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Allyl chloride epoxidation method for preparing epichlorohydrin

A technology of epichlorohydrin and chloropropene, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of low yield of epoxides, improve product selectivity, ease thermal effects, eliminate Acid effect

Active Publication Date: 2012-10-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because titanium-silicon molecular sieves can only show high catalytic activity in the reaction system with strong polar compounds such as alcohols as the solvent, and the surface acidity of the catalyst will cause the product epoxide to undergo a catalytic ring-opening reaction to generate by-product ethers, making the ring The selectivity of oxides is only about 85%, and the yield of epoxides is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In the polymerization kettle, add 7.5g of titanium-silicon molecular sieve powder, 90g of polymerized monomer styrene and 30g of divinylbenzene, pore-forming agent liquid wax (C 9-11 Normal alkanes) 60g, after stirring and mixing evenly, when the temperature of the water bath was raised to 60°C, 1.5g of initiator benzoyl peroxide was added, and the reaction temperature was polymerized at 90°C for 6 hours to obtain a block titanium silicon molecular sieve catalyst. Then carry out crushing and granulation, the catalyst obtained after sieving through Taylor standard sieve with 8~9 mesh, add 1,2-dichloroethane to swell, wherein the volume ratio of 1,2-dichloroethane to catalyst is 5:1, swelling at room temperature for 5 hours. After pouring out 1,2-dichloroethane, add ethyl acetate for solvent extraction, wherein the volume ratio of ethyl acetate to catalyst is 3:1, the extraction reaction temperature is 55°C, and the extraction time is 4 hours. The method carried out thre...

Embodiment 2

[0045] In the polymerization kettle, add 15g of titanium-silicon molecular sieve powder, 90g of polymerized monomer styrene, 15g of divinyltoluene, 25g of divinylxylene, and pore-forming agent C 5 60g of aliphatic alcohol, stirred and mixed evenly, when the temperature of the water bath was raised to 80°C, 2.0g of initiator azobisisobutanol was added, and the reaction temperature was polymerized at 100°C for 6 hours to obtain a block titanium silicon molecular sieve catalyst. Then carry out crushing and granulation, the catalyst obtained after sieving through Taylor standard sieve with 8~9 mesh, add 1,2-dichloroethane to swell, wherein the volume ratio of 1,2-dichloroethane to catalyst is 5:1, swelling at room temperature for 5 hours. After pouring out 1,2-dichloroethane, add xylene for solvent extraction, wherein the volume ratio of xylene to catalyst is 3:1, the extraction reaction temperature is 55°C, and the extraction time is 4 hours, and the same method is carried out E...

Embodiment 3

[0047] Change the weight of the titanium-silicon molecular sieve powder in Example 1 to 30g, and the treatment time in the tubular roaster is 48 hours. The rest are the same as in Example 1 to obtain a titanium-silicon molecular sieve and resin composite modified catalyst C, whose physicochemical properties are shown in Table 1 .

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PUM

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Abstract

The invention discloses an allyl chloride epoxidation method for preparing epichlorohydrin. According to the invention, under the existence of a titanium silicon molecular sieve and resin composite modified catalyst, with alcohol as a solvent, allyl chloride and hydrogen peroxide are subjected to an epoxidation reaction, such that epichlorohydrin is produced. According to the invention, a fixed bed reaction manner is adopted, such that a problem of separation difficulty of titanium silicon catalyst powder and a reaction liquid of a traditional slurry reactor is solved. The reaction efficiency is improved. Also, with the modification upon the catalyst, a ring-opening side reaction of the epoxide is eliminated, and product selectivity is improved.

Description

technical field [0001] The invention belongs to a method for the epoxidation of allyl chloride, in particular to a method for preparing epichlorohydrin through the epoxidation of allyl chloride in a fixed bed. Background technique [0002] Since Italy Enichem first synthesized titanium-silicon molecular sieve catalyst TS-1 in 1983, it has become a hotspot in the research of oxidation catalysts due to its excellent oxidation selectivity and mild reaction conditions. This discovery is regarded as a major milestone in the development of environmentally friendly catalysts. breakthrough. [0003] Titanium-silicon molecular sieve catalysts play a very important role in the selective oxidation of organic compounds, such as the epoxidation of propylene with hydrogen peroxide under the action of titanium-silicon molecular sieve catalysts to prepare propylene oxide. In industrial applications, titanium-silicon molecular sieve catalysts exhibit excellent shape-selective catalytic perf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/12B01J31/06
Inventor 王海波黎元生勾连科宋丽芝薛冬
Owner CHINA PETROLEUM & CHEM CORP
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