CN114735872A - Method for recycling and reusing sulfanilamide quinoxaline process wastewater - Google Patents
Method for recycling and reusing sulfanilamide quinoxaline process wastewater Download PDFInfo
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- CN114735872A CN114735872A CN202210263746.6A CN202210263746A CN114735872A CN 114735872 A CN114735872 A CN 114735872A CN 202210263746 A CN202210263746 A CN 202210263746A CN 114735872 A CN114735872 A CN 114735872A
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- process wastewater
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- 238000000034 method Methods 0.000 title claims abstract description 80
- 229940124530 sulfonamide Drugs 0.000 title claims abstract description 60
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002351 wastewater Substances 0.000 title claims abstract description 57
- XSCHRSMBECNVNS-UHFFFAOYSA-N quinoxaline Chemical compound N1=CC=NC2=CC=CC=C21 XSCHRSMBECNVNS-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000004064 recycling Methods 0.000 title claims abstract description 19
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 92
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000001103 potassium chloride Substances 0.000 claims abstract description 46
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 46
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229960003097 sulfaquinoxaline Drugs 0.000 claims abstract description 37
- NHZLNPMOSADWGC-UHFFFAOYSA-N 4-amino-N-(2-quinoxalinyl)benzenesulfonamide Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=CN=C(C=CC=C2)C2=N1 NHZLNPMOSADWGC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000012074 organic phase Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 23
- BYHVGQHIAFURIL-UHFFFAOYSA-N 2-chloroquinoxaline Chemical compound C1=CC=CC2=NC(Cl)=CN=C21 BYHVGQHIAFURIL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 20
- 239000012071 phase Substances 0.000 claims abstract description 19
- 238000006482 condensation reaction Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000012452 mother liquor Substances 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000006386 neutralization reaction Methods 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 239000008399 tap water Substances 0.000 claims description 5
- 235000020679 tap water Nutrition 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 150000003456 sulfonamides Chemical class 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000003472 neutralizing effect Effects 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000008346 aqueous phase Substances 0.000 description 12
- 239000003337 fertilizer Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 241000224483 Coccidia Species 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- MSTNYGQPCMXVAQ-RYUDHWBXSA-N (6S)-5,6,7,8-tetrahydrofolic acid Chemical compound C([C@H]1CNC=2N=C(NC(=O)C=2N1)N)NC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 MSTNYGQPCMXVAQ-RYUDHWBXSA-N 0.000 description 1
- 208000003495 Coccidiosis Diseases 0.000 description 1
- 206010023076 Isosporiasis Diseases 0.000 description 1
- DHKHZGZAXCWQTA-UHFFFAOYSA-N [N].[K] Chemical compound [N].[K] DHKHZGZAXCWQTA-UHFFFAOYSA-N 0.000 description 1
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 108010014404 dihydrofolate synthetase Proteins 0.000 description 1
- OZRNSSUDZOLUSN-LBPRGKRZSA-N dihydrofolic acid Chemical compound N=1C=2C(=O)NC(N)=NC=2NCC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OZRNSSUDZOLUSN-LBPRGKRZSA-N 0.000 description 1
- WZISDKTXHMETKG-UHFFFAOYSA-H dimagnesium;dipotassium;trisulfate Chemical group [Mg+2].[Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O WZISDKTXHMETKG-UHFFFAOYSA-H 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 1
- 235000019797 dipotassium phosphate Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000005460 tetrahydrofolate Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C01D3/04—Chlorides
-
- 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
- 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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
Abstract
The invention discloses a method for recycling sulfanilamide quinoxaline process wastewater, which comprises the steps of mixing sulfanilamide, 2-chloroquinoxaline and potassium carbonate, then sequentially carrying out decoloring, filtering, neutralizing, precipitating and filtering by using activated carbon to prepare solid sulfaquinoxaline and process wastewater, adding dichloromethane into the process wastewater to extract organic matters in the process wastewater to form a water phase and an organic phase, finally respectively treating the water phase and the organic phase to respectively obtain industrial sulfaquinoxaline mixture which can be repeatedly used for condensation reaction, high-purity potassium chloride solid, recyclable dichloromethane and recyclable secondary mother liquor, thus, zero discharge of process wastewater is realized, wastes generated in the production process are harmless, the discharge amount of pollutants is reduced, the environment is effectively protected, and resources are saved.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a method for recycling sulfanilamide quinoxaline process wastewater.
