Cross-linked air-entraining type water reducing agent and preparation method thereof
A technology of water reducer and monomer, which is applied in the field of cross-linked air-entraining water reducer and its preparation, can solve the problems of insufficient foam stability of concrete, and achieve the advantages of prolonging storage time, good dispersibility, and large steric hindrance Effect
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[0033] The invention provides a preparation method of a cross-linked air-entraining polycarboxylate water reducer, comprising the following steps:
[0034] Put vinyl ether macromonomer, reducing agent and appropriate amount of deionized water in the reactor, stir to dissolve, add dropwise the mixed solution of unsaturated acid and unsaturated ester, air-entraining monomer solution, oxidant And chain transfer agent, and adjust the temperature to 5 ~ 15 ° C to react, the dropping time is 0.5 ~ 1h, keep warm for 0.5 ~ 1.5h after the dropping, drop to room temperature after the reaction, adjust the pH to 6 ~ 7 with liquid alkali , that is, a cross-linked air-entraining retarding water reducer is obtained.
[0035] Wherein, the mass ratio of the vinyl ether macromonomer:monomer B:monomer C:monomer D is: 200:(1~30):(10~30):(1~10);
[0036] The oxidizing agent is preferably hydrogen peroxide or sodium persulfate;
[0037] The reducing agent is preferably at least one of ascorbic ac...
Embodiment 1
[0049] (1) Preparation of air-entraining monomer B1: 0.1mol of bis(hydroxyethyl)methyl dodecyl ammonium chloride, 0.115mol of acryloyl chloride, 40mL of 1,4 dioxane, and 0.1mol of pyridine were placed in the reaction In the reactor, under the condition of 15°C, the reaction was carried out for 10 h, and the product was purified by vacuum distillation and recrystallization to obtain the air-entraining monomer B1.
[0050] (2) Copolymerization reaction: by weight, 200 parts of 4-hydroxybutyl vinyl polyoxyethylene ether-2400, 1.5 parts of sodium formaldehyde sulfoxylate and deionized water are placed in the reactor, stirred and dissolved, and added to Add dropwise the mixed solution of 20 parts of acrylic acid, 2 parts of 2-methacryloxyethyl phosphate and 3 parts of air-entraining monomer B1, 2 parts of hydrogen peroxide solution, 1 part of thioglycolic acid solution, 5 ℃ The dropwise addition time is 45min under the condition, keep warm for 1h after the dropwise addition, cool d...
Embodiment 2
[0052] (1) Preparation of air-entraining monomer B2: 0.1mol octadecylbis(2-hydroxyethyl)methyl ammonium chloride, 0.115mol acryloyl chloride, 45mL1,4-dioxane, 0.1mol pyridine In the reactor, under the condition of 15°C, the reaction was carried out for 10 h, and the product was purified by vacuum distillation and recrystallization to obtain the air-entraining monomer B2.
[0053] (2) Copolymerization reaction: by weight, 200 parts of 4-hydroxybutyl vinyl polyoxyethylene ether-2400, 1 part of Brüggolit FF6 and deionized water are placed in the reactor, stirred and dissolved, and respectively added to the reactor Add dropwise a mixed solution of 21 parts of acrylic acid, 3 parts of 2-methacryloyloxyethyl phosphorylcholine and 4 parts of air-entraining monomer B2, 2 parts of hydrogen peroxide solution, and 1 part of thioglycolic acid solution at 10°C The time is 45 minutes. After the dropwise addition, keep warm for 1 hour. After the reaction, cool down to room temperature and ad...
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