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

An alkyl sulfate and alkyl end-capping technology is applied in the field of preparing alkyl-terminated polyether by using alkyl sulfate as end-capping agent, which can solve problems such as increasing end-capping agent, avoid decomposition, reduce usage, The effect of 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 end-capping agent alkyl sulfate will decompose when it meets water, these existing methods for preparing alkyl-terminated polyethers can only ensure sufficient end-capping efficiency by increasing the amount of end-capping agent used in large quantities.

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 200 grams of butanol polyether (EO / PO=50 / 50, random, hydroxyester 36), 14.0 grams of solid potassium hydroxide, and 4.0 grams of anhydrous sodium sulfite (antioxidant) in a 500 ml four-necked flask, add 9.3 grams of calcium oxide, stirred vigorously. Under stirring, it was replaced with nitrogen four times, and reacted at 90-100° C. for 1 hour. Cool down to 40-45°C, add 15.8 grams of dimethyl sulfate dropwise, continue to react at 40-45°C for 2 hours, 60°C for 1 hour, and 90°C for 1 hour after the dropwise addition. 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 water phase, vacuum dehydrate, and filter to remove solid impurities to obtain the end-capped polyether product

Embodiment 2

[0035] Add 200 grams of polyethylene glycol (hydroxyl value 78), 30.4 grams of solid potassium hydroxide, 4.0 grams of anhydrous sodium sulfite, 20.3 grams of calcium oxide, and 80 milliliters of xylene in a 500 milliliter four-necked flask, blow nitrogen for 10 minutes, and then Stirring is carried out at a temperature of 90-100°C for 1 hour. Cool down to 40-45°C, add 30.2 grams of dimethyl sulfate dropwise, and continue to react at 40-45°C for 2 hours after the dropwise addition, 1 hour at 60°C, and 1 hour at 90°C. 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 water phase, remove the solvent in a vacuum, and filter to remove solid impurities to obtain a blocked polyether product.

Embodiment 3

[0037] Add 200 grams of glycerol polyether (EO / PO=30 / 70, random, hydroxyl value 37), 14.4 grams of solid potassium hydroxide, 4.0 grams of anhydrous sodium sulfite, and 9.6 grams of calcium oxide in a 500 milliliter four-necked flask, and stir The mixture was replaced with nitrogen four times, and then stirred and reacted at 90-100° C. for 1 hour. Cool down to 40-45°C, add 16.2 g of dimethyl sulfate dropwise, and then maintain 40-45°C to continue the reaction for 2 hours, 1 hour at 60°C, and 1 hour at 90°C. 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 water phase, vacuum dehydrate, and filter to remove solid impurities to obtain a blocked polyether product.

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Abstract

A method for preparing an alkyl-terminated polyether by reacting a polyether containing a hydroxyl group in the molecular chain with an alkyl sulfate ester, comprising: 1) adding solid potassium hydroxide or sodium hydroxide to the polyether for reaction, and the reaction temperature is 25-25 140°C, the equivalent ratio of polyether to potassium hydroxide or sodium hydroxide is 1:1.50-1.95, calcium oxide powder is also added to the reaction system, and the weight ratio of calcium oxide powder to potassium hydroxide or sodium hydroxide is 1 : 1 ~ 6; 2) Add alkyl sulfate ester to the reaction system to continue the reaction, the reaction temperature is 25 ~ 100 ° C, the equivalent ratio of raw material polyether and alkyl sulfate ester is 1: 1.75 ~ 2.00; 3) reactant Products obtained after refining. In the present invention, since the water-absorbing agent calcium oxide is added to the reaction system, the decomposition of the reaction between water and the alkyl sulfate of the end-capping agent is avoided. The advantage is that it can reduce the amount of end-capping agent used and improve the end-capping efficiency.

Description

technical field [0001] The invention relates to a method for preparing an alkyl-terminated polyether by reacting a polyether containing a hydroxyl group in a molecular chain with an alkyl sulfate. Background technique [0002] Alkyl-terminated polyethers in which all hydroxyl groups in the molecular chain are substituted by alkyl groups have higher chemical stability than polyethers containing hydroxyl groups in the molecular chain. Utilizing the good heat resistance of alkyl-terminated polyether, it can be used as an excellent non-ionic surfactant in the oil 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 alkali, 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 monomers for defoamers or low-foaming deter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/48
Inventor 张士福
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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