CN100575328C - Process for preparing dichloroacetyl chloride - Google Patents
Process for preparing dichloroacetyl chloride Download PDFInfo
- Publication number
- CN100575328C CN100575328C CN200610098265A CN200610098265A CN100575328C CN 100575328 C CN100575328 C CN 100575328C CN 200610098265 A CN200610098265 A CN 200610098265A CN 200610098265 A CN200610098265 A CN 200610098265A CN 100575328 C CN100575328 C CN 100575328C
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- CN
- China
- Prior art keywords
- composite catalyst
- dichloroacetyl chloride
- trieline
- trichloroethylene
- weight ratio
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- FBCCMZVIWNDFMO-UHFFFAOYSA-N dichloroacetyl chloride Chemical compound ClC(Cl)C(Cl)=O FBCCMZVIWNDFMO-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 239000002131 composite material Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 239000012263 liquid product Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 24
- 235000019270 ammonium chloride Nutrition 0.000 claims description 12
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 12
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000002917 insecticide Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 abstract 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- UBCKGWBNUIFUST-YHYXMXQVSA-N tetrachlorvinphos Chemical compound COP(=O)(OC)O\C(=C/Cl)C1=CC(Cl)=C(Cl)C=C1Cl UBCKGWBNUIFUST-YHYXMXQVSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A preparation process of dichloroacetyl chloride. Relates to a preparation process of dichloroacetyl chloride used as an insecticide. The method takes trichloroethylene as a raw material and comprises the following steps: 1) placing trichloroethylene in a tower reactor, adding a composite catalyst, wherein the weight ratio of the composite catalyst to the trichloroethylene is 0.1-1.0: 100, and uniformly stirring; heating to 100-110 ℃, introducing dry air into the container at the temperature, and keeping for 9-11 hours; 2) and carrying out normal pressure distillation processing on the product obtained in the previous step, and collecting 105-108 ℃ fractions to obtain a colorless transparent liquid product, namely dichloroacetyl chloride. The invention uses dry air as oxidation source, and the reaction yield reaches 93.5% and the content is more than 99% by compressed air oxidation. Is suitable for industrialized energy-saving production, can reduce three wastes and improve economic benefit. The invention has simple process, no special requirement on equipment in the processing process, low equipment cost and greatly improved safety in the processing process.
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, described composite catalyst is this three of Vanadium Pentoxide in FLAKES, triphenyl phosphorus and ammonium chloride, perhaps is this three of Manganse Dioxide, triphenyl phosphorus and ammonium chloride; The weight ratio of composite catalyst and trieline is 0.1～1.0: 100, evenly stirs; 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.
When described composite catalyst was this three of Vanadium Pentoxide in FLAKES, triphenyl phosphorus and ammonium chloride, three's weight ratio was 1: 0.5～0.7: 2～2.5.
When described composite catalyst was this three of Manganse Dioxide, triphenyl phosphorus and ammonium chloride, three's weight ratio was 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 (3)
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, described composite catalyst is this three of Vanadium Pentoxide in FLAKES, triphenyl phosphorus and ammonium chloride, perhaps is this three of Manganse Dioxide, triphenyl phosphorus and ammonium chloride; The weight ratio of composite catalyst and trieline is 0.1～1.0: 100, evenly stirs; 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, when described composite catalyst was this three of Vanadium Pentoxide in FLAKES, triphenyl phosphorus and ammonium chloride, three's weight ratio was 1: 0.5～0.7: 2～2.5.
3, the preparation technology of dichloroacetyl chloride according to claim 1 is characterized in that, when described composite catalyst was this three of Manganse Dioxide, triphenyl phosphorus and ammonium chloride, three's weight ratio was 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 | Process for preparing dichloroacetyl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610098265A CN100575328C (en) | 2006-12-08 | 2006-12-08 | Process for preparing dichloroacetyl chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101195563A CN101195563A (en) | 2008-06-11 |
| CN100575328C true 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 | Process for preparing dichloroacetyl chloride |
Country Status (1)
| Country | Link |
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| CN (1) | CN100575328C (en) |
Families Citing this family (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 |
| 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 |
| CN115504879B (en) * | 2021-06-22 | 2024-08-30 | 联化科技股份有限公司 | Method for continuously preparing dichloroacetyl chloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1073369A (en) * | 1965-05-21 | 1967-06-28 | Shell Int Research | A processes for oxidizing trichloroethylene to dichloroacetyl chloride |
| CN1131140A (en) * | 1995-03-09 | 1996-09-18 | 济南市天桥天营科工贸开发中心 | Method for preparation of dichloracetyl chloride |
| CN1181370A (en) * | 1996-10-30 | 1998-05-13 | 济南市天桥天营科工贸开发中心 | Method for prepn. of trichlorine acetylchloride |
-
2006
- 2006-12-08 CN CN200610098265A patent/CN100575328C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1073369A (en) * | 1965-05-21 | 1967-06-28 | Shell Int Research | A processes for oxidizing trichloroethylene to dichloroacetyl chloride |
| CN1131140A (en) * | 1995-03-09 | 1996-09-18 | 济南市天桥天营科工贸开发中心 | Method for preparation of dichloracetyl chloride |
| CN1181370A (en) * | 1996-10-30 | 1998-05-13 | 济南市天桥天营科工贸开发中心 | Method for prepn. of trichlorine acetylchloride |
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| CN101195563A (en) | 2008-06-11 |
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| C06 | Publication | ||
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| C14 | Grant of patent or utility model | ||
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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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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: JI ZHIYANG WANG JIANRONG TO: YU GUOQUAN YU WEI JI ZHIYANG WANG JIANRONG |