CN103910337A - Treatment method for sulfur as byproduct generated in ethyl chloride production process - Google Patents
Treatment method for sulfur as byproduct generated in ethyl chloride production process Download PDFInfo
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- CN103910337A CN103910337A CN201410116483.1A CN201410116483A CN103910337A CN 103910337 A CN103910337 A CN 103910337A CN 201410116483 A CN201410116483 A CN 201410116483A CN 103910337 A CN103910337 A CN 103910337A
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Abstract
The invention relates to a treatment method for sulfur as a byproduct generated in an ethyl chloride production process. The treatment method comprises the steps of firstly, carrying out reduced pressure distillation on sulfur subjected to alkaline hydrolysis; then, adding liquid caustic soda and water, uniformly stirring, and carrying out suction filtration to obtain a filter cake; drying the filter cake to obtain sulfur as an industrial product with the purity of larger than 99.5%. The method is low in cost, high in recovery rate of ethyl chloride, reduced in field smell and suitable for large-scale industrial production.
Description
Technical field
The treatment process that the present invention relates to by product sulphur in a kind of diethylaluminum monochloride production process, belongs to fine chemical technology field.
Background technology
" diethylaluminum monochloride " is the efficient key intermediate of 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, 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 alkaline hydrolysis reaction, removes disulphur dichloride, obtains crude product diethylaluminum monochloride and sulphur; Then by refining crude product washing, obtain finished product.After this technique alkaline hydrolysis, diethylaluminum monochloride loss is more, only has percent seventy or eighty yield, and the thick sulphur producing after alkaline hydrolysis, complicated component, and 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 in the time processing, and processing cost is higher; And the treatment time is long, distillation temperature (110～120 ℃) height, has exceeded the isomerized temperature of diethylaluminum monochloride (100 ℃), and the diethylaluminum monochloride quality of subsequent recovery is affected greatly.Therefore, need provide a kind of is more suitable in 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 has not only reduced energy consumption and cost, has also improved product yield simultaneously, has greatly reduced 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, and 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, 80～90 ℃ of temperature, time 2～2.5h.
In above-mentioned treatment process, it is 30～35% sodium hydroxide solution that described liquid caustic soda is selected from massfraction; 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, add after liquid caustic soda and water, must treat that gained mixture temperature is down to 50 ℃ and just can carries out below suction filtration.
The treating method comprises following concrete steps:
1) sulphur after alkaline hydrolysis is placed in and processes still stratification, upper strata diethylaluminum monochloride further reclaims;
2) remaining step 1) mixture is decompressed to-0.095～-0.1MPa, in 80～90 ℃ of distillations 2～2.5 hours, gained distillment was diethylaluminum monochloride, recycled;
3) continue to add liquid caustic soda, water, stir, suction filtration in the time that temperature is down to below 50 ℃;
4) by step 3) gained filter cake process drying treatment, obtain industrial goods sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride is further recycled.
On-the-spot smell, is necessary suction filtration device portal to vacuumize when reducing suction filtration.
The present invention does not use catalyzer and emulsifying agent in sulphur treatment process, only by first underpressure distillation, then adds liquid caustic soda and water to process the industrial sulfur product of acquisition purity more than 99.5%.In by product sulphur treating processes of the present invention, the strict distillation temperature of controlling, within the scope of 80～90 ℃, not only shortens the treatment time, reduces and processes energy consumption and cost, has also improved the yield of diethylaluminum monochloride simultaneously; In addition,, owing to suction filtration device portal being vacuumized in putting sulphur, greatly reduced on-the-spot smell.
Embodiment
Following examples are used for illustrating 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 to sulphur and processes still stratification, upper strata crude product diethylaluminum monochloride is reclaimed;
2) closed system, starts and stirs, and sulphur is processed in still mixture at-0.096MPa, under 84 ℃ of conditions, distills 2h, and gained distillment is diethylaluminum monochloride, recycles; The mixed gas that distillation produces is through condenser, receiving tank, surge tank access vacuum pump, the vacuum pump withdrawing gas gas processing system that truncates.
3) continue to process in still and add 100kg liquid caustic soda (massfraction 32%), 600kg water to sulphur, stir, treat that temperature is down to 50 ℃ and emits below liquid to suction filtration device, suction filtration device portal is vacuumized simultaneously, reduce on-the-spot smell.
4) gained filter cake drying processing after suction filtration, obtains 99.5% purity industrial goods sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride recoverable, remaining filtrate further recycles.
Embodiment 2:
1) sulphur of the 1400kg after alkaline hydrolysis is placed in to sulphur and processes still stratification, upper strata crude product diethylaluminum monochloride is reclaimed;
2) closed system, starts and stirs, and sulphur is processed in still mixture at-0.098MPa, under 86 ℃ of conditions, distills 2.3h, and gained distillment is diethylaluminum monochloride, recycles; The mixed gas that distillation produces is through condenser, receiving tank, surge tank access vacuum pump, the vacuum pump withdrawing gas gas processing system that truncates.