Background
The sulfaquinoxaline belongs to sulfanilamide antibacterial drugs, is used for livestock coccidiosis, can generate competitive reaction with dihydrofolate synthetase in coccidian bodies to block the synthesis of dihydrofolate of the coccidian bodies, leads to the block of the synthesis of tetrahydrofolate, and consequently blocks the synthesis of nucleic acid to influence the growth and the propagation of the coccidian.
During the process of producing sulfaquinoxaline, a large amount of potassium chloride is generated. The reaction equation is as follows:
potassium chloride is an important raw material for preparing the nitrogen-potassium fertilizer, has good value, currently, potassium chloride and potassium sulfate are main varieties of the potassium fertilizer, and the balance is potassium magnesium sulfate, potassium hydrogen phosphate and potassium nitrate, so that the yield is low. The potassium chloride is the most water-soluble potassium salt in nature, so the potassium chloride is also the most potassium fertilizer, and accounts for more than 90 percent of the total amount of the potassium fertilizer in the world.
At present, the basic strategy of environmental pollution treatment in China is to establish an economic development mode taking circular economy as a main line so as to improve the resource utilization rate, reduce the discharge amount of pollutants and achieve the purposes of reducing and harmlessly treating wastes through a production link. The potassium chloride recovered by the process can be reused in the synthesis of the fertilizer, and the zero discharge standard of the wastewater of the process is really realized.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a harmless and zero-emission process wastewater recycling method for sulfaquinoxaline process wastewater.
In order to achieve the purpose, the scheme provided by the invention is as follows: a method for recycling sulfanilamide quinoxaline process wastewater comprises the following steps:
s1, mixing the raw materials in a molar ratio of 1.0-1.4: 1.2-1.7: 1.25-1.75 respectively weighing sulfanilamide: 2-chloroquinoxaline: potassium carbonate, then mixing and stirring sulfanilamide, 2-chloroquinoxaline and potassium carbonate, heating and then carrying out condensation reaction;
s2, after the reaction is finished in the step S1, adding a set amount of tap water, stirring and dissolving, adding activated carbon for decoloring, and filtering;
s3, adding hydrochloric acid into the filtrate filtered in the step S2 for neutralization, separating out a target product, and then sequentially filtering and centrifugally separating to obtain solid sulfaquinoxaline and process wastewater, wherein the pH value is neutralized to 6-6.5 by hydrochloric acid;
s4, adding a dichloromethane solvent into the process wastewater in the step S3 to form a water phase and an organic phase, then extracting the organic phase, distilling the organic phase at normal pressure to obtain a dichloromethane solvent, and evaporating to dryness to obtain a mixture of industrial sulfanilamide and sulfaquinoxaline;
s5, extracting the water phase in the step S4, adding activated carbon for decoloring, distilling, recovering water by distillation, gradually separating out potassium chloride when the water phase is distilled to a small volume, cooling until the potassium chloride is separated out to saturation, and finally performing centrifugal filtration to obtain potassium chloride solids meeting the requirements, wherein the secondary mother liquor can be circulated to the next batch for recovering potassium chloride.
The beneficial effects of the invention are as follows: the method comprises the steps of mixing and stirring sulfanilamide, 2-chloroquinoxaline and potassium carbonate, decoloring, filtering, neutralizing, separating out and filtering sequentially through activated carbon to obtain solid sulfanilamide quinoxaline and process wastewater, adding dichloromethane into the process wastewater to extract organic matters in the process wastewater to form a water phase and an organic phase, and finally treating the water phase and the organic phase respectively to obtain a mixture of industrial sulfanilamide and sulfanilamide quinoxaline which can be repeatedly used for condensation reaction, high-purity potassium chloride solid, dichloromethane which can be repeatedly used and secondary mother liquor which can be recycled.
