Preparation method of polyether macromonomer for polycarboxylate water reducer

A technology of polyether macromonomer and water reducing agent, which is applied in the field of synthesis of methallyl atactic polyether, and achieves the effects of high effective content, simple operation and stable quality

Active Publication Date: 2018-04-20
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the above-mentioned defects in the synthesis process of existing superplasticizer macromonomers, the present invention provides a random po

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Add 28.8 parts of methallyl alcohol into the reaction kettle, add 2.4 parts of catalyst metal sodium within 30 minutes, control the reaction temperature at 20-30°C, and the reaction time is 0.5-1.0 hours; after the reaction, put the product into In 259.2 parts of methallyl alcohol, replace with nitrogen, raise the temperature to 70°C, feed 638.4 parts of ethylene oxide and 273.6 parts of propylene oxide, control the reaction temperature at 70-95°C, and the reaction time is 3.0-4.0 hours; the reaction is over After cooling down to 70°C, a methallyl oligomer with a molecular weight of 300 was obtained.

[0031] 2) Add 540 parts of the methallyl oligomer with a molecular weight of 300 obtained in step 1) to the reactor, add 0.3 parts of catalyst 18-crown-6 and 1.5 parts of hexachlorocyclotri Phosphazene, control the reaction temperature at 30-50°C, and the reaction time is 0.5-1.0 hours; after the reaction is completed, replace with nitrogen, raise the temperature to 80...

Embodiment 2

[0034] 1) Add 25.2 parts of methallyl alcohol to the reaction kettle, add 3.7 parts of catalyst metal potassium within 30 minutes, control the reaction temperature at 25-30°C, and the reaction time is 0.5-1.0 hours; after the reaction, put the product into In 226.8 parts of methallyl alcohol, replace with nitrogen, raise the temperature to 70°C, feed 681.1 parts of ethylene oxide and 291.9 parts of propylene oxide, control the reaction temperature at 70-95°C, and the reaction time is 3.0-4.0 hours; the reaction is over After cooling down to 70°C, a methallyl oligomer with a molecular weight of 350 was obtained.

[0035] 2) Add 315 parts of the methallyl oligomer with a molecular weight of 350 obtained in step 1) to the reactor, add 0.35 parts of catalyst 18-crown-6 and 2.1 parts of hexachlorocyclotriacetate within 30 minutes For phosphazene, control the reaction temperature at 30-50°C, and the reaction time is 0.5-1.0 hours; after the reaction is completed, replace with nitrog...

Embodiment 3

[0038] 1) Add 21.6 parts of methallyl alcohol into the reaction kettle, add 1.8 parts of catalyst metal sodium and 2.4 parts of metal potassium within 30 minutes, control the reaction temperature at 30-40 ° C, and the reaction time is 0.5-1.0 hours; after the reaction Put the product into 194.4 parts of methallyl alcohol, replace it with nitrogen, raise the temperature to 80°C, feed 787.2 parts of ethylene oxide and 196.8 parts of propylene oxide, control the reaction temperature at 80-95°C, and the reaction time is 3.0- 4.0 hours; after the completion of the reaction, the temperature was lowered to 70° C. and discharged to obtain a methallyl oligomer with a molecular weight of 400.

[0039] 2) Add 300 parts of the methallyl oligomer with a molecular weight of 400 obtained in step 1) to the reactor, add 0.4 parts of catalyst 15-crown-5 and 2.3 parts of hexachlorocyclotriacetate within 30 minutes For phosphazene, control the reaction temperature at 35-55°C, and the reaction time ...

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Abstract

The invention discloses a preparation method of a polyether macromonomer for a polycarboxylate water reducer. The preparation method comprises the following steps: (1) taking a part of methyl allyl alcohol to react with a catalyst one, then putting a reacted product into the remaining methallyl alcohol, and introducing ethylene oxide and propylene oxide for reaction, so that a methylallyl random oligomer is obtained; and (2) allowing the methylallyl random oligomer to react with a catalyst two and a catalyst three, and then introducing ethylene oxide and propylene oxide for reaction; wherein the catalyst one is one or more of sodium, potassium and sodium hydride; the catalyst two is one or more of 18-crown-6 and 15-crown-5; and the catalyst three is phosphonitrilic chloride trimer. Compared with the prior art, the preparation method of the polyether macromonomer for the polycarboxylate water reducer has the advantages that the effective content is high, the by-product content is low, the molecular weight distribution is narrow, the double bond retention rate is high, and the likes, wherein a molecular weight distribution coefficient is less than 1.05, and the double bond retentionrate is greater than 98.0%.

Description

technical field [0001] The invention relates to a method for synthesizing methallyl atactic polyether, which belongs to the technical field of organic compound synthesis. Background technique [0002] With the development of construction technology, the continuous improvement of construction technology requirements and the rapid development of concrete technology, the level of polycarboxylate high-performance water reducer and its application technology in my country has been continuously improved. Polycarboxylate superplasticizer has outstanding advantages such as low dosage, good slump retention performance, low concrete shrinkage rate, strong molecular structure adjustability, high performance potential, and clean production process, which can greatly improve the working performance of concrete , greatly improve the compressive strength and durability of concrete, and are widely used in concrete engineering construction fields such as railways, highways, construction, por...

Claims

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Application Information

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IPC IPC(8): C08G65/26C04B24/32
CPCC04B24/32C04B2103/302C08G65/2609C08G65/2684C08G65/2696
Inventor 向松柏王月芬金一丰万庆梅董楠赵兴军
Owner ZHEJIANG HUANGMA TECH
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