CN101402495B - Process for treating waste water from thiol methyl tin production - Google Patents
Process for treating waste water from thiol methyl tin production Download PDFInfo
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- CN101402495B CN101402495B CN2008102335536A CN200810233553A CN101402495B CN 101402495 B CN101402495 B CN 101402495B CN 2008102335536 A CN2008102335536 A CN 2008102335536A CN 200810233553 A CN200810233553 A CN 200810233553A CN 101402495 B CN101402495 B CN 101402495B
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Abstract
The invention provides a method for treated wastewater generated in the process of producing methyltin mercaptide. The invnetion belongs to a wastewater treatment method, in particular to a method for performing the zero wastewater discharge treatment on special wastewater generated in the process of producing the methyltin mercaptide. In the method, according to characteristics of the methyltin wastewater, and by the combination of the technological flow of producing the methyltin, an adsorbent is used to adsorb the wastewater first; at the same time, potassium permanganate is used to remove organic matters in the wastewater, and ammonium chloride is extracted out of the wastewater; and finally, the water in which the organic matters and the ammonium chloride are removed is returned to the methyltin mercaptide production process for cyclic use. The method has the advantages of high efficiency of removing the organic matters, simple process, the obtaining of valued side products, low water consumption in the process of producing the methyltin and zero wastewater discharge in the whole flow.
Description
Technical field
The invention belongs to a kind of method of wastewater treatment, particularly the waste water that produces in the production process to thiol methyl tin carries out the treatment process of sewage zero-discharge.
Background technology
Thiol methyl tin also claims methyl tin or methyl tin stabilizer, is a kind of in the organotin stabilizer, is water white oily mater.Because it has advantages such as nontoxic, efficient, that tint permanence is good, is widely used as plastic heat stabilizer in recent years at home and abroad.With the PVC plastics that the thiol methyl tin used as stabilizers obtains, have characteristics such as unique processing characteristics and transparent, environmental protection, safety, be widely used as packing, decoration and engineering materials.
In the production process of thiol methyl tin, to produce waste water inevitably, produce 1 ton of wastewater flow rate that thiol methyl tin produced at present and be about about 3 cubic metres, mainly contain organism and inorganic salt in the waste water, must endanger otherwise can produce through handling environment.
Summary of the invention
The purpose of this invention is to provide a kind of process for treating waste water from thiol methyl tin production, organic removal efficiency height, process is easy, can obtain the valency byproduct, and methyl tin production water consumption is low, the whole process sewage zero-discharge.
Technical scheme of the present invention is: in conjunction with the methyl tin technological process of production, at first waste water is adopted absorption with sorbent material, remove organism in the waste water with potassium permanganate simultaneously, and then the ammonium chloride in the extraction waste water, will remove organism and ammonium chloride water afterwards at last and return thiol methyl tin Production Flow Chart use.
Technical scheme of the present invention also comprises: sorbent material adopts gac, cinder; Ammonium chloride in the waste water extracts and adopts distillation under vacuum, and service temperature is 70 ℃～80 ℃, and vacuum tightness is 75Kpa, and the purity of ammonium chloride is purified to more than 97%; Removing organism and ammonium chloride a part of water adjust pH afterwards is 6.9～7.1, as methyl tin bath water, between another part water adjust pH to 6～7, as the dissolving water of methyl tin intermediate.
To deviate from the water hydrochloric acid adjust pH after organism and the ammonium chloride, behind adjust pH, carry out with above-mentioned distillation under vacuum once more as the dissolving water of methyl tin intermediate; Gac filters behind the cinder absorption waste water, and sorbent material recirculation is used.
Concrete processing step of the present invention is as follows:
The first step: adsorbing and removing organism: get methyl tin factory effluent, add gac, cinder, potassium permanganate make it fully contact, adsorb after-filtration (gac of adding, cinder recycles), make organism obtain effective elimination, enter the processing of second step then;
Second step: the water that the first step is obtained carries out underpressure distillation, and 70 ℃～80 ℃ of temperature are collected water of condensation and the ammonium chloride that distillation obtains respectively, the salt master content that obtains is greater than the white crystal more than 97%, colorless and odorless can be used as byproduct and sells, and water of condensation enters the processing of the 3rd step;
The 3rd step: the pH value is adjusted: add micro-hydrochloric acid in water of condensation, carry out the adjustment of pH value, the pH value is transferred to neutrality about 7, and the moisture that obtains is become two partly, and some is directly as methyl tin bath water; Another partly enters the processing of the 4th step;
The 4th step: secondary underpressure distillation: handle in the water of condensation obtain to the 3rd step and to add hydrochloric acid, carry out the adjustment of pH value, the pH value is transferred between the neutrality 6～7, carries out the secondary underpressure distillation then, with the water that the obtains dissolving water as methyl tin intermediate.
