking 1ml to 10ml of titanium liquid sample, placing the titanium liquid sample in a conical flask, and adding distilled water at 15 +/-1 ℃; adding N1ml, N2ml, N3ml, N4ml, N5ml, N6ml and N7ml … … Nn ml in sequence, shaking for 8-12 seconds after adding water each time, standing for 18-22 seconds until turbidity appears, and recording the number of milliliters of added distilled water; wherein, the stability B of the titanium liquid is represented as:。

Further, the detection of the sulfuric acid content C in the titanium solution specifically comprises the following steps:

Taking titanium liquid after acidolysis leaching, sucking 1ml to 10ml of titanium liquid sample into a conical flask, adding 10ml of distilled water and 25ml of ammonium chloride-barium chloride mixed solution, adding a methyl orange indicator, and titrating by using a sodium hydroxide standard solution until the upper layer solution is transparent orange yellow as a terminal point after the solution precipitation rapidly descends; the content C of the sulfuric acid in the titanium solution is represented as:

(ii) a Wherein b is the concentration of the sodium hydroxide standard solution, H is the volume of the sodium hydroxide standard solution consumed, and H1 is the volume of the sample taken up.

Further, the method also comprises the step of detecting the F value of the sulfuric acid, wherein the F value is expressed as:

(ii) a Wherein the content of the first and second substances,Is the content of sulfuric acid in the sample,is the titanium dioxide content of the sample.

further, the detection of the residue content D in the titanium liquid specifically comprises the following steps:

S41: connecting the detection devices, and detecting the air tightness of the detection devices;

s42: placing two pieces of wet phi 70mm quantitative filter paper in a Buchner funnel, flatly attaching the filter paper to the bottom of the funnel, opening a detection device, and keeping the vacuum degree in a filter flask below-0.04 Mpa;

S43: taking titanium liquid after complete acidolysis leaching, preserving heat at 60-70 ℃ to ensure that the titanium liquid does not precipitate crystals, pouring the titanium liquid into a Buchner funnel for suction filtration, and after the titanium liquid is dried, using distilled water for suction washing for three to four times;

s44: and (3) transferring the filter paper and the residues into an evaporation dish, drying the evaporation dish in an oven preheated to 105 ℃ for 1 hour, taking out the evaporation dish, cooling and weighing to obtain the residue content D of the sample.

Further, the detection of the iron content E of the ilmenite in the titanium liquid specifically comprises the following steps:

S51: putting 0.200g of ilmenite sample into a ceramic crucible, adding 8-10 g of potassium pyrosulfate, covering the crucible cover, moving the crucible cover into a high-temperature furnace with the temperature of 400-500 ℃, placing the crucible cover for 9-11 min, heating the furnace to 700-750 ℃, melting for 13-15 min, taking out, and cooling to obtain a fusion cake;

s52: pouring the frit into a 400ml beaker, cleaning the crucible and a crucible cover with hot hydrochloric acid, adding 25ml hydrochloric acid, diluting to about 70ml with water, and heating to completely dissolve the frit to obtain a test solution;

s53: heating the test solution in the S52 to bubbling, dropwise adding a stannous chloride solution until the yellow color of the solution disappears, dropwise adding 1-2 drops of the stannous chloride solution in excess, cooling the solution to room temperature with running water, adding 10ml of mercury dichloride saturated solution, shaking up, standing for 3-5 min, adding 18ml of sulfuric acid-phosphoric acid mixed acid and 3-5 drops of sodium diphenylamine sulfonate solution, and using a potassium dichromate standard solution until the solution is stable purple, namely the end point;

S54: analyzing and calculating the iron content E of ilmenite in the titanium liquid; the iron content E of ilmenite in the titanium liquor is expressed as:

(ii) a Wherein k is the volume of the potassium dichromate standard titration solution consumed in the titration test solution;The volume of potassium dichromate standard titration solution consumed for the blank test; d is the molar concentration of the potassium dichromate standard titration solution;is the ilmenite sample mass.

Further, weighing 0.200g of ilmenite sample to be accurate to 0.0001 g; and/or the granularity of the ilmenite sample is not more than 90 mu m; and/or, the ilmenite sample needs to be dried for 2 hours at 105-110 ℃ in advance, placed in a dryer and cooled to room temperature; and/or detecting the iron content E of the ilmenite for not less than three times, and taking an average value.

further, sampling a titanium liquid sample after the leaching operation of the acidolysis process and before the reduction operation; and/or detecting the content A, the stability B, the content C of sulfuric acid and the content D of residues in the titanium liquid by the same titanium liquid sample at the same time.

