CN108557772B - Treatment method of sulfur mud of dicyclohexyl disulfide - Google Patents
Treatment method of sulfur mud of dicyclohexyl disulfide Download PDFInfo
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/027—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a treatment method of sulfur mud of dicyclohexyl disulfide, which comprises the steps of mixing sulfur mud waste residue with a sodium sulfide solution, stirring until the sulfur mud waste residue is not dissolved any more, then filtering, storing filtrate, and recycling the filtrate as a raw material of the dicyclohexyl disulfide; mixing the obtained residue with hydrochloric acid, stirring, standing, and filtering; and adding the filter residue into water, stirring and washing until no water-soluble substance is dissolved in the water, and drying the filter residue after washing to be treated as solid waste. The invention has good recovery effect on the sulfur mud waste residue generated in the production process of dicyclohexyl disulfide, can improve the recovery utilization rate of sulfur, avoids resource waste, saves chemical production cost, reduces waste generated in the production process, avoids environmental pollution to a certain extent, accords with the environment protection idea advocated by modern times, and practices the idea of green chemical industry.
Description
Technical Field
The invention relates to a method for treating sulfur mud generated in a dicyclohexyl disulfide production process, in particular to a method for recovering low-grade sulfur from the sulfur mud generated in the dicyclohexyl disulfide production process, and belongs to the technical field of dicyclohexyl disulfide waste treatment.
Background
The structural formula of dicyclohexyl disulfide (disulfide for short) is
Can be used as food spice and used in the fields of dye, medicine, pesticide, organic synthesis and the like; in the rubber auxiliaries sector, dicyclohexylThe disulfide is one of important intermediates for synthesizing a scorch retarder CTP (N-cyclohexyl thiophthalimide). Modern rubber processing technology is developing towards high temperature and high speed, the position of the anti-coking agent is more and more prominent, and the position of the intermediate product dicyclohexyl disulfide is more and more important.
Currently, the main methods for synthesizing disulfides are: with Na2S, S and chlorocyclohexane as raw materials, dissolving sodium sulfide in water, adding sulfur, stirring, adding chlorocyclohexane for reaction, separating disulfide product, and adding mother liquor into mother liquor tank. The mother liquor contains Na2S, NaCl, NaHS, S, water and the like, and at present, the conventional industrial treatment method for the mother liquor comprises the following steps: adding hydrochloric acid into the mother liquor for acidification, reacting HCl with NaHS to generate hydrogen sulfide gas, absorbing the generated hydrogen sulfide gas with alkali liquor, ending acidification when the pH value of the mother liquor reaches 6-7, carrying out plate-and-frame filter pressing on the mother liquor, feeding the obtained filtrate into a wastewater tank, and carrying out further water treatment, wherein the main component of the obtained filter residue is unreacted sulfur, the content of the unreacted sulfur is about 70-76%, and impurities brought by some raw materials are called sulfur mud. The obtained sulfur paste is generally sold to manufacturers specially used for waste solid treatment after being directly bagged as solid waste, which not only wastes resources in industrial production, but also is contrary to the modern environmental protection concept. Most of the current reports on disulfide are focused on the improvement of the synthetic method, and the reports and researches on how to better utilize and treat the sulfur mud are rare. At present, the country pays more and more attention to environmental protection and advocates the concept of green chemical industry, so that the development of a method with certain industrial value for treating sulfur mud generated in the reaction process is of great importance in the chemical industry.
Disclosure of Invention
Aiming at the problems of resource waste and environmental pollution of the sulfur mud in the prior art, the invention provides a treatment method of the sulfur mud of dicyclohexyl disulfide, which uses sodium sulfide to recover low-grade sulfur in the sulfur mud, avoids resource waste, improves the added value of the sulfur mud, reduces the environmental pollution and provides an effective way for reutilization and post-treatment of the sulfur mud.
The specific technical scheme of the invention is as follows:
a process for the treatment of sulphur sludge of dicyclohexyldisulphide, comprising the following steps:
(1) mixing the sulfur mud waste residue (detecting sulfur mud or waste residue, the same below) with sodium sulfide solution, stirring until the sulfur mud waste residue is not dissolved, filtering, storing the filtrate, and recycling the filtrate as the raw material of dicyclohexyl disulfide;
(2) taking the filter residue obtained after filtering in the step (1), fully stirring and mixing with hydrochloric acid, then standing, filtering after standing, and performing neutralization treatment on the obtained filtrate and then feeding the filtrate into a water treatment system for treatment or using the filtrate as industrial hydrochloric acid;
(3) and (3) adding the filter residue obtained after filtration in the step (2) into water, stirring and washing until no water-soluble substance is dissolved in the water, and drying the filter residue after washing to be treated as solid waste.