Further, in the step S1, the temperature is raised to 140-150 ℃, and the reaction time is 4-6 hours.
Further, in the step S1, the temperature was raised to 150 ℃, and the reaction time was 5 hours.
Further, in step S1, a stirring mixing reaction is performed using a reaction vessel.
Further, the sulfonamide: 2-chloroquinoxaline: the molar ratio of potassium carbonate is 1.2: 1.45:1.5.
Further, in the step S2, the decoloring temperature is 80-90 ℃, and the decoloring time is 1-2 hours.
Further, in the step S2, the decoloring temperature is 85 ℃ and the decoloring time is 1.5 hours.
Further, in step S3, a crystallization kettle is used for neutralization and precipitation.
Further, in the step S4, the dichloromethane solvent obtained by distillation may be recycled.
Further, in the step S5, the distilled and recovered water can be recycled.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention will be further illustrated with reference to specific examples:
the first embodiment is as follows:
referring to the attached figure 1, the method for recycling the p-sulfaquinoxaline process wastewater comprises the following steps:
s1, mixing the raw materials in a molar ratio of 1.0-1.4: 1.2-1.7: 1.25-1.75 respectively weighing sulfanilamide: 2-chloroquinoxaline: potassium carbonate, then respectively pouring sulfanilamide, 2-chloroquinoxaline and potassium carbonate into a 2000L reaction kettle, mixing and stirring, heating to 140 ℃, and then carrying out condensation reaction for 4 hours; specifically, taking sulfanilamide: 2-chloroquinoxaline: the molar ratio of potassium carbonate is 1.0: 1.2: 1.25, namely 200kg of sulfanilamide, 240kg of 2-chloroquinoxaline and 250kg of potassium carbonate, wherein the sulfanilamide is industrial sulfanilamide.
S2, after the reaction in the step S1 is completed, namely when the mass content of the sulfanilamide in the materials is less than 10%, stopping the condensation reaction, adding 1600L of tap water, stirring and dissolving, then adding 20kg of activated carbon for decoloring, and then filtering, wherein when the activated carbon is added for decoloring, the temperature needs to be raised to 80 ℃, and the decoloring time is 1 h.
S3, adding hydrochloric acid into the filtrate filtered in the step S2 for neutralization, separating out a target product, then sequentially filtering and centrifugally separating to obtain a solid sulfaquinoxaline and process wastewater, wherein the hydrochloric acid is used for neutralization until the PH value is 6-6.5, and the solid needs to be dried.
S4, adding 300L of dichloromethane solvent into the process wastewater in the step S3, uniformly stirring, standing for a period of time to form a water phase and an organic phase, extracting the organic phase, distilling the organic phase at normal pressure to obtain the dichloromethane solvent, and evaporating to dryness to obtain a mixture of industrial sulfanilamide and sulfaquinoxaline; wherein the dichloromethane solvent obtained by distillation can be reused for mixing with the process wastewater in the step S4, and the mixture of the industrial sulfanilamide and the sulfaquinoxaline obtained by evaporation can be directly reused for the condensation reaction in the step S1.
S5, extracting the water phase in the step S4, adding activated carbon for decoloring, distilling, recovering water by distillation, gradually separating out potassium chloride when the water phase is distilled to a small volume, cooling until the potassium chloride is separated out to saturation, and finally performing centrifugal filtration and drying to obtain potassium chloride solids meeting the requirements, wherein secondary mother liquor can be circulated to the next batch for recovering potassium chloride; wherein, the content of the potassium chloride in the obtained potassium chloride solid can reach more than 99 percent.