further, the detection device comprises a discharge valve, a Buchner funnel, a filter flask, a safety bottle, a ball valve, a vacuum pressure reducing valve and a vacuum pump; the discharge valve is arranged on a discharge pipe at the bottom of the filter flask; the buchner funnel is arranged on the feed inlet of the filter flask; the suction filter bottle is connected with the safety bottle through a first connecting pipe; the safety bottle is connected with the vacuum pump through a second connecting pipe; the ball valve and the vacuum reducing valve are arranged on the second connecting pipe in series.

the invention provides a method for analyzing the quality of titanium liquid after acidolysis leaching, which is used for expressing the comprehensive quality of the titanium liquid after acidolysis leaching by substituting the data of titanium dioxide content, sulfuric acid content, residue content and stability of the titanium liquid after acidolysis leaching and the iron content of pyrite which is a raw material for producing a sample into a specific formula. The method provided by the invention adds the residue content determination in the traditional titanium liquid quality analysis, supplements and perfects the quality index system of the titanium liquid after acidolysis leaching, introduces the iron content of the pyrite which is the raw material for producing the sample into the result representation of the analysis method, and enables the quality representation of the titanium liquid after acidolysis leaching to be more comprehensive, so that the comprehensive quality of the titanium liquid after acidolysis leaching can be monitored and controlled by a single and reliable index, and the method has important significance in production.

Drawings

FIG. 1 is a flow chart of a sulfuric acid process titanium dioxide production process in the prior art;

FIG. 2 is a flow diagram of an acid hydrolysis process in the prior art;

FIG. 3 is a flow chart of a method for analyzing the quality of titanium liquid after acidolysis leaching according to the present invention;

FIG. 4 is a schematic view of a titanium liquid residue content detection device according to the present invention;

FIG. 5 is a line graph plotting the titanium dioxide content of 200 consecutive samples of the present invention (ordinate units: g/L);

FIG. 6 is a line graph (in units of ordinate: mL) plotting stability data for 200 consecutive samples of the present invention;

FIG. 7 is a line graph plotting residue content (ordinate units: g) for 200 consecutive samples of the invention;

FIG. 8 is a line graph plotting the sulfuric acid content of 200 consecutive samples of the present invention (ordinate units: g/L);

FIG. 9 is a line graph depicting F values for 200 consecutive samples of the present invention;

FIG. 10 is a line graph plotting the iron content of 200 consecutive samples according to the invention (ordinate units:%);

FIG. 11 is a graph in which Q values of 200 consecutive samples are plotted according to the present invention;

FIG. 12 is a correlation analysis of titanium dioxide content, stability, residue content, sulfuric acid content, F-number, iron content of 200 consecutive samples according to the present invention.

FIG. 4 depicts a reference:

1-a discharge valve; 2-Buchner funnel; 3, a filter flask; 4, a safety bottle; 5-ball valve; 6-vacuum pressure reducing valve; 7-vacuum pump.

Detailed Description

The invention will be further explained with reference to the accompanying drawings:

As shown in figure 3, the invention provides a method for analyzing the quality of titanium liquid after acidolysis leaching, which takes the titanium liquid after acidolysis leaching and comprises the following steps:

s1: detecting the content A of titanium dioxide in the titanium liquid;

s2: detecting the stability B of the titanium liquid;

s3: detecting the sulfuric acid content C in the titanium liquid;

s4: detecting the residue content D in the titanium liquid;

S5: detecting the iron content E in the ilmenite for producing the batch of samples;

s6: the comprehensive quality Q of the titanium liquid after acidolysis leaching is calculated according to the following formula:

(ii) a Wherein R is a correction coefficient.

preferably, with reference to the above scheme, in this embodiment, the detecting the content a of titanium dioxide in the titanium solution specifically includes the following steps:

s11: taking 200ml of titanium liquid after acidolysis leaching, sucking 1ml to 10ml of titanium liquid into a conical flask, and adding 80 ml to 100ml of mixed sulfur and salt acid and 2g of aluminum sheet; preferably, 1ml is aspirated into a 500ml Erlenmeyer flask;

S12: installing a cover funnel and plugging a rubber plug, adding a saturated solution of sodium bicarbonate into the cover funnel to 1/3 of the volume of a container, heating the mixture on an electric furnace with small fire until the reaction starts, then leaving a heat source, heating the mixture with strong fire after an aluminum sheet is dissolved completely, completely removing hydrogen in the solution, leaving the heat source when the solution is clear, and cooling running water to room temperature;

S13: adding saturated sodium bicarbonate solution at any time during the cooling process, adding 2ml of ammonium thiocyanate indicator, and immediately titrating with ferric ammonium sulfate solution until light red is the end point; the titanium dioxide content a is expressed as:

(ii) a Wherein a is the concentration of the ammonium ferric sulfate standard solution, and the unit is mol/L; v is the volume of the ammonium ferric sulfate standard solution consumed, and the unit is ml; v1 is the volume as aspirated in ml; 0.0799 is the standard solution of ferric sulfate { C [ NH ] 1.00ml₄Fe(SO₄)₂]Mass of titanium dioxide expressed in grams, equivalent to =0.0001mol/L }.

