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Methylallyl alcohol random polyether and preparation method thereof

A technology of methallyl alcohol and random polyether, which is applied in the field of methallyl alcohol random polyether and its preparation, which can solve the problem that the reaction is difficult to control, cannot explain the polymer surfactant, the variety of monomers, etc. problems, to reduce the chemical process time, save the investment of slicing equipment, and improve the dispersion performance.

Active Publication Date: 2017-09-26
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For polymer copolymer superplasticizers, because the HLB theory cannot reflect the degree of polymerization of the copolymer, it cannot explain the polymer surfactant and is not applicable; and under the condition that the existing polycarboxylate superplasticizer macromonomer is fixed, Experts and scholars use small molecular monomers, such as methacrylic acid, acrylic acid, sodium methacrylate sulfonate, hydroxyethyl acrylate, etc. to design the hydrophilic-lipophilic balance value of polycarboxylate superplasticizers. Due to the variety of monomers, The reaction is difficult to control

Method used

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  • Methylallyl alcohol random polyether and preparation method thereof
  • Methylallyl alcohol random polyether and preparation method thereof
  • Methylallyl alcohol random polyether and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0051] A kind of preparation method of methallyl alcohol random polyether of the present embodiment, comprises the steps:

[0052] 1) Add 21.6 parts by weight of methallyl alcohol into the reaction kettle, add 0.45 parts by weight of catalyst metal sodium within 30 minutes, control the reaction temperature to 20-30°C, and the reaction time is 0.5h; after the reaction, put the product into In 411 parts by weight of methallyl alcohol, nitrogen is replaced, the temperature is raised to 90°C, and a mixture of 1970.7 parts by weight of ethylene oxide and propylene oxide (mass ratio is about 69:47) is introduced, and the reaction temperature is controlled to be 90-90°C. 105°C, the reaction time is 4.0h; after the reaction, the temperature is lowered to 40°C and discharged to obtain a methallyl alcohol random polyether oligomer with a molecular weight of 400.

[0053] 2) Add 90 parts by weight of step 1) in the reaction kettle to obtain the methallyl alcohol random polyether oligomer...

Embodiment 2

[0055] A kind of preparation method of methallyl alcohol random polyether of the present embodiment, comprises the steps:

[0056] 1) Add 18.8 parts by weight of methallyl alcohol into the reactor, add 0.32 parts by weight of catalyst metal potassium within 50 minutes, control the reaction temperature to 25-35°C, and the reaction time is 0.5h; after the reaction, put the product into In 200.5 parts by weight of methacrylic acid, replace with nitrogen, raise the temperature to 90°C, feed 1151.3 parts by weight of a mixture of ethylene oxide and propylene oxide (mass ratio is about 138:103), and control the reaction temperature to 90-105 °C, the reaction time is 5.0 h; after the reaction, the temperature is lowered to 40 °C and discharged to obtain a methallyl alcohol random polyether oligomer with a molecular weight of 450.

[0057] 2) Add 84 parts by weight of step 1) in the reaction kettle to obtain the molecular weight of methallyl alcohol random polyether oligomer of 450, a...

Embodiment 3

[0059] A kind of preparation method of methallyl alcohol random polyether of the present embodiment, comprises the steps:

[0060]1) Add 17 parts by weight of methallyl alcohol into the reaction kettle, add 0.21 parts by weight of sodium metal and 0.21 parts by weight of metal potassium catalyst within 50 minutes, control the reaction temperature to 30-40 °C, and the reaction time is 0.8h; the reaction is over Then put the product into 159.4 parts by weight of methallyl alcohol, replace it with nitrogen, raise the temperature to 90°C, and feed in a mixture of 926.1 parts by weight of ethylene oxide and alkoxypropane (mass ratio is about 345:262), The reaction temperature is controlled at 90-105°C, and the reaction time is 5.5h; after the reaction, the temperature is lowered to 40°C and discharged to obtain a methallyl alcohol random polyether oligomer with a molecular weight of 450.

[0061] 2) Add 84 parts by weight of the methallyl alcohol random polyether oligomer with mole...

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Abstract

The invention relates to methylallyl alcohol random polyether and a preparation method thereof, and belongs to polyether compound synthesis in organic chemistry. The method comprises the following steps: firstly, ensuring methylallyl alcohol with the prescription dosage being 5 to 20 percent to be reacted with a catalyst I, putting the methylallyl alcohol into the rest methylallyl alcohol, leading ethylene oxide and propene oxide mixed according to a specific ration into the methylallyl alcohol, and obtaining methylallyl alcohol random polyether low polymer with the molecular weight being 400 to 1000 after reaction; secondly, enabling 5 to 20 percent of methylallyl alcohol random polyether low polymer obtained in the first step to be reacted with a catalyst II, putting the methylallyl alcohol random polyether low polymer into the rest methylallyl alcohol random polyether low polymer, feeding ethylene oxide and propene oxide mixed according to a specific ration into the methylallyl alcohol random polyether low polymer, and obtaining methylallyl alcohol random polyether with the molecular weight being M after reaction. The methylallyl alcohol random polyether is applied to the synthesis of a polycarboxylate superplasticizer to be applied to a concrete additive, and has the advantages of good cement dispersity and good solubility with other compounds.

Description

technical field [0001] The invention relates to a methallyl alcohol random polyether and a preparation method thereof, and belongs to the technical field of synthesis of polyether compounds in organic chemistry. Background technique [0002] China's understanding and pilot research on polycarboxylic acid-based high-performance water reducers gradually began at the beginning of this century. Although it started late, due to the simultaneous introduction of some relevant support policies by the state, which laid the foundation for the preparation of high-performance water reducers, batches of research results have been released one after another. For example, Li Yongde and Li Chongzhi of Tsinghua University successfully developed acrylic acid, polyethylene glycol, and allyl sulfonate series of water reducing agents; Hu Jianhua of Fudan University used polyethylene glycol, maleic acid phenol, acrylic acid, etc. Copolymers of various functional groups, and then prepare water re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08F283/06C08F220/06C04B24/26C04B103/30
CPCC04B24/2605C08F283/065C08G65/2609C04B2103/302C08F220/06
Inventor 董楠金一丰尹红王新荣万庆梅向松柏
Owner ZHEJIANG HUANGMA TECH
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