In the invention, the sulfur mud is filter residue obtained by acidifying and filter-pressing mother liquor generated in the production process of dicyclohexyl disulfide, and the sulfur mud comprises the following components in percentage by weight: 70-76wt% of sulfur and 24-30wt% of other impurities. According to the invention, the low-grade sulfur in the sulfur mud is recycled according to the principle that the solubility of the sulfur in the sodium sulfide solution is higher than that of the sulfur in pure water and the sulfur can generate sodium disulfide in the sodium sulfide solution, so that the sulfur in the sulfur mud waste residue can be recycled, the utilization efficiency of the sulfur is improved, the production amount of the waste residue is reduced, the cost for treating the waste residue is reduced, and the production cost is further saved. Meanwhile, the sodium sulfide solution reacts with sulfur to generate sodium disulfide which is an important raw material for preparing the sulfur-containing organic compound, can be directly reused in the production of dicyclohexyl disulfide and has important industrial value.
Further, in the step (1), the mass ratio of the sodium sulfide solution to the sulfur mud waste residue is 1-1.5: 1; preferably, the concentration of the sodium sulfide solution is 10.0-30.0g/100 ml.
Further, in the step (1), the sulfur mud waste residue and the sodium sulfide solution are mixed and stirred at the temperature of 65-85 ℃, and the pressure is normal pressure. The temperature can be heated by steam circulation generated in the production process of dicyclohexyl disulfide. At the temperature, the sulfur paste can be fully dissolved after being mixed and stirred for 25 to 45 minutes. After the dissolution is completed, the solution is cooled by circulating water, and then the filtration and separation operations are carried out. The filtration can adopt various forms such as centrifugal filtration, filtration tank suction filtration, filter pressing, plate-and-frame filter pressing and the like. The filtrate obtained by filtration is stored intensively and used as a raw material for producing dicyclohexyl disulfide in a chemical industry.
Further, the filter residue obtained by filtering in the step (1) is subjected to further treatment in the step (2), and the mass ratio of the hydrochloric acid to the filter residue obtained by filtering in the step (1) is 1-1.2: 1; preferably, the concentration of the hydrochloric acid is 0.05-9.0 mol/L.
Further, in the step (2), the stirring time is 10-45 minutes, so that the hydrochloric acid and the filter residue obtained by filtering in the step (1) are fully mixed. After stirring, standing and settling for 10-45 minutes, and then filtering. The filtration can adopt various forms such as centrifugal filtration, filtration tank suction filtration, filter pressing, plate-and-frame filter pressing and the like.
Further, in the step (2), neutralization treatment is carried out on the filtrate, the pH value of the filtrate is controlled to be 6-8, and then the filtrate enters a water treatment system for treatment.
Further, in the step (2), the filtrate is purified and used as industrial hydrochloric acid. The purification treatment may be performed using an ion exchange resin.
Further, in the step (3), the filter residue is washed by multiple times of water washing, the total amount of water is 4-6 times of the mass of the filter residue, the filter residue is preferably washed for more than three times, for example, 3-6 times, and the water consumption for the first time is preferably more than that for the later times. The mode of cleaning for a small number of times is adopted, so that the cleaning is cleaner, and the water can be saved. Experiments prove that under the condition that the water consumption is the same, the cleaning can be carried out for multiple times to clean the water, and if the water is cleaned for one time, the effect is not as good as that of the cleaning for multiple times. And during each cleaning, mixing and stirring the filter residue and water for 30-50 minutes, and then filtering by adopting the forms of centrifugal filtration, filtration of a filter tank, filter pressing, plate-and-frame filter pressing and the like.
Further, in the step (3), the filtrate obtained after each washing and filtering is circularly used in the step (3) as washing water until crystals are precipitated in the filtrate, and the filtrate obtained after crystallization is put into a water treatment system for treatment. The filtrate can be used for washing the filter residue in the next batch independently, and can also be mixed with fresh water for washing the filter residue.
Further, in the step (3), the water vapor obtained by drying is cooled and stored for dissolving sodium sulfide.
