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Method for synthesizing decynediol ethoxylate

A technology of ethoxylates and synthesis methods, which is applied in the field of chemical synthesis, can solve the problems of restricting the application of products in high-end fine chemical products, low unsaturation, high chroma, etc., and achieve high product unsaturation, fast reaction rate, The effect of low chroma of the product

Active Publication Date: 2018-09-11
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The ethoxylated decynediol product synthesized by the prior art has high chroma and low unsaturation, which limits the application of the product in high-end fine chemical products

Method used

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  • Method for synthesizing decynediol ethoxylate
  • Method for synthesizing decynediol ethoxylate
  • Method for synthesizing decynediol ethoxylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Add 226g TMDD, 1181g 1-butyl-3-methylimidazolium dihydrogen phosphate and 7.923g triethylamine into a 2L stirred autoclave, heat the reactor to 60°C, and start stirring at the same time to fully mix TMDD and the catalyst .

[0057] After stirring for 20 minutes, replace the air in the reactor with nitrogen for five times, then vacuumize, and then raise the temperature of the reactor to 140°C.

[0058] Feed ethylene oxide into the reaction kettle, keep the pressure in the kettle stable at 0.2MPa by controlling the gas flow meter, continue feeding ethylene oxide until the cumulative amount reaches 10mol, and stop feeding ethylene oxide.

[0059] The temperature in the kettle was controlled simultaneously by the inner coil of the kettle and the outer jacket of the kettle, so that the reaction temperature in the kettle was stabilized at 140° C. until the pressure in the kettle was stabilized and the reaction was completed, and the temperature was lowered to 60° C. Add 600m...

Embodiment 2

[0063] Add 226g of TMDD, 1300g of 1-butyl-3-methylimidazolium bisulfate and 7.923g of trimethylamine into a 2L stirred autoclave. The temperature of the reactor is raised to 60°C, and at the same time, stirring is started to fully mix TMDD and the catalyst.

[0064] After stirring for 20 minutes, replace the air in the reactor with nitrogen for five times, then vacuumize, and then raise the temperature of the reactor to 130°C.

[0065] Feed ethylene oxide into the reaction kettle, keep the pressure in the kettle stable at 0.2MPa by controlling the gas flow meter, continue feeding ethylene oxide until the cumulative amount reaches 10mol, and stop feeding ethylene oxide.

[0066] The temperature in the kettle was controlled simultaneously by the inner coil of the kettle and the outer jacket of the kettle, so that the reaction temperature in the kettle was stabilized at 130° C. until the pressure in the kettle was stabilized and the reaction was completed, and the temperature was ...

Embodiment 3

[0070] Add 226g TMDD, 1211g 1-butyl-3-methylimidazolium trifluoromethanesulfonate and 7.923g triethylamine into a 2L stirred autoclave, heat the reactor to 60°C, and start stirring at the same time to make TMDD and catalyst Mix well.

[0071] After stirring for 20 minutes, replace the air in the reactor with nitrogen for five times, then vacuumize, and then raise the temperature of the reactor to 120°C.

[0072] Feed ethylene oxide into the reaction kettle, keep the pressure in the kettle stable at 0.2MPa by controlling the gas flow meter, continue feeding ethylene oxide until the cumulative amount reaches 10mol, and stop feeding ethylene oxide.

[0073] The temperature in the kettle was controlled simultaneously by the inner coil of the kettle and the outer jacket of the kettle, so that the reaction temperature in the kettle was stabilized at 120° C. until the pressure in the kettle was stabilized and the reaction was completed, and the temperature was lowered to 60° C. Add ...

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Abstract

The invention discloses a method for synthesizing decynediol ethoxylate. 2,4,7,9-tetramethyl-5 decyne-4,7-diol and ethylene oxide are used as raw materials, ethoxylated decynediol is synthesized through polymerization, acidic ionic liquid 1-butyl-3-methylimidazolium phosphate dihydrogen salt is used as an acidic catalyst and solvent, one or more of the organic bases are used as basic catalysts forreaction, and a product and the catalysts are separated by using ether as an extracting agent to obtain ethoxylated 2,4,7,9-tetramethyl-5-decyne-4,7-diol. The acid-base catalysts have good protectioneffect on the triple bond of alkynol, the product has high product unsaturation, by-products are few and product chroma is low. The components of the whole process are easy to separate, the catalystsand solvent can be recycled, the production cost is low, the process is green and environmentally friendly, and the method can be used for industrial production.

Description

technical field [0001] The present invention relates to the technical field of chemical synthesis, more specifically, to a method for synthesizing decynediol ethoxylates, in particular to 2,4,7,9-tetramethyl-5-decyne-4, The invention discloses a method for preparing ethoxylated 2,4,7,9-tetramethyl-5-decyne-4,7-diol by polymerization reaction of 7-diol and ethylene oxide as raw materials. Background technique [0002] Ethoxylated 2,4,7,9-tetramethyl-5-decyne-4,7-diol is also known as 2,4,7,9-tetramethyl-5-decyne-4, 7-diol polyoxyethylene ether is a new type of environmentally friendly acetylenic alcohol multifunctional surfactant, which has two hydrophilic groups and two lipophilic groups, and the triple bond is located in the center of the hydrocarbon chain. Ethoxy groups and hydroxyl groups are distributed symmetrically on both sides of the triple bond. This special molecular structure makes it have good ability to reduce surface tension, defoaming and foam suppression, wa...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08G65/30
CPCC08G65/2609C08G65/2672C08G65/2675C08G65/2678C08G65/2684C08G65/269C08G65/30Y02P20/54
Inventor 蒋乐乐陶川东余维新赖崇伟周飞李杰灵
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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