Whether the every quality index and the effect of the thiol methyl tin that the treated water of investigation use is produced be consistent with the thiol methyl tin that uses pure water to produce.
Advantage of the present invention:
1, organic removal efficiency height in the waste water, process is easy, and the agents useful for same cheapness is easily purchased.
2, the purity of the inorganic salt in the waste water reaches more than 97%, and outward appearance and smell are normal, can be used as byproduct and sells;
3, the water that obtains after the processing can successfully return and be used for the production of methyl tin, has not only reduced methyl Xi Shui consumption, and quality product and production unit are not had any impact, and realizes zero release truly;
4, whole waste water treatment process is simply effective, has tangible economic benefit, is easy to realize industrialization.
Description of drawings
Fig. 1 is the process flow sheet of invention.
Embodiment
Embodiment one
The first step: adsorbing and removing organism: get methyl tin factory effluent 800 grams, add gac, cinder, potassium permanganate makes it fully contact, adsorb the after-filtration (gac of adding, cinder recycles), make organism obtain effective elimination, enter the processing of second step then;
Second step: " water that the first step is obtained carries out underpressure distillation, 70 ℃～80 ℃ of temperature, and water of condensation 650 grams and the 85 gram ammonium chlorides that obtain are distilled in collection respectively, and the white crystal of the salt master content 97.5% that obtains, colorless and odorless, water of condensation enter the processing of the 3rd step;
The 3rd step: the pH value is adjusted: add micro-hydrochloric acid in water of condensation, carry out the adjustment of pH value, the pH value is transferred to 7.05, and the moisture that obtains become two partly, some is directly as methyl tin bath water, wash result shows, with identical with the effect of pure water washing, to the quality of thiol methyl tin without any influence; Another partly enters the processing of the 4th step;
The 4th step: secondary underpressure distillation: in the water of condensation that the processing of the 3rd step obtains, add hydrochloric acid, carry out the adjustment of pH value, the pH value is transferred to 6.5, carry out the secondary underpressure distillation then, with the water that obtains dissolving water as methyl tin intermediate, obtain the thiol methyl tin product after the reaction, investigate indexs such as quality and yield.The result shows, and is in full accord with the thiol methyl tin product that obtains with the pure water dissolving.
Index is as follows: Sn:19.33% S:11.92% Po-Co:5 transmittance: 99.5.
Embodiment two
The first step: adsorbing and removing organism: get methyl tin factory effluent 800 grams, add gac, cinder, potassium permanganate makes it fully contact, adsorb the after-filtration (gac of adding, cinder recycles), make organism obtain effective elimination, enter the processing of second step then;
Second step: the water that the first step is obtained carries out underpressure distillation, 70 ℃～80 ℃ of temperature, and water of condensation 620 grams and the 86 gram ammonium chlorides that obtain are distilled in collection respectively, and the white crystal of the salt master content 97.8% that obtains, colorless and odorless, water of condensation enter the processing of the 3rd step;
The 3rd step: the pH value is adjusted: add micro-hydrochloric acid in water of condensation, carry out the adjustment of pH value, the pH value is transferred to 6.95, and the moisture that obtains become two partly, some is directly as methyl tin bath water, wash result shows, with identical with the effect of pure water washing, to the quality of thiol methyl tin without any influence; Another partly enters the processing of the 4th step;
The 4th step: secondary underpressure distillation: in the water of condensation that the processing of the 3rd step obtains, add hydrochloric acid, carry out the adjustment of pH value, the pH value is transferred to 6.4, carry out the secondary underpressure distillation then, with the water that obtains dissolving water as methyl tin intermediate, obtain the thiol methyl tin product after the reaction, investigate indexs such as quality and yield.The result shows, and is in full accord with the thiol methyl tin product that obtains with the pure water dissolving.
Index is as follows: Sn:19.27% S:11.94% Po-Co:8 transmittance: 99.8.