3) continue to process in still and add 117kg liquid caustic soda (massfraction 30%), 700kg water to sulphur, stir, treat that temperature is down to 50 ℃ and emits below liquid to suction filtration device, suction filtration device portal is vacuumized simultaneously, reduce on-the-spot smell.
4) after suction filtration, gained filter cake, through drying treatment, obtains 99.6% purity industrial goods sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride recoverable, remaining filtrate further recycles.
Embodiment 3:
1) sulphur of the 1600kg after alkaline hydrolysis is placed in to sulphur and processes still stratification, upper strata crude product diethylaluminum monochloride is reclaimed;
2) closed system, starts and stirs, and sulphur is processed in still mixture at-0.1MPa, under 88 ℃ of conditions, distills 2.5h, and gained distillment is diethylaluminum monochloride, recycles; The mixed gas that distillation produces is through condenser, receiving tank, surge tank access vacuum pump, the vacuum pump withdrawing gas gas processing system that truncates.
3) continue to process in still and add 133kg liquid caustic soda (massfraction 35%), 800kg water to sulphur, stir, in the time that temperature is down to below 50 ℃, emit liquid in suction filtration device, suction filtration device portal is vacuumized simultaneously, reduce on-the-spot smell.
4) after suction filtration, gained filter cake, through drying treatment, obtains 99.8% purity industrial goods sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride recoverable, remaining filtrate further recycles.
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 (6)
1. a treatment process for by product sulphur in diethylaluminum monochloride production process, is characterized in that, first by the sulphur underpressure distillation after alkaline hydrolysis, then adds liquid caustic soda and water, stirs, and suction filtration, obtains industrial goods sulphur after gained filtration cakes torrefaction.
2. treatment process according to claim 1, is characterized in that, described underpressure distillation condition: pressure-0.095～-0.1MPa, 80～90 ℃ of temperature, 2～2.5 hours time.
3. treatment process according to claim 1, is characterized in that, described liquid caustic soda is the sodium hydroxide solution of massfraction 30～35%.
4. 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.
5. treatment process according to claim 1, is characterized in that, adds after liquid caustic soda and water, and palpus thing temperature to be mixed is down to 50 ℃ and is carried out below suction filtration again.
6. treatment process according to claim 1, is characterized in that, the treating method comprises following concrete steps:
1) sulphur after alkaline hydrolysis is placed in and processes still stratification, upper strata diethylaluminum monochloride further reclaims;
2) remaining step 1) mixture is decompressed to-0.095～-0.1MPa, in 80～90 ℃ of distillations 2～2.5 hours, gained distillment diethylaluminum monochloride was recycled;
3) continue to add liquid caustic soda, water, stir, suction filtration in the time that temperature is down to below 50 ℃;
4) by step 3) gained filter cake process drying treatment, obtain industrial goods sulphur; Gained filtrate stratification, lower floor's diethylaluminum monochloride is further recycled.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621370A (en) * | 2016-02-29 | 2016-06-01 | 湖北仙隆化工股份有限公司 | Technology and equipment for recycling sulfur in ethyl chloride |
| CN107673313A (en) * | 2017-09-30 | 2018-02-09 | 杨波 | The processing recovery process of sulfur waste sulphur in a kind of chloride |
| CN108557772A (en) * | 2018-05-03 | 2018-09-21 | 山东戴瑞克新材料有限公司 | A kind of processing method of the sulphur mud of dicyclohexyl bisulfide |
| CN109467058A (en) * | 2018-12-21 | 2019-03-15 | 浙江埃森化学有限公司 | A kind of melting and oxidative purification of diethylaluminum monochloride by-product sulphur |
| CN109553074A (en) * | 2019-01-31 | 2019-04-02 | 扬州帮手科技有限公司 | A kind of recovery method of environment amenable diethylaluminum monochloride production by-product sulphur |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109455674B (en) * | 2018-12-21 | 2022-04-12 | 浙江埃森化学有限公司 | Solvent purification method of ethyl chloride byproduct sulfur |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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2014
- 2014-03-26 CN CN201410116483.1A patent/CN103910337B/en active Active
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 (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621370A (en) * | 2016-02-29 | 2016-06-01 | 湖北仙隆化工股份有限公司 | Technology and equipment for recycling sulfur in ethyl chloride |
| CN107673313A (en) * | 2017-09-30 | 2018-02-09 | 杨波 | The processing recovery process of sulfur waste sulphur in a kind of chloride |
| CN108557772A (en) * | 2018-05-03 | 2018-09-21 | 山东戴瑞克新材料有限公司 | A kind of processing method of the sulphur mud of dicyclohexyl bisulfide |
| 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 |
| CN109467058A (en) * | 2018-12-21 | 2019-03-15 | 浙江埃森化学有限公司 | A kind of melting and oxidative purification of diethylaluminum monochloride by-product sulphur |
| 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 |
| CN109553074A (en) * | 2019-01-31 | 2019-04-02 | 扬州帮手科技有限公司 | A kind of recovery method of environment amenable diethylaluminum monochloride production 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. |
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