阅读说明：本技术 一种褐煤综合利用微波提取环保装置及工艺 (Microwave extraction environment-friendly device and process for comprehensive utilization of lignite ) 是由 刘冠诚 于 2021-01-14 设计创作，主要内容包括：本发明公开了一种褐煤综合利用微波提取环保装置与工艺,所述装置包括湿式粉碎机、螺旋分级机,所述的湿式粉碎机与螺旋分级机相连,所述的螺旋分级机分别与一号储料罐和二号储料罐相连,一号储料罐分别顺序与一号微波提取器、一号板框过滤机相连,一号板框过滤机与一号冷凝器相连；二号储料罐连分别顺序连接二号微波提取器、二号板框过滤机、酸解罐、沉淀池、三号板框过滤机,所述酸解罐的物料进口与酸储罐的物料出口相连,所述三号板框过滤机的液体出口连接药液池,滤渣出口与一号微波干燥器相连；所述的一号板框过滤机分别顺序与二号微波干燥器、混炼机、热解炉相连接,所述热解炉炉顶与分离器相连,炉底连接三号冷凝器。所述工艺包括褐煤蜡提取、腐殖酸提取和热解。(The invention discloses a microwave extraction environment-friendly device and process for comprehensively utilizing lignite, wherein the device comprises a wet-type pulverizer and a spiral classifier, the wet-type pulverizer is connected with the spiral classifier, the spiral classifier is respectively connected with a first storage tank and a second storage tank, the first storage tank is respectively connected with a first microwave extractor and a first plate-frame filter in sequence, and the first plate-frame filter is connected with a first condenser; the second storage tank is connected with a second microwave extractor, a second plate-frame filter, an acidolysis tank, a sedimentation tank and a third plate-frame filter which are sequentially connected, a material inlet of the acidolysis tank is connected with a material outlet of the acid storage tank, a liquid outlet of the third plate-frame filter is connected with a liquid medicine tank, and a filter residue outlet is connected with a first microwave dryer; the first plate-frame filter is connected with the second microwave dryer, the mixing roll and the pyrolysis furnace in sequence, the top of the pyrolysis furnace is connected with the separator, and the bottom of the pyrolysis furnace is connected with the third condenser. The process comprises montan wax extraction, humic acid extraction and pyrolysis.)

1. The microwave extraction environment-friendly device for comprehensively utilizing lignite comprises a wet grinder (1) and a spiral classifier (2), and is characterized in that the wet grinder (1) is connected with the spiral classifier (2), the spiral classifier (2) is respectively connected with a first storage tank (3) and a second storage tank (9), the first storage tank (3) is respectively connected with a first microwave extractor (4) and a first plate-frame filter (5) in sequence, and the first plate-frame filter (5) is connected with a first condenser (6);

the second material storage tank (9) is connected with a second microwave extractor (10), a second plate-frame filter (11), an acidolysis tank (12), a sedimentation tank (14) and a third plate-frame filter (15) in sequence, a material inlet of the acidolysis tank (12) is connected with a material outlet of an acid storage tank (13), a liquid outlet of the third plate-frame filter (15) is connected with a liquid medicine tank (16), and a filter residue outlet is connected with a first microwave dryer (18);

the first plate-frame filter (5) is respectively connected with a second microwave dryer (22), a mixing roll (25) and a pyrolysis furnace (26) in sequence, the top of the pyrolysis furnace (26) is connected with a separator (30), and the bottom of the furnace is connected with a third condenser.

2. The lignite comprehensive utilization microwave extraction environment-friendly device according to claim 1, characterized in that the first microwave dryer (18) is connected with a condensation water tank (17) and a Raymond mill (19), and the Raymond mill (19) is connected with a dust collector (20).

3. The lignite comprehensive utilization microwave extraction environment-friendly device according to claim 1, characterized in that a steam outlet of the second microwave dryer (22) is connected with a second condenser (23), and the second condenser (23) is connected with a water storage tank (24).

4. The lignite comprehensive utilization microwave extraction environment-friendly device as claimed in claim 1, wherein the second plate-frame filter (11) is connected with the first storage tank (3).

