CN101195563A - Technique of preparing dichloroacetyl chloride - Google Patents
Technique of preparing dichloroacetyl chloride Download PDFInfo
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- CN101195563A CN101195563A CNA2006100982655A CN200610098265A CN101195563A CN 101195563 A CN101195563 A CN 101195563A CN A2006100982655 A CNA2006100982655 A CN A2006100982655A CN 200610098265 A CN200610098265 A CN 200610098265A CN 101195563 A CN101195563 A CN 101195563A
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- composite catalyst
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- dichloroacetyl chloride
- trieline
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Abstract
A technique for preparing dichloracetyl chloride is provided. The invention relates to a technique for preparing dichloracetyl chloride as insecticide, which adopts trichloroethylene as raw material and comprises 1) placing trichloroethylene the tower reactor to charge composite catalyst, wherein the weight ratio of the composite catalyst and trichloroethylene is 0.1-1.0: 100, the raw materials are stirred evenly and heated to 100-110 DEG C and the container is aerated by dry air under the temperature to keep 9-11 h; 2) distilling the obtained product of the step one and processing under normal pressure and collecting fraction at 105-108 DEG C, the colorless transparent liquid product dichloracetyl chloride is obtained. The invention uses dry air as oxidizing source, the reaction yield reaches 93.5% and the content is more than 99% through compressing air and oxidizing, thereby fitting for industrialized energy-saving production, reducing three-waste and improving economic benefit. The invention is simple in technique without special requirement of equipment in the processing procedure and low in equipment cost, which improves the security in the processing procedure greatly.
Description
Technical field
The present invention relates to the synthesis technique of agricultural insecticide tetrachlorvinphos, particularly a kind of preparation technology of the dichloroacetyl chloride as sterilant.
Background technology
What the dichloroacetyl chloride synthetic method was reported at present is that oxidation source carries out oxidation with oxygen, needs pressure higher, and yield can only reach 89%.This method production oxygen utilization rate is not high, and yield and content are low, directly influence production cost, and quantity of three wastes is bigger simultaneously, and safety coefficient is not high.
State Intellectual Property Office's application number is: 95110365.2, name is called: the technical scheme of " a kind of preparation method of dichloroacetyl chloride ", disclosed a kind of be main raw material with the trieline, azo-bis-iso-butyl is a catalysts, triethylamine is the technical scheme of reaction initiator.Wherein the adding proportion for catalyzer and initiator requires accurately; When catalyst levels is lower than setting range, can cause reaction not carry out, do not reach the catalyzed reaction effect, when being higher than setting range, reaction is fierce, and is wayward; And reaction pressure sharply increases, equipment is withstand voltage conditional request height.Has certain risk in the production process.The control of the consumption of initiator and temperature needs accurately equally, otherwise can not react or speed of response slow, temperature is too high also may cause danger.The technical program is very high to equipment requirements, requires to have very high voltage endurance capability.Long processing time needs 15 hours approximately simultaneously.
Summary of the invention
The object of the invention is to provide a kind of reaction yield height, the preparation technology of the dichloroacetyl chloride that technological process is simple, safe.
Technical scheme of the present invention is: with the trieline is raw material, and it may further comprise the steps:
1), trieline is placed tower reactor, and add composite catalyst, the weight ratio of composite catalyst and trieline is 0.1～1.0: 100, evenly stirring; Reheat to 100～110 ℃ under this temperature, feed the exsiccant air in container, kept 9～11 hours;
2), last step gains are carried out air distillation processing, collect 105～108 ℃ of cuts, promptly get colourless transparent liquid product dichloroacetyl chloride.
Described composite catalyst is Vanadium Pentoxide in FLAKES or Manganse Dioxide, triphenyl phosphorus, ammonium chloride.
Described composite catalyst is Vanadium Pentoxide in FLAKES, triphenyl phosphorus, ammonium chloride, and three's weight ratio is 1: 0.5～0.7: 2～2.5.
Described composite catalyst is Manganse Dioxide, triphenyl phosphorus, ammonium chloride, and three's weight ratio is 1: 0.3～0.5: 0.8～1.2.
The present invention is an oxidation source with the dry air under the catalysis of Vanadium Pentoxide in FLAKES or Manganse Dioxide, triphenyl phosphorus, ammonium chloride, product content, and promptly purity can reach 99%, and yield reaches 93%.Be fit to industrialized energy-saving production, can reduce the three wastes, increase economic efficiency.Among the present invention, the composite catalyst of adding and the weight ratio of trieline are 0.1～1.0: 100.The appropriate catalyst add-on not only can not cause cost to strengthen to production, and can reach purpose of design.Technology of the present invention is simple, in the course of processing equipment is not had particular requirement, and equipment cost is low, and has improved the security in the course of processing greatly.
Embodiment
Example 1
1, in the tower reactor of 1000ml, drops into trieline 400g, Vanadium Pentoxide in FLAKES 0.3g, triphenyl phosphorus 0.2g, ammonium chloride 0.6g.
2, be warming up to 100 ℃, fed the exsiccant air reaction 11 hours down at 100 ℃.