In this embodiment, firstly, a condensation reaction is performed, hydrochloric acid is added to neutralize, precipitation and filtration processes are performed to prepare sulfaquinoxaline and corresponding process wastewater, then dichloromethane is added to the process wastewater to extract organic matters (organic matters are industrial sulfanilamide and sulfaquinoxaline) in the process wastewater, the process wastewater is left for a period of time, a precipitate is formed into an aqueous phase and an organic phase, the organic phase and the aqueous phase are respectively treated, wherein the organic phase is distilled to obtain a reusable industrial sulfanilamide and sulfaquinoxaline mixture, after the aqueous phase is decolored by adding activated carbon, potassium chloride solids are precipitated by distillation, high-purity potassium chloride is recovered, and the remaining secondary mother liquor can be recycled to the next batch to recover potassium chloride.
Example two:
referring to the attached figure 1, the method for recycling the sulfaquinoxaline process wastewater comprises the following steps:
s1, mixing the raw materials in a molar ratio of 1.0-1.4: 1.2-1.7: 1.25-1.75 respectively weighing sulfanilamide: 2-chloroquinoxaline: potassium carbonate, then respectively pouring sulfanilamide, 2-chloroquinoxaline and potassium carbonate into a 2000L reaction kettle, mixing and stirring, heating to 140 ℃, and then carrying out condensation reaction for 4 hours; specifically, taking sulfanilamide: 2-chloroquinoxaline: the molar ratio of potassium carbonate is 1.4: 1.7: 1.75, namely 280kg of sulfanilamide, 340kg of 2-chloroquinoxaline and 350kg of potassium carbonate, wherein the sulfanilamide is industrial sulfanilamide.
S2, after the reaction in the step S1 is completed, namely when the mass content of the sulfanilamide in the materials is less than 10%, stopping the condensation reaction, adding 1600L of tap water, stirring and dissolving, then adding 20kg of activated carbon for decoloring, and then filtering, wherein when the activated carbon is added for decoloring, the temperature needs to be raised to 90 ℃, and the decoloring time is 2 hours.
S3, adding hydrochloric acid into the filtrate filtered in the step S2 for neutralization, separating out a target product, then sequentially filtering and centrifugally separating to obtain a solid sulfaquinoxaline and process wastewater, wherein the hydrochloric acid is used for neutralization until the PH value is 6-6.5, and the solid needs to be dried.
S4, adding 300L of dichloromethane solvent into the process wastewater in the step S3, uniformly stirring, standing for a period of time to form a water phase and an organic phase, extracting the organic phase, distilling the organic phase at normal pressure to obtain the dichloromethane solvent, and evaporating to dryness to obtain a mixture of industrial sulfanilamide and sulfaquinoxaline; wherein the dichloromethane solvent obtained by distillation can be reused for mixing with the process wastewater in the step S4, and the mixture of the industrial sulfanilamide and the sulfaquinoxaline obtained by evaporation can be directly reused for the condensation reaction in the step S1.
S5, extracting the water phase in the step S4, adding activated carbon for decoloring, distilling, recovering water by distillation, gradually separating out potassium chloride when the water phase is distilled to a small volume, cooling until the potassium chloride is separated out to saturation, and finally performing centrifugal filtration and drying to obtain potassium chloride solids meeting the requirements, wherein secondary mother liquor can be circulated to the next batch for recovering potassium chloride; wherein, the content of the potassium chloride in the obtained potassium chloride solid can reach more than 99 percent.
In this embodiment, firstly, a condensation reaction is performed, hydrochloric acid is added to neutralize, precipitation and filtration processes are performed to prepare sulfaquinoxaline and corresponding process wastewater, then dichloromethane is added to the process wastewater to extract organic matters (organic matters are industrial sulfanilamide and sulfaquinoxaline) in the process wastewater, the process wastewater is left for a period of time, a precipitate is formed into an aqueous phase and an organic phase, the organic phase and the aqueous phase are respectively treated, wherein the organic phase is distilled to obtain a reusable industrial sulfanilamide and sulfaquinoxaline mixture, after the aqueous phase is decolored by adding activated carbon, potassium chloride solids are precipitated by distillation, high-purity potassium chloride is recovered, and the remaining secondary mother liquor can be recycled to the next batch to recover potassium chloride.
