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Method for synthesizing adduct of alkynediol and epoxyethane

A technology for the synthesis of ethylene oxide, which is applied in the preparation of ether from alkylene oxide, chemical instruments and methods, transportation and packaging, etc. It can solve the problems of complex operation, large equipment investment, and difficult control of reaction temperature, etc., and achieve production safety Improve performance, reduce equipment investment, and reduce volatilization

Inactive Publication Date: 2012-01-04
杨朝辉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But it should be pointed out that this synthesis process has the following disadvantages: (1) high-pressure reaction equipment and high-pressure feeding device need to be used, the equipment investment is large, and the operation is complicated; (2) in the pro

Method used

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  • Method for synthesizing adduct of alkynediol and epoxyethane
  • Method for synthesizing adduct of alkynediol and epoxyethane
  • Method for synthesizing adduct of alkynediol and epoxyethane

Examples

Experimental program
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Embodiment 1

[0033] Synthesis of 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethylene oxide adduct (1:1.5).

[0034] Add 226 grams (1.0mol) of 2,4,7,9-tetramethyl-5-decyne-4,7-diol in a 5-liter three-necked round-bottomed flask, 500 milliliters of anhydrous ether and 0.1mol Under reflux with mechanical stirring, slowly add dropwise a mixed solution of 1.5 mol of ethylene oxide dissolved in 500 ml of anhydrous diethyl ether, after the dropwise addition, continue to stir and reflux for 5 hours. After the reaction is completed, anhydrous ether is removed by rotary evaporation, and a small amount of trimethylamine is extracted under reduced pressure to obtain 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethylene oxide adduct compound (1:1.5), code-named CHEM-10.

Embodiment 2

[0036] Synthesis of 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethylene oxide adduct (1:3.5).

[0037] Add 316 g (1.0 mol) of CHEM-10, 500 ml of anhydrous ether and 0.1 mol of trimethylamine in a 5-liter three-necked round-bottomed flask, slowly add 2.0 mol of ethylene oxide dropwise under mechanical stirring and reflux Dissolve the mixed solution in 500 ml of anhydrous ether, after the dropwise addition, continue to stir and reflux for 10 hours. After the reaction is completed, anhydrous ether is removed by rotary evaporation, and a small amount of trimethylamine is extracted under reduced pressure to obtain 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethylene oxide adduct compound (1:3.5), code-named CHEM-20.

Embodiment 3

[0039]Synthesis of 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethylene oxide adduct (1:10).

[0040] Add 436 grams (1.0mol) of CHEM-20, 500 milliliters of anhydrous ether and 0.1mol of trimethylamine in a 5-liter three-necked round-bottomed flask, slowly add 6.5mol of ethylene oxide dropwise under mechanical stirring and reflux Dissolve the mixed solution in 1000 ml of anhydrous ether, after the dropwise addition, continue to stir and reflux for 20 hours. After the reaction is completed, anhydrous ether is removed by rotary evaporation, and a small amount of trimethylamine is extracted under reduced pressure to obtain 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethylene oxide adduct compound (1:10), code-named CHEM-30.

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Abstract

The invention discloses a method for synthesizing adduct of alkynediol and epoxyethane. In the method, alkynediol and epoxyethane are used as raw materials, triethylamine is used as a catalyst, absolute ether, benzene or toluene is used as a solvent, a reflux reaction is performed under a low-temperature and high-efficiency refluxing and condensing conditions, the organic solvent and catalyst are removed by rotary evaporation, and thus, the short-chain epoxyethane adduct is obtained. Meanwhile, the short-chain epoxyethane adduct can be added with a certain amount of epoxyethane by a one-step or multi-step process to react under the reaction conditions to obtain adducts with different chain lengths. In the invention, reaction under normal temperature is realized, and expensive high-voltage equipment is not used; the reaction conditions, such as reaction temperature, can be regulated by using solvents with different boiling points and are easy to control; and the method ahs a great significance for reducing equipment investment and production cost, promoting safety operation and the like and has a wide prospect.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and in particular relates to a method for preparing ethoxylated acetylenic glycol surfactants by reacting acetylene glycol and ethylene oxide, that is, a synthesis method of an adduct of acetylene glycol and ethylene oxide. Background technique [0002] Alkyne diols are a new class of non-ionic surfactants with a wide range of uses [Information Institute of the Ministry of Chemical Industry. World Fine Chemical Products Handbook [M]. Beijing: Chemical Industry Press, 1985, 535. Zhong Chuanrong, Lu Ai , Application and Production of Alkyne Alcohols, Oilfield Chemistry, 2000, 17(3), 285-288. Tang Dexiang, Synthesis of Alkyne Alcohol Corrosion Inhibitors, Science and Technology Information, 2009, 1, 46-47. Lu Ai, Zhong Chuanrong, Wang Jianhua, Zhou Hongying, Synthesis and corrosion inhibition effects of several alkyne alcohols, 2001, 18(9), 550-553]. [0003] Due to the small hydrophilic group...

Claims

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Application Information

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IPC IPC(8): C07C43/11C07C41/03C08G65/28B01F17/42C09K23/42
Inventor 杨朝辉
Owner 杨朝辉
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