CN102101848A - Method for producing epichlorohydrin - Google Patents
Method for producing epichlorohydrin Download PDFInfo
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- CN102101848A CN102101848A CN2010105212380A CN201010521238A CN102101848A CN 102101848 A CN102101848 A CN 102101848A CN 2010105212380 A CN2010105212380 A CN 2010105212380A CN 201010521238 A CN201010521238 A CN 201010521238A CN 102101848 A CN102101848 A CN 102101848A
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- hydrogen peroxide
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- chloropropene
- chlorallylene
- catalyzer
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Abstract
The invention provides a method for producing epichlorohydrin. A phase transfer method is adopted, 3-chloropropene is taken as a raw material and hydrogen peroxide is taken as an oxidant to produce the epichlorohydrin. The method comprises the following steps of: adding the 3-chloropropene and quaternary ammonium phosphotungstate serving as a catalyst into a reactor, stirring and heating to reaction temperature; and adding hydrogen peroxide, wherein reaction heat in the reaction process is condensed, refluxed and brought away by organic steam, a mass ratio of 50 percent hydrogen peroxide to the 3-chloropropene is (0.21-0.27):1, the hydrogen peroxide is added at a constant speed in 1 hour, and the total reaction time is 2 hours. In the reaction, other solvents are not added, and the conversion rate of epoxidation is controlled to be lower than 30 percent. By controlling the ratio of the 3-chloropropene to the hydrogen peroxide and the conversion rate of the epoxidation of the 3-chloropropene, the peroxide cumulated amount in the distillation procedure can be greatly reduced, and the explosion danger caused by overlarge peroxide cumulated amount in the subsequent distillation procedure is eliminated.
Description
Technical field
The present invention relates to a kind of production method of epoxy chloropropane, particularly relate to a kind of epoxy chloropropane production method of controlling chlorallylene epoxidation reaction transformation efficiency.
Background technology
Epoxy chloropropane is a kind of important Organic Chemicals and fine chemical product, and purposes is very extensive.Traditional epichlorohydrin production process mainly is propylene high-temperature chlorination process and allyl acetate method, has the governing problem that a large amount of " three wastes " pollute in the water discharge process under the saponification.Propelling along with the strategy of sustainable development, green synthetic route with epoxy chloropropane of industrial value becomes the focus of research in the industry, present research mainly concentrates on the exploration of the direct epoxidation technique route of propenyl chloride, adopting HTS or Lin Wusuanyan as catalyzer, is the epoxidation reaction that oxygenant carries out propenyl chloride with the hydrogen peroxide.
The direct epoxidation system epoxy chloropropane of phase transfer method propenyl chloride and hydrogen peroxide technology is arisen at the historic moment under this environment just.Adopt phosphotungstic acid quaternary as catalyzer, be oxygenant with the hydrogen peroxide, successfully solved the problem that traditional technology produces a large amount of waste water, and tool has high conversion and selectivity very much.But transformation efficiency is too high, and the portable a large amount of catalyzer of reaction solution causes follow-up distillation process superoxide semi-invariant too high, brings explosion hazard for the distillation tower still.
Summary of the invention
The technical problem to be solved in the present invention is, a kind of production method of epoxy chloropropane is provided, proportioning by control chlorallylene and hydrogen peroxide, the transformation efficiency of control chlorallylene epoxidation reaction, can greatly reduce the superoxide semi-invariant of distillation process, eliminate follow-up distillation process because of the too high explosion hazard that brings of superoxide semi-invariant.
The invention provides a kind of production method of epoxy chloropropane, adopt phase transfer method, with the chlorallylene is raw material, hydrogen peroxide is the oxidant production epoxy chloropropane, chlorallylene, catalyzer are added earlier in the reactor, after stirring is warming up to temperature of reaction, adds hydrogen peroxide again and react, the reaction heat of reaction process is taken away by the organic steam condensing reflux, and the mass ratio that feeds intake of 50% hydrogen peroxide/chlorallylene is 0.21～0.27: 1.
Phosphotungstic acid quaternary as catalyzer, is at the uniform velocity added hydrogen peroxide in the 1h, reaction total time 2h.The charging mass ratio is a propenyl chloride: 50% (mass ratio) hydrogen peroxide: catalyzer is 1: 0.23: 0.07.
Do not add any other solvent in the reaction.
The transformation efficiency of gate ring oxidizing reaction of the present invention is lower than 30%.Separate and promptly obtain the oil-phase product that propenyl chloride/epoxy chloropropane is the main body composition.On the one hand catalyst dissolution amount in the reaction product is dropped to extremely lowly, still can guarantee the highly selective of reacting and the high utilization rate of hydrogen peroxide on the other hand.
Embodiment
A kind of production method of epoxy chloropropane, adopt phase transfer method, with the chlorallylene is raw material, and phosphotungstic acid quaternary is a catalyzer, and hydrogen peroxide is the oxidant production epoxy chloropropane, add chlorallylene, catalyzer in the reactor earlier, after stirring is warming up to temperature of reaction, add hydrogen peroxide again, at the uniform velocity add hydrogen peroxide in the 1h, reaction total time 2h, the reaction heat of reaction process is taken away by the organic steam condensing reflux.The mass ratio that feeds intake of 50% hydrogen peroxide/chlorallylene is 0.21～0.27: 1.
