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

A technology of alkyl end-capping and molecular chain, which is applied in the synthesis field of end-capping polyether, and can solve the problem of low end-capping rate

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

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 400 g of allyl alcohol polyoxypropylene ether (hydroxyl value 73) and 188 g of alcoholic solution of sodium methylate in a 1000 ml round bottom flask equipped with an electronic constant speed stirrer, a reflux condenser, a thermometer and a dropping funnel. Under the condition of -0.085~-0.098, react at 90~95°C for 1 hour, cool down to 45~50°C, add 164g of bromobutane dropwise, and finish dropping in about 3 hours. After the dropwise addition, continue to react at 45~50°C for 4 hours. 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, 176g 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 148g of bromobutane dropwise, drop for about 3 hours After completion of the dropwise addition, the reaction was continued 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 halide, 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 halide is C1-C4 alkyl chloride or alkyl bromide. 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): C08G65/48C08G65/329
Inventor 王伟松王新荣孟照平万庆梅
Owner ZHEJIANG HUANGMA TECH
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