CN114988435A - Harmless treatment method for saline water in polyphenylene sulfide resin production - Google Patents
Harmless treatment method for saline water in polyphenylene sulfide resin production Download PDFInfo
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- CN114988435A CN114988435A CN202210668084.0A CN202210668084A CN114988435A CN 114988435 A CN114988435 A CN 114988435A CN 202210668084 A CN202210668084 A CN 202210668084A CN 114988435 A CN114988435 A CN 114988435A
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 33
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 33
- 239000011780 sodium chloride Substances 0.000 title claims abstract description 28
- 239000011347 resin Substances 0.000 title claims abstract description 23
- 229920005989 resin Polymers 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 51
- 230000008020 evaporation Effects 0.000 claims abstract description 48
- 150000003839 salts Chemical class 0.000 claims abstract description 32
- 239000012267 brine Substances 0.000 claims abstract description 29
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims abstract description 29
- 239000012452 mother liquor Substances 0.000 claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000001632 sodium acetate Substances 0.000 claims abstract description 12
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 11
- 238000005374 membrane filtration Methods 0.000 claims abstract description 10
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000012535 impurity Substances 0.000 claims description 12
- 238000005485 electric heating Methods 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 4
- 239000002910 solid waste Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 17
- 239000007788 liquid Substances 0.000 description 9
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 8
- 229910052808 lithium carbonate Inorganic materials 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 229910052977 alkali metal sulfide Chemical class 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 230000019086 sulfide ion homeostasis Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a harmless treatment method of brine in polyphenylene sulfide resin production, which comprises the following steps: primary evaporation: carrying out primary evaporation crystallization on the washing strong brine to generate miscellaneous salt, cooling, crystallizing and centrifugally drying the evaporation mother liquor to obtain a product sodium acetate, and recycling the product sodium acetate system; pyrolyzing miscellaneous salt; dissolving the solution; membrane filtration; and (3) secondary evaporation, namely, performing multistage evaporation or MVR evaporation crystallization on the brine after membrane filtration, drying by a fluidized bed to obtain a product sodium chloride with the water content lower than 0.2%, and conveying the mother liquor to primary evaporation for recycling. The harmless treatment method of the brine in the production of the polyphenylene sulfide resin solves the difficult problems in the polyphenylene sulfide industry, reduces the industrial bottleneck again, reduces the environmental protection risk, has simple process, is easy to operate and control, has small equipment investment and high recovery rate.
Description
Technical Field
The invention relates to the technical field of polyphenylene sulfide production, in particular to a harmless treatment method of saline water in polyphenylene sulfide resin production.
Background
Polyphenylene sulfide is a special engineering plastic with excellent mechanical properties, has excellent heat resistance, electrical properties and rigidity, and is widely applied to various material fields, such as automobiles and electronic and electrical parts. At present, the method for producing polyphenylene sulfide usually employs a condensation polymerization reaction of a dihalo-substituted aromatic compound and an alkali metal sulfide in a polar organic solvent, for example, p-dichlorobenzene and sodium sulfide are polymerized in an N-methyl-2-pyrrolidone solvent at high temperature and high pressure to prepare a slurry containing polyphenylene sulfide resin, and the slurry is filtered and recovered to obtain the polyphenylene sulfide resin. However, in the above-mentioned production process of polyphenylene sulfide resin, p-dichlorobenzene and sodium sulfide are polymerized to produce polyphenylene sulfide resin, and sodium chloride as a by-product is also produced, and the produced sodium chloride is insoluble in N-methyl-2-pyrrolidone solvent, and at the same time, a small amount of polyphenylene sulfide oligomer, that is, low molecular weight substances such as polyphenylene sulfide trimer, polyphenylene sulfide tetramer, etc. is also produced during the polymerization. In the existing production process of polyphenylene sulfide resin, a large amount of brine is generated, the brine contains sodium chloride, lithium carbonate, low-carbon chain organic matters and the like, and no effective utilization method is available for the brine so far, so that the environment is polluted.
Disclosure of Invention
The invention aims to provide a harmless treatment method of brine in polyphenylene sulfide resin production, which solves the difficult problems in the polyphenylene sulfide industry, reduces the industrial bottleneck again, reduces the environmental protection risk, has simple process, is easy to operate and control, has small equipment investment and high recovery rate.