5. The lignite comprehensive utilization microwave extraction environment-friendly device according to claim 1, characterized in that the pyrolysis furnace (26) is powered by a medium-frequency power supply (27).

6. The lignite comprehensive utilization microwave extraction environment-friendly device according to claim 1, wherein the separator (30) is connected with a gas tank (31), and the gas tank (31) is connected with the pyrolysis furnace (26).

7. The environmentally-friendly microwave extraction device for comprehensive lignite utilization according to claim 6, wherein the first condenser (6) is respectively connected with a liquid medicine recovery device (7) and a lignite wax product collection device (8).

8. An environment-friendly microwave extraction process for comprehensively utilizing montan wax is characterized by comprising the following steps:

(1) montan wax extraction

Lignite is crushed by adding water through a wet type crusher (1) and then classified, fine pulp is used for standby, coarse pulp is used for adjusting the concentration of ore pulp by tap water, ammonium chloride is added for stirring and dissolving, microwave extraction is carried out after the flow is adjusted, the extracted ore pulp is subjected to heat filtration, filter residue is dried, the filtrate is subjected to wax and liquid medicine separation, a montan wax product is obtained after montan wax is completely solidified and floats on the liquid medicine, and the liquid medicine is recycled;

(2) humic acid extraction

Adjusting the solid-to-liquid ratio of the fine slurry obtained in the step (1), adding sodium hydroxide, stirring, dissolving, adjusting the pH value, adjusting the flow rate, performing microwave extraction on the fine slurry, filtering the fine slurry after extraction, recycling filter residues, acidifying the filtrate, performing precipitation, concentrating, drying and crushing the filtrate to obtain a fulvic acid product, and drying the filter residues to obtain brownish black humic acid;

(3) pyrolysis

Drying the filter residue subjected to heat filtration in the step (1), condensing dried water vapor for later use, crushing the dried mineral, fully crushing, performing electric heating pyrolysis in a reducing atmosphere, controlling the pyrolysis temperature at 650-800 ℃ for medium-temperature pyrolysis, heating at the heating speed of 10-200 ℃ per second, generating main components of coal gas in the temperature range, separating the main components of the coal gas, separating tar and the coal gas, performing decoking on the molten semicoke to obtain a semicoke product, filling and collecting the separated tar, and adjusting the separated coal gas to be used as reducing gas for recycling.

9. An environment-friendly process for extracting montan wax by comprehensively utilizing microwaves is characterized in that tap water with the mass 5-9 times that of montan is added in the step (1) for crushing, the concentration of ore pulp is adjusted by water with the solid-liquid ratio of 1: 5-8, ammonium chloride with the total amount of 3-7% of the ore pulp is added for stirring and dissolving, the extraction temperature is controlled to be 90-95 ℃ for extracting montan wax, and the heat filtering temperature is 75-85 ℃.

10. An environment-friendly microwave extraction process for comprehensively utilizing montan wax is characterized in that in the step (2), the solid-to-liquid ratio is 1: 8-10, 1-1.5% of sodium hydroxide is added according to the total mass of ore pulp, stirring and dissolving are carried out, the pH value is adjusted to 10.5-11.5, and the extraction temperature is controlled to be 45-50 ℃ for extracting humic acid.

Technical Field

The invention belongs to the technical field of coal chemical industry, and particularly relates to a microwave extraction environment-friendly device and process for comprehensively utilizing lignite.

