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Preparation method of initiator for polycarboxylate superplasticizer polyether macromonomer

A technology of polyether macromonomer and water reducer, which is applied in the direction of ether preparation, chemical instruments and methods, and preparation of ether by addition of unsaturated compounds. The effect of shortening the reaction time

Inactive Publication Date: 2021-10-22
安徽海螺材料科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the synthesis process of existing monovinyl macromonomers such as ethylene glycol monovinyl polyoxyethylene ether (EPEG) and 4-hydroxybutyl vinyl polyoxyethylene ether (VPEG) is relatively complicated.

Method used

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  • Preparation method of initiator for polycarboxylate superplasticizer polyether macromonomer
  • Preparation method of initiator for polycarboxylate superplasticizer polyether macromonomer
  • Preparation method of initiator for polycarboxylate superplasticizer polyether macromonomer

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Experimental program
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Effect test

Embodiment 1

[0035] A preparation method for a polycarboxylate water reducer polyether macromonomer starter, comprising the following steps:

[0036] (1) Under a nitrogen protective atmosphere, add 6.0mol (624.9g) neopentyl glycol and 1% neopentyl glycol quality (6.25g) co-catalyst 18-crown-6 in a 2L pressure reactor, and simultaneously add block 16.4g (7% of neopentyl glycol moles) of granular potassium metal is used as a catalyst, heated to 115°C until the potassium metal is completely dissolved;

[0037] (2) Then heat up to 175 ° C, maintain the pressure at 3.5 MPa and continuously feed the acetylene gas with a flow rate of 140 mL / min in the prepared potassium neopentyl glycolate solution, and the reaction residence time is 8 hours;

[0038] (3) After the reaction is finished, cool to normal temperature and replace the acetylene gas in the kettle. The obtained product is distilled at 128°C to remove unreacted neopentyl glycol, and further distilled under reduced pressure at 140-145°C an...

Embodiment 2

[0040] A preparation method for a polycarboxylate water reducer polyether macromonomer starter, comprising the following steps:

[0041] (1) Under a nitrogen protective atmosphere, add 8.0mol (833.2g) neopentyl glycol and 2.5% neopentyl glycol quality (20.8g) cocatalyst 15-crown ether-3 in a 2L pressure reactor, and add block Particle metal potassium 1.73g (0.55% of neopentyl glycol moles) is used as a catalyst, heated to 120°C until metal potassium is completely dissolved;

[0042] (2) Then the temperature was raised to 190°C, and the pressure was maintained at 4.0MPa to continuously feed the acetylene gas with a flow rate of 150mL / min into the prepared potassium neopentyl glycolate solution, and the reaction residence time was 8 hours;

[0043] (3) After the reaction is over, cool to normal temperature and replace the acetylene gas in the kettle. The obtained product is distilled at 128°C to remove unreacted neopentyl glycol, and further distilled under reduced pressure at 1...

Embodiment 3

[0045] A preparation method for a polycarboxylate water reducer polyether macromonomer starter, comprising the following steps:

[0046] (1) Under a nitrogen protective atmosphere, add 7.0mol (729.1g) neopentyl glycol and 2.0% (14.6g) cocatalyst 20-crown ether-4 in a 2L pressure reactor, and add metal potassium 13.65g of block particles simultaneously (5.0% of neopentyl glycol molar number) as catalyst, be heated to 120 ℃ to metal potassium and dissolve completely;

[0047] (2) Then heat up to 180 ° C, maintain the pressure at 2.8 MPa and continuously feed the acetylene gas with a flow rate of 40 mL / min in the prepared potassium neopentyl glycolate solution, and the reaction residence time is 8 hours;

[0048](3) After the reaction is finished, cool to normal temperature and replace the acetylene gas in the kettle. The obtained product is distilled at 128°C to remove unreacted neopentyl glycol, and further distilled under reduced pressure at 140-145°C and 0.066MPa pressure 29...

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Abstract

The invention discloses a preparation method of an initiator for a polycarboxylate superplasticizer polyether macromonomer. The method comprises the following steps: by taking neopentyl glycol and acetylene as reaction raw materials and an alkali metal catalyst as a catalyst, carrying out addition reaction on the reaction raw materials under the catalyst, and carrying out reduced pressure distillation on the obtained product to obtain the initiator monovinyl neopentyl glycol ether for the polycarboxylate superplasticizer polyether macromonomer. The monovinyl neopentyl glycol ether has the condensation reaction with ethylene oxide under the action of a basic catalyst, and glacial acetic acid or phosphoric acid is added for neutralization after the reaction is finished to obtain neopentyl glycol monovinyl polyoxyethylene ether which is suitable for the polycarboxylate superplasticizer polyether macromonomer. The monovinyl neopentyl glycol ether obtained by the invention is used for the polycarboxylate superplasticizer vinyl ether macromonomer and has better wrapping property and winding property, so that the synthesized polycarboxylate superplasticizer has the characteristics of lower doping amount and better adaptability.

Description

technical field [0001] The invention belongs to the technical field of water reducers, and in particular relates to a method for preparing an initiator for polycarboxylate water reducers and polyether macromonomers. Background technique [0002] As the third-generation concrete water-reducing agent, polycarboxylate high-performance water-reducing agent has high water-reducing rate, low dosage, good dispersion, good slump retention, wide application range, green environmental protection, and no "three wastes" in the whole process "Emissions and other advantages are the research hotspots and development trends in the field of concrete admixtures at this stage. Among the polyether macromonomers commonly used in polycarboxylate high-performance water reducers at this stage, methallyl alcohol polyoxyethylene ether (HPEG) and methallyl butanol polyoxyethylene ether (TPEG) products account for the majority of them. the vast majority. With the deepening of technology, monovinyl st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/08C07C43/178C08G65/28C08F283/06C08F220/06C04B24/26B01J23/04B01J31/02C04B103/30
CPCC07C41/08C08G65/2609C08F283/065C04B24/2605B01J23/04B01J31/0204C04B2103/302B01J35/19C08F220/06C07C43/178
Inventor 张瑞涛许庚友陈烽司宏振曾君宋南京姚杰
Owner 安徽海螺材料科技股份有限公司