Example three:
referring to the attached figure 1, the method for recycling the sulfaquinoxaline process wastewater comprises the following steps:
s1, mixing the raw materials in a molar ratio of 1.0-1.4: 1.2-1.7: 1.25-1.75 respectively weighing sulfanilamide: 2-chloroquinoxaline: potassium carbonate, then respectively pouring sulfanilamide, 2-chloroquinoxaline and potassium carbonate into a 2000L reaction kettle, mixing and stirring, heating to 140 ℃, and then carrying out condensation reaction for 4 hours; specifically, taking sulfanilamide: 2-chloroquinoxaline: the molar ratio of potassium carbonate is 1.2: 1.4: 1.5, namely 240kg of sulfanilamide, 280kg of 2-chloroquinoxaline and 300kg of potassium carbonate, wherein the sulfanilamide is industrial sulfanilamide.
S2, after the reaction in the step S1 is completed, namely when the mass content of the sulfanilamide in the materials is less than 10%, stopping the condensation reaction, adding 1600L of tap water, stirring and dissolving, then adding 20kg of activated carbon for decoloring, and then filtering, wherein when the activated carbon is added for decoloring, the temperature needs to be raised to 85 ℃, and the decoloring time is 1.5 h.
And S3, adding hydrochloric acid into the filtrate filtered in the step S2 for neutralization, separating out a target product, and then sequentially filtering and centrifugally separating to obtain a solid sulfaquinoxaline and process wastewater, wherein the hydrochloric acid is used for neutralization until the PH value is 6-6.5, and the solid needs to be dried.
S4, adding 300L of dichloromethane solvent into the process wastewater in the step S3, uniformly stirring, standing for a period of time to form a water phase and an organic phase, extracting the organic phase, distilling the organic phase at normal pressure to obtain the dichloromethane solvent, and evaporating to dryness to obtain a mixture of industrial sulfanilamide and sulfaquinoxaline; wherein the dichloromethane solvent obtained by distillation can be reused for mixing with the process wastewater in the step S4, and the mixture of the industrial sulfanilamide and the sulfaquinoxaline obtained by evaporation can be directly reused for the condensation reaction in the step S1.
S5, extracting the water phase in the step S4, adding activated carbon for decoloring, distilling, recovering water by distillation, gradually separating out potassium chloride when the water phase is distilled to a small volume, cooling until the potassium chloride is separated out to saturation, and finally performing centrifugal filtration and drying to obtain potassium chloride solids meeting the requirements, wherein secondary mother liquor can be circulated to the next batch for recovering potassium chloride; wherein, the content of the potassium chloride in the obtained potassium chloride solid can reach more than 99 percent.
In this embodiment, firstly, a condensation reaction is performed, hydrochloric acid is added to neutralize, precipitation and filtration processes are performed to prepare sulfaquinoxaline and corresponding process wastewater, then dichloromethane is added to the process wastewater to extract organic matters (organic matters are industrial sulfanilamide and sulfaquinoxaline) in the process wastewater, the process wastewater is left for a period of time, a precipitate is formed into an aqueous phase and an organic phase, the organic phase and the aqueous phase are respectively treated, wherein the organic phase is distilled to obtain a reusable industrial sulfanilamide and sulfaquinoxaline mixture, after the aqueous phase is decolored by adding activated carbon, potassium chloride solids are precipitated by distillation, high-purity potassium chloride is recovered, and the remaining secondary mother liquor can be recycled to the next batch to recover potassium chloride.