Background

In China, the reserve of lignite accounts for 55% of the total amount of coal, and lignite contains abundant montan wax and humic acid. Montan wax is a raw material for manufacturing coatings, paints, rubber additives, lubricating oil, high-grade wax paper and cosmetics. Humic acid extracted from lignite can be used as organic fertilizer, and the composite water-retaining agent can improve soil and promote the growth of crops. The humic acid can be used as a heavy metal adsorbent for sewage treatment, and the humic acid of lignite can be used as a slurry regulator in various deep well drilling. The products such as organic chemical raw material tar and light oil, high-quality power fuel, gasification raw material semi-coke, coke oven gas and the like can be extracted from the lignite. Lignite is large in water content, low in calorific value and high in volatile matter, and lignite, particularly young lignite, often contains rare resources such as montan wax and humic acid. The classification and quality-based utilization is to develop related products or clean energy according to the characteristics of coal, so that the resources and benefits are maximized. The classification and quality-separation utilization generally refers to extracting humic acid, montan wax, volatile matters (oil and gas) and fixed carbon (semi-coke), and then respectively developing and utilizing. After humic acid and montan wax are extracted, clean energy is obtained through pyrolysis, and meanwhile, the external dependence of China on petroleum and natural gas can be effectively relieved, and a good supplement effect is achieved for guaranteeing national energy safety. The grading and quality-grading utilization of coal is to realize the clean and efficient utilization of coal. The existing humic acid extraction process is extraction after drying, because the moisture contained in the lignite is about 30-60 percent and most of the moisture is capillary tube moisture, the lignite can only be dehydrated in a heating evaporation mode, the traditional drying method is that the lignite is heated by indirectly contacting with a rotary kiln, and the moisture is evaporated and dried, but the ignition point of the lignite is low, the coal quality is poor due to local overheating in the coal drying process, valuable components in the lignite are damaged, the control is poor, explosion is caused, and the energy consumption of the process is particularly high and violates the purposes of energy conservation and emission reduction. The existing extraction process of the montan wax uses benzene and xylene organic solvents for extraction, the extracting agent is a flammable and explosive volatile raw material, great influence is caused to the environment, and once leakage occurs, explosion danger can be caused.

Disclosure of Invention

The invention aims to provide a microwave extraction environment-friendly device for comprehensive utilization of lignite.

The second purpose of the invention is to provide a microwave extraction process for comprehensive utilization of lignite.

The first purpose of the invention is realized by the following steps that the wet type pulverizer and the spiral classifier are included, the wet type pulverizer is connected with the spiral classifier, the spiral classifier is respectively connected with a first storage tank and a second storage tank, the first storage tank is respectively connected with a first microwave extractor and a first plate-frame filter in sequence, and the first plate-frame filter is connected with a first condenser;

the second storage tank is connected with a second microwave extractor, a second plate-frame filter, an acidolysis tank, a sedimentation tank and a third plate-frame filter in sequence, a material inlet of the acidolysis tank is connected with a material outlet of an acid storage tank, a liquid outlet of the third plate-frame filter is connected with a liquid medicine tank, and a filter residue outlet is connected with a first microwave dryer;

the first plate-frame filter is connected with the second microwave dryer, the mixing roll and the pyrolysis furnace in sequence, the top of the pyrolysis furnace is connected with the separator, and the bottom of the pyrolysis furnace is connected with the third condenser.

The second object of the present invention is achieved by the steps of:

(1) montan wax extraction

Lignite is crushed by a wet type crusher 1 through adding water and then classified, fine pulp is used for standby, coarse pulp is used for adjusting the concentration of ore pulp by tap water, ammonium chloride is added for stirring and dissolving, microwave extraction is carried out after the flow is adjusted, the extracted ore pulp is subjected to heat filtration, filter residue is dried, the filtrate is subjected to wax and liquid medicine separation, a montan wax product is obtained after montan wax is completely solidified and floats on the liquid medicine, and the liquid medicine is recycled;

(2) humic acid extraction

Adjusting the solid-to-liquid ratio of the fine slurry obtained in the step (1), adding sodium hydroxide, stirring, dissolving, adjusting the pH value, adjusting the flow rate, performing microwave extraction on the fine slurry, filtering the fine slurry after extraction, recycling filter residues, acidifying the filtrate, performing precipitation, concentrating, drying and crushing the filtrate to obtain a fulvic acid product, and drying the filter residues to obtain brownish black humic acid;

(3) pyrolysis

Drying the filter residue subjected to heat filtration in the step (1), condensing dried water vapor for later use, crushing the dried mineral, fully crushing, performing electric heating pyrolysis in a reducing atmosphere, controlling the pyrolysis temperature at 650-800 ℃ for medium-temperature pyrolysis, heating at the heating speed of 10-200 ℃ per second, generating main components of coal gas in the temperature range, separating the main components of the coal gas, separating tar and the coal gas, performing decoking on the molten semicoke to obtain a semicoke product, filling and collecting the separated tar, and adjusting the separated coal gas to be used as reducing gas for recycling.

