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

A technology with comb-like structure and end-group functions, which is applied in the field of pH-responsive polycarboxylic acid materials, can solve problems that have not been reported before, and achieve the effects of reducing capillary pressure, inhibiting shrinkage cracking, and increasing contact angle

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

Therefore, it is required that the prepared polycarboxylic acid materials are not limited to the currently reported synthesis methods, and use innovative synthetic routes to obtain pH response characteristics at the molecular structure level. It is also conducive to industrialized production and popularization and application. There is no report on this aspect at home and abroad.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] First, 360g 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 30g of N,N-diethyl-2-acrylamide and 11.06 g2-mercaptoethanol mixed solution 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-diethyl-2-acrylamide solution; 10.71g allyl chloride, 217.14 Add gN,N-diisopropylethylamine and 0.72g tetraethylammonium iodide to the self-polymerization product solution in turn, stir and adjust the temperature to 120°C, react at a constant temperature of 120°C for 2 hours, and then distill under reduced pressure to remove tetrahydrofuran and Excessive reagent, obtain unsaturated poly N,N-diethyl-2-acrylamide macromonomer; 46.66g unsaturated poly N,N-diethyl-2-acrylamide macromonomer is dissolved in In 56.10g of solvent water, heat up to 90°C, stir for 1...

Embodiment 2

[0036] First, 270g of dimethyl sulfoxide was added to the reactor, the temperature was raised to 110°C, 5.54g of tert-butyl peroxybenzoate was added and stirred for 12 minutes until it was evenly mixed, then 30g of 4-vinylpyridine and 11.15g of 2- The mixed solution of mercaptoethanol was added for 3 hours. After the dropwise addition, the reaction was continued at a constant temperature of 110°C for 2 hours to obtain a self-polymerized product poly-4-vinylpyridine solution; , N-diisopropylethylamine and 1.35g tetrabutylammonium bromide were added to the self-polymerization product solution in turn, stirred and adjusted to 110°C, reacted at a constant temperature of 110°C for 4 hours, and then distilled off dimethyl under reduced pressure sulfoxide and excess reagent to obtain unsaturated poly-4-vinylpyridine macromonomer; 50.68g unsaturated poly-4-vinylpyridine macromonomer was dissolved in 50.68g solvent water, heated to 85°C, stirred Wait for 12 minutes to mix it evenly, th...

Embodiment 3

[0038] First, 150g of aniline was added to the reactor, the temperature was raised to 90°C, 5.10g of dibenzoyl peroxide was added and stirred for 20 minutes until it was evenly mixed, then 30g of diethylaminoethyl methacrylate and 2.98g of 3-mercapto Mixed solution of propanol for 8 hours, continue to react at a constant temperature of 90° C. for 4 hours after the dropwise addition, to obtain a self-polymerized product polydiethylaminoethyl methacrylate solution; Add methylethylenediamine 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 under reduced pressure to remove aniline and excess reagents. Obtain unsaturated polydiethylaminoethyl methacrylate macromonomer; 34.61g unsaturated polydiethylaminoethyl methacrylate macromonomer is dissolved in 27.68g solvent water, be warmed up to 70 ℃, stir Wait for 20 minutes to mix it...

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Abstract

The invention relates to a method for preparing pH-responsive comb-structure polycarboxylic acid through terminal group functionalization. According to the method, with a pH-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 pH-responsive monomer as a reactant, a terminal group-functionalized pH-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 pH-responsive polymer chain and the unsaturated halogenated hydrocarbon to obtain a pH-responsive macromonomer, and finally a copolymerization reaction is performed on the pH-responsive macromonomer and the small 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 pH-responsive function. By the method, the process is high-efficiency and energy-saving, the conversion rate of a product is high, the functional modification of the polycarboxylic acid is successfully achieved through introduction of the pH-responsive polymer side chain by a terminal group functionalization method, an excellent characteristic of inhibiting shrinkage of cement mortar is shown, and the market competitiveness and the application prospect are very good.

Description

technical field [0001] The invention relates to the technical field of a pH-responsive polycarboxylic acid material for cement concrete, in particular to a pH-responsive macromonomer that uses a pH-responsive monomer to self-polymerize and then replace to obtain a terminal functionalized pH-responsive macromonomer combined with carboxylate The invention discloses a specific preparation method for copolymerizing small acid monomers into a comb-shaped polycarboxylic acid material. Background technique [0002] Concrete is the most widely used building material in modern construction projects. With the needs of construction projects and the advancement of science and technology, it has been widely used in industries, water conservancy, agriculture, transportation and seaports. However, concrete is prone to chemical deterioration and other problems during the application process. The shrinkage cracking in concrete will reduce the ability of concrete to resist the erosion of exte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F265/10C08F220/06C08F222/02C08F222/06C08F265/04C08F271/02C04B24/26C04B103/30
CPCC04B24/2652C04B2103/006C04B2103/302C08F265/04C08F265/10C08F271/02C08F220/06C08F222/02C08F222/06
Inventor 刘晓许谦白夏冰管佳男王子明王杰
Owner BEIJING UNIV OF TECH
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