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Method for continuously producing epoxy chloropropane

A technology of epichlorohydrin and chloropropene, applied in chemical recovery, organic chemistry, etc., can solve the problems of difficult separation catalysts, achieve the effect of solving separation difficulties, realizing automatic separation, and reducing losses

Active Publication Date: 2010-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the difficulty of separating the original powder catalyst of titanium-silicon molecular sieve from the liquid product and the shortcomings of frequently regenerating the catalyst, and provide a method for continuously and stably producing epichlorohydrin in a fixed-bed reactor for a long period of time

Method used

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  • Method for continuously producing epoxy chloropropane
  • Method for continuously producing epoxy chloropropane
  • Method for continuously producing epoxy chloropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] In the embodiment, the titanium-silicon molecular sieve catalyst used is extruded TS-1 catalyst, shaped according to the method disclosed in CN200710120615.8, and the mass fraction of TS-1 in the shaped catalyst is 60%. TS-1 is produced by Hunan Jianchang Petrochemical Co., Ltd., the brand is HTS; chloropropene is industrial chloropropene, the mass content of 3-chloropropene is greater than 97%, and it is produced by Baling Petrochemical Co., Ltd.; hydrogen peroxide is As an analytically pure reagent, the mass content of hydrogen peroxide is 30%; methanol is an analytically pure reagent, and the mass content of methanol is greater than 99.5%.

[0059] The epoxidation reaction of 3-chloropropene and hydrogen peroxide was carried out in a jacketed tubular fixed-bed reactor, and the loading amount of the catalyst was 100 mL. The temperature of the reactor was regulated by an automatic thermostatic oil bath flowing through the reactor jacket. The pressure of the reactor wa...

Embodiment 2

[0076] Epichlorohydrin was produced in the same manner as in Example 1, except that ammonia was not added to the reaction raw materials, the temperature of the reactor jacket oil bath was kept constant at 60°C, and the reaction temperature rise did not exceed 10°C. The process and results of the continuous epoxidation reaction are shown in Table 3, and the accumulated continuous epoxidation reaction results are shown in Table 4.

[0077] table 3

[0078] Catalyst status

reactor

Reaction time / h

Regeneration time / h

X HPO / %

S ECH / %

fresh

1

165

0

98.6

94.4

fresh

2

173

0

98.8

94.1

first wash regenerated

1

115

16

98.2

94.6

first wash regenerated

2

119

16

98.2

93.9

second wash regenerated

1

102

16

97.9

94.2

second wash regenerated

2

90

16

98.1

94.6

third wa...

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Abstract

The invention relates to a method for continuously producing epoxy chloropropane, comprising the following steps: leading 3-chloropropene, hydrogen peroxide and solvent in a plurality of fixed bed reactors filled with titanium silicalite catalyst; enabling the 3-chloropropene and the hydrogen peroxide to carry out epoxidation; and stopping epoxidation in at least one fixed bed reactor and regenerating the catalyst therein, wherein when regeneration is carried out in any one of the reactors, at least one reactor in the rest reactors is in epoxidation. The method provided by the invention has the advantages of simplifying the separation process of the catalyst and the reaction products, realizing long-period continuous and stable operation in the production process of epoxy chloropropane, reducing the loss caused by equipment downtime, and having simple technology process and convenient process realization.

Description

technical field [0001] The present invention relates to a method for continuously producing epichlorohydrin, in particular, the present invention relates to a method for continuously producing epichlorohydrin through the epoxidation reaction of 3-chloropropene and hydrogen peroxide. Background technique [0002] Epichlorohydrin is a basic organic chemical raw material. The current production methods of epichlorohydrin include propylene high-temperature chlorination method and allyl acetate method. Since these two processes contain chlorohydrinization and saponification processes, there are serious environmental protection problems such as large wastewater discharge and difficult waste residue treatment. At the same time, there are also defects such as serious corrosion, many by-products, and high material consumption. It is urgent to develop clean and efficient epoxy resins. Chloropropane production technology. [0003] In the late 1980s, US4833260 disclosed a method for p...

Claims

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Application Information

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IPC IPC(8): C07D303/08C07D301/12
CPCY02P20/584
Inventor 张永强杜泽学刘易
Owner CHINA PETROLEUM & CHEM CORP
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