Preferably, with reference to the above scheme, in this embodiment, the detecting the stability B of the titanium solution specifically includes the following steps: taking 200ml of titanium solution after acidolysis leaching, sucking 1-10 ml of sample, placing the sample in a conical flask, and adding distilled water at 15 +/-1 ℃; preferably, 10ml of the diluted sample is sucked into a 100ml volumetric flask, and after shaking up, 10ml of the diluted sample is sucked into a 500ml conical flask; further, N1ml, N2ml, N3ml, N4ml, N5ml, N6ml and N7ml … … Nn ml can be added in the order, specifically, N1ml can be selected as 100ml, N2ml can be selected as 100ml, N3ml can be selected as 50ml, N4ml can be selected as 50ml, N5ml can be selected as 20ml, N6ml can be selected as 20ml, and N7ml can be selected as 10 ml; shaking for 8-12 seconds, specifically 10 seconds, after adding water each time; standing for 18 to 22 seconds, specifically 20 seconds; recording the amount of the added distilled water milliliter until turbidity appears; wherein, the stability B of the titanium liquid is represented as:。

preferably, with reference to the above scheme, in this embodiment, the detecting the sulfuric acid content C in the titanium solution specifically includes the following steps: taking 200ml of titanium solution after acidolysis leaching, sucking 1ml to 10ml into a conical flask, adding 100ml of distilled water and 25ml of ammonium chloride-barium chloride mixturecombining the solution, adding a methyl orange indicator, titrating by using a sodium hydroxide standard solution until the upper layer solution is transparent orange yellow as a terminal point after the precipitation of the solution rapidly drops; preferably, 1ml is pipetted into a 500ml Erlenmeyer flask; the content C of the sulfuric acid in the titanium solution is represented as:(ii) a Wherein b is the concentration of the sodium hydroxide standard solution, and the unit is mol/L; h is the volume of the sodium hydroxide standard solution consumed, and the unit is ml; h1 is the volume of the sample taken up in ml; 0.04904 is prepared by mixing with 1.00ml of sodium hydroxide standard solution [ C (NaOH) =1.000 mol%]equivalent mass of sulfuric acid expressed in grams.

Preferably, with reference to the above scheme, in this embodiment, the method further includes detecting an F value of the sulfuric acid, where the F value is a ratio of the sulfuric acid content to the titanium dioxide content after the determination of the sulfuric acid content and the titanium dioxide content, and calculating according to a formula; this value is often used to compare the amount of sulfuric acid per unit of titanium dioxide in the titanium liquor during production; the value of F is expressed as:(ii) a Wherein the content of the first and second substances,Is the content of sulfuric acid in the sample,is the titanium dioxide content of the sample.

preferably, with reference to the above scheme, in this embodiment, the detecting the residue content D in the titanium solution specifically includes the following steps:

S41: connecting the detection devices, and detecting the air tightness of the detection devices;

s42: placing two pieces of wet phi 70mm quantitative filter paper in a Buchner funnel, flatly attaching the filter paper to the bottom of the funnel, opening a detection device, and keeping the vacuum degree in a filter flask below-0.04 Mpa;

S43: taking titanium liquid after complete acidolysis leaching, preserving heat at 60-70 ℃ to ensure that the titanium liquid does not precipitate crystals, pouring the titanium liquid into a Buchner funnel for suction filtration, and after the titanium liquid is dried, using distilled water for suction washing for three to four times;

S44: and (3) transferring the filter paper and the residues into an evaporation dish, drying the evaporation dish in an oven preheated to 105 ℃ for 1 hour, taking out the evaporation dish, cooling and weighing to obtain the residue content D of the sample.

Preferably, with reference to the above scheme, in this embodiment, detecting the iron content E of ilmenite in the titanium liquid raw material is: melting an ilmenite sample by using potassium pyrosulfate, adding a little excessive stannous chloride to reduce ferric iron into ferrous iron in a hot dilute hydrochloric acid solution, oxidizing the excessive stannous chloride by using mercury dichloride, adding sulfuric acid-phosphoric acid mixed acid, using sodium diphenylamine sulfonate as an indicator, and titrating by using a potassium dichromate standard titration solution to a stable purple color as a terminal point; the method specifically comprises the following steps:

S51: putting 0.200g ilmenite sample into a 30ml ceramic crucible, adding 8-10 g potassium pyrosulfate, covering the crucible cover, moving the crucible cover into a high-temperature furnace with the temperature of 400-500 ℃, placing the crucible cover for about 10min, heating the furnace to 700-750 ℃, melting for 13-15 min, taking out, and cooling to obtain a fusion cake;

s52: pouring the frit into a 400ml beaker, washing the crucible and a crucible cover with a small amount of hot hydrochloric acid, adding 25ml of hydrochloric acid, diluting the mixture to about 70ml with water, and heating the mixture to completely dissolve the frit to obtain a test solution;