Further, in the step (3), the dried waste residue is subjected to screening and other operations, and finally enters a packaging line for packaging, and then is treated as solid waste. Such as in landfills, or sold to a manufacturer dedicated to waste disposal.
The invention has the following advantages:
1. the invention has good recovery effect on the sulfur mud waste residue generated in the production process of dicyclohexyl disulfide, can improve the recovery utilization rate of sulfur, avoid the waste of resources, save the chemical production cost, reduce the waste generated in the production process, avoid the pollution to the environment to a certain extent, accord with the environment protection idea advocated in the modern times, and practice the idea of green chemical industry.
2. The invention recovers low-grade sulfur by using the sodium sulfide solution used in the reaction process of dicyclohexyl disulfide, the sulfur is converted into sodium disulfide, the product sodium disulfide is an important raw material for preparing sulfur-containing organic compounds, can be directly used for producing dicyclohexyl disulfide, and has important industrial value and practical significance.
3. The invention recycles the filtrate generated in the recycling process as much as possible, for example, the filtrate of the washing waste residue is circularly used as washing water, thereby saving water resources and having strong practicability.
Detailed Description
The invention will be illustrated below by means of specific examples of how the sodium sulphide solution is used to recover sulphur sludge produced during the production of dicyclohexyldisulphide. The following description is intended to be illustrative of the invention and should not be taken to be limiting.
The sulphur sludge waste and the sodium sulphide solution used in the following examples were both taken directly from the dicyclohexyldisulphide plant. The used sulfur mud waste residue comprises the following components (wt%): 74% of sulfur and 26% of other impurities.
Example 1
1. Taking 400.0g of sulfur mud waste residue in a 1000ml beaker. 400.0g of sodium sulfide solution (with the concentration of 10.0g/100 ml) is weighed and poured into the beaker, the beaker is placed into a water bath kettle at 70 ℃ for stirring, and after stirring for 30 minutes, the filter residue is not dissolved any more. And (4) carrying out suction filtration operation by using a suction filtration machine, and weighing the filter residue with the mass of 132.5g and the filtrate with the mass of 667.5g after the suction filtration is finished. The filtrate can be used as a raw material for workshop production of dicyclohexyl disulfide.
2. And (2) putting the filter residue obtained by suction filtration in the step (1) into a beaker, measuring 133 g of hydrochloric acid (with the concentration of 0.5 mol/L) and putting into the beaker, stirring for 30 minutes at normal temperature and normal pressure, dissolving part of substances in the hydrochloric acid, standing for 30 minutes, carrying out suction filtration operation by using a suction filtration machine, and obtaining 105.9g of filter residue after the suction filtration is finished. Neutralizing the filtrate, controlling the pH value of the filtrate to be 6-8, and then treating the neutralized filtrate in a water treatment system according to a water treatment process, wherein the water treatment system is not described; or the filtrate is purified to be used as industrial hydrochloric acid.
3. And (4) carrying out successive water washing on the filter residue subjected to suction filtration in the step (2). The mass of the primary water for the first time (primary water, namely fresh clean water) is 200g, stirring is carried out for 30 minutes, suction filtration operation is carried out, and the operation is repeated, wherein the water consumption is respectively 150g, 50g, 50g and 50g in sequence, namely the water consumption is 500 g. After washing, the filter residue was dried in an oven, and after two hours, the filter residue was weighed to a mass of 84.2 g. And mixing the filtrate obtained by washing and filtering the filter residue with the next batch of primary water, entering the next washing operation cycle until crystals are separated out, and entering the water-washing filtrate after the crystals are separated out into a water treatment system for unified treatment.
Example 2
1. Taking 400.0g of sulfur mud waste residue in a 1000ml beaker. 400.0g of sodium sulfide solution (with the concentration of 10.0g/100 ml) is weighed and poured into the beaker, the beaker is placed into a 65 ℃ water bath kettle to be stirred, and after stirring for 25 minutes, the filter residue is not dissolved any more. And (4) carrying out suction filtration by using a suction filtration machine, and weighing the filter residue with the mass of 134.1g and the filtrate with the mass of 665.9g after the suction filtration is finished. The filtrate can be used as a raw material for workshop production of dihexyl polar disulfide.
