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Method for Purifying Cationic Etherifying Agent with Phosphate Ester Extractant

A technology of cationic etherification agent and phosphate esters, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of restricting sustainable development, difficult and difficult treatment of organic wastewater, etc., and achieve good use effect , less investment in equipment and easy operation

Inactive Publication Date: 2016-08-24
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the lower the impurity content in the waste water, the more difficult it is to treat. Therefore, it is difficult to treat the organic waste water produced by cationic etherification agent stripping method, and the cost is high. This is also a major technical bottleneck restricting the sustainable development of enterprises.

Method used

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  • Method for Purifying Cationic Etherifying Agent with Phosphate Ester Extractant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take trioctyl phosphate as an example to purify cationic etherification agent:

[0021] 1. Extraction

[0022] The content of epichlorohydrin in the crude product cationic etherification agent 3-chloro-2-hydroxypropyltrimethylammonium chloride is 1622mg kg -1 , the content of 1,3-dichloro-2-propanol is 18472mg·kg -1 . Extractant with V 粗产品 :V 萃取剂 =1:0.7 ratio, after one continuous extraction, the content of epichlorohydrin in the cationic etherification agent is 15mg·kg -1 , the content of 1,3-dichloro-2-propanol is 32mg·kg -1 ; After 2 consecutive extractions, the content of epichlorohydrin in the cationic etherification agent is 6 mg kg -1 , the content of 1,3-dichloro-2-propanol is 12mg·kg -1 .

[0023] 2. Regeneration

[0024] The regeneration conditions of trioctyl phosphate: the concentration is 7% NaOH aqueous solution, the temperature is 120 ° C, the regeneration time is 3 hours, after recycling 6 times, epichlorohydrin and 1,3-dichloro-2- Propanol con...

Embodiment 2

[0026] Take triisobutyl phosphate as the extraction agent to purify cationic etherification agent as an example:

[0027] 1. Extraction

[0028] The content of epichlorohydrin in the crude product cationic etherification agent 3-chloro-2-hydroxypropyltrimethylammonium chloride is 1622mg kg -1 , the content of 1,3-dichloro-2-propanol is 18472mg·kg -1 . Extractant with V 粗产品 :V 萃取剂 =1:0.8 ratio, after one continuous extraction, the content of epichlorohydrin in cationic etherifying agent is 36mg·kg -1 , the content of 1,3-dichloro-2-propanol is 70mg·kg -1 ; After 2 consecutive extractions, the content of epichlorohydrin in the cationic etherifying agent is 10 mg kg -1 , the content of 1,3-dichloro-2-propanol is 15mg·kg -1 ; After 4 consecutive extractions, epichlorohydrin and 1,3-dichloro-2-propanol were not detected by the cationic etherifying agent.

[0029] 2. Regeneration

[0030] The regeneration condition of triisobutyl phosphate: the concentration is 6%Na 2 CO ...

Embodiment 3

[0032] Take tributyl phosphate as the extraction agent to purify cationic etherification agent as an example:

[0033] 1. Extraction

[0034] The ECH content in the crude product cationic etherification agent 3-chloro-2-hydroxypropyltrimethylammonium chloride is 1885mg kg -1 , DCP content is 23265mg·kg -1 . Extractant with V 粗产品 :V 萃取剂 =1:1.1 ratio, after one continuous extraction, the content of epichlorohydrin in the cationic etherification agent is 46mg·kg -1 , the content of 1,3-dichloro-2-propanol is 82mg·kg -1 ; After 2 consecutive extractions, the content of epichlorohydrin in the cationic etherifying agent is 18 mg kg -1 , the content of 1,3-dichloro-2-propanol is 25mg·kg -1 .

[0035] 2. Regeneration

[0036] The regeneration conditions of tributyl phosphate: the concentration is 5% tetrabutylammonium hydroxide aqueous solution, the temperature is 120 ℃, the regeneration time is 6 hours, after recycling 6 times, epichlorohydrin and 1,3- The content of dichloro...

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Abstract

The invention discloses a method for purifying a cationic etherifying agent via a phosphate ester extraction agent. According to the method, the crude product of the cationic etherifying agent is extracted and purified by taking a phosphate ester compound as an extraction agent so as to remove epoxy chloropropane and 1,3-dichloro-2-propanol remaining in the cationic etherifying agent product. When the extraction is carried out, the final extraction agent rich in the epoxy chloropropane and the 1,3-dichloro-2-propanol is regenerated, wherein a regeneration environment is maintained as an alkaline environment by adopting an alkaline liquor; the regenerated extraction agent is recycled aiming at the extraction of the crude product of the cationic etherifying agent; and meanwhile, the recycled epoxy chloropropane is cycled into the synthesized cationic etherifying agent to be utilized. Compared with the prior art, the method disclosed by the invention is simple in process, simple and convenient to operate, less in equipment investment, economical and environmentally friendly.

Description

technical field [0001] The invention belongs to a purification process of fine chemical products, and more specifically relates to a method for extraction, purification and regeneration of a cationic etherification agent. Background technique [0002] At present, most of the cationic etherifying agents used in the domestic production of high-quality modified starch are imported from abroad. However, with the continuous development of natural product modified chemicals such as starch, the amount of 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHPTMAC), as an etherification agent with excellent performance, will continue to increase. Therefore, it is of great significance to seek the optimal process for the production of CHPTMAC to improve the market competitiveness of etherifying agents in my country. However, the cationic etherification agent crude products produced by domestic manufacturers contain high contents of epichlorohydrin (ECH) and 1,3-dichloro-2-propanol (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/10C07C215/40
Inventor 程发朱森张春晓刘丽娟牛吉峰魏玉萍
Owner TIANJIN UNIV
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