Synthesis method of methyl allyl alcohol polyethenoxy ether

A technology of methallyl alcohol polyoxyethylene ether and methallyl alcohol, which is applied in the field of synthesis of polyether compounds in organic chemistry

Active Publication Date: 2013-01-30
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]The existing synthesis technology of methallyl alcohol polyoxyethylene ether, the US published patent number is US2003199616, and the patent name is: Cement admixture and cement composition. Under the catalysis of sodium hydroxide, methallyl alcohol reacts with ethylene oxide to generate methallyl alcohol polyoxyethylene ether, but it will produce more by-products such as polyethylene glycol, etc., resulting in a decrease in effective content , Molecular weight distribution widens, double bond retention rate decreases, thus affecting its application performance
The patent number is CN 102134313 A, and the patent name is: the preparation method of methallyl alcohol polyoxyethylene ether introduces the methallyl alcohol under the catalysis of sodium methallylate or potassium methallylate and Ethylene oxide reacts to produce methallyl alcohol polyoxyethylene ether. The amount of catalyst is based on methallyl alcohol, which is 0.1~0.6wt%, which can increase the degree of unsaturation of the product by 10%, but the catalyst methyl The preparation conditions and quality of sodium allyl alcoholate and the addition method of catalyst sodium methallyl alcoholate will still affect the quality of methallyl alcohol polyoxyethylene ether, resulting in the generation of by-products such as polyethylene glycol and the broadening of molecular weight distribution , The double bond retention rate is reduced, thereby reducing the application effect of methallyl alcohol polyoxyethylene ether

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for synthesizing methallyl alcohol polyoxyethylene ether in this embodiment includes the following steps: 1) Add 21.6 parts of methallyl alcohol into the reaction kettle, add 0.45 parts of catalyst metal sodium within 30 minutes, and control The reaction temperature is 20~30°C, and the reaction time is 0.5h; after the reaction, put the product into 410.4 parts of methallyl alcohol, replace it with nitrogen, raise the temperature to 90°C, and feed 1368 parts of ethylene oxide to control the reaction temperature 90~105°C, the reaction time is 4.0h; after the reaction, the temperature is lowered to 70°C and the material is discharged to obtain a methallyl alcohol polyoxyethylene ether oligomer with a molecular weight of 300; 2) Add 90 parts of the above-mentioned Step 1) To obtain the methallyl alcohol polyoxyethylene ether oligomer with a molecular weight of 300, add 1.8 parts of catalyst sodium metal within 30 minutes, control the reaction temperature at 30~40°C,...

Embodiment 2

[0032]The synthesis method of a kind of methallyl alcohol polyoxyethylene ether of the present embodiment comprises the following steps: 1) add 17.9 parts of methallyl alcohol in the reaction kettle, add 0.32 parts of catalyst metal potassium in 50 minutes, control The reaction temperature is 25~35°C, and the reaction time is 0.5h; after the reaction, put the product into 198.1 parts of methallyl alcohol, replace it with nitrogen, raise the temperature to 90°C, and feed 834 parts of ethylene oxide to control the reaction temperature 90~105°C, the reaction time is 5.0h; after the reaction, the temperature is lowered to 70°C and the material is discharged to obtain a methallyl alcohol polyoxyethylene ether oligomer with a molecular weight of 350; 2) Add 84 parts of the above-mentioned Step 1) For the obtained methallyl alcohol polyoxyethylene ether oligomer with a molecular weight of 350, add 2.4 parts of catalyst metal potassium within 50 minutes, control the reaction temperatur...

Embodiment 3

[0039] A method for synthesizing methallyl alcohol polyoxyethylene ether in this embodiment includes the following steps: 1) Add 17 parts of methallyl alcohol into the reaction kettle, add 0.21 parts of sodium metal and 0.21 parts of sodium metal in 50 minutes Metal potassium catalyst, the reaction temperature is controlled at 30~40°C, and the reaction time is 0.8h; after the reaction, the product is put into 155.8 parts of methallyl alcohol, replaced by nitrogen, the temperature is raised to 90°C, and 656 parts of ethylene oxide are introduced Alkanes, the reaction temperature is controlled at 90~105°C, and the reaction time is 5.5h; after the reaction, the temperature is lowered to 70°C and the material is discharged to obtain a methallyl alcohol polyoxyethylene ether oligomer with a molecular weight of 350; 2) Add 84 parts of the methallyl alcohol polyoxyethylene ether oligomer with a molecular weight of 350 obtained in the step 1) described above, add 1.5 parts of metal sod...

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Abstract

The invention discloses a synthesis method of methyl allyl alcohol polyethenoxy ether, which comprises the following steps: 1) reacting 5-20 wt% of prescribed methyl allyl alcohol and a catalyst, adding the reaction product into residual prescribed methyl allyl alcohol, and introducing epoxyethane to react, thereby obtaining methyl allyl alcohol polyethenoxy ether low polymer; and 2) reacting 5-20 wt% of prescribed methyl allyl alcohol polyethenoxy ether low polymer obtained in the step 1) and a catalyst, adding the reaction product into residual prescribed methyl allyl alcohol polyethenoxy ether low polymer, and introducing epoxyethane to react, thereby obtaining the methyl allyl alcohol polyethenoxy ether. The methyl allyl alcohol polyethenoxy ether product prepared by the method disclosed by the invention has the advantages of low content of byproducts (polyethyleneglycol and the like), narrow molecular weight distribution, high double-bond protective rate and the like, and is suitable for synthesizing polycarboxylic-acid high-performance water reducing agents.

Description

technical field [0001] The invention relates to a synthesis method of methallyl alcohol 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 copolymerize...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
Inventor 王胜利金一丰马定连万庆梅董楠
Owner ZHEJIANG HUANGMA TECH
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