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Comprehensive utilization method of hydrogen-peroxide-process epichlorohydrin by-product

A technology of epichlorohydrin and by-products, which is applied in the field of comprehensive utilization of epichlorohydrin by-products in the hydrogen peroxide method, and can solve the problems of difficult processing and high cost

Active Publication Date: 2021-10-08
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

[0003] Since the hydrogen peroxide method generally uses methanol as a solvent, epichlorohydrin and methanol will react to generate 1-chloro-3-methoxy-2-propanol (2-CMP) and 3-chloro-2-methoxy in the production process. Base-1-propanol (1-CMP) two impurities, these two impurities are usually collectively referred to as by-products together with epichlorohydrin hydrolysis product 3-chloro-1,2-propanediol, and its main composition is 1-chloro- 3-methoxy-2-propanol 60~70%, 3-chloro-2-methoxy-1-propanol 10~20%, 3-chloro-1,2-propanediol 5~10%, the rest is Low polymer; often these by-products are disposed of as hazardous waste, which is difficult and costly due to the chlorine content of the components

Method used

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  • Comprehensive utilization method of hydrogen-peroxide-process epichlorohydrin by-product
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  • Comprehensive utilization method of hydrogen-peroxide-process epichlorohydrin by-product

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add epichlorohydrin by-product 200g in the 500ml reaction flask with desolventizer, (composition is 2-CMP 68%, 1-CMP 18%, 3-chloro-1,2-propanediol 9%, low polymer 5 %), be warming up to 75 DEG C, start stirring, continuously dropwise add 470g40% hydroiodic acid, control dropwise time at 3hr, continue to insulate at reaction temperature for 2hr after dropping, and the reaction process collects light components by precipitation device;

[0023] Dehydrate the above materials under negative pressure, vacuum control -0.1Mpa, and the kettle temperature does not exceed 80°C;

[0024] Packing TiO in a fixed bed 2 Type solid superacid catalyst, the dehydrated material is passed into the fixed bed under the protection of nitrogen, the reaction temperature is controlled at 170 °C, and the mass space velocity is 1h -1 ;

[0025] The reaction material of fixed bed is carried out negative pressure rectification, vacuum control-0.1Mpa, kettle temperature is no more than 110 ℃, colle...

Embodiment 2~5

[0034] Investigate the hydroiodic acid consumption, have carried out different parameter experiments, all the other conditions are identical with embodiment 1. The data is as follows:

[0035] Example Hydroiodic acid: CMP ECH content (%) Yield (%) 2 1.0 99.2 89.5 3 1.05 99.4 92.8 1 1.065 99.7 93.2 4 1.10 99.7 93.0 5 1.2 99.7 90.2

[0036] It can be seen from the above table that the best dosage of hydroiodic acid is between 1.05 and 1.1.

Embodiment 6~11

[0038] Investigate the influence of temperature of reaction in S1 on reaction, have carried out different parameter experiment, all the other conditions are identical with embodiment 1, and data are as follows:

[0039]

[0040]

[0041] It can be seen from the above table that the reaction temperature is 70-80°C.

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Abstract

The invention provides a comprehensive utilization method of a hydrogen-peroxide-process epichlorohydrin byproduct. The comprehensive utilization method comprises the following steps: subjecting hydriodic acid to reacting with 1-CMP and 2-CMP to convert 1-CMP and 2-CMP into 3-chloro-1,2-propanediol, recovering the byproduct iodomethane generated by the reaction through a desolventizing device, and carrying out negative-pressure dehydration to obtain a material with high content of 3-chloro-1,2-propanediol; and dehydrating 3-chloro-1,2-propanediol by using an oxide super solid acid in a fixed bed as a catalyst, converting 3-chloro-1,2-propanediol into epichlorohydrin, and carrying out negative-pressure rectification to obtain an epichlorohydrin product. According to the invention, 1-CMP and 2-CMP in by-products and the hydrolysis by-product 3-chloro-1,2-propanediol in the production process of epichlorohydrin are fully utilized in the whole reaction process; on one hand, the yield of the hydrogen-peroxide-process epichlorohydrin is improved and value is created; and on the other hand, the treatment amount of hazardous wastes is greatly reduced, cost is reduced, and the popularization of a hydrogen peroxide process for epichlorohydrin is facilitated.

Description

technical field [0001] The invention relates to a comprehensive utilization method of by-products of chemical products, in particular to the comprehensive utilization of epichlorohydrin by-products of the hydrogen peroxide method. Background technique [0002] Epichlorohydrin is a volatile and unstable colorless oily liquid, slightly soluble in water, mainly used in the manufacture of epoxy resins, and is also the main raw material for epoxy and phenoxy resins. At present, the production methods of epichlorohydrin include chlorohydrin method, glycerin method, and hydrogen peroxide method. The hydrogen peroxide method epichlorohydrin process uses hydrogen peroxide as the oxygen source, methanol as the solvent, and titanium silicon molecular sieve as the catalyst. Oxychloropropane, this process has high atomic utilization rate and less waste, and is a clean process encouraged by the state. [0003] Since the hydrogen peroxide method generally uses methanol as a solvent, epich...

Claims

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Application Information

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IPC IPC(8): C07D303/08C07D301/12C07D301/32
CPCC07D303/08C07D301/12C07D301/32
Inventor 史雪芳吴翔马勇沈杰田宇宋佳孟宪跃胡凯滕彦虎
Owner JIANGSU RUIHENG NEW MATERIAL TECH CO LTD
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