Process for preparing epoxy chloropropane

A technology of epichlorohydrin and chloropropene, applied in the direction of organic chemistry, can solve the problems of large calcium chloride-containing wastewater, environmental pollution, and unindustrialization

Inactive Publication Date: 2007-01-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0012] A common disadvantage of the chlorohydrin method and the propylene acetate method is that from dichloropropanol to epichlorohydrin must pass through a Ca(OH) 2 The process of dehydrochlorination brings a large amount of calcium chloride-containing wastewater, which seriously pollutes the environment
[Appl.Catal., 138,27(1996)] but because there is the cost problem of titanium silicon molecular sieve and needs to use a large amount of solvents, this method has not been industrialized so far

Method used

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  • Process for preparing epoxy chloropropane
  • Process for preparing epoxy chloropropane

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0029] Example 1. Epoxidation of allyl chloride:

[0030] Get 0.23g catalyzer (the total package is composed of {π-C 5 h 5 N + C 12 h 25} 3 {PMo 4 o 16} 3- ), 3.30gH 2 o 2 Solution (33.5wt%) was added with 10 g of allyl chloride, and reacted at 65° C. for 2 hours. Allyl chloride to H 2 o 2 The conversion rate was 92.7%, the epichlorohydrin selectivity was 92.2%, and the yield was 85.5%. The catalyst recovery rate was 99.8%.

example 2

[0031] Example 2. Epoxidation of allyl chloride

[0032] Take 0.38g catalyst {C 16 h 33 N + (CH 3 ) 3} 3 {PO 4 [WO(O 2 ) 2 ] 2 [WO(O 2 ) 2 (H 2 O)]} 3- , 0.02g potassium hydrogen phthalate, 2.50gH 2 o 2 solution (35.0wt%), add 10g of allyl chloride, and react at 65° C. for 2.5 hours. Allyl chloride to H 2 o 2 The conversion rate was 95%, the epichlorohydrin selectivity was 90%, and the yield was 85.5%. Centrifuge to recover the catalyst. After washing with toluene, dry it. Gained reclaimed catalyst can be recycled, and its reaction result is as table 1:

[0033] catalyst cycle

example 3

[0034] Example 3. Epoxidation of allyl chloride

[0035] Get 0.29g catalyzer (the total package is composed of {π-C 5 h 5 N + C 14 h 29} 3 {PW 3.75 h 0.5 o 15.5} 3- ), add 0.02gNaH 2 PO 4 / 0.02gNa 2 HPO 4 Mixed Phosphates, 1.65gH 2 o 2 Solution (33.5wt%) was added with 10 g of allyl chloride, and reacted at 45° C. for 3 hours. Allyl chloride to H 2 o 2 The conversion rate was 93.3%, the epichlorohydrin selectivity was 95.1%, and the yield was 88.7%. Centrifuge to recover the catalyst. After washing with allyl chloride, dry it. Gained recovery catalyst can be recycled, and its activity is shown in Table 2:

[0036] catalyst cycle

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Abstract

In the preparation of epoxy chloropropane, chloropropene is oxidized with H2O2 aqua as oxygen source in no solvent condition and under the action of heteropoly acid catalyst of phosphomolybdic acid or phosphotungestic acid to produce epoxy chloropropane, with the catalyst being recovered for reuse. The preparation process has mild reaction condition, high epoxy chloropropane yield, single product, high selectivity and no pollution, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a kind of method for preparing epichlorohydrin, specifically, relate to a kind of chloropropene under solvent-free condition with H 2 o 2 Solution catalyzed epoxidation method for preparing epichlorohydrin. Background technique [0002] Epichlorohydrin is an important petrochemical product, mainly used in the production of epoxy resin and synthetic glycerin. At present, there is a great demand for epichlorohydrin in my country, and the domestic production is seriously in short supply. [0003] At present, there are mainly two kinds of process routes for the epoxidation of chloropropene. One is the chlorohydrin method, which accounts for more than 90% of the output of epichlorohydrin. The process is mainly composed of 3 reaction units: [0004] ① High temperature chlorination of propylene to produce chloropropene; [0005] ②Allyl chloride is electrophilicly substituted by hypochlorous acid to generate dichloropropan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/12
Inventor 奚祖威李健高爽
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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