CN103910337B - The treatment process of by product sulphur in a kind of diethylaluminum monochloride production process - Google Patents
The treatment process of by product sulphur in a kind of diethylaluminum monochloride production process Download PDFInfo
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- CN103910337B CN103910337B CN201410116483.1A CN201410116483A CN103910337B CN 103910337 B CN103910337 B CN 103910337B CN 201410116483 A CN201410116483 A CN 201410116483A CN 103910337 B CN103910337 B CN 103910337B
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Abstract
The present invention relates to the treatment process of by product sulphur in a kind of diethylaluminum monochloride production process, first by the sulphur underpressure distillation after alkaline hydrolysis, then add liquid caustic soda and water, stir, suction filtration, after gained filtration cakes torrefaction, obtain the industrial goods sulphur of purity more than 99.5%.Present method cost is low, and the diethylaluminum monochloride rate of recovery is high, and on-the-spot smell reduces, and is suitable for large-scale commercial production.
Description
Technical field
The present invention relates to the treatment process of by product sulphur in a kind of diethylaluminum monochloride production process, belong to technical field of fine.
Background technology
" diethylaluminum monochloride " is the efficient key intermediate producing higher effective and lower toxic pesticide Chlorpyrifos 94 and triazophos etc., and product meets the requirement of green chemical industry and recycling economy.At present, go up both at home and abroad and generally adopt thiophosphoric anhydride legal system to get diethylaluminum monochloride, namely thiophosphoric anhydride and dehydrated alcohol react and generate sulfide under pyridine catalysis, then pass into chlorinated with chlorine and obtain muriate; The sodium sulphite that muriate and vulcanization reaction generate carries out Basic fluxing raction, and removing disulphur dichloride, obtains crude product diethylaluminum monochloride and sulphur; Then by refining for crude product washing, finished product is obtained.After this technique alkaline hydrolysis, diethylaluminum monochloride loss is more, only has percent seventy or eighty yield, and the thick sulphur produced after alkaline hydrolysis, and complicated component, impurity is many, comprises the organism such as diethylaluminum monochloride and other unserviceable salt inorganics.
CN10151005A discloses the treatment process of by product sulphur in a kind of o,o-diethylthiophosphoryl chloride production process, and its method will add liquid caustic soda, catalyzer and emulsifying agent when processing, and processing cost is higher; And the treatment time is long, distillation temperature (110 ~ 120 DEG C) is high, has exceeded the isomerized temperature of diethylaluminum monochloride (100 DEG C), has affected greatly the ethylmercury chloride amount of subsequent recovery.Therefore, need provide a kind of and be more suitable for industrial production, the wider method of application.
Summary of the invention
In order to overcome above-mentioned purpose, the invention provides the treatment process of by product sulphur in a kind of diethylaluminum monochloride production process, the method not only reduces energy consumption and cost, also improves product yield simultaneously, greatly reduces on-the-spot smell.
To achieve these goals, the present invention adopts following technical scheme:
A treatment process for by product sulphur in diethylaluminum monochloride production process, first by the sulphur underpressure distillation after alkaline hydrolysis, then adds liquid caustic soda and water, stirs, suction filtration, obtains the industrial goods sulphur of purity more than 99.5% after gained filtration cakes torrefaction.
In above-mentioned treatment process, described underpressure distillation condition: pressure-0.095 ~-0.1MPa, temperature 80 ~ 90 DEG C, time 2 ~ 2.5h.
In above-mentioned treatment process, described liquid caustic soda is selected from the sodium hydroxide solution that massfraction is 30 ~ 35%; Preferred mass mark 32%.
In above-mentioned treatment process, after described alkaline hydrolysis, the mass ratio of sulphur and liquid caustic soda, water is 12 ~ 16:1 ~ 1.5:6 ~ 8.
In above-mentioned treatment process, after adding liquid caustic soda and water, must treat that gained mixture temperature is down to less than 50 DEG C and just can be carried out suction filtration.
The treating method comprises following concrete steps:
1) sulphur after alkaline hydrolysis is placed in process still stratification, upper strata diethylaluminum monochloride reclaims further;
2) remaining for step 1) mixture is decompressed to-0.095 ~-0.1MPa, in 80 ~ 90 DEG C of distillations 2 ~ 2.5 hours, gained distillment was diethylaluminum monochloride, recycled;
3) continue to add liquid caustic soda, water, stir, suction filtration when temperature is down to below 50 DEG C;
4) by step 3) gained filter cake through drying treatment, obtain industrial goods sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride is recycled further.
During in order to reduce suction filtration, on-the-spot smell, is necessary to vacuumize Suction filtration device entrance.
The present invention does not use catalyzer and emulsifying agent in sulphur treatment process, by means of only first underpressure distillation, then adds liquid caustic soda and water and carries out process and obtain the industrial sulfur product of purity more than 99.5%.In by product sulphur treating processes of the present invention, the strict distillation temperature that controls is within the scope of 80 ~ 90 DEG C, not only shortens the treatment time, reduces process energy consumption and cost, also improve the yield of diethylaluminum monochloride simultaneously; In addition, owing to vacuumizing Suction filtration device entrance while putting sulphur, on-the-spot smell is greatly reduced.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
1) sulphur of the 1200kg after alkaline hydrolysis is placed in sulphur process still stratification, upper strata crude product diethylaluminum monochloride is reclaimed;
2) closed system, start and stir, in sulphur process still, mixture is at-0.096MPa, distills 2h under 84 DEG C of conditions, and gained distillment is diethylaluminum monochloride, recycles; The mixed gas that distillation produces is through condenser, receiving tank, surge tank access vacuum pump, and vacuum pump withdrawing gas truncates gas processing system.