In order to achieve the aim, the invention provides a harmless treatment method of brine in polyphenylene sulfide resin production, which comprises the following steps:
s1, primary evaporation: carrying out primary evaporation crystallization on the washing strong brine to generate mixed salt, cooling, crystallizing and centrifugally drying the evaporation mother liquor to obtain a product sodium acetate, and recycling the product sodium acetate system;
s2, pyrolyzing miscellaneous salts: continuously adding the miscellaneous salt into a special electric heating furnace through a spiral pusher, controlling the environment and the temperature in the electric heating furnace and keeping the retention time, and converting organic matters in the miscellaneous salt into crude salt;
s3, dissolving the solution: dissolving the pyrolyzed crude salt in a first reaction kettle by using an aqueous solution doped with hydrochloric acid, wherein the pH value is less than 2, overflowing the saline water dissolved in the first reaction kettle into a second reaction kettle, adding sodium hydroxide, and changing impurities dissolved in a liquid phase into solid impurities, wherein the pH value is 6.5 to obtain saline water;
s4, membrane filtration: separating solid impurities out of the system by the saline water through a multistage tubular membrane filter to be used as common solid waste filter residues;
and S5, secondary evaporation, namely, carrying out multistage evaporation or MVR evaporation crystallization on the brine filtered by the membrane in the S4, drying the brine by a fluidized bed to obtain a product sodium chloride with the water content of less than 0.2%, and conveying the mother liquor to primary evaporation for recycling.
Preferably, the primary evaporative crystallization in step S1 is specifically: the washing concentrated brine is directly introduced into a multi-stage countercurrent evaporator at 70 ℃ at 60 ℃, the mixed salt is taken out from the last stage at 110 ℃, and then centrifugal separation is carried out to keep impurities in the evaporation mother liquor.
Preferably, the cooling crystallization in step S1 specifically includes: and (3) putting the evaporation mother liquor into a cooling kettle, cooling the evaporation mother liquor to less than 10 ℃ through circulating water and low-temperature water, and then centrifugally drying and separating until the moisture content is less than 3% to obtain the product sodium acetate.
Preferably, the temperature of the circulating water is reduced to 60 ℃, and the temperature of the low-temperature water is reduced to 10 ℃.
Preferably, the environment of the special electric heating furnace in the miscellaneous salt pyrolysis of the step S2 is an oxygen-insulated environment, the temperature is 500-750 ℃, and the retention time is kept for 2-4 h.
Preferably, the temperature of the special electric heating furnace is lower than the melting temperature of sodium chloride and higher than the decomposition temperature of organic matters.
Preferably, the dissolution temperature of the first reaction kettle in the step S3 is 40-70 ℃.
Preferably, the membrane filtration temperature of the step S4 is 40-60 ℃.
Preferably, the temperature of the secondary evaporation in the step S5 is 120 ℃, and the reflux amount of the mother liquor conveyed to the primary evaporation is 0.5m 3 /h。
Therefore, the harmless treatment method for the brine in the production of the polyphenylene sulfide resin has the following beneficial effects:
(1) the process is simple, easy to operate and control, the equipment investment is small, the recovery rate is high, the product purity is high, no production wastewater is discharged, the requirement of environmental protection is met, and better economic and social benefits are achieved;
(2) the pyrolysis temperature is controlled to be 300-500 ℃, the calcination time is 1-3 hours, the time is reduced by 50% compared with the time of the existing process on the market, the organic matter removal rate is 99.5% higher than that of the existing process, the sodium acetate product is white in color and high in purity and can be recycled, and a tail gas treatment system is installed in the pyrolysis furnace, so that toxic and harmful substances in the smoke are eliminated, and the environment is protected;
(3) the purity of the refined sodium chloride product is more than or equal to 98.5 percent and the TOC is less than or equal to 30 after twice evaporation and crystallization, the purity is higher than the standards of T/CCT002-2019 coal chemical industry byproduct industrial sodium chloride and QBT5270-2018 ionic membrane caustic soda salt, and the economic value is high;
(4) no hazardous waste is generated, the filter residue is common solid waste, the difficult problem of the polyphenylene sulfide industry is thoroughly solved, the industrial bottleneck is reduced again, the environmental protection risk is reduced, and the industrial value is very high.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a flow chart of an embodiment of the present invention, wherein the crude salt A is a mixed salt of sodium chloride and sodium acetate.
