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Method for preparing epoxy chloropropane

A technology of epichlorohydrin and chloropropene, which is applied in the direction of organic chemistry, can solve the problem of catalyst activity reduction, achieve the effects of no activity reduction, easy recovery and recycling, and reduce production costs

Active Publication Date: 2012-05-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to overcome the problem of catalyst activity reduction in the above-mentioned epoxy system, and provide a new process for preparing epichlorohydrin from propylene chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 200g purity is 98% allyl chloride (ALC), 12g catalyst [(C 16 h 33 )N(CH 3 ) 3 ] 3 PW 4 o 16 and 2g additive [(C 16 h 33 )N(CH 3 ) 3 ] 3 PO 4 Put it into a 500mL glass reactor, raise the temperature to 65°C, and slowly pump in 68g of 50% H 2 o 2After the addition, continue to react at this temperature for 3 hours, cool with ice water, separate the liquid and solid, use the solid catalyst for the next reaction, separate the oil phase from the liquid, and perform gas chromatography analysis to obtain the yield and selectivity of epichlorohydrin . The step of reclaiming catalyst and reacting is the same as above, carries out altogether 10 times of reaction results and is shown in Table 1.

[0025] Table 1

[0026] Responses

[0027] Visible by table 1, additive [(C 16 h 33 )N(CH 3 ) 3 ] 3 PO 4 Adding can improve the stability of catalyst, and the yield of epichlorohydrin is maintained at about 87% when catalyst is recycled 9 times (10 times of...

Embodiment 2

[0029] 200g purity is 98% allyl chloride (ALC), 8g catalyst [(C 12 h 25 )N(CH 3 ) 3 ] 3 PW 4 o 16 and 1g additive [(C 12 h 25 )N(CH 3 ) 3 ] 3 PO 4 Put it into a 500mL glass reactor, raise the temperature to 55°C, and slowly pump in 70g of 30% H 2 o 2 After the addition, continue to react at this temperature for 3 hours, cool with ice water, separate the liquid and solid, use the solid catalyst for the next reaction, separate the oil phase from the liquid, and perform gas chromatography analysis to obtain the yield and selectivity of epichlorohydrin . The step of reclaiming catalyst and carrying out reaction is the same as above, carries out altogether 8 times of reaction results and is shown in Table 2.

[0030] Table 2

[0031] Responses

[0032] It can be seen from Table 2 that the yield and the selectivity of epichlorohydrin are maintained at about 84% and 94% when the catalyst is recycled 7 times (reacted 8 times), without decreasing, and the stabi...

Embodiment 3

[0034] 300g purity is 98% allyl chloride (ALC), 10g catalyst [(C 18 h 37 )N(CH 3 ) 3 ] 3 PW 4 o 16 and 0.5g additive [(C 18 h 37 )N(CH 3 ) 3 ] 3 PO 4 Put it into a 500mL glass reactor, raise the temperature to 48°C, and slowly pump in 50g of 50% H 2 o 2 After the addition, continue to react at this temperature for 4h, cool with ice water, separate the liquid and solid, use the solid catalyst for the next reaction, separate the oil phase from the liquid, and perform gas chromatography analysis to obtain the yield and selectivity of epichlorohydrin . The step of reclaiming catalyst and carrying out reaction is the same as above, carries out altogether 15 times of reaction results and is shown in Table 3.

[0035] table 3

[0036] Responses

[0037] 10

[0038] It can be seen from Table 3 that the yield and selectivity of epichlorohydrin for 14 times of catalyst recycling (reaction 15 times) are maintained at about 83% and 94%, indicating that...

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PUM

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Abstract

The invention discloses a method for preparing epoxy chloropropane. The method comprises the following step of: oxidizing chloropropene by using a phosphotungstic acid quaternary ammonium salt, a phosphoric acid quaternary ammonium salt and hydrogen peroxide under a solvent-free condition to generate the epoxy chloropropane.

Description

technical field [0001] The invention relates to the preparation of epichlorohydrin, in particular to a method for preparing epichlorohydrin by epoxidation of propylene chloride. Background technique [0002] Epichlorohydrin (ECH) is an important organic chemical raw material and intermediate, widely used in the production of epoxy resin and epichlorohydrin rubber. There are two processing routes for epichlorohydrin: chlorohydrin method and allyl acetate method. In the chlorohydrin method, propylene is chlorinated at high temperature to generate Allyl Chloride, which then reacts with aqueous chlorine solution to generate 1,3-dichloro-2-propanol, which is cyclized under the action of alkali solution to generate epichlorohydrin. One equivalent of epichlorohydrin is produced with one equivalent of CaCl 2 Into the water phase, this process is very serious to environmental pollution. The allyl acetate method is to first oxidize propylene in acetic acid to form allyl acetate, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/12
Inventor 高爽李军赵公大张毅吕迎张恒耘
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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