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Method for preparing blocked allyl polyether

A technology of allyl polyether and hydroxyl-terminated polyether, which is applied in the field of preparation of end-capped allyl polyether, can solve the problems of low yield and low end-capping efficiency of end-capped allyl polyether, Achieve the effects of improving yield and capping efficiency, avoiding hydrolysis, and good technical effects

Inactive Publication Date: 2012-05-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the end-capping agent decomposes due to the generation of water in the etherification reaction process of the prior art, resulting in low yield of end-capped allyl polyether and low end-capping efficiency. A kind of preparation method of new capped allyl polyether

Method used

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  • Method for preparing blocked allyl polyether
  • Method for preparing blocked allyl polyether
  • Method for preparing blocked allyl polyether

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 176 grams of nonylphenol polyoxyethylene (15) ether (EO=15), 12 grams of solid potassium hydroxide and 200 milliliters of toluene in a 500 milliliter glass reactor, and replace it with nitrogen for 3 times under stirring. React with water at an azeotropic temperature of 85°C for 4 hours, and separate the water generated by the reaction through the azeotropy of toluene and water, control the amount of water output until the synthesis reaction of potassium nonylphenol polyether alcohol is completed, and lower the reaction temperature to 60°C , slowly add 20 grams of chloropropene dropwise, after the dropwise addition, heat up to 120°C and stir for 4 hours to react. After the etherification reaction is completed, carry out vacuum distillation to recover toluene, filter and desalt to separate the generated salt, and finally refine to obtain nonyl phenol-terminated allyl polyether.

Embodiment 2

[0023] Add 132 grams of nonylphenol polyoxyethylene (10) ether (EO=10), 12 grams of solid potassium hydroxide and 200 milliliters of toluene in a 500 milliliter glass reactor, and replace it with nitrogen for 3 times under stirring. React with water at an azeotropic temperature of 85°C for 4 hours, and separate the water generated by the reaction through the azeotropy of toluene and water, control the amount of water output until the synthesis reaction of potassium nonylphenol polyether alcohol is completed, and lower the reaction temperature to 60°C , slowly add 20 grams of chloropropene dropwise, after the dropwise addition, heat up to 120°C and stir for 4 hours to react. After the etherification reaction is completed, carry out vacuum distillation to recover toluene, filter and desalt to separate the generated salt, and finally refine to obtain nonyl phenol-terminated allyl polyether.

Embodiment 3

[0025] Add 176 grams of nonylphenol polyoxyethylene (15) ether (EO=15) 12 grams of solid potassium hydroxide and 200 milliliters of toluene in a glass reactor of 500 milliliters, replace with nitrogen gas 3 times under stirring, in two Toluene and water were reacted at an azeotropic temperature of 95°C for 4 hours, and the water generated by the reaction was separated by the azeotropy of xylene and water, and the amount of water was controlled until the synthesis reaction of potassium nonylphenol polyether alkoxide was completed, and the reaction temperature was lowered to Slowly add 20 grams of chloropropene dropwise at 60°C. After the dropwise addition, raise the temperature to 130°C and stir for 4 hours. After the etherification reaction is complete, carry out vacuum distillation to recover toluene, filter and desalt to separate the generated salt, and finally refine A nonylphenol-terminated allyl polyether is obtained.

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Abstract

The invention relates to a method for preparing blocked allyl polyether and mainly aims to solve the problem that the water generated by the etherification in the prior art results in the decomposition of the blocking agent. To solve the problem, the invention adopts the technical scheme comprising the following steps of: (1) adding hydroxyl terminated polyether and alkali metal hydroxide with mole ratio of 1: 0.5 to 5 to organic solvent, then making the mixture react for 0.5 to 15 hours at the azeotropic temperature of the organic solvent and the water, and separating the generated water by the azeotropic reaction of the organic solvent and water to prepare the solution of polyether polyol alkali metal salt; (2) reducing the temperature of the solution prepared in the step (1) to 40 to 80 DEG C, adding halide to the reaction system, etherifying the mixture for 0.5 to 15 hours at the reaction temperature of 80 to 150 DEG C, carrying out the reduced pressure distillation, filtering anddesalting and refining after the reaction is finished, finally, obtaining the blocked allyl polyether. The invention is applied to the industrial production of the blocked allyl polyether.

Description

technical field [0001] The invention relates to a preparation method of end-capped allyl polyether. Background technique [0002] Polymerizable surfactant is a kind of surfactant containing polymerizable groups. As a functional surfactant, it not only has significant surface activity, but also can undergo homogeneous (co)polymerization reaction under certain triggering conditions. Due to its unique structure and superior performance, polymerizable surfactants can be used in many emerging industries and scientific research fields, thus opening up a new field of surfactant synthesis and application. [0003] Polymerizable surfactants can be divided into allyl type, styrene type, (meth)acrylic acid type, acrylamide type and maleic acid type according to the polymerization active group, and can be divided into anion, Nonionic and cationic. Among them, allyl polyether has good hydrophilicity, emulsifying ability and chemical stability, and is a polymerizable nonionic surfactant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/338C08G65/32C08G65/324C08G65/337C08G65/48
Inventor 周承俊杨为民周文乐夏燕敏虞子牛沈之芹宋晓芳陈安猛
Owner CHINA PETROLEUM & CHEM CORP
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