Method for preparing alkyl end capping polyether using alkyl halide as end capping reagent

A technology of alkyl end-capping and haloalkane, which is applied in the field of preparation of alkyl-termination polyether with haloalkane as the end-capping agent, which can solve the problems of increasing the end-capping agent, achieve the effect of reducing the usage amount and improving the end-capping efficiency

Inactive Publication Date: 2005-06-01
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Since the haloalkane end-capping agent will decompose when it meets water, these existing alkyl-terminated polyether preparation methods usually can only ensure sufficient end-capping efficiency by greatly increasing the amount of end-capping agent used

Method used

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  • Method for preparing alkyl end capping polyether using alkyl halide as end capping reagent

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Effect test

Embodiment 1

[0033] In a 500 ml four-necked flask, add 200 g of butanol polyether (EO / PO=50 / 50, random, hydroxyl value 36), 13.0 g of solid potassium hydroxide, and 4.0 g of anhydrous sodium sulfite (antioxidant). It was replaced with nitrogen 4 times with stirring, and then reacted at a temperature of 90 to 100° C. for 1 hour. 3.3 grams of calcium oxide powder was added, vigorously stirred, and 11.7 grams of methylene chloride was added dropwise, and the reaction was continued at 120-130° C. for 4 hours after the dropwise addition. Add 100 ml of water to wash the reaction product, stir at 90 ° C for 1 hour, maintain 80 ~ 90 ° C to make the reactant stand for stratification, remove the water phase, vacuum dehydration, filter to remove solid impurities, and obtain the end-capped polyether product.

Embodiment 2

[0035] In a 500 ml four-necked flask, add 200 grams of butanol polyether (EO / PO=50 / 50, random, hydroxyl value 36), 14.0 grams of solid potassium hydroxide, 4.0 grams of anhydrous sodium sulfite, and 9.3 grams of calcium oxide, Stir vigorously. It was replaced with nitrogen four times under stirring, and the reaction was carried out at 90 to 100° C. for 1 hour. 11.7 g of monochloromethane was added dropwise, and the reaction was continued at 110-120° C. for 4 hours after the dropwise addition was completed. Add 100 ml of water, stir at 90°C for 1 hour, maintain 80-90°C to allow the reactants to stand for stratification, remove the aqueous phase, dehydrate in vacuo, and filter to remove solid impurities to obtain the end-capped polyether product

Embodiment 3

[0037] In a 500 ml four-necked flask, add 200 g of polyethylene glycol (hydroxyl value 78), 30.4 g of solid potassium hydroxide, 4.0 g of anhydrous sodium sulfite, 12.2 g of calcium oxide, and 80 ml of xylene. A stirring reaction was performed at a temperature of 90 to 100° C. for 1 hour. 27.4 g of monochloromethane was added dropwise, and the reaction was continued at 110-120° C. for 4 hours after the dropwise addition was completed. Add 100 ml of water, stir at 90°C for 1 hour, maintain 80-90°C to allow the reactant to stand for stratification, remove the aqueous phase, remove the solvent in vacuo, and filter to remove solid impurities to obtain the end-capped polyether product.

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Abstract

A method for preparing an alkyl-terminated polyether by reacting a polyether with a hydroxyl group in its molecular chain with an alkyl halide, comprising: 1) adding a solid base to the polyether for reaction, and the solid base is obtained from one of potassium hydroxide or sodium hydroxide species or a mixture thereof, the reaction temperature is 25-140°C, the equivalent ratio of polyether to potassium hydroxide or sodium hydroxide is 1:1.50-1.95, and calcium oxide powder, calcium oxide powder and potassium hydroxide are also added to the reaction system Or the feeding weight ratio of sodium hydroxide is 1: 1-6; 2) adding haloalkane to the reaction system to continue the reaction, the reaction temperature is 40-140°C, and the feeding equivalent ratio of raw material polyether and haloalkane is 1: 1.75-1.95; 3) The reactant is refined to obtain the product. In the present invention, since the water-absorbing agent calcium oxide is added to the reaction system, the reaction between water and the end-capping agent haloalkane is avoided to cause its decomposition. Its advantage is that it can reduce the usage amount of end-capping agent and improve the end-capping efficiency.

Description

technical field [0001] The invention relates to a method for preparing alkyl-terminated polyether by reacting polyether containing hydroxyl group in molecular chain with halogenated alkyl. Background technique [0002] Compared with the polyether containing hydroxyl groups in the molecular chain, the alkyl-terminated polyether in which the hydroxyl groups in the molecular chain are all substituted by alkyl groups has higher chemical stability. Utilizing the good heat resistance of alkyl-terminated polyether, it can be used as a non-ionic surfactant with excellent performance in the oiling agent for high-speed spinning of chemical fibers, and can also be used as an additive in high-temperature-resistant lubricating oil or heat-conducting oil. Utilizing its stability to strong alkalis, it can be used in strong alkaline detergent formulations. In addition, most alkyl-terminated polyethers also have anti-foaming and low-foaming properties, so they are often used as defoamers or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/332
Inventor 张士福
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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