3, after reaction is finished, change over to and carry out air distillation in the 500ml there-necked flask, collect 108 ℃ of cuts, obtain colourless transparent liquid product dichloroacetyl chloride 461g, purity 99%.
4, the cut below 105 ℃ is mainly trieline, recycles.
Example 2
1, in the tower reactor of 1000ml, drops into trieline 400g, Manganse Dioxide 0.6g, triphenyl phosphorus 0.2g, ammonium chloride 0.6g.
2, be warming up to 100 ℃, fed the exsiccant air reaction 10 hours down at 105 ℃.
3, after reaction is finished, change over to and carry out air distillation in the 500ml there-necked flask, collect 106 ℃ of cuts, obtain colourless transparent liquid product dichloroacetyl chloride 462g, purity 99%.
4, the cut below 105 ℃ is mainly trieline, recycles.
Example 3
1, in the tower reactor of 1000ml, drops into trieline 400g, Manganse Dioxide 0.6g, triphenyl phosphorus 0.2g, ammonium chloride 0.6g.
2, be warming up to 100 ℃, fed the exsiccant air reaction 9 hours down at 110 ℃.
3, after reaction is finished, change over to and carry out air distillation in the 500ml there-necked flask, collect 105 ℃ of cuts, obtain colourless transparent liquid product dichloroacetyl chloride 462g, purity 99%.
4, the cut below 105 ℃ is mainly trieline, recycles.
Claims (4)
1. the preparation technology of dichloroacetyl chloride is a raw material with the trieline, it is characterized in that it may further comprise the steps:
1), trieline is placed tower reactor, and add composite catalyst, the weight ratio of composite catalyst and trieline is 0.1～1.0: 100, evenly stirring; Reheat to 100～110 ℃ under this temperature, feed the exsiccant air in container, kept 9～11 hours;
2), last step gains are carried out air distillation processing, collect 105～108 ℃ of cuts, promptly get colourless transparent liquid product dichloroacetyl chloride.
2. the preparation technology of dichloroacetyl chloride according to claim 1 is characterized in that, described composite catalyst is Vanadium Pentoxide in FLAKES or Manganse Dioxide, triphenyl phosphorus, ammonium chloride.
3. the preparation technology of dichloroacetyl chloride according to claim 2 is characterized in that, described composite catalyst is Vanadium Pentoxide in FLAKES, triphenyl phosphorus, ammonium chloride, and three's weight ratio is 1: 0.5～0.7: 2～2.5.
4. the preparation technology of dichloroacetyl chloride according to claim 2 is characterized in that, described composite catalyst is Manganse Dioxide, triphenyl phosphorus, ammonium chloride, and three's weight ratio is 1: 0.3～0.5: 0.8～1.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610098265A CN100575328C (en) | 2006-12-08 | 2006-12-08 | The preparation technology of dichloroacetyl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610098265A CN100575328C (en) | 2006-12-08 | 2006-12-08 | The preparation technology of dichloroacetyl chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101195563A true CN101195563A (en) | 2008-06-11 |
| CN100575328C CN100575328C (en) | 2009-12-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610098265A Active CN100575328C (en) | 2006-12-08 | 2006-12-08 | The preparation technology of dichloroacetyl chloride |
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| CN (1) | CN100575328C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573242A (en) * | 2017-09-07 | 2018-01-12 | 盐城顺恒化工有限公司 | A kind of preparation method of ethyl bromide difluoride |
| CN111318246A (en) * | 2020-04-24 | 2020-06-23 | 东营银桥化工有限责任公司 | Dichloroacetyl chloride synthesis reactor and synthesis method |
| CN115504879A (en) * | 2021-06-22 | 2022-12-23 | 联化科技股份有限公司 | Method for continuously preparing dichloroacetyl chloride |
-
2006
- 2006-12-08 CN CN200610098265A patent/CN100575328C/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573242A (en) * | 2017-09-07 | 2018-01-12 | 盐城顺恒化工有限公司 | A kind of preparation method of ethyl bromide difluoride |
| CN111318246A (en) * | 2020-04-24 | 2020-06-23 | 东营银桥化工有限责任公司 | Dichloroacetyl chloride synthesis reactor and synthesis method |
| CN111318246B (en) * | 2020-04-24 | 2023-05-12 | 东营银桥化工有限责任公司 | Dichloro acetyl chloride synthesis reactor and synthesis method |
| CN115504879A (en) * | 2021-06-22 | 2022-12-23 | 联化科技股份有限公司 | Method for continuously preparing dichloroacetyl chloride |
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| Publication number | Publication date |
|---|---|
| CN100575328C (en) | 2009-12-30 |
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Inventor after: Yu Guoquan Inventor after: Yu Wei Inventor after: Ji Zhiyang Inventor after: Wang Jianrong Inventor before: Ji Zhiyang Inventor before: Wang Jianrong |
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Free format text: CORRECT: INVENTOR; FROM: JI ZHIYANG WANG JIANRONG TO: YU GUOQUAN YU WEI JI ZHIYANG WANG JIANRONG |