A kind of unsaturated polyether monomer and its preparation method, application and prepared polymer

A polyether monomer and unsaturated technology, applied in the field of application and prepared polymers, unsaturated polyether monomer and preparation method thereof, can solve the problem of low polymerization activity, single structure of polyether monomer, and concrete retention performance. Not good enough, etc., to achieve the effect of improving retention performance

Active Publication Date: 2019-09-10
联泓(江苏)新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to provide a kind of unsaturated polyether monomer for synthesizing polycarboxylate water reducer and its preparation method and application, to solve the single structure of polyether monomer in the prior art, low polymerization activity, concrete retention performance Not good enough to meet the actual needs of concrete transportation, construction and material quality changes

Method used

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  • A kind of unsaturated polyether monomer and its preparation method, application and prepared polymer
  • A kind of unsaturated polyether monomer and its preparation method, application and prepared polymer
  • A kind of unsaturated polyether monomer and its preparation method, application and prepared polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Under nitrogen protection, put 215 parts of dimethylallyl alcohol in a reaction flask, add 0.45 parts of NaH powder, stir and heat up to 90 ° C, then slowly add 233 parts of butyl glycidyl ether dropwise to the reaction flask at a constant speed, control The reaction temperature is about 90°C, the dropwise addition time is 120 minutes, the temperature is kept for 2 hours after the dropwise addition is completed, and the intermediate (1-1#) is obtained by cooling.

[0062] Add 416 parts of the above-mentioned synthetic intermediate (1-1#) to the reaction kettle, add 7.0 parts of NaH powder, under vacuum conditions, stir and heat up to 120 ° C, slowly feed 970 parts of ethylene oxide into the reaction kettle to carry out In the polymerization reaction, the temperature is maintained at about 120 °C, and the pressure is relatively constant at about 0.4 MPa, until all ethylene oxide is added to the reactor, and the temperature is kept for about 1 hour. material to obtain an ...

Embodiment 2

[0066] Place 300 parts of dimethylallyl alcohol in a three-necked flask with a nitrogen protection device, a thermometer and a stirrer, add 4.5 parts of NaH powder, quickly perform nitrogen replacement, turn on the heating, stir and heat up to 100 ° C, and then add 4.5 parts of NaH powder to the flask. Slowly add 744 parts of butyl glycidyl ether dropwise at a constant speed, control the reaction temperature to 100°C, and dropwise for 180 minutes.

[0067] Add 500 parts of the above-mentioned synthetic intermediate (2-1#) to the autoclave, replace with nitrogen, then under stirring, vacuum the reactor, turn on heating, and slowly feed into the reactor after being warmed up to 120°C 993 parts of ethylene oxide were polymerized, the temperature was maintained at 120°C, and the pressure was relatively constant at about 0.3 MPa, until all the ethylene oxide was added to the reactor, and the temperature was kept for about 1 hour until the pressure of the reactor no longer decreased....

Embodiment 3

[0071]Place 403 parts of dimethylallyl alcohol in a three-necked flask with a nitrogen protection device, a thermometer and a stirrer, add 3.4 parts of NaH powder, quickly carry out nitrogen replacement, turn on the heating, stir and heat up to 100 ° C, then add 3.4 parts of NaH powder to the flask. Slowly add 325 parts of butyl glycidyl ether dropwise at a constant speed, control the reaction temperature to 100°C, dropwise for 180 minutes, keep the temperature for 2 hours after the dropwise addition, and cool to obtain the intermediate (3-1#).

[0072] Then add 360 parts of the above-mentioned synthetic intermediate to the autoclave, add 1.3 parts of sodium hydride, carry out nitrogen replacement, and then under stirring, the reaction kettle is evacuated, the heating is turned on, and the temperature is raised to 120 ℃. Introduce 6375 parts of ethylene oxide to carry out the polymerization reaction, maintain the temperature at 120°C, and keep the pressure relatively constant a...

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Abstract

The invention relates to the technical field of concrete admixtures and in particular relates to an unsaturated polyether monomer, a preparation method and application of the unsaturated polyether monomer, and a polymer prepared thereby. According to the structural design of introducing glycidyl ether into hydrophobic blocks, a certain amount of hydrophobic units and hydrophobic groups are introduced and controlled in a carboxylic copolymer molecular structure, so that the viscidity of a cement-based material is reduced under the action of a water reducing agent, and the dispersion property of the water reducing agent and slump retaining performance are improved. The unsaturated polyether monomer disclosed by the invention comprises multiple polymerization units, and has high double bond retention rate and excellent polymerization activity; by controlling the reaction conditions, the main chain and side chains of the product can be subjected to accurate design at different positions and lengths, so that the prepared water reducing agent is rich in product structure and is slightly influenced by factors such as high-temperature environment change, material quality fluctuation and the like, the concrete workability and high slump retaining performance are maintained, and convenience is brought to production and transportation and construction control.

Description

technical field [0001] The invention relates to the technical field of concrete admixtures, in particular to an unsaturated polyether monomer and its preparation method, application and prepared polymer. Background technique [0002] Concrete water reducer is one of the most widely used and most used additives in concrete admixtures. In recent years, the research and production of concrete admixtures have tended to develop in the direction of high performance, green environmental protection, and no pollution. The polycarboxylate superplasticizer with comb-shaped molecular structure is a high-performance water-reducing agent, because of its high water-reducing rate, good slump retention, low dosage, no pollution, The production process is simple to operate, low cost and other excellent properties, suitable for the preparation of high-strength, ultra-high-strength, high-fluidity and self-compacting concrete, and has become a hot field of research and development for professio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/06C08F228/02C08G65/28C04B24/16C04B103/30
Inventor 朱军成黄海李华威李方
Owner 联泓(江苏)新材料研究院有限公司
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