2. And (2) putting the filter residue obtained by suction filtration in the step (1) into a beaker, measuring 160 g of hydrochloric acid (with the concentration of 0.05 mol/L) and putting into the beaker, stirring for 45 minutes at normal temperature and normal pressure, dissolving part of substances in the hydrochloric acid, standing for 30 minutes, carrying out suction filtration operation by using a suction filtration machine, and obtaining 112.3g of filter residue after the suction filtration is finished. Neutralizing the filtrate, controlling the pH value of the filtrate to be 6-8, and then treating the neutralized filtrate in a water treatment system according to a water treatment process, wherein the water treatment system is not described; or the filtrate is purified and used as industrial hydrochloric acid.
3. And (4) carrying out successive water washing on the filter residue subjected to suction filtration in the step (2). The mass of the primary water for the first time (primary water, namely fresh clean water) is 200g, stirring is carried out for 30 minutes, suction filtration operation is carried out, and the operation is repeated, wherein the water consumption is respectively 100g, 50g and 50g in sequence, namely the water consumption is 450g in total. After washing, the filter residue was dried in an oven, and after two hours, the filter residue was weighed to a mass of 89.3 g. And mixing the filtrate obtained by washing and filtering the filter residue with the next batch of primary water, entering the next washing operation cycle until crystals are separated out, and entering the water-washing filtrate after the crystals are separated out into a water treatment system for unified treatment.
Example 3
1. 400.0g of sulfur mud waste residue is taken to be put in a 1000ml beaker. 600.0g of sodium sulfide solution (with the concentration of 10.0g/100 ml) is measured and poured into the beaker, the beaker is placed into a water bath kettle at 70 ℃ for stirring, and after stirring for 25 minutes, the filter residue is not dissolved any more. And (4) carrying out suction filtration by using a suction filtration machine, and weighing the filter residue with the mass of 130.9g and the filtrate with the mass of 869.1g after the suction filtration is finished. The filtrate can be used as a raw material for workshop production of dicyclohexyl disulfide.
2. And (2) putting the filter residue obtained by suction filtration in the step (1) into a beaker, measuring 131.0 g of hydrochloric acid (with the concentration of 0.1 mol/L) and putting into the beaker, stirring for 30 minutes at normal temperature and normal pressure, dissolving part of substances in the hydrochloric acid, standing for 30 minutes, carrying out suction filtration operation by using a suction filtration machine, and obtaining 103.5g of filter residue after the suction filtration is finished. Neutralizing the filtrate, controlling the pH value of the filtrate to be 6-8, and then treating the neutralized filtrate in a water treatment system according to a water treatment process, wherein the water treatment system is not described; or the filtrate is purified and used as industrial hydrochloric acid.
3. And (4) carrying out successive water washing on the filter residue subjected to suction filtration in the step (2). The mass of the primary water for the first time (primary water, namely fresh clean water) is 300g, stirring is carried out for 30 minutes, suction filtration operation is carried out, and the operation is repeated, wherein the water consumption is respectively 150g, 50g, 50g and 50g in sequence, namely the water consumption is 600 g. After washing, the filter residue was dried in an oven, and after two hours, the filter residue was weighed to a mass of 82.9 g. And mixing the filtrate obtained by washing and filtering the filter residue with the next batch of primary water, entering the next washing operation cycle until crystals are separated out, and entering the water-washing filtrate after the crystals are separated out into a water treatment system for unified treatment.
Example 4
1. 400.0g of sulfur mud waste residue is taken to be put in a 1000ml beaker. 400.0g of sodium sulfide solution (with the concentration of 30.0g/100 ml) is weighed and poured into the beaker, the beaker is placed into a water bath kettle at 70 ℃ for stirring, and after stirring for 25 minutes, the filter residue is not dissolved any more. And (4) performing suction filtration by using a suction filtration machine, and weighing filter residue with the mass of 132.9g and filtrate with the mass of 667.1g after the suction filtration is finished. The filtrate can be used as a raw material for workshop production of dicyclohexyl disulfide.
2. And (2) putting the filter residue obtained by suction filtration in the step (1) into a beaker, measuring 160 g of hydrochloric acid (with the concentration of 1.0 mol/L) and putting into the beaker, stirring for 10 minutes at normal temperature and normal pressure, dissolving part of substances in the hydrochloric acid, standing for 15 minutes, carrying out suction filtration operation by using a suction filtration machine, and obtaining 106.1g of filter residue after the suction filtration is finished. Neutralizing the filtrate, controlling the pH value of the filtrate to be 6-8, and then treating the neutralized filtrate in a water treatment system according to a water treatment process, wherein the water treatment system is not described; or the filtrate is purified and used as industrial hydrochloric acid.