S53: heating the test solution in the S52 to bubble, namely, to be nearly boiling, wherein the near boiling refers to a state that the bottom of the solution begins to bubble in large particles and is nearly boiled; specifically, taking an aqueous solution as an example, the temperature is generally about 95 ℃; dropwise adding a stannous chloride solution until the yellow color of the solution just disappears, then adding 1-2 drops of stannous chloride solution, cooling the solution to room temperature by running water, adding 10ml of saturated solution of mercury dichloride, shaking the solution evenly, standing the solution for 3-5 min, adding 18ml of mixed sulfuric acid-phosphoric acid and 3-5 drops of sodium diphenylamine sulfonate solution, preferably 4 drops of sodium diphenylamine sulfonate solution, and using a standard potassium dichromate solution until the solution is stable purple, namely the end point;

S54: analyzing and calculating the iron content E of ilmenite in the titanium liquid; the iron content E of ilmenite in the titanium liquor is expressed as:

(ii) a Wherein k is the volume of the potassium dichromate standard titration solution consumed in the titration test solution, and the unit is milliliter (ml);the volume of potassium dichromate standard titration solution consumed for the blank test in milliliters (ml); d is the molar concentration of the potassium dichromate standard titration solution, and the unit is mol per liter (mol/L);is the ilmenite sample mass in grams (g); 55.85 is the molar mass of iron in grams per mole (g/mol).

preferably, in combination with the above scheme, in this embodiment, the ratio of sulfuric acid-phosphoric acid mixed acid: 150ml of sulfuric acid (. rho.about.1.84 g/ml) was slowly poured into 700ml of water with stirring, cooled to room temperature, added with 150ml of phosphoric acid (. rho.about.1.70 g/ml) and mixed well.

preferably, in combination with the above scheme, in this embodiment, the ratio of stannous chloride solution: weighing 10g of stannous chloride (SnCl)_2·2H₂o) was dissolved in 10ml of hot hydrochloric acid (. rho.about.1.19 g/ml), diluted to 100ml with water and filtered; the solution is prepared on site at the time of use.

preferably, in combination with the above scheme, in the present embodiment, the potassium dichromate standard titration solution (C)_1/6K2Cr2O7=0.03000 mol/L) 2.9418g of standard reagent potassium dichromate (dried in advance for 2h at 150 h and cooled to room temperature in a desiccator), dissolved in a suitable amount of water, transferred into a 2000ml volumetric flask, diluted to the mark with water and mixed well.

Preferably, in combination with the above scheme, in this example, the ilmenite sample is selected to be 0.200g, to the nearest 0.0001 g.

Preferably, in combination with the above scheme, in the present embodiment, the particle size of the ilmenite sample should not be larger than 90 μm.

preferably, in combination with the above scheme, in this embodiment, the ilmenite sample needs to be baked at 105 ℃ to 110 ℃ for 2 hours in advance, placed in a dryer, and cooled to room temperature.

Preferably, in combination with the above scheme, in this embodiment, the number of times of detecting the iron content E of ilmenite is not less than three, and an average value is taken; blank test was performed along with the sample.

Preferably, in combination with the above scheme, in this embodiment, the titanium liquid sample is sampled after the leaching operation and before the reduction operation in the acidolysis process.

preferably, with reference to the above scheme, in this embodiment, the content a of titanium dioxide, the stability B, the content C of sulfuric acid, and the content D of residue in the titanium solution are detected by using the same titanium solution sample.

Preferably, in combination with the above solution, as shown in fig. 3, in the present embodiment, the detection device includes a discharge valve 1, a buchner funnel 2, a filtration bottle 3, a safety bottle 4, a ball valve 5, a vacuum pressure reducing valve 6, and a vacuum pump 7; the discharge valve is arranged on a discharge pipe at the bottom of the filter flask; the buchner funnel is arranged on the feed inlet of the filter flask; the suction flask is connected with the safety flask 4 through a first connecting pipe; the safety bottle 4 is connected with the vacuum pump 7 through a second connecting pipe; the ball valve 5 and the vacuum reducing valve 6 are arranged on the second connecting pipe in series and used for adjusting the flow of the second connecting pipe.

by adopting the scheme, relatively complete quality data of the titanium liquid is obtained at the first time after the feeding production, the use condition of various ilmenite and other production raw materials on the production line and the adaptability of the production line to the change of the production raw materials are analyzed, and the quality of the titanium liquid in the acidolysis process of titanium white production is comprehensively monitored; the invention provides an analysis method of titanium liquid after acidolysis leaching, which comprehensively monitors the titanium dioxide content, the sulfuric acid content, the stability, the iron content and the residue content of the titanium liquid.