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Preparation method of polycarboxylic acid water reducer macromonomer ethylene glycol monovinyl polyoxyethylene ether

A technology of ethylene glycol monovinyl polyoxyethylene ether and ethylene glycol monovinyl ether is applied in the field of preparation of polycarboxylate water reducing agent macromonomer ethylene glycol monovinyl polyoxyethylene ether, which can solve the problem of Reaction control accuracy requirements are high, double bond retention rate decreases, molecular weight distribution broadens, etc., to achieve the effect of narrow relative molecular weight distribution, high double bond retention rate, and improved application performance

Inactive Publication Date: 2019-07-12
山东卓星化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its ethoxylation is prepared by a one-step method, which also has the problems of high precision of reaction control, changes in temperature, pressure and catalytic rate, etc., which may easily lead to a decrease in the retention rate of double bonds and a broadening of the molecular weight distribution.

Method used

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  • Preparation method of polycarboxylic acid water reducer macromonomer ethylene glycol monovinyl polyoxyethylene ether
  • Preparation method of polycarboxylic acid water reducer macromonomer ethylene glycol monovinyl polyoxyethylene ether

Examples

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Effect test

Embodiment 1

[0033] The preparation of ethylene glycol monovinyl polyoxyethylene (46) ether:

[0034] Catalyst preparation: Add 1.135mol (100g) ethylene glycol monovinyl ether to a 100ml round-bottom single-necked flask, put it on an electromagnetic stirrer with a water bath and slowly add 0.0908mol (2.65g) lithium tetrahydrogen, and the reaction temperature is 25 °C, reacted for 2.5 hours, and prepared a catalyst after the reaction was complete.

[0035] Add 1.135mol (100g) ethylene glycol monovinyl ether and the above-mentioned catalyst into a 10L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. The air in the kettle was replaced with nitrogen for 3 times, and when the temperature of the kettle rose to 80-85°C, 68.1mol (3000g) of ethylene oxide was passed through for 3.5 hours, and the reaction was continued for 1 hour. Then add 3.03g of sodium hydride, stir and raise the temperature to 100-120°C, and then feed 158.9mol (7000g) of ethylene oxide fo...

Embodiment 2

[0037] The preparation of ethylene glycol monovinyl polyoxyethylene (53) ether:

[0038] Catalyst preparation: Add 1.135mol (100g) ethylene glycol monovinyl ether to a 100ml round-bottom single-necked flask, put it on an electromagnetic stirrer with a water bath and slowly add 0.1135mol (4.31g) lithium tetrahydrogen, and the reaction temperature is 20 °C, react for 3 hours, and prepare the catalyst after the reaction is complete.

[0039] Add 1.135mol (100g) ethylene glycol monovinyl ether and the above-mentioned catalyst into a 10L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. Replace the air in the kettle with nitrogen for 3 times, and when the temperature of the kettle rises to 80-85° C., 90.8 mol (4000 g) of ethylene oxide is passed through for 3.5 hours, and the reaction is continued for 0.5 hours. Then add 6.05g of sodium hydride, stir to raise the temperature to 100-120°C, and feed 181.6mol (8000g) of ethylene oxide for 8 hours...

Embodiment 3

[0041] The preparation of ethylene glycol monovinyl polyoxyethylene (55) ether:

[0042] Catalyst preparation: Add 50 (100 g) ethylene glycol monovinyl ether into a 100 ml round-bottomed single-necked flask, put it into an electromagnetic stirrer with a water bath and slowly add 0.102 mol (3.87 g) lithium aluminum tetrahydride, and the reaction temperature is 15°C , reacted for 4h, and the catalyst was prepared after the reaction was complete.

[0043] Add 1.135mol (100g) ethylene glycol monovinyl ether and the above-mentioned catalyst into a 10L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. Replace the air in the kettle with nitrogen for 3 times, and when the temperature of the kettle rises to 80-85° C., 56.75 mol (2500 g) of ethylene oxide is passed through for 4 hours, and the reaction is continued for 0.5 hours. Then add 0.91 sodium hydride and 0.91 sodium, stir and raise the temperature to 100-120°C, and feed 147.55 mol (6500 g) of...

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Abstract

The invention relates to a polycarboxylic acid water reducer, and concretely relates to a preparation method of a polycarboxylic acid water reducer macromonomer ethylene glycol monovinyl polyoxyethylene ether. The method comprises the following steps: reacting ethylene glycol monovinyl ether with lithium aluminum hydride to obtain a catalyst, carrying out a condensation reaction on the ethylene glycol monovinyl ether and ethylene oxide under the action of the catalyst to obtain an ethylene glycol monovinyl ether oligomer, carrying out a condensation reaction on the ethylene glycol monovinyl ether oligomer and ethylene oxide under the action of an alkaline catalyst, performing termination with epoxypropane, and adding glacial acetic acid to neutralize in order to obtain the ethylene glycolmonovinyl polyoxyethylene ether. The ethylene glycol monovinyl polyoxyethylene ether obtained in the invention has the advantages of narrow relative molecular weight distribution, high double-bond reservation rate, simple process, safety, low reaction temperature, short reaction time and low production cost.

Description

technical field [0001] The invention relates to a polycarboxylate water reducer, in particular to a method for preparing a polycarboxylate water reducer macromonomer ethylene glycol monovinyl polyoxyethylene ether. Background technique [0002] With the rapid development of the national economy, high-performance concrete, self-compacting concrete, high-strength concrete and high-fluidity concrete are used as building materials for civil, railway, highway, bridge, tunnel, hydropower, seaport, wharf, airport and other major and key projects Demand has grown rapidly. High-performance water-reducing agent has important application value as an indispensable component in various performance concrete. [0003] As the third generation of concrete superplasticizer, polycarboxylate high-performance superplasticizer has high water reducing rate, low dosage, large degree of freedom in molecular structure design, good dispersion, good slump retention, wide application range, and environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
CPCC08G65/2609
Inventor 王双平王建军
Owner 山东卓星化工有限公司
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