Method for synthesizing nusaturated hydrophilic methyl or ethyl end capping polyether

A synthetic method and hydrophilic technology, which is applied in the field of synthesis of unsaturated hydrophilic methyl or ethyl-terminated polyether, and can solve the problems of many by-products, deep color of the product, and low capping rate.

Inactive Publication Date: 2005-01-12
王伟松
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The above synthesis method is because the alkalinity in the reaction system is too strong, so the end-capping rate of the unsaturated hydrophilic methyl (ethyl) group-terminated polyether synthesized is lower, the product color is deep, and there are many by-products

Method used

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  • Method for synthesizing nusaturated hydrophilic methyl or ethyl end capping polyether
  • Method for synthesizing nusaturated hydrophilic methyl or ethyl end capping polyether
  • Method for synthesizing nusaturated hydrophilic methyl or ethyl end capping polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Firstly, alkaline sustained-release microcapsules were prepared. Under the protection of nitrogen, add 300 grams of sodium hydroxide particles (particle size is 100-200 μm) in a small glass fluidized bed with an inner diameter of 20 cm and a height of 80 cm. The nitrogen gas velocity was increased to suspend the alkali particles. Then spray into alkaline earth metal salt calcium chloride aqueous solution, the weight ratio of calcium chloride to sodium hydroxide is 0.3:1. When drying, the nitrogen temperature is 125°C. After drying for 2-3 hours, cool to room temperature and store in airtight condition until use.

[0032] Add allyl alcohol polyoxyethylene ether (average degree of addition is 8) 100g, sodium hydroxide microcapsule 35g in the 500ml round bottom flask that is equipped with electronic constant speed stirrer, reflux condenser, thermometer and dropping funnel, Stirring was started, and the temperature was kept at 30-35°C. At the same time, 33.5 g of dimethyl...

Embodiment 2-6

[0034] Use potassium hydroxide, sodium hydroxide or their mixture with sodium carbonate, potassium carbonate instead

[0035] Example

[0036] (The capping rate is determined by quantitative 13 CNMR analysis value is calculated as a benchmark)

Embodiment 7-12

[0038] Example

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Abstract

In the synthetic method, allyl alcohol polyether and dimethyl sulfate or diethyl sulfate are etherified at temperature of 0-80 deg.C, under action of basic microcapsule catalyst in slow release and unsaturated hydrophilicity methyl or ethyl end capped polyether is obtained after neutralizing with acid-base and washing. The catalyst slowly releases alkali microcapsule prepard by alkali metal hydroxide or by mixed alkali metal chamicals.

Description

technical field [0001] The invention relates to a method for synthesizing unsaturated hydrophilic methyl or ethyl capped polyether, which belongs to the technical field of capping polyether synthesis. Background technique [0002] Unsaturated hydrophilic methyl- or ethyl-terminated polyether, as a polyether with special structure and performance, has been widely used in the fields of synthetic lubricating oil, daily chemical industry and chemical fiber oil. Previously, there were multiple methods for producing methyl or ethyl-terminated polyethers. Among them, the Williamson (Williamson) method using dimethyl (ethyl) sulfate as the first (ethyl) reagent was because of its high reactivity and low price. Inexpensive and has attracted the attention of researchers. The known Williamson (Williamson) method discloses in Japanese Patent Publication No. 48-22198 and No. 51-203500, using an aqueous or alcoholic solution of sodium methylate, sodium hydroxide or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48
Inventor 王伟松
Owner 王伟松
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