The invention has the beneficial effects that:

the invention replaces the traditional process, the lignite is reselected by water, light matters are used for extracting humic acid by microwave without drying, heavy matters are used for extracting lignite wax by a microwave hydrolysis method, the lignite wax and the humic acid are extracted and then dried by microwave, and other products are produced by pyrolysis after drying. Because microwaves have distinctive selective heating characteristics and the absorption capacity of water to the microwaves is stronger than that of other polar solvents, water in the lignite capillary tube is quickly evaporated from inside to outside, and therefore energy is saved. And the traditional process heats from outside to inside, and the moisture is wrapped by the materials and is difficult to evaporate, thereby consuming energy. In the extraction aspect, water is used as a solvent, an auxiliary agent is added, the material vibrates in the frequency of microwave 915 plus 2450MHz/s, and water vapor generated by water in the lignite capillary tube is beneficial to oxidative decomposition of the humic acid of macromolecules, so that the separation purpose of the extract is achieved. No organic solvent is used, so that the potential safety hazard is eliminated, and the environment is not influenced.

Drawings

FIG. 1 is a schematic view of the overall structure of the present invention;

in the figure: 1-wet type pulverizer, 2-spiral classifier, 3-first storage tank, 4-first microwave extractor, 5-first plate frame filter, 6-first condenser, 7-liquid medicine recovery device, 8-montan wax product collection device, 9-second storage tank, 10-second microwave extractor, 11-second plate frame filter, 12-acidolysis tank, 13-acid storage tank, 14-sedimentation tank, 15-third plate frame filter, 16-liquid medicine tank, 17-condensate tank, 18-first microwave dryer, 19-Raymond mill, 20-dust collector, 21-humic acid product collection device, 22-second microwave dryer, 23-second condenser, 24-water storage tank, 25-mixing mill, 26-pyrolysis furnace, 27-intermediate frequency power supply, 28-third condenser, 29-semicoke product collecting device, 30-separator, 31-gas tank and 32-tar product collecting device.

Detailed Description

The invention is further described with reference to the accompanying drawings, but the invention is not limited in any way and any variations or modifications based on the teachings of the invention are within the scope of the invention.

As shown in fig. 1, the device of the invention comprises a wet type pulverizer 1 and a spiral classifier 2, wherein the wet type pulverizer 1 is connected with the spiral classifier 2, the spiral classifier 2 is respectively connected with a first storage tank 3 and a second storage tank 9, the first storage tank 3 is respectively connected with a first microwave extractor 4 and a first plate-frame filter 5 in sequence, and the first plate-frame filter 5 is connected with a first condenser 6;

the second material storage tank 9 is connected with a second microwave extractor 10, a second plate frame filter 11, an acidolysis tank 12, a sedimentation tank 14 and a third plate frame filter 15 which are sequentially connected, a material inlet of the acidolysis tank 12 is connected with a material outlet of an acid storage tank 13, a liquid outlet of the third plate frame filter 15 is connected with a liquid medicine tank 16, and a filter residue outlet is connected with a first microwave dryer 18;

the first plate frame filter 5 is respectively connected with a second microwave dryer 22, a mixing roll 25 and a pyrolysis furnace 26 in sequence, the top of the pyrolysis furnace 26 is connected with a separator 30, and the bottom of the pyrolysis furnace is connected with a third condenser.

The first microwave dryer 18 is connected with a condensation water tank 17 and a Raymond mill 19, and the Raymond mill 19 is connected with a dust collector 20.

The steam outlet of the second microwave dryer 22 is connected with a second condenser 23, and the second condenser 23 is connected with a water storage pool 24.

And the second plate frame filter 11 is connected with the first material storage tank 3.

The pyrolysis furnace 26 is powered by a medium frequency power supply 27.

The separator 30 is connected with a gas tank 31, and the gas tank 31 is connected with the pyrolysis furnace 26.

The first condenser 6 is respectively connected with a liquid medicine recovery device 7 and a montan wax product collecting device 8.