In this embodiment, firstly, a condensation reaction is performed, hydrochloric acid is added to neutralize, precipitation and filtration processes are performed to prepare sulfaquinoxaline and corresponding process wastewater, then dichloromethane is added to the process wastewater to extract organic matters (organic matters are industrial sulfanilamide and sulfaquinoxaline) in the process wastewater, the process wastewater is left for a period of time, a precipitate is formed into an aqueous phase and an organic phase, the organic phase and the aqueous phase are respectively treated, wherein the organic phase is distilled to obtain a reusable industrial sulfanilamide and sulfaquinoxaline mixture, after the aqueous phase is decolored by adding activated carbon, potassium chloride solids are precipitated by distillation, high-purity potassium chloride is recovered, and the remaining secondary mother liquor can be recycled to the next batch to recover potassium chloride.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way. Those skilled in the art can make many changes and modifications to the disclosed embodiments, or modify equivalent embodiments to practice the disclosed embodiments, without departing from the scope of the disclosed embodiments. Therefore, equivalent variations made according to the idea of the present invention should be covered within the protection scope of the present invention without departing from the contents of the technical solution of the present invention.
Claims (10)
1. A method for recycling sulfanilamide quinoxaline process wastewater is characterized by comprising the following steps: the method comprises the following steps:
s1, mixing the raw materials in a molar ratio of 1.0-1.4: 1.2-1.7: 1.25-1.75 respectively weighing sulfanilamide: 2-chloroquinoxaline: potassium carbonate, then mixing and stirring sulfanilamide, 2-chloroquinoxaline and potassium carbonate, heating and then carrying out condensation reaction;
s2, after the reaction is finished in the step S1, adding a set amount of tap water, stirring and dissolving, adding activated carbon for decoloring, and filtering;
s3, adding hydrochloric acid into the filtrate filtered in the step S2 for neutralization, separating out a target product, and then sequentially filtering and centrifugally separating to obtain solid sulfaquinoxaline and process wastewater, wherein the pH value is neutralized to 6-6.5 by hydrochloric acid;
s4, adding a dichloromethane solvent into the process wastewater in the step S3 to form a water phase and an organic phase, then extracting the organic phase, distilling the organic phase at normal pressure to obtain a dichloromethane solvent, and evaporating to dryness to obtain a mixture of industrial sulfanilamide and sulfaquinoxaline;
s5, extracting the water phase in the step S4, adding activated carbon for decoloring, distilling, recovering water by distillation, gradually separating out potassium chloride when the water phase is distilled to a small volume, cooling until the potassium chloride is separated out to saturation, and finally performing centrifugal filtration to obtain potassium chloride solids meeting the requirements, wherein the secondary mother liquor can be circulated to the next batch for recovering potassium chloride.
2. The method for recycling p-sulfaquinoxaline process wastewater according to claim 1, which is characterized in that: in the step S1, the temperature is raised to 140-150 ℃, and the reaction time is 4-6 hours.
3. The method for recycling p-sulfaquinoxaline process wastewater according to claim 2, which is characterized in that: in step S1, the temperature is raised to 150 ℃ and the reaction time is 5 hours.
4. The method for recycling p-sulfaquinoxaline process wastewater according to claim 3, which is characterized in that: in the step S1, a reaction kettle is used for stirring and mixing reaction.
5. The method for recycling p-sulfaquinoxaline process wastewater according to claim 4, which is characterized in that: the sulfonamide: 2-chloroquinoxaline: the molar ratio of potassium carbonate is 1.2: 1.45:1.5.
6. The method for recycling sulfanilamide quinoxaline process wastewater according to claim 5, which is characterized in that: in the step S2, the decoloring temperature is 80-90 ℃, and the decoloring time is 1-2 hours.
7. The method for recycling sulfanilamide quinoxaline process wastewater according to claim 6, which is characterized in that: in the step S2, the decoloring temperature is 85 ℃, and the decoloring time is 1.5 h.
8. The method for recycling sulfanilamide quinoxaline process wastewater according to claim 7, which is characterized in that: in the step S3, a crystallization kettle is used for neutralization and precipitation.
9. The method for recycling sulfanilamide quinoxaline process wastewater according to claim 8, which is characterized in that: in the step S4, the methylene chloride solvent obtained by distillation is recovered and reused.
10. The method for recycling sulfanilamide quinoxaline process wastewater according to claim 9, which is characterized in that: in step S5, the water recovered by distillation is recovered and reused.
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