Method for preparing temperature-responsive comb-structure polycarboxylic acid through terminal group functionalization

A temperature-responsive, comb-like structure technology, applied in the field of temperature-responsive polycarboxylic acid materials, can solve the problems of limiting industrial application potential and not considering the application of temperature response behavior, so as to reduce the dependence on preparation methods, inhibit shrinkage cracking, reduce The effect of pressure

Active Publication Date: 2019-01-18
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned preparation methods all have a certain degree of inadequacy. The achievement of the shrinkage reduction effect still relies on the traditional ideas and means of reducing surface tension, and does not consider the application of the temperature response behavior in the field of surface and interface chemistry to the shrinkage reduction and cracking of cement concrete. In the field of materials, and in the preparation of materials, most of them use a single method such as physical blending or transformation process, but rarely realize the real control of their application performance through the method of molecular structure design.
Experiments have proved that temperature-responsive macromolecules can effectively improve the shrinkage and crack resistance of concrete, but most living polymerization methods limit their industrial application potential due to the complexity and harshness of the reaction process.
Therefore, this requires the preparation of polycarboxylic acid materials to fundamentally carry out subversive molecular structure design, to determine a reasonable synthesis method, to ensure operability and universality, so as to achieve the suppression of cement concrete shrinkage and The characteristic performance of cracking has the value of industrial production application, and there is no report on this aspect at home and abroad

Method used

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  • Method for preparing temperature-responsive comb-structure polycarboxylic acid through terminal group functionalization
  • Method for preparing temperature-responsive comb-structure polycarboxylic acid through terminal group functionalization
  • Method for preparing temperature-responsive comb-structure polycarboxylic acid through terminal group functionalization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First, 72.81g of N,N-dimethylformamide was added to the reactor, the temperature was raised to 70°C, 7.11g of azobisisoheptanonitrile was added and stirred for 25 minutes until it was evenly mixed, and then 24.27g of N-isopropyl Mixed solution of methacrylamide and 1.49g 2-mercaptoethanol for 10 hours, after the dropwise addition, continue to react at a constant temperature of 70°C for 5 hours to obtain a self-polymerized product poly-N-isopropylmethacrylamide solution; 9.68g allyl Add bromine, 10.34g N,N-diisopropylethylamine and 0.19g benzyltrimethylammonium chloride to the self-polymerization product solution in sequence, stir and adjust the temperature to 50°C, react at a constant temperature of 50°C for 12 hours and then depressurize N,N-dimethylformamide and excess reagents were removed by distillation to obtain unsaturated poly-N-isopropylmethacrylamide macromonomer; 27.37g of unsaturated poly-N-isopropylmethacrylamide Dissolve acrylamide macromonomer in 16.42g o...

Embodiment 2

[0036] First, add 91.60g of aniline into the reactor, raise the temperature to 90°C, add 5.10g of dibenzoyl peroxide and stir for 20 minutes until it is evenly mixed, then add dropwise 18.32g of N-propylacrylamide and 2.98g of 3-mercapto Mixed solution of propanol for 8 hours, after the dropwise addition, continue to react at a constant temperature of 90°C for 4 hours to obtain a self-polymerized product poly-N-propylacrylamide solution; mix 8.15g 3-chloro-2-methylpropene, 13.95g tetramethyl Add ethylenediamine and 0.27g benzyltriethylammonium chloride to the self-polymerization product solution in turn, stir and adjust the temperature to 70°C, react at a constant temperature of 70°C for 9 hours, and then distill off aniline and excess reagents under reduced pressure to obtain Unsaturated poly-N-propylacrylamide macromonomer; dissolve 23.05g of unsaturated poly-N-propylacrylamide macromonomer in 18.44g of solvent water, heat up to 70°C, stir for 20 minutes and wait It is mixed...

Embodiment 3

[0038] First, 280.56g of tetrahydrofuran was added to the reactor, the temperature was raised to 120°C, 1.72g of di-tert-butyl peroxide was added and stirred for 10 minutes until it was evenly mixed, then 23.38g of N,N-dimethylacrylamide and 11.06g2 -The mixed solution of mercaptoethanol for 1 hour, after the dropwise addition, continue to react at a constant temperature of 120°C for 1 hour to obtain a self-polymerized product poly N,N-dimethylacrylamide solution; 10.71g of allyl chloride, 217.14g of N,N- Diisopropylethylamine and 0.72g tetraethylammonium iodide were added to the self-polymerization product solution in sequence, stirred and adjusted to 120°C, reacted at a constant temperature of 120°C for 2 hours, and then distilled off tetrahydrofuran and excess reagents under reduced pressure to obtain Unsaturated poly N,N-dimethylacrylamide macromonomer; dissolve 29.05g of unsaturated poly N,N-dimethylacrylamide macromonomer in 34.86g of solvent water, heat up to 90°C, Stir...

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Abstract

The invention relates to a method for preparing temperature-responsive comb-structure polycarboxylic acid through terminal group functionalization. According to the method, with a temperature-responsive monomer, unsaturated halogenated hydrocarbon, a small carboxylic acid momonomer and the like as raw materials, a polycarboxylate material is prepared through self-polymerization first, then substitution and then copolymerization; namely, with the temperature-responsive monomer as a reactant, a terminal group-functionalized temperature-responsive polymer chain is produced through the self-polymerization under the actions of an initiator and a terminal group functionalizing agent, then a substitution reaction is performed on the terminal group-functionalized temperature-responsive polymer chain and the unsaturated halogenated hydrocarbon to obtain a temperature-responsive macromonomer, and finally a copolymerization reaction is performed on the temperature-responsive macromonomer and thesmall carboxylic acid momonomer under the action of the initiator to obtain a comb-structure polymer which uses polycarboxylic acid as a main chain and has a side chain with a temperature-responsive function. By the method, the process is simple, convenient and fast, the molecular weight of a product is controllable, graft polymerization of the temperature-responsive functional macromonomer on polycarboxylic acid is successfully achieved by a terminal group functionalization method, the effects of inhibiting shrinkage and resisting cracking of cement mortar are excellent, and the scientific research value and economic and social benefits are very good.

Description

technical field [0001] The invention relates to the technical field of a temperature-responsive polycarboxylic acid material for cement concrete, in particular to a temperature-responsive macromonomer that uses a temperature-responsive monomer to first self-polymerize and then replace to obtain a terminal functionalized temperature-responsive macromonomer combined with carboxylate The invention discloses a specific preparation method for synthesizing a comb-shaped structure polycarboxylic acid material by copolymerization reaction of small acid monomers. Background technique [0002] As a building material, concrete has the characteristics of strong compressive capacity, convenient material acquisition, and good durability. Due to a series of problems such as concrete construction, its own deformation and constraints, concrete cracks have become the most common engineering diseases in civil engineering, water conservancy, bridges, tunnels and other projects. The main reason...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F265/10C08F220/06C08F222/02C08F222/06C04B24/26C04B103/30
CPCC04B24/2652C04B2103/006C04B2103/302C08F265/10C08F220/06C08F222/02C08F222/06
Inventor 刘晓许谦管佳男赖光洪王子明王剑锋
Owner BEIJING UNIV OF TECH
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