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Preparation method of epoxy chloropropane

A technology of epichlorohydrin and chlorinated liquid, which is applied in the direction of organic chemistry, can solve the problems of high requirements for process equipment, complex synthesis process, and large amount of three wastes, and achieve the advantages of small usage, high output, and short reaction time Effect

Active Publication Date: 2021-08-10
JIANGSU RUIHENG NEW MATERIAL TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a method for synthesizing epichlorohydrin by a one-step method in view of the shortcomings of the existing glycerol method, such as complex synthesis process, large amount of three wastes, and high requirements for process equipment

Method used

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  • Preparation method of epoxy chloropropane
  • Preparation method of epoxy chloropropane
  • Preparation method of epoxy chloropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Put SO4 into the autoclave 2- / TIO 2 Type solid superacid 3.75g and glycerin 750g (feeding coefficient 0.6), with N 2 Replace the air in the autoclave, stir, heat, control the reaction temperature at 170°C, pass hydrogen chloride gas into the autoclave through the gas cylinder, remove the heat of reaction through cooling water, maintain the reaction temperature, and keep the reaction pressure at 2.5MPa, and the reaction time is 15 minutes , to obtain chlorinated solution; after the reaction is completed, cool down to normal temperature, and use N 2 Bubble and purge the chlorinated liquid to remove the excess hydrogen chloride gas in the kettle to the water absorption system; open the kettle, put the chlorinated liquid into the crude distillation device, carry out negative pressure distillation, and control the vacuum degree to -0.085MPa~-0.1MPa, Control the temperature of the kettle not to exceed 100°C, pour the crude fraction into the separatory funnel for stratifica...

Embodiment 1～2

[0035] In order to investigate the impact of different solid superacids on the reaction, different types of solid superacids and mixed solid superacids were used in the reaction to carry out experiments, and all the other conditions were constant. The data are shown in Table 1:

[0036] Table 1

[0037] Example catalyst Product content (%) Yield (%) 1 SO4 2- / TIO 2 type solid superacid

[0038] As can be seen from Table 1, compared with the blank experiment example 2, the solid superacid has a catalytic effect on this reaction, and can greatly improve the product content and yield.

Embodiment 3～8

[0040] In order to investigate the impact of the ratio of solid superacid and glycerol on the reaction, with respect to Example 1, change SO4 2- / TIO 2 The consumption of type solid superacid is tested, and all the other conditions are constant, and data are as shown in table 2:

[0041] Table 2

[0042]

[0043] As can be seen from Table 2, solid superacid: glycerol=0.001~0.01, all have catalytic effect, wherein solid superacid: glycerol=0.002~0.008 effect is better, solid superacid: glycerol=0.003~0.006 effect is particularly good.

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Abstract

The invention provides a preparation method of epoxy chloropropane. The solid superacid is used as the catalyst to perform chlorination reaction, so that the epoxy chloropropane is synthesized by hydrogen chloride and glycerol in one step, and a large amount of salt-containing wastewater generated by a chlorination and saponification two-step method in an original synthesis route is avoided; the reaction route provided by the invention is short in reaction time and high in yield, and a larger production task can be completed by using a relatively small device; the catalyst used in the invention is not easy to esterify with glycerol, the pipeline is not blocked in the reaction process, and the production device can operate stably; in addition, the catalyst adopted in the reaction route is easy to obtain, small in usage amount and capable of being recycled; and the preparation method of epichlorohydrin has the advantages of green and environment-friendly reaction route, conventional raw materials, no generation of difficult-to-treat wastes, low equipment operation cost and suitability for popularization and application.

Description

technical field [0001] The invention relates to a production technology of a chemical intermediate, in particular to a preparation method of epichlorohydrin. Background technique [0002] Epichlorohydrin (ECH) is an organic compound, the main purpose is to make epoxy resin, the current production methods of epichlorohydrin include chlorohydrin method, glycerin method, propylene acetate method and DECH method, glycerol method Due to the advantages of short process, low consumption and less investment, the production has developed rapidly in China in recent years. Companies such as Jiangsu Yangnong, Yihai Kerry, and Dongying Hebang have already successfully operated glycerin-based projects. [0003] There are deficiencies in the existing glycerin production process: ①A two-step method is used for preparation, using hydrogen chloride and alkali as raw materials, acid-base neutralization results in a large amount of high-salt wastewater, which needs to be treated separately; ②C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/02C07D301/32
CPCC07D303/08C07D301/02C07D301/32
Inventor 吴翔史雪芳马勇沈杰田宇侯申础王奇孟宪跃胡凯宋佳滕彦虎
Owner JIANGSU RUIHENG NEW MATERIAL TECH CO LTD
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