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Synthesis method of hyperbranched unsaturated polyoxyethylene ether as well as product and application thereof

A technology of polyoxyethylene ether and synthesis method, which is applied in the synthesis of unsaturated polyoxyethylene ether and the field of hyperbranched unsaturated polyoxyethylene ether, which can solve the problem of being unable to further increase the molecular chain density and relative molar ratio of polyoxyethylene ether Can not be further improved, polycarboxylate water reducer performance bottleneck and other problems, to achieve excellent retarding effect, broad application prospects and market potential, high water reducing rate effect

Active Publication Date: 2017-11-24
SHANGHAI TAIJIE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, in the prior art, the unsaturated polyoxyethylene ether used as the reaction raw material of the polycarboxylate water reducer generally has a single straight chain structure or a double straight chain structure, and this unsaturated polyoxyethylene ether is synthesized as the reaction raw material The relative molar ratio of the linear polyoxyethylene ether molecular structure of the polycarboxylate water reducer cannot be further increased. There is a performance bottleneck in the water agent, so it is difficult to meet the high index demand for polycarboxylate water reducers in actual construction projects

Method used

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  • Synthesis method of hyperbranched unsaturated polyoxyethylene ether as well as product and application thereof
  • Synthesis method of hyperbranched unsaturated polyoxyethylene ether as well as product and application thereof
  • Synthesis method of hyperbranched unsaturated polyoxyethylene ether as well as product and application thereof

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preparation example Construction

[0022] According to the synthetic method of the hyperbranched unsaturated polyoxyethylene ether of the first aspect, comprise the following steps: S1: add polyhydroxyl compound and unsaturated carboxylic acid X in reaction container:

[0023]

[0024] Wherein, R is H or an alkyl group of C1-C8; an esterification catalyst and a polymerization inhibitor are added, and an esterification reaction is carried out at a reaction temperature of 65°C-95°C to obtain intermediate A; wherein, the esterification The catalyst is p-toluenesulfonic acid, and the polymerization inhibitor is hydroquinone or / and p-quinone; S2: adding the intermediate A, ethylene oxide, and anionic ring-opening polymerization to the pressurized reaction device Catalyst, under the reaction temperature of 160 DEG C to 185 DEG C and the pressure in the reaction vessel of 0.15 Mpa to 0.25 Mpa, the anionic ring-opening polymerization reaction is carried out to obtain the hyperbranched unsaturated polyoxyethylene ethe...

Embodiment 1

[0035] S1: Add 500 g of tetramethanol, 380 g of acrylic acid, 10 g of p-toluenesulfonic acid, and 1.2 g of hydroquinone into the reaction vessel, and mechanically stir for 5 hours at a reaction temperature of 80° C. to complete the esterification reaction to obtain intermediate A1;

[0036] S2: Add 150g of the intermediate A1, 2000g of ethylene oxide, and 20g of sodium ethoxide to the pressurized reaction device, and carry out anionic ring-opening polymerization reaction at a reaction temperature of 170°C and a pressure of 0.15Mpa in the reaction vessel. The time is 6 hours, and the hyperbranched unsaturated polyoxyethylene ether P1 is prepared.

Embodiment 2

[0038] S1: Add 550g of pentaerythritol, 500g of methacrylic acid, 15g of p-toluenesulfonic acid and 1.8g of p-quinone to the reaction vessel, and mechanically stir for 4.5h at a reaction temperature of 90°C to complete the esterification reaction and obtain intermediate A2 ;

[0039] S2: Add 175g of the intermediate A2, 3000g of ethylene oxide, and 25g of potassium ethylate to the pressurized reaction device, and carry out anionic ring-opening polymerization at a reaction temperature of 165°C and a pressure of 0.20Mpa in the reaction vessel. The time is 5.5h, and the hyperbranched unsaturated polyoxyethylene ether P2 is prepared.

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Abstract

The invention provides a synthesis method of hyperbranched unsaturated polyoxyethylene ether, hyperbranched unsaturated polyoxyethylene ether obtained by adopting the synthesis method and application thereof. The synthesis method mainly comprises the steps of firstly, carrying out esterification reaction on a polyhydroxy compound and unsaturated carboxylic acid, wherein massive hydroxyls are reserved in the obtained ester intermediate; then in presence of an anionic ring opening polymerization catalyst, carrying out anionic ring opening polymerization on the ester intermediate and ethylene oxide, thus obtaining the target product. A polycarboxylic acid water reducer which has higher polyoxyethylene ether molecular chain density and is prepared by taking the hyperbranched unsaturated polyoxyethylene ether as a raw material shows higher water reducing rate, higher cement paste expansion degree and then shows more excellent retarding effect. Therefore, the provided synthesis method and the hyperbranched unsaturated polyoxyethylene ether obtained by adopting the synthesis method have broad application prospect and great market potential.

Description

technical field [0001] The invention belongs to the field of concrete admixtures, in particular to a synthesis method of hyperbranched unsaturated polyoxyethylene ether, and the hyperbranched unsaturated polyoxyethylene ether prepared by the synthesis method and its application. Background technique [0002] In modern concrete construction projects, polycarboxylate water reducers are the most widely used construction admixtures. The polycarboxylate water reducers are different from those that improve the dispersion of concrete through electrostatic repulsion. Lignosulfonate water reducer and naphthalene water reducer, polycarboxylate water reducer have both electrostatic repulsion and steric hindrance, and the steric hindrance is mainly provided by the linear polyoxyethylene ether structure , The relative molar ratio and structural molecular weight of the linear polyoxyethylene ether molecular structure directly affect the overall performance of the polycarboxylate water red...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C04B24/26C04B103/30
Inventor 朱伟亮
Owner SHANGHAI TAIJIE CHEM
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