Solid anti-mud ultra-slow release polycarboxylate slump retention agent and preparation method thereof
An ultra-sustained-release, polycarboxylic acid technology, applied in the field of building materials, can solve the problems of loss of polycarboxylic acid slump-retaining agent, expensive equipment, and influence of slump-retaining effect, and achieves improved adsorption, good material adaptability, and maintenance of slump effect
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Embodiment 1
[0036] (1) Preparation of unsaturated esterified small monomers:
[0037] Under normal pressure, 41 parts of methacrylic acid, 71 parts of propionic acid, 130 parts of 3-bis(2-hydroxyethyl)amino-2-hydroxypropanesulfonic acid (DIPSO) were added to the reactor, and 0.25 1 part of copper chloride, 0.13 part of benzyltributylammonium chloride and 13 parts of chloroform, carry out esterification reaction, the esterification reaction temperature is 100 ℃, and the reaction time is 3 hours, after the reaction is finished, it is down to room temperature, that is to say, Saturated esterified small monomers.
[0038] (2) Melt polymerization
[0039] Add 80 parts by weight of unsaturated polyether P-1 and 20 parts by weight of 4-hydroxybutyl vinyl polyoxyethylene ether with a molecular weight of 500 into the reactor, raise the temperature to 85°C to make it in a molten state, and then once Add 1 part by weight of benzyltriphenylphosphine chloride, and stir evenly;
[0040] Mix 1 part b...
Embodiment 2
[0044] (1) Preparation of unsaturated esterified small monomers:
[0045]Under normal pressure, 60 parts of methacrylic acid, 162 parts of butyric acid, 130 parts of 3-bis(2-hydroxyethyl)amino-2-hydroxypropanesulfonic acid (DIPSO) were added to the reactor, and 0.55 Part of zinc chloride, 0.45 part of three (N-nitroso-N-phenylhydroxylamine) aluminum and 18 parts of carbon tetrachloride, carry out esterification reaction, the esterification reaction temperature is 110 ℃, and the reaction time is 4 hours, After the reaction is finished, it is lowered to room temperature, and the unsaturated esterified small monomer is obtained.
[0046] (2) Melt polymerization
[0047] Add 60 parts by weight of unsaturated polyether P-2 and 40 parts by weight of 4-hydroxybutyl vinyl polyoxyethylene ether with a molecular weight of 800 into the reactor, raise the temperature to 90°C to make it in a molten state, and then once 1 weight part tetrakis (triphenylphosphine) palladium was added, and ...
Embodiment 3
[0052] (1) Preparation of unsaturated esterified small monomers:
[0053] Under normal pressure, 90 parts of methacrylic acid, 85 parts of butyric acid, 130 parts of 3-bis(2-hydroxyethyl)amino-2-hydroxypropanesulfonic acid (DIPSO) were added to the reactor, and 0.6 1 part of copper chloride, 0.35 part of benzyltributylammonium chloride and 40 parts of chloroform, carry out esterification reaction, the esterification reaction temperature is 120 ℃, and the reaction time is 5 hours, and after the reaction is finished, it is down to room temperature, that is, no Saturated esterified small monomers.
[0054] (2) Melt polymerization
[0055] Add 20 parts by weight of unsaturated polyether P-3 and 80 parts by weight of 4-hydroxybutyl vinyl polyoxyethylene ether with a molecular weight of 1500 into the reactor, raise the temperature to 80°C to make it in a molten state, and then once Add 2 parts by weight of tetrakis (triphenylphosphine) palladium, and stir evenly;
[0056] Mix 5 p...
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