Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing epoxy chloropropane

A technology of epichlorohydrin and chloropropene, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of low selectivity of hydrogen peroxide epoxidation, peroxidation Low hydrogen conversion rate and other problems, to achieve the effect of improving hydrogen peroxide conversion rate and good hydrophobicity

Active Publication Date: 2012-05-23
CHINA PETROLEUM & CHEM CORP +1
View PDF6 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is the low conversion rate of hydrogen peroxide and the low selectivity of hydrogen peroxide epoxidation when producing epichlorohydrin in the prior art, and a new method for preparing epichlorohydrin is provided

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Silica sol (40% by weight), bis(triethoxysilyl)methane, TiCl 4 , tetrapropylammonium hydroxide, ammoniacal liquor and water are mixed uniformly according to the stoichiometric ratio, wherein the molar ratio of each component of the raw material is inorganic silicon source: organic silicon source: titanium source: organic templating agent: basic compound: water=1: 0.01 :0.01:0.03:0.4:20. Crystallize at 160° C. for 1 day, and the product is filtered, washed with water, and dried to obtain MFI titanium-silicon molecular sieves containing skeleton organic groups.

[0012] In a 250 ml three-necked flask, add 0.2 g of the above synthesized organic silicon titanium silicon molecular sieve catalyst, 20 g of methanol solvent, and 5 g of chloropropene, heat up to 50 ° C, and then add 3 g of 30% H 2 o 2 The solution was reacted under stirring conditions for 1 hour, and after the reaction was completed, the three-neck flask was cooled to 7° C. with ice water. Finally, the molecu...

Embodiment 2

[0014] Solid silica (2000 mesh), bis(triethoxysilyl)methane, TiCl 3 , tetrapropylammonium bromide, ethylamine and water are mixed uniformly by stoichiometric ratio, wherein the molar ratio of each component of the raw material is inorganic silicon source: organic silicon source: titanium source: organic templating agent: basic compound: water=1: 0.05:0.03:0.15:2.0:100. It was crystallized at 170°C for 5 days, and the product was filtered, washed with water and dried to obtain MFI titanium silicon molecular sieves containing skeleton organic groups.

[0015] In a 250 ml three-necked flask, add 0.1 g of the above-mentioned synthesized catalyst containing organosilicon-titanium-silicon molecular sieve, 10 g of 3-chloropropene, raise the temperature to 40° C., and then add 3 g of H with a mass fraction of 30%. 2 o 2 The solution was reacted for 2 hours under stirring conditions, and after the reaction was completed, the three-neck flask was cooled to 7° C. with ice water. Final...

Embodiment 3

[0017] Ethyl orthosilicate, bis(triethoxysilyl)methane, TiOCl 2 , Tetrabutylammonium hydroxide, n-propylamine and water are mixed uniformly in a stoichiometric ratio, wherein the molar ratio of each component of the raw material is inorganic silicon source: organic silicon source: titanium source: organic templating agent: basic compound: water=1: 0.03: 0.02:0.09:1.2:60. Crystallize at 180°C for 10 days, and the product is filtered, washed with water, and dried to obtain an MFI titanium-silicon molecular sieve containing a skeleton organic group.

[0018] Add 0.4 g of the organosilicon-titanium-silicon molecular sieve catalyst synthesized above, 40 g of ethanol solvent, and 20 g of 2-methyl-3-chloropropene into a 250 ml three-necked flask, heat up to 60° C., and then add 3 g of a mass fraction of 30 %H 2 o 2 The solution was reacted under stirring conditions for 3 hours, and after the reaction was completed, the three-neck flask was cooled to 7° C. with ice water. Finally,...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a method for preparing epoxy chloropropane. The problems of low conversion rate and low epoxidation selectivity of hydrogen peroxide when the epoxy chloropropane is produced in the prior art are solved. The hydrogen peroxide and chloropropene serve as raw materials, and under the condition that: the reaction temperature is 40 to 90 DEG C, the weight ratio between the hydrogen peroxide and the chloropropene is 0.02 to 0.2, and the weight ratio between a catalyst and the hydrogen peroxide is 0.1 to 1.2, the hydrogen peroxide and the chloropropene are reacted for 1 to 5 hours. The preparation method for the catalyst comprises the following steps of: mixing an inorganic silicon source, an organic silicon source, a titanium source, an organic template agent, an alkali compound and water; and after crystallizing the mixture for 1 to 30 days at 160 to 220 DEG C, and filtering, washing and drying the crystal to obtain the catalyst. The problems are better solved through the technical scheme and the method can be applied to the industrial production of the epoxy chloropropane.

Description

technical field [0001] The invention relates to a method for preparing epichlorohydrin. Background technique [0002] The industrialized production technologies of epichlorohydrin include chloropropene method and propylene acetate method. The former is a classic method of industrial production, accounting for more than 90% of the total global ECH production capacity; while the latter is only adopted by a few companies. The high-temperature chlorination of propylene was successfully developed and applied to industrial production for the first time in 1948 by Shell Company. The process mainly includes three reaction units: high-temperature chlorination of propylene to produce allyl chloride, hypochlorination of allyl chloride to synthesize dichloropropanol, and saponification of dichloropropanol to synthesize epichlorohydrin. The high-temperature chlorination of propylene is characterized by flexible production process, mature technology and stable operation. In addition to ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/12B01J31/38
Inventor 何欣高焕新刘志成李宏旭
Owner CHINA PETROLEUM & CHEM CORP