Do not add any other solvent in the reaction.
The transformation efficiency of epoxidation reaction is controlled at is lower than in 30% the scope.
Embodiment one
Chlorallylene, catalyzer are added earlier in the reactor, after stirring is warming up to temperature of reaction, at the uniform velocity add hydrogen peroxide in the 1h, reaction total time 2h, the reaction heat of reaction process is taken away by the organic steam condensing reflux.The charging mass ratio, propenyl chloride: 50% hydrogen peroxide: catalyzer is 1: 0.21: 0.07.
The propenyl chloride transformation efficiency is 23%, and catalyst concn is 0.19% in the oil-phase product.
Embodiment two:
Chlorallylene, catalyzer are added earlier in the reactor, after stirring is warming up to temperature of reaction, at the uniform velocity add hydrogen peroxide in the 1h, reaction total time 2h, the reaction heat of reaction process is taken away by the organic steam condensing reflux.The charging mass ratio, propenyl chloride: 50% hydrogen peroxide: catalyzer is 1: 0.27: 0.08.
The propenyl chloride transformation efficiency is 30%, and catalyst concn is 0.29% in the oil-phase product.
Embodiment three (counter-example):
Chlorallylene, catalyzer are added earlier in the reactor, after stirring is warming up to temperature of reaction, at the uniform velocity add hydrogen peroxide in the 1h, reaction total time 2h.The charging mass ratio, propenyl chloride: 50% hydrogen peroxide: catalyzer is 1: 0.35: 0.1.
The propenyl chloride transformation efficiency is 40%, and catalyst concn is 0.91% in the oil-phase product.
Claims (4)
1. the production method of an epoxy chloropropane, adopt phase transfer method, with the chlorallylene is raw material, hydrogen peroxide is the oxidant production epoxy chloropropane, it is characterized in that, chlorallylene, catalyzer are added earlier in the reactor, after stirring is warming up to temperature of reaction, add hydrogen peroxide again, the mass ratio that feeds intake of 50% hydrogen peroxide/chlorallylene is 0.21～0.27: 1.
2. production method as claimed in claim 1 is characterized in that, catalyzer is a phosphotungstic acid quaternary.
3. production method as claimed in claim 2 is characterized in that, at the uniform velocity adds hydrogen peroxide in the 1h, reaction total time 2h.
4. production method as claimed in claim 3 is characterized in that, does not add any other solvent in the reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105212380A CN102101848A (en) | 2010-10-27 | 2010-10-27 | Method for producing epichlorohydrin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105212380A CN102101848A (en) | 2010-10-27 | 2010-10-27 | Method for producing epichlorohydrin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102101848A true CN102101848A (en) | 2011-06-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105212380A Pending CN102101848A (en) | 2010-10-27 | 2010-10-27 | Method for producing epichlorohydrin |
Country Status (1)
| Country | Link |
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| CN (1) | CN102101848A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557787A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Method for preparing epoxy chloropropane |
| CN116514741A (en) * | 2023-07-04 | 2023-08-01 | 山东民基新材料科技有限公司 | Process for producing epoxy chloropropane by utilizing micro-interface reaction |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1534030A (en) * | 2003-03-28 | 2004-10-06 | 中国石油化工股份有限公司 | Production method of epoxy chloropropane |
| CN1900071A (en) * | 2005-07-21 | 2007-01-24 | 中国科学院大连化学物理研究所 | Process for preparing epoxy chloropropane |
| CN101205220A (en) * | 2006-12-22 | 2008-06-25 | 中国科学院大连化学物理研究所 | Preparation method of methyl epichlorohydrin |
| CN101279961A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for preparing epoxy chloropropane by epoxidation of propylene chloride |
-
2010
- 2010-10-27 CN CN2010105212380A patent/CN102101848A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1534030A (en) * | 2003-03-28 | 2004-10-06 | 中国石油化工股份有限公司 | Production method of epoxy chloropropane |
| CN1900071A (en) * | 2005-07-21 | 2007-01-24 | 中国科学院大连化学物理研究所 | Process for preparing epoxy chloropropane |
| CN101205220A (en) * | 2006-12-22 | 2008-06-25 | 中国科学院大连化学物理研究所 | Preparation method of methyl epichlorohydrin |
| CN101279961A (en) * | 2007-04-04 | 2008-10-08 | 中国石油化工股份有限公司 | Method for preparing epoxy chloropropane by epoxidation of propylene chloride |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557787A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Method for preparing epoxy chloropropane |
| CN104557787B (en) * | 2013-10-28 | 2017-04-19 | 中国石油化工股份有限公司 | Method for preparing epoxy chloropropane |
| CN116514741A (en) * | 2023-07-04 | 2023-08-01 | 山东民基新材料科技有限公司 | Process for producing epoxy chloropropane by utilizing micro-interface reaction |
| CN116514741B (en) * | 2023-07-04 | 2023-09-26 | 山东民基新材料科技有限公司 | Process for producing epoxy chloropropane by utilizing micro-interface reaction |
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Application publication date: 20110622 |