Detailed Description
The invention provides a harmless treatment method of brine in polyphenylene sulfide resin production, which comprises the following steps:
s1, primary evaporation: washing strong brine (brine to be treated) is subjected to primary evaporation crystallization, and the primary evaporation crystallization is specifically to be used for washing strong brineDirectly introducing the mixed salt into a 70 ℃ multistage countercurrent evaporator at 60 ℃, taking out the mixed salt from the last stage at 110 ℃, then performing centrifugal separation, retaining impurities in evaporation mother liquor, putting the evaporation mother liquor into a cooling kettle, cooling the evaporation mother liquor to less than 10 ℃ through circulating water and low-temperature water, then performing centrifugal drying separation until the moisture content is less than 3 percent to obtain a product sodium acetate, and recycling the product sodium acetate system, wherein the circulating water is cooled to 60 ℃, and the low-temperature water is cooled to 10 ℃. Primary evaporation crystallization procedure H is added into the solution separated from the water washing procedure 2 O 2 Adjusting and maintaining the pH value to be 7-8, evaporating and concentrating by 20-40 times, drying, screening, and producing crude sodium chloride. The preferred conditions are countercurrent evaporation and 120 deg.c high temperature discharge, and 98% organic matter is maintained in the evaporating mother liquid to the maximum.
S2, pyrolyzing miscellaneous salts: continuously adding the miscellaneous salt into a special electric heating furnace through a spiral pusher, controlling the environment of the electric heating furnace to be an anaerobic environment at the temperature of 500-; the temperature of the special electric heating furnace is lower than the melting temperature of sodium chloride and higher than the decomposition temperature of organic matters. Organic matters in the salt are removed, and a tail gas treatment system is arranged in the furnace, so that the smoke gas is discharged up to the standard. The electric furnace for pyrolysis has simple and safe structure compared with natural gas, convenient maintenance and temperature control precision of +/-0.5 ℃.
S3, dissolving the solution: dissolving the pyrolyzed crude salt in a first reaction kettle by using an aqueous solution doped with hydrochloric acid, wherein the dissolving temperature is 40-70 ℃, the pH value is less than 2, overflowing the saline water dissolved in the first reaction kettle into a second reaction kettle, adding sodium hydroxide, and changing impurities dissolved in a liquid phase into solid impurities, wherein the pH is 6.5, so as to obtain saline water; and washing crude lithium carbonate obtained in the water leaching filtration and precipitation filtration process by deionized water for several times, carrying out solid-liquid separation and drying to obtain a lithium carbonate product, and returning washing liquor to the solution in the evaporation crystallization process.
S4, membrane filtration: the salt water passes through a multi-stage tubular membrane filter to separate solid impurities out of the system to be used as common solid waste filter residues, and the membrane filtration temperature is 40-60 ℃. The membrane filtration process is that salt water enters a multi-stage tubular ultrafiltration membrane element after passing through a bag filter by a pump, clear liquid enters a collection tank, concentrated liquid returns to a raw material tank, the membrane precision is preferably 30nm, and the number of components is more than 8. In the washing procedure, hot deionized water is used for washing 3-5 times according to the solid-liquid ratio of 1: 0.5-1.5.
S5, secondary evaporation, namely, carrying out multistage evaporation or MVR evaporation crystallization on the salt water subjected to membrane filtration in the S4 at 120 ℃, drying the salt water by a fluidized bed to obtain a product sodium chloride with the water content of less than 0.2%, conveying the mother liquor to primary evaporation for recycling, and conveying the mother liquor to the primary evaporation with the reflux amount of 0.5m 3 /h。
The technical scheme of the invention is further explained by the attached drawings and the embodiment.
