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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 end capping efficiency

Inactive Publication Date: 2004-06-16
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

Examples

Experimental program
Comparison scheme
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 process for preparing alkyl blocking polyether through reaction of polyethers with molecular chains including hydroxyl with alkyl sulfate comprising the steps of, (1) adding solid solid potassium hydroxide or sodium hydroxide into polyether for reaction, at a reaction temperature of 25-140 deg. C and the charge equivalent weight ratio of polyether and potassium hydrate or sodium hydroxide is 1:1.50-1.95%, (2) adding alkyl sulfate into the reaction system for continuance reaction, at a reaction temperature of 25-140 deg. C and the charge equivalent weight ratio of raw material polyether and alkyl sulfate is 1:1.75-2.00, (3) refining the reactant to obtain the produce. The invention can be utilized to lower the application of blocking agent and increase closing 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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IPC IPC(8): C08G65/48
Inventor 张士福
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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