3) continue to add 100kg liquid caustic soda (massfraction 32%), 600kg water in sulphur process still, stir, treat that temperature is down to less than 50 DEG C and is released liquid to Suction filtration device, Suction filtration device entrance is vacuumized simultaneously, reduce on-the-spot smell.
4) gained filter cake drying process after suction filtration, obtains 99.5% grade industrial product sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride recoverable, remaining filtrate recycles further.
Embodiment 2:
1) sulphur of the 1400kg after alkaline hydrolysis is placed in sulphur process still stratification, upper strata crude product diethylaluminum monochloride is reclaimed;
2) closed system, start and stir, in sulphur process still, mixture is at-0.098MPa, distills 2.3h under 86 DEG C of conditions, and gained distillment is diethylaluminum monochloride, recycles; The mixed gas that distillation produces is through condenser, receiving tank, surge tank access vacuum pump, and vacuum pump withdrawing gas truncates gas processing system.
3) continue to add 117kg liquid caustic soda (massfraction 30%), 700kg water in sulphur process still, stir, treat that temperature is down to less than 50 DEG C and is released liquid to Suction filtration device, Suction filtration device entrance is vacuumized simultaneously, reduce on-the-spot smell.
4) after suction filtration, gained filter cake, through drying treatment, obtains 99.6% grade industrial product sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride recoverable, remaining filtrate recycles further.
Embodiment 3:
1) sulphur of the 1600kg after alkaline hydrolysis is placed in sulphur process still stratification, upper strata crude product diethylaluminum monochloride is reclaimed;
2) closed system, start and stir, in sulphur process still, mixture is at-0.1MPa, distills 2.5h under 88 DEG C of conditions, and gained distillment is diethylaluminum monochloride, recycles; The mixed gas that distillation produces is through condenser, receiving tank, surge tank access vacuum pump, and vacuum pump withdrawing gas truncates gas processing system.
3) continue to add 133kg liquid caustic soda (massfraction 35%), 800kg water in sulphur process still, stir, when temperature is down to below 50 DEG C, release liquid in Suction filtration device, Suction filtration device entrance is vacuumized simultaneously, reduce on-the-spot smell.
4) after suction filtration, gained filter cake, through drying treatment, obtains 99.8% grade industrial product sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride recoverable, remaining filtrate recycles further.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (3)
1. the treatment process of by product sulphur in diethylaluminum monochloride production process, is characterized in that, comprise following concrete steps:
1) sulphur after alkaline hydrolysis is placed in process still stratification, upper strata diethylaluminum monochloride reclaims further;
2) by step 1) remaining mixture is decompressed to-0.095 ~-0.1MPa, and in 80 ~ 90 DEG C of distillations 2 ~ 2.5 hours, gained distillment diethylaluminum monochloride was recycled;
3) continue to add liquid caustic soda, water, stir, suction filtration when temperature is down to below 50 DEG C;
4) by step 3) gained filter cake through drying treatment, obtain industrial goods sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride is recycled further.
2. treatment process according to claim 1, is characterized in that, described liquid caustic soda is the sodium hydroxide solution of massfraction 30 ~ 35%.
3. treatment process according to claim 1, is characterized in that, after described alkaline hydrolysis, the mass ratio of sulphur and liquid caustic soda, water is 12 ~ 16:1 ~ 1.5:6 ~ 8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455674A (en) * | 2018-12-21 | 2019-03-12 | 浙江埃森化学有限公司 | A kind of solvent purifications method of diethylaluminum monochloride by-product sulphur |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621370B (en) * | 2016-02-29 | 2017-12-15 | 湖北仙隆化工股份有限公司 | The recovery process and equipment of sulphur in a kind of diethylaluminum monochloride |
| CN107673313B (en) * | 2017-09-30 | 2019-12-27 | 杨波 | Treatment and recovery process of waste sulfur in chloride |
| CN108557772B (en) * | 2018-05-03 | 2022-06-10 | 山东戴瑞克新材料有限公司 | Treatment method of sulfur mud of dicyclohexyl disulfide |
| CN109467058B (en) * | 2018-12-21 | 2022-06-17 | 浙江埃森化学有限公司 | Melting and oxidation purification method of ethyl chloride byproduct sulfur |
| CN109553074B (en) * | 2019-01-31 | 2020-07-28 | 扬州帮手科技有限公司 | Environment-friendly recovery method of byproduct sulfur in ethyl chloride production |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101293897A (en) * | 2008-06-06 | 2008-10-29 | 武汉工程大学 | Method for preparing O,O-ethyl thioether substituted phosphorus oxychloride |
| CN101591005A (en) * | 2008-05-31 | 2009-12-02 | 阳新县晨天化工有限责任公司 | The treatment process of attached product sulphur in the o,o-diethylthiophosphoryl chloride production process |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591005A (en) * | 2008-05-31 | 2009-12-02 | 阳新县晨天化工有限责任公司 | The treatment process of attached product sulphur in the o,o-diethylthiophosphoryl chloride production process |
| CN101293897A (en) * | 2008-06-06 | 2008-10-29 | 武汉工程大学 | Method for preparing O,O-ethyl thioether substituted phosphorus oxychloride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455674A (en) * | 2018-12-21 | 2019-03-12 | 浙江埃森化学有限公司 | A kind of solvent purifications method of diethylaluminum monochloride by-product sulphur |
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Address after: 441300 No. 9 High-tech Industrial Development Zone, Suizhou City, Hubei Province Patentee after: Hubei Gongxing New Materials Co., Ltd. Address before: 441300 No. 9 Economic and Technological Development Zone, Suizhou City, Hubei Province Patentee before: Hubei Benxing Chemical Co., Ltd. |