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Method for preparing epoxy chloropropane

A technology of epichlorohydrin and chloropropane, applied in the direction of organic chemistry and the like, can solve the problems of pollution, low catalyst use efficiency, etc., and achieve the effect of simple process, reduction of use cost and operation cost, and realization of convenience.

Inactive Publication Date: 2019-05-28
山东玉江源环保科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a novel method for preparing epichlorohydrin aiming at the problems of serious pollution and low catalyst use efficiency in the traditional production process of epichlorohydrin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1, first add 1 g of titanium-silicon molecular sieve catalyst with a particle size range of 2-50 microns, and simultaneously add 0.5 g of a mixture of ethylamine and dimethylamine with a mass ratio of 1:1, add 100 g of methanol, and then add 20 g of chloropropene Add 10g of hydrogen peroxide solution with a mass fraction of 10% into the reactor, control the rotation speed at 100 rpm, then raise the temperature to 50°C at a heating rate of 5°C / min, raise the pressure to 0.5MPa, and maintain this temperature and Reaction under pressure for 9h. Then cool down to room temperature, exhaust, and the solvent and catalyst are used for the next reaction. The solvent can be recycled by fractional distillation, and the catalyst can be recovered by filtration or evaporation.

Embodiment 2

[0018] Example 2, first add 5 g of titanium-silicon molecular sieve catalysts with a particle size range of 2-50 microns, and simultaneously add 0.5 g of a mixture of ethylamine and dimethylamine with a mass ratio of 1:2, add 200 g of methanol, and then add 50 g of chloropropene Add 10g of hydrogen peroxide solution with a mass fraction of 10% into the reactor, control the rotation speed at 200 rpm, then raise the temperature to 80°C at a heating rate of 8°C / min, raise the pressure to 1.5MPa, and maintain this temperature and Reaction under pressure for 5h. Then cool down to room temperature, exhaust, and the solvent and catalyst are used for the next reaction. The solvent can be recycled by fractional distillation, and the catalyst can be recovered by filtration or evaporation.

Embodiment 3

[0019] Example 3, first add 3 g of titanium-silicon molecular sieve catalysts with a particle size range of 2-50 microns, and simultaneously add 0.5 g of a mixture of ethylamine and dimethylamine with a mass ratio of 1:1, add 150 g of methanol, and then add 30 g of chloropropene Add 10g of hydrogen peroxide solution with a mass fraction of 10% into the reactor, control the rotation speed at 200 rpm, then raise the temperature to 70°C at a heating rate of 6°C / min, raise the pressure to 1.2MPa, and maintain this temperature and Reaction under pressure for 6h. Then cool down to room temperature, exhaust, and the solvent and catalyst are used for the next reaction. The solvent can be recycled by fractional distillation, and the catalyst can be recovered by filtration or evaporation.

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Abstract

The invention belongs to the technical field of epoxide preparation, and relates to a method for preparing epoxy chloropropane. The method comprises the following steps: that firstly, a catalyst and alkali are added into a reaction kettle, then a reaction raw material, an oxidizing agent and a solvent are added, the reaction temperature and the pressure are controlled for reaction, and after the reaction is finished, the solvent and filtered and concentrated catalyst slurry are added into the reaction kettle again for reaction, wherein the reaction raw material is chloropropene, the oxidizingagent is a hydrogen peroxide solution with the mass concentration of 10%, and the catalyst is titanium-silicon molecular sieve particles. Compared with the prior art, the method for producing the epoxy chloropropane has the advantages that under the premise of ensuring the reaction conversion rate and selectivity, by means of condition optimization and addition of alkali substances, the activity and the stability of the catalyst are greatly enhanced, and the use cost and the operation cost of the catalyst are remarkably lowered; and the technological process is simple, and implementation is convenient.

Description

technical field [0001] The invention belongs to the technical field of oxide preparation, and relates to a method for preparing epichlorohydrin. Background technique [0002] Because epichlorohydrin contains active epoxy groups and chlorine atoms in its molecules, its chemical properties are quite active, and it has become an important basic organic chemical raw material and intermediate, and is widely used in the synthesis of epoxy resin, glycerin, and alcohol rubber. , pharmaceuticals, pesticides, surfactants, FRP, ion exchange resins, coatings and plasticizers, etc. Epichlorohydrin is a basic organic chemical raw material. The current production methods of epichlorohydrin include propylene high-temperature chlorination method and allyl acetate method. Since these two processes contain chlorohydrinization and saponification processes, there are serious environmental protection problems such as large wastewater discharge and difficult waste residue treatment. At the same ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/12
Inventor 李正胡景华李玉江吴青伟李钉锐郭芳
Owner 山东玉江源环保科技股份有限公司
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