Synthesis method of 4-hydroxybutyl vinyl ether polyoxyethylene ether

A technology of hydroxybutyl vinyl ether and polyoxyethylene ether, which is applied in the field of synthesis of polyether compounds in organic chemistry, to achieve the effect of simple operation and reasonable process

Inactive Publication Date: 2014-03-19
ZHEJIANG LYUKEAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few reports about the synthesis process of 4-hydroxybutyl vinyl ether polyoxyethylene ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The synthetic method of the 4-hydroxybutyl vinyl ether polyoxyethylene ether of present embodiment, comprises the steps:

[0018] (1) Preliminary synthesis: Add 21.6 parts by weight of 4-hydroxybutyl vinyl ether into the reactor, add 0.45 parts by weight of sodium metal as the primary synthesis catalyst within 30 minutes, control the pre-reaction temperature at 20~30°C, and the pre-reaction time 0.5 hours; after the pre-reaction is completed, the pre-reaction product is dropped into 411.8 parts by weight of 4-hydroxybutyl vinyl ether, after nitrogen replacement, the temperature is raised to 90 ° C, and 685.5 parts by weight of ethylene oxide are introduced for primary synthesis. Control the reaction temperature at 90~105°C, and the reaction time is 4.0 hours; after the reaction, cool down to 70°C and discharge to obtain the initial product, which is 4-hydroxybutyl vinyl ether polyoxyethylene ether oligomer with a molecular weight of 300 ;

[0019] (2) Final synthesis: ...

Embodiment 2

[0023] The synthetic method of present embodiment 4-hydroxybutyl vinyl ether polyoxyethylene ether comprises the steps:

[0024] (1) Preliminary synthesis: Add 19.2 parts by weight of 4-hydroxybutyl vinyl ether into the reactor, add 0.32 parts by weight of primary synthesis catalyst metal potassium within 50 minutes, control the pre-reaction temperature at 25~35°C, and the pre-reaction time 0.5 hours; after the pre-reaction is finished, the pre-reaction product is dropped into 200.4 parts by weight of 4-hydroxybutyl vinyl ether, and after nitrogen replacement, the temperature is raised to 90° C., and 441.8 parts by weight of ethylene oxide are introduced for initial synthesis, and the controlled The reaction temperature is 90~105°C, and the reaction time is 5.0h; after the primary synthesis reaction is completed, the temperature is lowered to 70°C and the material is discharged to obtain the primary product, which is 4-hydroxybutyl vinyl ether polyoxyethylene ether oligomer wit...

Embodiment 3

[0029] The synthetic method of the 4-hydroxybutyl vinyl ether polyoxyethylene ether of present embodiment, comprises the steps:

[0030] (1) Initial synthesis: Add 17.2 parts by weight of 4-hydroxybutyl vinyl ether into the reactor, add 0.21 parts by weight of sodium metal and 0.21 parts by weight of potassium metal for the primary synthesis catalyst within 50 minutes, and control the pre-reaction temperature at 30~ 40°C, the pre-reaction time is 0.8 hours; after the pre-reaction is completed, put the pre-reaction product into 159.4 parts by weight of 4-hydroxybutyl vinyl ether, after nitrogen replacement, the temperature is raised to 90°C, and 355.3 parts by weight of epoxy Ethane, the reaction temperature is controlled at 90~105°C, the reaction time is 5.5 hours, and the primary synthesis is carried out; after the primary synthesis reaction is completed, the temperature is lowered to 70°C and the material is discharged to obtain the primary product, which is 4-hydroxybutyleth...

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Abstract

The invention relates to a synthesis method of 4- hydroxybutyl vinyl ether polyoxyethylene ether, and belongs to the technical field of polyether compound synthesis in organic chemistry. The synthesis method comprises two phases, namely a primary synthesis phase and a final synthesis phase, and specifically comprises the following steps: subjecting a part of 4-hydroxybutyl vinyl ether to a pre-reaction with a primary synthesis catalyst, adding the pre-reaction product into the rest part of 4-hydroxybutyl vinyl ether, introducing ethylene oxide to carry out primary synthesis so as to obtain a primary product, adding a final synthesis catalyst into a part of the primary product to carry out a secondary pre-reaction, and subjecting the secondary pre-reaction product to final synthesis reactions with the rest part of the primary product and ethylene oxide so as to obtain the final product. The product obtained by the technical scheme provided by the invention has the advantages of low by-product content, narrow molecular weight distribution, and high double-bond protection rate.

Description

technical field [0001] The invention relates to a synthesis method of 4-hydroxybutyl vinyl ether polyoxyethylene ether, which belongs to the technical field of synthesis of polyether compounds in organic chemistry. Background technique [0002] Polycarboxylate water reducer has the advantages of high water reducing rate, small slump loss over time, low dosage, low concrete shrinkage, strong controllable molecular structure and environmental friendliness, which can greatly improve the working performance of concrete , greatly improve the compressive strength and durability of concrete, and are widely used in the field of concrete engineering construction such as railways and bridges. There are two ways to synthesize polycarboxylic acid-based water reducers. One is polyether without unsaturated double bonds, such as polyethylene glycol monomethyl ether MPEG. Acrylic acid is reacted to produce methacrylate or acrylate of polyethylene glycol monomethyl ether, and then it is cop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C04B24/24
Inventor 王胜利金一丰董楠向松柏杜明强
Owner ZHEJIANG LYUKEAN CHEM
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