3. And (4) carrying out successive water washing on the filter residue subjected to suction filtration in the step (2). The mass of the primary water for the first time (primary water, namely fresh clean water) is 200g, stirring is carried out for 30 minutes, suction filtration operation is carried out, and the operation is repeated, wherein the water consumption is respectively 150g, 50g, 50g and 50g in sequence, namely the water consumption is 500 g. After washing, the filter residue was dried in an oven, and after two hours, the filter residue was weighed to a mass of 85.3 g. And mixing the filtrate obtained by washing and filtering the filter residue with the next batch of primary water, entering the next washing operation cycle until crystals are separated out, and entering the water-washing filtrate after the crystals are separated out into a water treatment system for unified treatment.
Example 5
1. 400.0g of sulfur mud waste residue is taken to be put in a 1000ml beaker. 400.0g of sodium sulfide solution (with the concentration of 30.0g/100 ml) is weighed and poured into the beaker, the beaker is placed into a water bath kettle at 85 ℃ for stirring, and after stirring for 45 minutes, the filter residue is not dissolved any more. And (4) carrying out suction filtration by using a suction filtration machine, and weighing 133.1g of filter residue and 666.9g of filtrate after the suction filtration is finished. The filtrate can be used as a raw material for workshop production of dicyclohexyl disulfide.
2. And (2) putting the filter residue obtained by suction filtration in the step (1) into a beaker, measuring 134.0 g of hydrochloric acid (with the concentration of 3.0 mol/L) and putting into the beaker, stirring for 20 minutes at normal temperature and normal pressure, dissolving part of substances in the hydrochloric acid, standing for 30 minutes, carrying out suction filtration operation by using a suction filtration machine, and obtaining 106.3g of filter residue after the suction filtration is finished. Neutralizing the filtrate, controlling the pH value of the filtrate to be 6-8, and then treating the neutralized filtrate in a water treatment system according to a water treatment process, wherein the water treatment system is not described; or the filtrate is purified and used as industrial hydrochloric acid.
3. And (4) carrying out successive water washing on the filter residue subjected to suction filtration in the step (2). The mass of the primary water for the first time (primary water, namely fresh clean water) is 300g, stirring is carried out for 30 minutes, suction filtration operation is carried out, and the operation is repeated, wherein the water consumption is respectively 200g and 100g in sequence, namely the common water quantity is 600 g. After washing, the filter residue was put into an oven to be dried, and after two hours, the filter residue was weighed to a mass of 85.0 g. And mixing the filtrate obtained by washing and filtering the filter residue with the next batch of primary water, entering the next washing operation cycle until crystals are separated out, and entering the water-washing filtrate after the crystals are separated out into a water treatment system for unified treatment.
Example 6
1. Taking 400.0g of sulfur mud waste residue in a 1000ml beaker. 600.0g of sodium sulfide solution (with the concentration of 30.0g/100 ml) is weighed and poured into the beaker, the beaker is placed into a water bath kettle at 85 ℃ for stirring, and after stirring for 45 minutes, the filter residue is not dissolved any more. And (4) carrying out suction filtration by using a suction filtration machine, and weighing the filter residue with the mass of 132.7g and the filtrate with the mass of 867.3g after the suction filtration is finished. The filtrate can be used as a raw material for workshop production of dicyclohexyl disulfide.
2. And (2) putting the filter residue obtained by suction filtration in the step (1) into a beaker, measuring 159.2 g of hydrochloric acid (with the concentration of 5.0 mol/L) and putting into the beaker, stirring for 20 minutes at normal temperature and normal pressure, dissolving part of substances in the hydrochloric acid, standing for 30 minutes, carrying out suction filtration operation by using a suction filtration machine, and obtaining 106.0g of filter residue after the suction filtration is finished. Neutralizing the filtrate, controlling the pH value of the filtrate to be 6-8, and then treating the neutralized filtrate in a water treatment system according to a water treatment process, wherein the water treatment system is not described; or the filtrate is purified and used as industrial hydrochloric acid.
