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Method of synthesizing methoxypolyethylene glycol allyl methyl ether of water reducer macromonomer

A technology of polyethylene glycol methyl allyl ether and methoxy polyethylene glycol, which is used in the synthesis of water reducing agent macromonomers, water reducing agent macromonomer methoxy polyethylene glycol methylene In the field of synthesis of propyl ether, the effects of cheap and easy-to-obtain raw materials, cost reduction and high end capping rate are achieved.

Active Publication Date: 2011-03-16
德纳新材料(茂名)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis method of the macromonomer methoxy polyethylene glycol methyl allyl ether of the water reducing agent has not yet been reported, especially when preparing the macromonomer of the polycarboxylate water reducing agent, no solvent and polymerization inhibitor are added. The synthetic method of the last report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put 1200g of methoxypolyethylene glycol (polymerization degree 22) into a 2000ml four-neck flask, 48g of solid N a OH, stirred and warmed up. Control the temperature at 110~120°C, vacuum degree -0.09Mpa~-0.098Mpa, and react for 30~120min. Then cool to 50-60°C for use. Add 108.6 g of methyl chloride propene into the constant pressure dropping funnel, the molar ratio of methyl chloride propene to methoxypolyethylene glycol is 1.0:1.0, and the dropwise addition is completed within 60 minutes. Then heat up to 80-85°C and react for 180-400min, cool to 50-60°C, add diethylene glycol dimethyl ether to dissolve, wash with saturated solution of sodium chloride, separate phases to take the upper layer solution, and finally remove the solvent by distillation under reduced pressure and moisture. To obtain methoxypolyethylene glycol methyl allyl ether, the measured hydroxyl value is less than 2mgKOH / g, and the end-capping rate is more than 98%.

Embodiment 2

[0038] Put 1200g of methoxypolyethylene glycol (polymerization degree 26.5) into a 2000ml four-neck flask, 60g parts of N a OH, stirred and warmed up. Control the temperature at 80-150°C, vacuum degree -0.09Mpa--0.098Mpa, and react for 30-120min. Then cool to 50-60°C for use. Add 135.8 g of methyl chloride propene to the constant pressure dropping funnel, the molar ratio of methyl chloride propene to methoxypolyethylene glycol is 1.5:1.0, and the dropwise addition is completed within 60 minutes. Then heat up to 80-85°C and react for 180-400min, cool to 50-60°C, add diethylene glycol dimethyl ether to dissolve, wash with saturated solution of sodium chloride, separate phases to take the upper layer solution, and finally remove the solvent by distillation under reduced pressure and moisture. To obtain methoxypolyethylene glycol methyl allyl ether, the measured hydroxyl value is less than 2mgKOH / g, and the end-capping rate is more than 98%.

Embodiment 3

[0040] In a 2000ml four-neck flask, 1200g of methoxypolyethylene glycol (polymerization degree 33.3), 64g of N a OH, stirred and warmed up. Control the temperature at 80-150°C, vacuum degree -0.09Mpa--0.098Mpa, and react for 30-120min. Then cool to 50-60°C for use. Add 117.7 g of methyl chloride propene to the constant pressure dropping funnel, the molar ratio of methyl chloride propene to methoxypolyethylene glycol is 1.3:1.0, and the dropwise addition is completed within 60 minutes. Then heat up to 70-80°C to react for 180-400min, cool to 50-60°C, add ethylene glycol dimethyl ether to dissolve, wash with a saturated solution of sodium chloride, separate phases to take the upper solution, and finally distill under reduced pressure to remove the solvent and moisture. To obtain methoxypolyethylene glycol methyl allyl ether, the measured hydroxyl value is less than 2mgKOH / g, and the end-capping rate is more than 98%.

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PUM

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Abstract

The invention discloses a method of synthesizing methoxypolyethylene glycol allyl methyl ether of water reducer macromonomer. In a NaOH or KOH solution, the methoxypolyethylene glycol allyl methyl ether is condensed by a methoxypolyethylene glycol and a methyl allyl chloride. The raw material used in the method of the invention is the methyl allyl chloride which is cheap and easily obtained. The technological process is simple and the cost is low. The method is suitable for industrial production of an allyl methyl ether compound. Simultaneously, the reaction conditions are mild. The method is environment-friendly due to no use of a toxic solvent as a water-carrying agent.

Description

technical field [0001] The present invention relates to a method for synthesizing a macromonomer of a water reducing agent, in particular to a method for synthesizing a macromonomer of a water reducing agent, methoxypolyethylene glycol methallyl ether, which belongs to the category of capping in organic chemistry. The field of synthetic technology. Background technique [0002] The structure of methallyl ether has the properties of isomerization, oxygen binding and polymerization. It is often used in the fields of polymer monomers or crosslinking agents and water reducing agents. It is an important class of organic compounds. Methoxypolyethylene glycol methyl allyl ether has a polymerizable double bond at one end of its molecular structure, and is a new type of active macromonomer for polycarboxylic acid water reducers. [0003] The polycarboxylate water reducer has been continuously developed and improved for more than 20 years. Compared with the previous water reducer, th...

Claims

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Application Information

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IPC IPC(8): C08G65/48C04B24/24C04B103/30
Inventor 秦怡生陈荣福王伟徐平张学军蒋大智秦旭东
Owner 德纳新材料(茂名)有限公司
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