Embodiment three
The first step: adsorbing and removing organism: get methyl tin factory effluent 750 grams, add gac, cinder, potassium permanganate makes it fully contact, adsorb the after-filtration (gac of adding, cinder recycles), make organism obtain effective elimination, enter the processing of second step then;
Second step: the water that the first step is obtained carries out underpressure distillation, 70 ℃～80 ℃ of temperature, and water of condensation 600 grams and the 73 gram ammonium chlorides that obtain are distilled in collection respectively, and the white crystal of the salt master content 97.9% that obtains, colorless and odorless, water of condensation enter the processing of the 3rd step;
The 3rd step: the pH value is adjusted: add micro-hydrochloric acid in water of condensation, carry out the adjustment of pH value, the pH value is transferred to 7.01, and the moisture that obtains become two partly, some is directly as methyl tin bath water, wash result shows, with identical with the effect of pure water washing, to the quality of thiol methyl tin without any influence; Another partly enters the processing of the 4th step;
The 4th step: secondary underpressure distillation: in the water of condensation that the processing of the 3rd step obtains, add hydrochloric acid, carry out the adjustment of pH value, the pH value is transferred to 6.8, carry out the secondary underpressure distillation then, with the water that obtains dissolving water as methyl tin intermediate, obtain the thiol methyl tin product after the reaction, investigate indexs such as quality and yield.The result shows, and is in full accord with the thiol methyl tin product that obtains with the pure water dissolving.
Index is as follows: Sn:19.23% S:11.96% Po-Co:14 transmittance: 99.5.
Claims (2)
1. process for treating waste water from thiol methyl tin production, it is characterized in that: in conjunction with the methyl tin technological process of production, at first waste water is adopted absorption with sorbent material, remove organism in the waste water with potassium permanganate simultaneously, and then the ammonium chloride in the extraction waste water, will remove organism and ammonium chloride water afterwards at last and return thiol methyl tin Production Flow Chart use; Sorbent material adopts gac, cinder; Ammonium chloride in the waste water extracts and adopts distillation under vacuum, and service temperature is 70 ℃～80 ℃, and vacuum tightness is 75Kpa, and the purity of ammonium chloride is purified to more than 97%; Removing organism and ammonium chloride a part of water adjust pH afterwards is 6.9～7.1, as methyl tin bath water, between another part water adjust pH to 6～7, as the dissolving water of methyl tin intermediate.
2. process for treating waste water from thiol methyl tin production according to claim 1, it is characterized in that being: will deviate from the water hydrochloric acid adjust pH after organism and the ammonium chloride, and behind adjust pH, carry out with above-mentioned distillation under vacuum once more as the dissolving water of methyl tin intermediate; Gac filters behind the cinder absorption waste water, and sorbent material recirculation is used.
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| CN108976254A (en) * | 2018-07-04 | 2018-12-11 | 湖北犇星化工有限责任公司 | A kind of dry method for waste water of reduction thiol methyl tin synthesis |
| CN108751225A (en) * | 2018-07-16 | 2018-11-06 | 浙江大学 | Adsorb the ammonia chloride crystal purification system and method for purification of organic matter azane and oxygen alkane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4347385A (en) * | 1981-04-14 | 1982-08-31 | Phillips Petroleum Company | Process for the separation of sulfur compounds from water |
| CN1280214C (en) * | 2003-12-19 | 2006-10-18 | 天津市海跃水处理高科技有限公司 | Ammonia chloride waste water zero release treating process |
| CN101250017A (en) * | 2008-04-02 | 2008-08-27 | 总装备部工程设计研究总院 | Purification technique for methyl stannum mercaptide industrial sewage |
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- 2008-11-12 CN CN2008102335536A patent/CN101402495B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4347385A (en) * | 1981-04-14 | 1982-08-31 | Phillips Petroleum Company | Process for the separation of sulfur compounds from water |
| CN1280214C (en) * | 2003-12-19 | 2006-10-18 | 天津市海跃水处理高科技有限公司 | Ammonia chloride waste water zero release treating process |
| CN101250017A (en) * | 2008-04-02 | 2008-08-27 | 总装备部工程设计研究总院 | Purification technique for methyl stannum mercaptide industrial sewage |
Non-Patent Citations (1)
| Title |
|---|
| 胡晓斌.甲基硫醇锡生产废水的预处理试验.《内蒙古石油化工》.2005,(第1期), * |
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Assignee: Yunnan Tin Chemical Company Assignor: Yunnan Tin Group (Holding) Co., Ltd Contract record no.: 2012530000027 Denomination of invention: Process for treating waste water from thiol methyl tin production Granted publication date: 20110907 License type: Exclusive License Open date: 20090408 Record date: 20120522 |