Examples
In the chemical production process of the chlor-alkali industry, a large amount of waste salt containing sodium chloride, lithium carbonate and a small amount of low-carbon chain organic matters is generated. The waste salt was calcined at 550 ℃ for 4h to give a white mixture. And (3) leaching the calcined mixture by using deionized water, and filtering insoluble substances to obtain a crude lithium carbonate product. Adding hydrochloric acid into the filtrate, adjusting the pH of the solution to 5-6, and evaporating and concentrating until Li is obtained + >20g/L, filtering, washing with deionized water at a solid-to-liquid ratio of 1:0.5-1.0 for 2-3 times, wherein the obtained sodium chloride product meets the quality requirement of GB/T5462-2016. And keeping the temperature of the filtrate to 80 ℃, precipitating lithium by using a hot sodium carbonate solution, carrying out solid-liquid separation to obtain a crude lithium carbonate product, and returning the obtained filtrate to the evaporation and crystallization process. Washing and drying the lithium carbonate product by using deionized water at 90 ℃ to the crude lithium carbonate product in five times according to the solid-to-liquid ratio of 1:1, and returning the washing liquid to the solution in the evaporation and crystallization process. The primary yield of lithium is more than or equal to 85 percent, and the product meets the GB/T11075-2013 quality requirement.
Therefore, the harmless treatment method for the brine in the production of the polyphenylene sulfide resin solves the difficult problems in the polyphenylene sulfide industry, reduces the industrial bottleneck again, reduces the environmental protection risk, and has the advantages of simple process, easy operation and control, small equipment investment and high recovery rate.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the disclosed embodiments without departing from the spirit and scope of the present invention.
Claims (9)
1. A harmless treatment method of saline water in polyphenylene sulfide resin production is characterized by comprising the following steps:
s1, primary evaporation: carrying out primary evaporation crystallization on the washing strong brine to generate mixed salt, cooling, crystallizing and centrifugally drying the evaporation mother liquor to obtain a product sodium acetate, and recycling the product sodium acetate system;
s2, pyrolyzing miscellaneous salts: continuously adding the miscellaneous salt into a special electric heating furnace through a spiral pusher, controlling the environment and the temperature in the electric heating furnace and keeping the retention time, and converting organic matters in the miscellaneous salt into crude salt;
s3, dissolving the solution: dissolving the pyrolyzed crude salt in a first reaction kettle by using an aqueous solution doped with hydrochloric acid, wherein the pH value is less than 2, overflowing the saline water dissolved in the first reaction kettle into a second reaction kettle, adding sodium hydroxide, and changing impurities dissolved in a liquid phase into solid impurities, wherein the pH value is 6.5 to obtain saline water;
s4, membrane filtration: separating solid impurities out of the system by the saline water through a multistage tubular membrane filter to be used as common solid waste filter residues;
and S5, secondary evaporation, namely, carrying out multistage evaporation or MVR evaporation crystallization on the brine filtered by the membrane in the S4, drying the brine by a fluidized bed to obtain a product sodium chloride with the water content of less than 0.2%, and conveying the mother liquor to primary evaporation for recycling.
2. The method for harmless treatment of brine in polyphenylene sulfide resin production as defined in claim 1, wherein said one-time evaporative crystallization in step S1 comprises: the washing concentrated brine is directly introduced into a multi-stage countercurrent evaporator at 70 ℃ at 60 ℃, the mixed salt is taken out from the last stage at 110 ℃, and then centrifugal separation is carried out to keep impurities in the evaporation mother liquor.
3. The method as claimed in claim 1, wherein the cooling crystallization in step S1 is specifically as follows: and putting the evaporation mother liquor into a cooling kettle, cooling the evaporation mother liquor to be less than 10 ℃ through circulating water and low-temperature water, and then centrifugally drying and separating until the moisture content is less than 3% to obtain the product sodium acetate.
4. The method for harmless treatment of the brine in the production of polyphenylene sulfide resin as claimed in claim 3, wherein: the temperature of the circulating water is reduced to 60 ℃, and the temperature of the low-temperature water is reduced to 10 ℃.
5. The method for the harmless treatment of the brine in the production of polyphenylene sulfide resin as claimed in claim 1, wherein the method comprises the following steps: the environment of the special electric heating furnace in the miscellaneous salt pyrolysis in the step S2 is an anaerobic environment, the temperature is 500-750 ℃, and the retention time is kept for 2-4 h.
6. The method for harmless treatment of brine in polyphenylene sulfide resin production as claimed in claim 5, wherein: the temperature of the special electric heating furnace is lower than the melting temperature of sodium chloride and higher than the decomposition temperature of organic matters.
