Process of preparing alkyl dead-end polyether by polyether with parahydroxyl at molecular chain end

A technology of alkyl-terminated, molecular chain

Active Publication Date: 2010-02-10
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the polyether with secondary hydroxyl at the end of the molecular chain, it is difficult to make the polyether generate the corresponding alkoxide with conventional solid alkali metal hydroxide or its solution, resulting in a very low end-capping rate

Method used

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  • Process of preparing alkyl dead-end polyether by polyether with parahydroxyl at molecular chain end
  • Process of preparing alkyl dead-end polyether by polyether with parahydroxyl at molecular chain end
  • Process of preparing alkyl dead-end polyether by polyether with parahydroxyl at molecular chain end

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Experimental program
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Effect test

Embodiment 1

[0027] Add allyl alcohol polyoxypropylene ether (hydroxyl value 73) 400g in the 1000ml round bottom flask that is equipped with electronic constant speed stirrer, reflux condenser, thermometer and dropping funnel, the alcoholic solution 14Gg of sodium methylate, in vacuum degree Under the condition of -0.085~-0.098, react at 90~95°C for 1 hour, cool down to 45~50°C, add 131g of dimethyl sulfate dropwise, finish dropping in about 3 hours, and continue to react at 45~50°C for 4 hours after the dropwise addition . Add 200g of water, stir at 40-45°C for 0.5 hours, then let stand to separate layers, remove the water phase, neutralize with alkali until the pH is 6-8, dehydrate in vacuum, add diatomaceous earth filter aid and filter to obtain alkyl End-capped polyether products.

Embodiment 2

[0031] Add allyl alcohol polyether (EO / PO=55 / 45, block, PO chain segment at the end, hydroxyl The value is 36) 600g, 173g of alcohol solution of sodium methoxide, under the condition of vacuum degree of -0.085~-0.098, react at 90~95°C for 1 hour, cool down to 40~45°C, add 136g of dimethyl sulfate dropwise for about 3 hours After the dropwise addition, continue to react at 40-45° C. for 4 hours. Add 300g of water, stir at 40-45°C for 0.5 hours, then let stand to separate layers, remove the water phase, neutralize with alkali until the pH is 6-8, vacuum dehydrate, add diatomaceous earth filter aid and filter to obtain alkyl End-capped polyether products.

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Abstract

The process of preparing polyether with end capping alkyl group belongs to the field of polyether synthesis technology. The process includes the reaction of polyether with sec hydroxyl group in the end of molecular chain and strong nucleophilic reagent alkali, the further reaction with alkyl sulfate, neutralizing with alkali, water washing and filtering to obtain polyether with end capping alkyl group. The strong nucleophilic reagent alkali is alcohol solution of sodium methoxide, alcohol solution of potassium methoxide, solid sodium methoxide, solid potassium methoxide or their mixture; and the alkyl sulfate is dimethyl sulfate or diethyl sulfate. The present invention has very high reaction activity and effectively raised end capping rate.

Description

technical field [0001] The invention relates to a method for preparing an alkyl-capped polyether from a polyether whose molecular chain terminal is a secondary hydroxyl group, and belongs to the technical field of synthesizing the capped polyether. Background technique [0002] Alkyl-terminated polyether not only maintains many good properties of the original mono-alkyl polyether, but also improves the chemical properties of the entire molecule because the active hydrogen on the terminal hydroxyl group of the original mono-alkyl polyether compound is replaced by a hydrophobic alkyl group. Stability, thus showing a unique function. Alkyl-terminated polyether is mainly used in the following aspects: (1) It can be used in low-foaming detergents by taking advantage of its stability against strong alkali; (2) It can be used as polyurethane foam modified silicone Foam stabilizer in the production of foam materials; (3) as a chemical fiber oil monomer with excellent performance; (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/334C08G65/48
Inventor 王伟松王新荣孟照平万庆梅
Owner ZHEJIANG HUANGMA TECH
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