3. And (4) carrying out successive water washing on the filter residue subjected to suction filtration in the step (2). The mass of the primary water for the first time (primary water, namely fresh clean water) is 300g, stirring is carried out for 30 minutes, suction filtration operation is carried out, and the operation is repeated, wherein the water consumption is respectively 150g, 50g, 50g and 50g in sequence, namely the water consumption is 600 g. After washing, the filter residue was dried in an oven, and after two hours, the filter residue was weighed to a mass of 84.9 g. And mixing the filtrate obtained by washing and filtering the filter residue with the next batch of primary water, entering the next washing operation cycle until crystals are separated out, and entering the water-washing filtrate after the crystals are separated out into a water treatment system for unified treatment.
Example 7
1. 400.0g of sulfur mud waste residue is taken to be put in a 1000ml beaker. 400.0g of sodium sulfide solution (with the concentration of 10.0g/100 ml) is weighed and poured into the beaker, the beaker is placed into a water bath kettle at 85 ℃ for stirring, and after stirring for 30 minutes, the filter residue is not dissolved any more. And (4) performing suction filtration by using a suction filtration machine, and weighing filter residue with the mass of 132.8g and filtrate with the mass of 667.2g after the suction filtration is finished. The filtrate can be used as a raw material for workshop production of dicyclohexyl disulfide.
2. And (2) putting the filter residue obtained by suction filtration in the step (1) into a beaker, measuring 132.8g of hydrochloric acid (with the concentration of 9.0 mol/L) and putting into the beaker, stirring for 30 minutes at normal temperature and normal pressure, dissolving part of substances in the hydrochloric acid, standing for 30 minutes, carrying out suction filtration operation by using a suction filtration machine, and obtaining 106.1g of filter residue after the suction filtration is finished. Neutralizing the filtrate, controlling the pH value of the filtrate to be 6-8, and then treating the neutralized filtrate in a water treatment system according to a water treatment process, wherein the water treatment system is not described; or the filtrate is purified and used as industrial hydrochloric acid.
3. And (4) carrying out successive water washing on the filter residue subjected to suction filtration in the step (2). The mass of the primary water for the first time (primary water, namely fresh clean water) is 300g, stirring is carried out for 30 minutes, suction filtration operation is carried out, and the operation is repeated, wherein the water consumption is respectively 150g, 50g, 50g and 50g in sequence, namely the water consumption is 600 g. After washing, the filter residue was dried in an oven, and after two hours, the filter residue was weighed to a mass of 84.8 g. And mixing the filtrate obtained by washing and filtering the filter residue with the next batch of primary water, entering the next washing operation cycle until crystals are separated out, and entering the water-washing filtrate after the crystals are separated out into a water treatment system for unified treatment.
Claims (1)
1. A treatment method of sulfur mud of dicyclohexyl disulfide is characterized by comprising the following steps:
(1) mixing the sulfur mud waste residue and a sodium sulfide solution at 65-85 ℃, stirring for 25-45 minutes until the sulfur mud waste residue is not dissolved, then filtering, storing the filtrate, and recycling the filtrate as a raw material of dicyclohexyl disulfide; the sulfur mud is filter residue obtained by acidifying and filter-pressing mother liquor generated in the production process of dicyclohexyl disulfide; the mass ratio of the sodium sulfide solution to the sulfur mud waste residue is 1-1.5: 1; the concentration of the sodium sulfide solution is 10.0-30.0g/100 ml;
(2) taking the filter residue obtained after filtration in the step (1), fully stirring and mixing with hydrochloric acid for 10-45 minutes, then standing for 10-45 minutes, filtering after standing, and allowing the obtained filtrate to enter a water treatment system for treatment or be used as industrial hydrochloric acid after neutralization treatment; the mass ratio of the hydrochloric acid to the filter residue obtained after filtering in the step (1) is 1-1.2:1, and the concentration of the hydrochloric acid is 0.05-9.0 mol/L;
(3) adding the filter residue obtained after filtration in the step (2) into water, stirring and washing for 3-6 times, wherein the total using amount of the water is 4-6 times of the mass of the filter residue until no water-soluble substance is dissolved in the water, and drying the filter residue after washing to be used as solid waste for treatment; circularly sleeving the filtrate after water washing as washing water in the step (3) until crystals are separated out from the filtrate, and treating the filtrate after crystallization in a water treatment system; cooling and storing the dried water vapor for dissolving sodium sulfide;
In the steps (1) - (3), the filtration mode is centrifugal filtration, suction filtration of a filter tank, filter pressing or plate-and-frame filter pressing.
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