7. The method for harmless treatment of brine in polyphenylene sulfide resin production as claimed in claim 1, wherein: the dissolution temperature of the first reaction kettle in the step S3 is 40-70 ℃.
8. The method for harmless treatment of brine in polyphenylene sulfide resin production as claimed in claim 1, wherein: the membrane filtration temperature of the step S4 is 40-60 ℃.
9. The method for harmless treatment of brine in polyphenylene sulfide resin production as claimed in claim 1, wherein: the temperature of the secondary evaporation in the step S5 is 120 ℃, and the reflux quantity of the mother liquor conveyed to the primary evaporation is 0.5m 3/h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115432720A (en) * | 2022-10-09 | 2022-12-06 | 宜宾学院 | Process for recovering byproduct salt in polyphenylene sulfide synthesis |
| CN116672797A (en) * | 2023-07-19 | 2023-09-01 | 东莞市曼塔新材料科技有限公司 | Purification and filtration device and method for polyphenylene sulfide melt |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395862A (en) * | 2016-08-29 | 2017-02-15 | 四川理工学院 | Recovery method of by-product sodium chloride in production process of polyphenylene sulfide |
| CN106495190A (en) * | 2016-09-12 | 2017-03-15 | 天津科技大学 | A kind of calcining of abraum salt containing lithium recovery method |
| CN106565956A (en) * | 2016-10-21 | 2017-04-19 | 天津科技大学 | Method for comprehensive recycling of by-product slurry in polyphenylene sulfide productive process |
| CN106745076A (en) * | 2016-11-21 | 2017-05-31 | 大唐国际化工技术研究院有限公司 | A kind of method that Industrial Wastewater Treatment is produced carnallite resource |
| CN111574713A (en) * | 2020-06-16 | 2020-08-25 | 四川明道和化学新材料有限公司 | Method for recovering polyphenylene sulfide byproduct salt |
| CN112320822A (en) * | 2020-10-20 | 2021-02-05 | 绍兴凤登环保有限公司 | Waste salt recycling treatment method |
| CN113772692A (en) * | 2021-09-03 | 2021-12-10 | 江苏海普功能材料有限公司 | Method for treating and recycling waste salt |
| CN114349026A (en) * | 2021-04-08 | 2022-04-15 | 李广柱 | Treatment process of high-risk waste salt |
-
2022
- 2022-06-14 CN CN202210668084.0A patent/CN114988435A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106395862A (en) * | 2016-08-29 | 2017-02-15 | 四川理工学院 | Recovery method of by-product sodium chloride in production process of polyphenylene sulfide |
| CN106495190A (en) * | 2016-09-12 | 2017-03-15 | 天津科技大学 | A kind of calcining of abraum salt containing lithium recovery method |
| CN106565956A (en) * | 2016-10-21 | 2017-04-19 | 天津科技大学 | Method for comprehensive recycling of by-product slurry in polyphenylene sulfide productive process |
| CN106745076A (en) * | 2016-11-21 | 2017-05-31 | 大唐国际化工技术研究院有限公司 | A kind of method that Industrial Wastewater Treatment is produced carnallite resource |
| CN111574713A (en) * | 2020-06-16 | 2020-08-25 | 四川明道和化学新材料有限公司 | Method for recovering polyphenylene sulfide byproduct salt |
| CN112320822A (en) * | 2020-10-20 | 2021-02-05 | 绍兴凤登环保有限公司 | Waste salt recycling treatment method |
| CN114349026A (en) * | 2021-04-08 | 2022-04-15 | 李广柱 | Treatment process of high-risk waste salt |
| CN113772692A (en) * | 2021-09-03 | 2021-12-10 | 江苏海普功能材料有限公司 | Method for treating and recycling waste salt |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115432720A (en) * | 2022-10-09 | 2022-12-06 | 宜宾学院 | Process for recovering byproduct salt in polyphenylene sulfide synthesis |
| CN116672797A (en) * | 2023-07-19 | 2023-09-01 | 东莞市曼塔新材料科技有限公司 | Purification and filtration device and method for polyphenylene sulfide melt |
| CN116672797B (en) * | 2023-07-19 | 2024-05-24 | 威海旭日过滤器股份有限公司 | Purification and filtration device and method for polyphenylene sulfide melt |
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