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Preparation method of polycarboxylate water reducer macromonomer methallyl alcohol polyoxyethylene ether

A technology of methallyl alcohol polyoxyethylene ether and methallyl alcohol, which is applied in the field of preparation of polycarboxylate superplasticizer macromonomer methallyl alcohol polyoxyethylene ether, and can solve the difficulty of controlling the reaction process Large, prone to production accidents, complicated production process, etc., to achieve the effect of narrow relative molecular weight distribution, shortened production cycle, and simple production process

Active Publication Date: 2014-06-25
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

Because methallyl alcohol, the raw material of methallyl alcohol polyoxyethylene ether, has double bonds, is easy to polymerize, has low boiling point, and is easy to gasify, etc., the reaction process is easy to overpressure, overtemperature, and production accidents are easy to occur. Therefore, The production process is relatively complicated, and the control of the reaction process is difficult

Method used

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  • Preparation method of polycarboxylate water reducer macromonomer methallyl alcohol polyoxyethylene ether
  • Preparation method of polycarboxylate water reducer macromonomer methallyl alcohol polyoxyethylene ether

Examples

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Effect test

Embodiment 1

[0032] Preparation of methallyl alcohol polyoxyethylene (55) ether:

[0033] Catalyst preparation: Add 1.39mol (100g) methallyl alcohol to a 100ml round-bottomed single-necked flask, put it on an electromagnetic stirrer with a water bath, and slowly add 0.0695mol (2.65g) lithium aluminum tetrahydride, the reaction temperature is 30°C, After 2 hours of reaction, the catalyst was prepared after the reaction was complete.

[0034] Add 1.39mol (100g) methallyl alcohol and the above-mentioned catalyst in 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., 22.24 mol (979 g) of ethylene oxide is passed through for 4 hours, and the reaction is continued for 0.5 hours. Then add 2 g of potassium hydroxide, stir and heat up to 100-110° C., feed 130.6 mol (5749 g) of ethylene oxide for 8 hours, and continue the reaction for 0.5 hour...

Embodiment 2

[0036] Preparation of methallyl alcohol polyoxyethylene (57) ether:

[0037] Catalyst preparation: Add 1.39mol (100g) methallyl alcohol to a 100ml round-bottomed single-necked flask, put it on an electromagnetic stirrer with a water bath and slowly add 0.139mol (5.28g) lithium aluminum tetrahydride, the reaction temperature is 20°C, After 3 hours of reaction, the catalyst was prepared after the reaction was complete.

[0038] Add 1.39mol (100g) methallyl alcohol and the above-mentioned catalyst in 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., 55.6 mol (2447 g) of ethylene oxide is passed through for 4 hours, and the reaction is continued for 0.5 hours. Then add 2g of sodium hydroxide, stir and raise the temperature to 110-120°C, and feed 102.9mol (4526g) of ethylene oxide for 8 hours to continue the reaction for 0....

Embodiment 3

[0040] Preparation of methallyl alcohol polyoxyethylene (60) ether:

[0041] Catalyst preparation: Add 1.39mol (100g) methallyl alcohol to a 100ml round-bottomed single-necked flask, put it on an electromagnetic stirrer with a water bath, and slowly add 0.104mol (3.97g) lithium aluminum tetrahydride, the reaction temperature is 10°C, After 5 hours of reaction, the catalyst was prepared after the reaction was complete.

[0042] Add 1.39mol (100g) methallyl alcohol and the above-mentioned catalyst in 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., 38.92 mol (1713 g) of ethylene oxide is passed through for 4 hours, and the reaction is continued for 0.5 hours. Then add 1 g of sodium hydroxide and 1 g of potassium hydroxide, stir and heat up to 105-115° C., feed 127.9 mol (5627 g) of ethylene oxide for 8 hours, and contin...

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Abstract

The invention relates to a polycarboxylate water reducer and specifically relates to a preparation method of polycarboxylate water reducer macromonomer methallyl alcohol polyoxyethylene ether. The method comprises the following steps: performing condensation reaction with ethylene oxide by taking lithium aluminum tetrahydride as a catalyst and taking an intermediate product obtained by reaction of methallyl alcohol and lithium aluminum tetrahydride and methallyl alcohol as raw materials to obtain a methallyl alcohol oligomer, further enabling the methallyl alcohol oligomer to perform condensation reaction with the added ethylene oxide under the action of an alkaline catalyst, terminating with propylene oxide, and adding glacial acetic acid to neutralize to obtain methallyl alcohol polyoxyethylene ether. The preparation method provided by the invention has the advantages of simple process, safety, low reaction temperature, short reaction time and low production cost; and obtained methallyl alcohol polyoxyethylene ether has narrow distribution of relative molecular weight and high retention rate of double bonds.

Description

technical field [0001] The invention relates to a polycarboxylate water reducer, in particular to a method for preparing a polycarboxylate water reducer macromonomer methallyl alcohol polyoxyethylene ether. Background technique [0002] With the rapid development of the national economy, the amount of domestic construction is also increasing. The construction of various civil, railway, highway, bridge, tunnel, hydropower, seaport, wharf, airport and other major and key projects cannot do without high performance concrete. , Self-compacting concrete, high-strength concrete, and high-fluidity concrete, the amount of concrete required is increasing, and the quality requirements are increasing. The production of various performance concrete is inseparable from high-performance water reducing agents. [0003] Polycarboxylate high-performance water-reducing agent is called the third-generation concrete water-reducing agent. It has low dosage, high water-reducing rate, large degree...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/331C08G65/28
Inventor 王建军王双平
Owner 山东卓星化工有限公司
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