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A kind of preparation method of pH-responsive comb structure polycarboxylic acid

A technology of comb-like structure and polycarboxylate, which is applied in the field of pH-responsive polycarboxylate for cement concrete, to achieve the effects of low energy consumption, simple and controllable reaction process, and prevention of cracking

Active Publication Date: 2021-01-05
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, this requires the synthetic pH-responsive polycarboxylate material to realize the innovation of molecular structure, which can not only have application properties such as shrinkage reduction and crack resistance according to the change of the pH environment of cement concrete, but also ensure convenient process operation and low cost. Preparation cost, simple and easy-to-obtain reaction raw materials are conducive to industrial production and popularization and application, and there are no reports on this aspect of work at home and abroad

Method used

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  • A kind of preparation method of pH-responsive comb structure polycarboxylic acid
  • A kind of preparation method of pH-responsive comb structure polycarboxylic acid
  • A kind of preparation method of pH-responsive comb structure polycarboxylic acid

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Experimental program
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Effect test

Embodiment 1

[0034]First, 90g of N,N-dimethylformamide, 30g of ethyl acrylate and 32.75g of 3-mercaptopropionic acid isooctyl ester were added to the reactor, stirred and heated to 60°C, and then 5.96g of azobisisoheptaonitrile was added dropwise A mixed solution with 8.94g of N,N-dimethylformamide for 10 hours, after the dropping, continue to react at a constant temperature of 60°C for 5 hours to obtain a self-polymerized product polyethyl acrylate solution; adjust the temperature of the obtained self-polymerized product to 60°C , Add 24.29g tert-dodecyl mercaptan and stir for 35 minutes until it is evenly mixed, then add 377.31g dimethylaminoethyl methacrylate, 29.80g azobisisoheptonitrile and 44.71g N,N-dimethyl The mixed solution of methyl formamide was added for 10 hours. After the addition, the reaction was continued at 60°C for 5 hours, and then N,N-dimethylformamide was removed by vacuum distillation to obtain the graft copolymerized product; 407.31 g of graft copolymer was obtained. The...

Embodiment 2

[0036]First, 30g of tetrahydrofuran, 30g of methyl acrylate and 12.54g of isopropanol were added to the reactor, stirred and heated to 50°C, and then a mixed solution of 2.86g of azobisisobutyronitrile and 2.86g of tetrahydrofuran was added dropwise for 12 hours. After the addition, continue to react at a constant temperature of 50°C for 6 hours to obtain a self-polymerized product polymethyl acrylate solution; adjust the temperature of the obtained self-polymerized product to 50°C, add 35.22g of n-dodecyl mercaptan and stir for 40 minutes until it is mixed Evenly, add dropwise a mixed solution of 498.27g dimethylaminoethyl acrylate, 28.57g azobisisobutyronitrile and 28.57g tetrahydrofuran for 12 hours. After the addition, continue to react at a constant temperature of 50°C for 6 hours, and then remove by distillation under reduced pressure. Tetrahydrofuran to obtain graft copolymerization product; mix 528.27g graft copolymerization product with 62.64g deionized water, stir and heat...

Embodiment 3

[0038]First, 270g of dimethyl sulfoxide, 30g of amyl acrylate and 1.27g of isopropanol were added to the reactor, stirred and heated to 70°C, and then 6.56g of tert-butyl peroxybenzoate and 59.02g of dimethyl The mixed solution of sulfoxide was 8 hours, and after the dropping, the reaction was continued at 70°C for 4 hours to obtain the self-polymerization product polypentyl acrylate solution; adjust the temperature of the obtained self-polymerization product to 80°C, and add 32.03g n-dodecyl Stir the mercaptan for 25 minutes until it is evenly mixed, then add dropwise a mixed solution of 66.55g 4-vinylpyridine, 19.67g tert-butyl peroxybenzoate and 177.04g dimethyl sulfoxide for 6 hours, and continue to keep constant temperature after the addition is complete React at 80°C for 3 hours, then remove the dimethyl sulfoxide by vacuum distillation to obtain the graft copolymerization product; mix 96.55g of the graft copolymerization product with deionized water, stir and raise the temper...

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Abstract

The invention relates to a preparation method of a pH responsive polycarboxylic acid of a comb-shaped structure. The preparation method comprises the following steps: by taking acrylate and a pH responsive monomer as raw materials, preparing a polycarboxylic acid material by self-polymerization and graft copolymerization and hydrolysis: by taking acrylate as a reaction monomer, carrying out polymerization under the action of an initiator and a chain transfer agent to generate polyacrylate with controllable molecular weight and then copolymerizing with the pH responsive monomer to obtain a grafted copolymer taking the polyacrylate polymer as a main chain and the pH responsive polymer as a side chain; and finally, hydrolyzing the grafted copolymer to prepare the polycarboxylic acid of the comb-shaped structure taking polyacrylic acid as the main chain and the pH responsive polymer as the side chain. The preparation method is mild in condition and energy-saving and efficient. By introducing the pH responsive polymer by means of a molecular structural design, the polycarboxylic acid with a special functional side chain is synthesized, so that a pH responsive behavior is achieved successfully. The polycarboxylic acid shows an excellent characteristic of inhibiting shrinkage of cement mortar and has a wide market prospect and a popularizing and applying potential.

Description

Technical field[0001]The invention relates to the technical field of a pH-responsive polycarboxylic acid for cement concrete, in particular to a comb-like structure polycarboxylic acid material that adopts acrylic monomers to self-polymerize and then graft pH-responsive monomers and then hydrolyze to synthesize a comb-like structure polycarboxylic acid material The specific preparation method.Background technique[0002]Concrete is currently one of the most widely used building materials in the field of construction engineering. It is an important structural engineering material, but it is prone to shrinkage and deformation in a low-water dry environment, causing cracks and other defects in hardened concrete. Cracks in large-scale foundation slabs, building exterior walls, underground structures, floor slabs, and beams are common quality problems in construction projects. With the continuous development of green concrete and high-strength concrete, the types of concrete are changing w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F265/04C08F220/34C08F226/06C08F220/54C08F8/12C04B24/26C04B103/30
CPCC04B24/2688C04B2103/006C04B2103/302C08F8/12C08F265/04C08F220/34C08F226/06C08F220/54
Inventor 刘晓许谦赖光洪管佳男王子明张琳
Owner BEIJING UNIV OF TECH
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