The process comprises the following steps:

(1) montan wax extraction

Lignite is crushed by adding water through a wet type crusher (1) and then classified, fine pulp is used for standby, coarse pulp is used for adjusting the concentration of ore pulp by tap water, ammonium chloride is added for stirring and dissolving, microwave extraction is carried out after the flow is adjusted, the extracted ore pulp is subjected to heat filtration, filter residue is dried, the filtrate is subjected to wax and liquid medicine separation, a montan wax product is obtained after montan wax is completely solidified and floats on the liquid medicine, and the liquid medicine is recycled;

(2) humic acid extraction

Adjusting the solid-to-liquid ratio of the fine slurry obtained in the step (1), adding sodium hydroxide, stirring, dissolving, adjusting the pH value, adjusting the flow rate, performing microwave extraction on the fine slurry, filtering the fine slurry after extraction, recycling filter residues, acidifying the filtrate, performing precipitation, concentrating, drying and crushing the filtrate to obtain a fulvic acid product, and drying the filter residues to obtain brownish black humic acid;

(3) pyrolysis

Drying the filter residue subjected to heat filtration in the step (1), condensing dried water vapor for later use, crushing the dried mineral, performing electric heating pyrolysis in a reducing atmosphere after fully crushing, supplying power by a medium-frequency power supply (27), performing medium-temperature pyrolysis at the pyrolysis temperature of 650-800, heating at the heating speed of 10-200 ℃ per second, generating main components of coal gas in the temperature range, separating the coal gas from the coal gas, performing decoking on the molten semicoke to obtain a semicoke product, filling and collecting the separated tar, and adjusting the separated coal gas to be used as reducing gas for recycling.

Adding tap water with the mass 5-9 times of that of the lignite into the lignite, crushing, adjusting the concentration of ore pulp by using water with the solid-to-liquid ratio of 1: 5-8, adding ammonium chloride accounting for 3% -7% of the total amount of the ore pulp, stirring and dissolving, controlling the extraction temperature to be 90-95 ℃, extracting lignite wax, and controlling the heat filtering temperature to be 75-85 ℃.

And (3) adding 1-1.5% of sodium hydroxide according to the total mass of the ore pulp, stirring and dissolving to adjust the pH value to 10.5-11.5, and extracting humic acid at the extraction temperature of 45-50 ℃.

Examples

Adding tap water with the mass 5-9 times of that of lignite into lignite through a wet grinder 1 for grinding, classifying ore pulp through a spiral classifier 2, sending fine pulp to a second storage tank 9 for standby, combining coarse pulp and filter residue of a second plate-frame filter 11, sending the coarse pulp and the filter residue into a first storage tank 3, adjusting the concentration of the ore pulp by using the tap water according to the solid-to-liquid ratio of 1: 5-8, adding ammonium chloride accounting for 3-7% of the total amount of the ore pulp, stirring and dissolving, adjusting the flow rate, sending the mixture into a first microwave extractor 4, extracting lignite wax at the extraction temperature of 90-95 ℃, extracting for 30-60 minutes, sending the extracted ore pulp into a first plate-frame filter 5 through a conveying pipeline with a water bath sleeve and the constant temperature of 75-85 ℃, carrying out heat filtration, sending the filter residue to a second microwave dryer 22, sending filtrate to a first condenser 6 for wax and liquid medicine separation, and completely solidifying the lignite wax on, the liquid medicine is sent to a liquid medicine recovery device 7 to be recycled after the concentration of the liquid medicine is adjusted, and the montan wax is cleaned out from a first condenser 6 and sent to a montan wax product collection device 8 to be cleaned to obtain montan wax products;

