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Hyperbranched polymer, hyperbranched polycarboxylic acid-series super plasticizer and preparation method thereof

A technology of hyperbranched polymers and polycarboxylic acids, which is applied in the preparation of sulfonates, organic chemistry, etc., can solve the problems of complex synthesis process, high cost, and difficulty in realizing industrialization.

Active Publication Date: 2012-06-20
安徽海螺材料科技股份有限公司
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Problems solved by technology

[0008] For the synthesis of hyperbranched superplasticizers, Shou Chongqi's research group has carried out a lot of work: using sodium methacrylate, allyl polyoxyethylene ether and tert-butyl methacrylate as monomers, azo Dicyanovaleric acid initiates a polymerization reaction, synthesizes a water-reducing agent main chain with carboxyl groups at both ends, and then grafts a polycarboxylic acid superplasticizer of hyperbranched polyamide at both ends (Shou Chongqi, etc. Concrete, 2010, 243:55~57.); They also synthesized a bromine-terminated hyperbranched poly(amine-ester) by combining acrylic acid with monomethoxy-terminated allyl polyethylene glycol (APEG-27) Grafted to the end of hyperbranched poly(amine-ester), a new type of hyperbranched polycarboxylate superplasticizer was formed (Xu Lei, et al. Concrete, 2011, 257:84~87.), cement net The fluidity test of the slurry shows that the obtained hyperbranched superplasticizer has good dispersibility, but the method for synthesizing the hyperbranched superplasticizer is complicated in synthesis process and high in cost, and it is difficult to realize industrialization

Method used

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  • Hyperbranched polymer, hyperbranched polycarboxylic acid-series super plasticizer and preparation method thereof
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  • Hyperbranched polymer, hyperbranched polycarboxylic acid-series super plasticizer and preparation method thereof

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preparation example Construction

[0095] The invention provides a kind of preparation method with the hyperbranched polymer of formula (I) structure, comprises the following steps:

[0096] Alkenylamine and 2-acrylamido-2-sodium methylpropanesulfonate undergo an addition reaction to obtain a hyperbranched polymer having a structure of formula (I);

[0097] The alkenylamine is allylamine, acrylamide, diallylamine, 9-octadecenylamine or chloroenylamine.

[0098] Firstly, alkenylamine and sodium 2-acrylamido-2-methylpropanesulfonate are dissolved in an organic solvent to obtain a mixed solution of alkenylamine and sodium 2-acrylamido-2-methylpropanesulfonate. The alkenylamine is allylamine, acrylamide, diallylamine, 9-octadecenylamine or chloroenylamine, preferably allylamine, diallylamine, more preferably allyl amine. Wherein the molar ratio of alkenylamine to 2-acrylamido-2-methylpropanesulfonate sodium is 1: (1~5), preferably 1: (1.2~4); more preferably 1: (1.5 ~3); the organic solvent is preferably an alco...

Embodiment 1

[0225] Dissolve 1 mol of allylamine and 2 mol of sodium 2-acrylamido-2-methylpropanesulfonate in 1 mL of methanol, react the resulting mixed solution at 25°C for 1 hour, and then raise the temperature of the reaction system to 80°C React for 5 hours. After the reaction is completed, the obtained reaction solution is evaporated under reduced pressure to remove methanol to obtain hyperbranched polymer powder.

[0226] Will obtain hyperbranched polymer powder to carry out infrared test, the result is as follows figure 1 shown. figure 1 For the infrared spectrogram of the hyperbranched polymer prepared by the embodiment of the present invention 1, in figure 1 Medium, 1580cm -1 is the characteristic vibration of the amide group, 619cm -1 Be the characteristic vibration of sulfonic acid group, illustrate that allylamine and 2-acrylamido-2-sodium methyl propane sulfonate have undergone addition reaction, and the hyperbranched polymer powder that obtains has formula (I) structure. ...

Embodiment 2

[0228] Dissolve 1 mol of allylamine and 2 mol of methyl acrylate with 2 mL of methanol, react the resulting mixed solution at 25°C for 12 hours, then evaporate the obtained reaction solution under reduced pressure, remove methanol, and obtain the first intermediate product; Add 2.5 mol of ethylenediamine and 1 mL of methanol to an intermediate product, react the reaction system at 25°C for 12 hours, then gradually raise the temperature to 80°C for 5 hours, evaporate the obtained reaction solution under reduced pressure, and remove methanol to obtain the first The second intermediate product; the obtained second intermediate product and 4mol 2-acrylamido-2-methylpropanesulfonate were dissolved in 2 mL of methanol, and the resulting mixed solution was reacted at 70°C for 5 hours to obtain a hyperbranched polymer .

[0229] The obtained hyperbranched polymer is carried out infrared test, the result is as follows figure 2 mentioned. figure 2 Be the infrared spectrogram of the ...

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Abstract

The invention provides a hyperbranched polymer, a hyperbranched polycarboxylic acid-series super plasticizer and a preparation method thereof. The preparation method comprises the following steps of: undergoing an addition reaction and an ammonolysis reaction on alkenyl amine, polymethylmethacrylate, ethylene diamine and 2-acrylamide-2-sodium methylacrylsulfonate serving as raw materials to obtain a hyperbranched polymer with a structure shown as a formula (I), (II), (III) or (IV); undergoing a polymerization reaction on the hyperbranched polymer, an esterification monomer and a crosslinking agent; and preparing a hyperbranched polycarboxylic acid-series super plasticizer with a two-step process. The preparation method provided by the invention has the advantages of simple process, easiness for controlling a preparing process and operating, readily-available raw materials, low production cost and suitability for industrial production. Due to the adoption of the hyperbranched polycarboxylic acid-series super plasticizer, the comprehensive performance of concrete is improved. As proved by an experiment result, the hyperbranched polycarboxylic acid super plasticizer provided by the invention has high slump loss resistance, high water-reducing rate and high compressive strength.

Description

technical field [0001] The invention relates to the technical field of building materials, in particular to a hyperbranched polymer, a hyperbranched polycarboxylic acid superplasticizer and a preparation method thereof. Background technique [0002] At present, in the construction of large-scale projects, high-performance concrete construction projects are widely used. In the technology of preparing high-performance concrete, in addition to high requirements for cement and aggregates, the most important feature is the use of ultra-fine Powder admixtures and admixtures, especially superplasticizers. Incorporating superplasticizers into concrete is an effective measure to improve the workability of concrete, increase the strength of concrete, improve the long-term durability of concrete, reduce the shrinkage of hardened concrete, save cement, and reduce energy consumption. important means. [0003] Traditional comb-shaped polycarboxylate superplasticizers are widely used bec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00C08F299/00C07C309/16C07C303/32C04B24/16
Inventor 付新建赵洪义朱化雨朱孔赞张战营吕新璐夏宗艳
Owner 安徽海螺材料科技股份有限公司
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