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Method for preparing epoxy chloropropane by using hydrochloric acid water solution of dichlorohydrin

A technology of dichloropropanol hydrochloric acid and epichlorohydrin, which is applied in the direction of organic chemistry and the like, can solve the problems of increased energy consumption, difficult treatment of organic wastewater, and many separation steps, so as to reduce the cost of wastewater treatment, be easy to recycle, shorten the The effect of the separation process

Inactive Publication Date: 2011-04-13
SHANGHAI CHLOR ALKALI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can recover hydrochloric acid and greatly reduce the discharge of waste water, it has many separation steps, increases energy consumption, and cannot solve the problem of saline organic waste water produced in the saponification process. The salty organic waste water produced per ton of product about 4 tons
[0007] In a word, no matter the dichloropropanol hydrochloric acid solution obtained by the propylene method or the glycerin method is generally directly saponified or purified and then saponified, but the saponification reaction is carried out in a low-concentration aqueous phase solution. This method will not only waste a lot of water, resulting in a large amount of wastewater, and because the organic wastewater contains salt, not only the inorganic chloride is not easy to recycle, but also the organic wastewater containing salt is difficult to treat

Method used

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  • Method for preparing epoxy chloropropane by using hydrochloric acid water solution of dichlorohydrin
  • Method for preparing epoxy chloropropane by using hydrochloric acid water solution of dichlorohydrin

Examples

Experimental program
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Effect test

Embodiment 1

[0032] In the dichloropropanol hydrochloric acid solution, the weight concentration of dichloropropanol is 45.2%, the weight content of monochloroglycerin is 0.3%, the weight content of hydrochloric acid is 23.2%, and the balance is water;

[0033] Dichloropropanol hydrochloric acid solution 500g, under normal temperature conditions, with n-butyl ether as extractant, adopt separatory funnel to carry out 3 times of cross-flow extraction to dichloropropanol hydrochloric acid aqueous solution, n-butyl ether consumption is 500g, extract each time The final oil phase was collected to obtain 712 g of the extract phase, and the extraction yield of dichloropropanol was 86.9%.

[0034] The 712g extraction phase obtained above and 93g sodium hydroxide (98.5%, weight, the same below) are stirred and mixed in a reactor, and heated to 50°C to start the reaction, and the temperature of the reaction is controlled to be no higher than 100°C. Azeotropic distillation was carried out, and the or...

Embodiment 2

[0038] In the dichloropropanol hydrochloric acid solution, the weight concentration of dichloropropanol is 30%, the weight content of monochloroglycerin is 0%, the weight content of hydrochloric acid is 15%, and the balance is water;

[0039] Dichloropropanol hydrochloric acid solution 500g, under normal temperature conditions, with n-butyl ether as extractant, adopt separatory funnel to carry out 5 times of cross-flow extraction to dichloropropanol hydrochloric acid aqueous solution, n-butyl ether consumption is 1000g, extract each time The final oil phase was collected to obtain 1138 g of the extract phase, and the extraction yield of dichloropropanol was 96.4%.

[0040] The above obtained extract phase and 90g potassium hydroxide (95.0%) were stirred and mixed in a reactor, and heated to 100° C. for the reaction. Other conditions were the same as in Example 1. After 2.5 hours, the reaction was completed, and the distilled water phase was 30 g. Filter to obtain potassium chl...

Embodiment 3

[0042] In the dichloropropanol hydrochloric acid solution, the weight concentration of dichloropropanol is 40%, the weight content of monochloroglycerol is 0.5%, the weight content of hydrochloric acid is 20%, and the balance is water;

[0043]Dichloropropanol hydrochloric acid solution 500g, under normal temperature conditions, with n-octanol as extractant, adopt separatory funnel to carry out 3 times of cross flow extraction to dichloropropanol hydrochloric acid aqueous solution, n-octanol consumption is 600g, extract each time The final oil phase was collected to obtain 841 g of the extract phase, and the extraction yield of dichloropropanol was 97.1%.

[0044] Stir and mix the above-obtained extract phase with 110 g of sodium hydroxide in a reactor, heat to 95° C. for reaction, and control the reaction temperature not higher than 150° C., other conditions are the same as in Example 1, and 43 g of the distilled water phase is obtained after the reaction. After the liquid in...

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Abstract

The invention discloses a method for preparing epichlorohydrin by dichloropropanol hydrochloric acid aqueous solution. The method comprises the following steps: extracting the dichloropropanol hydrochloric acid aqueous solution by an organic solvent, collecting an extract phase, allowing saponification reaction between the extract phase and alkali, simultaneously distilling to remove water, ending the reaction when no water is generated, filtering to remove the generated salt, collecting filtrate, separating by a rectification method to obtain the epichlorohydrin. The method has the advantages of small wastewater discharge, easy recovery of inorganic chloride and a reaction solvent, shortened separation process of the dichloropropanol hydrochloric acid aqueous solution, and reduced energyconsumption.

Description

technical field [0001] The present invention relates to the preparation method of epichlorohydrin. Background technique [0002] Epichlorohydrin (ECH), also known as epichlorohydrin, is an important organic chemical raw material and fine chemical product, mainly used in the production of epoxy resins in the fields of coatings, composite materials, electronic appliances, and adhesives. In addition, it can also be used in various products such as surfactants, dyes, medicines, pesticides, ion exchange resins, glycidyl derivatives, and chlorohydrin rubber. [0003] At present, there are three industrialized epichlorohydrin production processes: propylene high-temperature chlorination method, propylene acetate method and glycerin method. Regardless of the process method, dichloropropanol is the key intermediate in the production process. Although the composition of dichloropropanol obtained by different processes is quite different, it will produce a homogeneous solution of dich...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/08C07D301/26
Inventor 马斌全陈斌武袁茂全沈帅朱莉
Owner SHANGHAI CHLOR ALKALI CHEM