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Preparation method of methyl epichlorohydrin

A technology of methyl epichlorohydrin and methyl chloropropene is applied in the field of preparation of methyl epichlorohydrin, which can solve the problems of low route economy, inability to look back on catalysts and the like

Inactive Publication Date: 2008-06-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Recently, a Japanese patent (JP05170,754) reported that using heteropolyacid as catalyst and hydrogen peroxide as oxygen source, in the system where toluene was used as solvent, a good result of 100% conversion rate and 92% selectivity was obtained. , but the catalyst cannot be turned back, and the economics of the route are not high. Therefore, it is very important to develop an environmentally friendly, economically reasonable synthetic route for methyl epichlorohydrin

Method used

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  • Preparation method of methyl epichlorohydrin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In the 50mL jacketed reaction flask, add 10g 30% hydrogen peroxide aqueous solution, the catalyst of 0.4g [(n-C 8 h 17 ) 4 N] 3 (PO 4 )(MoO 3 ) 4 ], add 15.7g methyl chloride propene,,, at 65 ℃, after reacting for 2 hours, the conversion ratio of methyl chloride propene is 49.0%, and the selectivity of methyl epichlorohydrin is 92%. At this time, the catalyst is precipitated from the reaction system, and the catalyst is recovered after centrifugation.

Embodiment 2

[0015] In the 50mL jacketed reaction flask, add 10g 30% hydrogen peroxide aqueous solution, the catalyst of 0.4g [(C 2 h 5 ) 3 NCH 2 pH] 2 H(PO 4 ) (WO 3 ) 2.54 ], add 15.7g methyl chloride propene, 15 milliliters of chloroform, after vigorous stirring at 55 ℃ for 4 hours, the conversion rate of methyl chloride propene is 49.0%, and the selectivity of methyl epichlorohydrin is 95%. At this time, the catalyst is precipitated from the reaction system, and the catalyst is recovered after centrifugation.

Embodiment 3

[0017] In the 50mL jacketed reaction flask, add 10g 30% hydrogen peroxide aqueous solution, the catalyst of 0.8g [(n-C 4 h 9 ) 4 N] 3 (PV 2 o 16 ], add 15.7g methyl chloride propene, 15 milliliters of chloroform, after vigorous stirring at 45 ℃ for 5 hours, the conversion rate of methyl chloride propene is 47.0%, and the selectivity of methyl epichlorohydrin is 95%. At this time, the catalyst is precipitated from the reaction system, and the catalyst is recovered after centrifugation.

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Abstract

The invention relates to novel method for obtaining a methyl epichlorohydrin transferring the catalyst of epoxidation by using a Methallyl Chloride. The catalyst does not dissolve into a reaction medium, but under the effect of the hydrogen peroxide, the catalyst can dissolve into active species and further react with the Methallyl Chloride, thus leading to an epoxidation reaction under high selectivity. The Methallyl Chloride has a conversion rate of 96 percent for hydrogen peroxide, and the methyl epichlorohydrin has a selectivity of 95 percent for the Methallyl Chloride. When the hydrogen peroxide is fully consumed, the catalyst is precipated from the reaction system. Through a simple separation, the catalyst can be recycled and reused again. The separation of the catalyst, compared with the multi-phase catalyst, fully presents the characteristics of the even-phase catalyst in the reaction process. The invention has the advantages of easy recycling and simple reaction system. The product is a single methyl epichlorohydrin which is environmentally-friendly and has a low cost which meets the request for economical technology; therefore the invention is a novel method which is suitable for lager-scale industrial production of the methyl epichlorohydrin.

Description

technical field [0001] The invention relates to a method for preparing methyl epichlorohydrin. The methyl epichlorohydrin is prepared by directly oxidizing methyl chloride propene with a heteropolyacid salt compound as a catalyst and hydrogen peroxide as an oxygen source. The by-product of the reaction is only water, and the catalyst It can be recycled and reused, the technical route is clean and simple, and it is suitable for industrial applications. Background technique [0002] Methyl epichlorohydrin is an important organic chemical raw material and intermediate with a wide range of uses. Around the 1970s, the United States, Japan and many countries in Europe successively developed this product. The hypochlorous acidification and saponification production process they adopt will produce a large amount of three wastes in the production process, causing environmental pollution, and the yield of the product is very low, so there is no large-scale industrial production so fa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/08B01J31/02
CPCY02P20/584
Inventor 高爽赵公大奚祖威
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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