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Preparation method of macromonomer with Y-shaped structure

A technology of macromonomers and intermediates, which is applied in the field of preparation of macromonomers with Y-shaped structure, can solve problems such as affecting copolymerization, affecting copolymerization reaction, and unsatisfactory actual performance, and achieves the effect of improving yield and good homogeneity

Pending Publication Date: 2021-07-13
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the polyether long chain before modification, the long chain of this polycarboxylic acid molecule can extend wider, and the steric hindrance effect is greatly enhanced; but the actual performance is still unsatisfactory, the main reason is that the catalyst used in the esterification process has a negative effect on Toluenesulfonic acid has strong acidity, and it is easy to destroy the double bond of polyoxyethylene ether at the high temperature required for esterification reaction, thereby affecting the subsequent copolymerization reaction, and the actual effect of using hydroquinone and other polymerization inhibitors is not ideal. Its residual components will also affect the subsequent copolymerization

Method used

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  • Preparation method of macromonomer with Y-shaped structure
  • Preparation method of macromonomer with Y-shaped structure
  • Preparation method of macromonomer with Y-shaped structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Mix 800 parts by mass of isobutylene polyoxyethylene ether (HPEG) with a molecular weight of 2400 and 176.12 parts by mass of glyceric acid with a molecular weight of 176.12, heat up to 110° C. under a nitrogen atmosphere, and add 14.64 parts by mass of 4-dimethylaminopyridine ( DMAP), the process nitrogen removes the by-product water of the esterification reaction, and reacts for 5h to obtain a mixture of carboxyl-terminated esterification product and unreacted glyceric acid. Weigh 120 parts by mass of the aforementioned mixture, add 50 parts by mass of water to dissolve, then add 50 parts by mass of ethyl bromide, shake to make it evenly mixed, let stand for 30min, keep the ethyl bromide phase after the liquid level is layered, and then add Add 30 parts by mass of water into the ethyl bromide phase, oscillate to mix evenly, let stand for 0.5h, keep the ethyl bromide phase after the liquid level is separated, and then remove the solvent in the ethyl bromide phase by rot...

Embodiment 2

[0037] Mix 800 parts by mass of isobutylene polyoxyethylene ether (HPEG) with a molecular weight of 2400 and 176.12 parts by mass of glyceric acid with a molecular weight of 176.12, heat up to 110° C. under a nitrogen atmosphere, and add 9.76 parts by mass of 4-dimethylaminopyridine ( DMAP), the process nitrogen removes the by-product water of the esterification reaction, and reacts for 5h to obtain a mixture of Y-type intermediate and unreacted glyceric acid. Weigh 120 parts by mass of the aforementioned mixture, add 50 parts by mass of water to dissolve, then add 50 parts by mass of ethyl bromide, shake to make it evenly mixed, let stand for 30min, keep the ethyl bromide phase after the liquid level is layered, and then add Add 30 parts by mass of water into the ethyl bromide phase, oscillate to mix evenly, let stand for 0.5h, keep the ethyl bromide phase after the liquid level is separated, and then remove the solvent in the ethyl bromide phase by rotary evaporation to obtai...

Embodiment 3

[0039] Mix 800 parts by mass of isobutylene polyoxyethylene ether (HPEG) with a molecular weight of 2400 and 176.12 parts by mass of glyceric acid with a molecular weight of 176.12, heat up to 110° C. under a nitrogen atmosphere, and add 19.52 parts by mass of 4-dimethylaminopyridine ( DMAP), the process nitrogen removes the by-product water of the esterification reaction, and reacts for 5h to obtain a mixture of Y-type intermediate and unreacted glyceric acid. Weigh 120 parts by mass of the aforementioned mixture, add 50 parts by mass of water to dissolve, then add 50 parts by mass of ethyl bromide, shake to make it evenly mixed, let stand for 30min, keep the ethyl bromide phase after the liquid level is layered, and then add Add 30 parts by mass of water into the ethyl bromide phase, oscillate to mix evenly, let stand for 0.5h, keep the ethyl bromide phase after the liquid level is separated, and then remove the solvent in the ethyl bromide phase by rotary evaporation to obta...

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Abstract

The invention discloses a preparation method of a macromonomer with a Y-shaped structure. According to the invention, 4-dimethylaminopyridine and / or triethylamine is used as an esterification catalyst to prepare the macromonomer with the Y-type structure, so the defect of low polymerization activity of an esterification product in the prior art is greatly improved; and the obtained macromonomer with the Y-type structure has good polymerization reaction activity with acrylic acid. The macromonomer mixture with the Y-type structure prepared by the method is used for preparing a Y-type side-chain polycarboxylic acid water reducing agent, and the intrinsic viscosity of the obtained water reducing agent is 10-20 mL / g and can reach 20.19 mL / g to the maximum; the Y-type side-chain polycarboxylic acid water reducing agent has better dispersing performance, and the highest fluidity of neat paste can reach 318 mm when a doping amount is 0.2 wt%; when the doping amount is 0.3 wt%, a water reducing rate can reach 25.32%, and the standard of a current commercial high-efficiency water reducing agent is met; the 28-day compressive strength ratio of the macromonomer can reach 128.3%; and concrete obtained after mixing has good homogeneity and workability.

Description

technical field [0001] The invention belongs to the technical field of concrete water reducers, and in particular relates to a preparation method of a Y-shaped structure macromonomer. Background technique [0002] As the latest generation of high-performance water reducer, polycarboxylate water reducer has the characteristics of low dosage, high water reducing rate, environmental friendliness, and strong structural design. With the continuous advancement of large-scale projects such as bridges at home and abroad, its proportion in the water reducing agent market has increased year by year, and it has become the most mainstream water reducing agent product at present. [0003] Most of the early polycarboxylate superplasticizers were polyester-based products, and the necessary esterification process had harsh reaction conditions, high energy consumption, and low esterification efficiency. Nippon Shokubai Co., Ltd. has done a lot of work in improving the synthesis process of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08F283/06C08F220/06C08G65/332C04B24/26C04B103/30
CPCC08G81/00C08F283/065C08G65/3322C04B24/2641C04B2103/30
Inventor 楼宏铭刘海周天凤金宇庞煜霞邱学青
Owner SOUTH CHINA UNIV OF TECH
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