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Method for preparing epoxy chloropropane by using novel catalyst

A technology for epichlorohydrin and a catalyst is applied in the field of preparing epichlorohydrin by using a novel catalyst, which can solve the problems of low selectivity of allyl chloride, low yield of epichlorohydrin and the like, and achieve the effects of improving catalytic performance and eliminating acidity

Inactive Publication Date: 2017-06-06
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] What the present invention is to solve is the problem of low selectivity of chloropropene and low yield of epichlorohydrin in the process of producing epichlorohydrin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Dissolve 9.8 kg TPABr in water, then add it into silica sol and stir vigorously to obtain liquid A, take 0.95 kg tetrabutyl titanate and add 10 L isopropanol and stir to obtain liquid B, and add B dropwise into liquid A under vigorous stirring, Then stir vigorously for 1 h, evaporate the alcohol at 80 °C for 3 h, add ammonia water and stir, then transfer to the reaction kettle. Crystallized at 150 °C for 3 days, the obtained product was filtered and washed, dried at 110 °C, and calcined at 540 °C for 5 h to obtain solid powder TS. Take 9 kg of nitric acid (mass fraction=5%), 0.1 kg of solid powder TS, 0.05 kg of HAuCl 4 In a reactor, it was modified at 170 °C for 24 h, then washed by centrifugation, dried at 110 °C, and calcined at 500 °C for 10 h to obtain the Au-TS catalyst.

[0015] Take 2 kg of chloropropene, 0.05 kg of Au-TS catalyst, 0.5 kg of 30% hydrogen peroxide and 10 L of methanol in a 25 L reactor, react in a homogeneous reactor at 80 °C for 2 h, and then t...

Embodiment 2

[0017] Dissolve 9.8 kg TPABr in water, then add it into silica sol and stir vigorously to obtain liquid A, take 0.95 kg tetrabutyl titanate and add 10 L isopropanol and stir to obtain liquid B, and add B dropwise into liquid A under vigorous stirring, Then stir vigorously for 1 h, evaporate the alcohol at 80 °C for 3 h, add ammonia water and stir, then transfer to the reaction kettle. Crystallized at 150 °C for 3 days, the obtained product was filtered and washed, dried at 110 °C, and calcined at 540 °C for 5 h to obtain solid powder TS. Take 10 kg nitric acid (mass fraction=5%), 0.1 kg solid powder TS, 0.07 kgAgNO 3 In a reactor, it was modified at 160 °C for 40 h, then washed by centrifugation, dried at 110 °C, and calcined at 450 °C for 12 h to obtain the Ag-TS catalyst.

[0018] Take 1 kg of chloropropene, 0.05 kg of Ag-TS catalyst, 0.3 kg of 30% hydrogen peroxide and 10 L of methanol in a 25 L reactor, react in a homogeneous reactor at 80 °C for 2 h, and then take it out...

Embodiment 3

[0020] Dissolve 9.8 kg TPABr in water, then add it into silica sol and stir vigorously to obtain liquid A, take 0.95 kg tetrabutyl titanate and add 10 L of isopropanol and stir to obtain liquid B, and add B dropwise into liquid A under vigorous stirring, Then stir vigorously for 1 h, evaporate the alcohol at 80 °C for 3 h, add ammonia water and stir, then transfer to the reaction kettle. Crystallized at 150 °C for 3 days, the obtained product was filtered and washed, dried at 110 °C, and calcined at 540 °C for 5 h to obtain solid powder TS. Take 8.5 kg nitric acid (mass fraction=5%), 0.1 kg solid powder TS, 0.02 kg Ce(NO 3 ) 3 In a reactor, it was modified at 160 °C for 24 h, then washed by centrifugation, dried at 110 °C, and calcined at 550 °C for 10 h to obtain the Ce-TS catalyst.

[0021] Take 2 kg of chloropropene, 0.05 kg of Ce-TS catalyst, 0.7 kg of 30% hydrogen peroxide and 10 L of methanol in a 25 L reactor, react in a homogeneous reactor at 70 °C for 2 h, and then ...

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Abstract

The invention relates to a method for preparing epoxy chloropropane by using a novel catalyst, mainly aiming at solving the problems that in a preparation process of the epoxy chloropropane, the selectivity of chloropropene is low, and the yield of the epoxy chloropropane is low. The epoxy chloropropane is prepared by using chloropropene and hydrogen peroxide as reaction raw materials, the mass ratio of the hydrogen peroxide to the chloropropene is within a range of (1 to 5)-(1 to 20), the mass ratio of the catalyst to the chloropropene is within a range of (1 to 15)-(1 to 100), the reaction temperature is 35-100 DEG C, and the reaction time is 1.5-3.5h. The novel catalyst can obviously improve the selectivity of the chloropropene and the yield of the epoxy chloropropane, so that the problems are better solved. The method can be used in industrial production of the epoxy chloropropane.

Description

technical field [0001] The invention relates to a method for preparing epichlorohydrin by catalyzing the epoxidation of chloropropene with a novel catalyst. Background technique [0002] Epichlorohydrin is an important fine chemical product and organic chemical raw material. Its application range is very wide. It is mainly used in the production of epoxy resin. The epoxy resin synthesized by epichlorohydrin has strong adhesion and corrosion resistance to chemical media. , good chemical stability, widely used in coatings and adhesives. Epichlorohydrin is also used in the synthesis of various products such as glycerin, glass fiber reinforced plastics, electrical insulation products, templating agents, medicine, nitroglycerin explosives, and chlorohydrin rubber. The development and utilization prospects are very broad. Due to the wide range of uses of epichlorohydrin, the supply exceeds demand, and the global production capacity has increased sharply. The production capacity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/08B01J29/89
CPCC07D301/12B01J29/89C07D303/08
Inventor 孙国新汉吉勋张真真
Owner UNIV OF JINAN
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