(2) humic acid extraction

Detecting the solid-liquid ratio of a second storage tank 9, adjusting the solid-liquid ratio to be 1: 8-10, adding 1-1.5% of sodium hydroxide according to the total mass of the ore pulp, stirring, dissolving, adjusting the pH value to be 10.5-11.5, adjusting the flow rate, sending the mixture into a second microwave extractor 10, controlling the extraction temperature to be 45-50 ℃ for extracting humic acid, extracting for 10-30 minutes, sending the extract into a second plate-frame filter 11 for filtering, sending filter residues into a first storage tank 3 for combining with coarse materials, sending filtrate into an acidolysis tank 12, providing 5% hydrochloric acid by an acid storage tank 13, adding the hydrochloric acid into the ore pulp of the acidolysis tank 12 for acidification, sending the ore pulp into a sedimentation tank 14 for sedimentation, sending the solution to a first microwave dryer 18 for drying, sending the sediment to a third plate-frame filter 15 for filtering, sending the filtrate into a liquid tank 16 for concentration, drying and crushing to obtain a humic acid product, sending the filter residues into a first microwave dryer 18 for drying, sending water vapor in a condensation water tank 17 for later use, conveying the dried brown black humic acid to a Raymond mill 19 for crushing to qualified mesh number, collecting and packaging by a dust collector 20, and conveying to a humic acid product collecting device 21 for collection;

(3) pyrolysis

Slag from a first plate-frame filter 5 is sent to a second microwave dryer 22 for drying, steam of the dryer is sent to a second condenser 23 for condensing and then sent to a water storage tank 24 for standby, minerals dried by the second microwave dryer 22 are sent to a mixing roll 25 for grinding, the minerals are sent to a pyrolysis furnace 26 for electric heating pyrolysis in a reducing atmosphere after being sufficiently ground, power is supplied by a medium-frequency power supply 27, the pyrolysis temperature is controlled to be 650-800 ℃ for medium-temperature pyrolysis, the heating speed is increased between 10-200 ℃ per second, main components of coal gas such as hydrogen, methane, carbon monoxide or reducing gas mixture are firstly generated in the temperature range, tar and coal gas are separated from the top of the furnace and sent to a separator 30, the molten semicoke is discharged from the bottom of the pyrolysis furnace into a third condenser 28 for decoking, the molten semicoke is sent to a semicoke product collecting device 29 by a gap feeding mechanism for collecting, the tar separated from the separator 30 is sent to a tar product collecting device 32 for collecting, the coal gas is sent to a gas tank 31 for storage and is returned to the pyrolysis furnace 26 to be used as reducing gas after being adjusted.

Acidification in step (2) resulted in pH =2 of the extract.

The principle of the invention is illustrated below by experiments with lignite samples:

lignite samples were provided by a Yunnan seek Dian coal mine and the test reports are as follows.

Crushing 1Kg of sample by a small ball mill, sieving with a 80-mesh sieve for standby, dissolving 150g of sodium hydroxide in 3L of water for standby, adding 5L of tap water into a 15L plastic container, placing the container in a water bath kettle with a constant temperature of 50 ℃, slowly adding 1Kg of 80-mesh sample under the condition of stirring, continuously stirring and gradually adding sodium hydroxide solution, alternately adding tap water and alkali liquor to adjust the pH =11 to 10L scale, heating to 50 ℃, immediately placing the container and ore pulp into a self-made 1kw microwave extractor with a frequency of 2450MHz, extracting filter residue for 2 minutes by microwaves, pouring out the ore pulp for filtering, transferring filtrate into a 15L container for standby, and placing into a drying box for drying for standby.

Extracting humic acid, adjusting the pH of the microwave extracting solution to be =2 by using a 5% hydrochloric acid solution, carrying out acidolysis for 30 minutes, filtering the supernatant to obtain fulvic acid, precipitating the fulvic acid to obtain a mixture of the fulvic acid and the fulvic acid, concentrating and drying the supernatant to obtain 4.23g of fulvic acid, wherein the recovery rate is 92%. The deposits of the brown humic acid and the black humic acid are dried to obtain 490g, and the recovery rate is 90 percent.

Extracting montan wax, adding 4L of tap water into a 5L container, adding 25g of ammonium chloride, stirring and dissolving, continuously stirring and slowly adding 500g of slag after extracting humic acid, putting into a microwave extractor, heating to 95 ℃, extracting for 3 minutes at constant temperature, filtering while hot, cooling filtrate to 10 ℃ in a water chiller through water separation, filtering to obtain 68g of montan wax, and the recovery rate is 85%.