Preparation method of fluorine-containing shrink-reduced polycarboxylate water reducing agent
A technology of water reducer and polycarboxylate, which is applied in the field of preparation of shrinkage-reducing polycarboxylate water reducer, can solve problems such as complex synthesis process and increased engineering cost, and achieve rich sources, low gas content and surface tension, and excellent performance stable effect
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Embodiment 1
[0024] 1) Preparation of carbonyl-containing polycarboxylate superplasticizer prepolymer: 0.1mol 2-keto-3-butene, 2mol acrylic acid and 1mol allyl polyethylene glycol (800g / mol) in 0.01mol sodium persulfate , under the action of 0.03mol sodium metabisulfite and 0.005mol sodium methacryl sulfonate, keep at 50°C for free radical polymerization for 3 hours to obtain a polycarboxylate superplasticizer prepolymer containing carbonyl groups;
[0025] 2) Preparation of fluorine-containing shrinkage-reducing polycarboxylate superplasticizer: mix 1 mol of carbonyl-containing polycarboxylate superplasticizer prepolymer with 0.01 mol of Prakash reagent (TMSCF 3 ) for 10 minutes of nucleophilic substitution reaction, after the reaction was completed, the pH value was adjusted to 5 with sodium hydroxide, and water was added to obtain a shrinkage-reducing polycarboxylate water reducer with a mass concentration of 5%.
Embodiment 2
[0027] 1) Preparation of carbonyl-containing polycarboxylate superplasticizer prepolymer: 0.2mol 3-methyl-4-penten-2-one, 3mol maleic anhydride and 1mol methallyl polyethylene glycol (2500g / mol) Under the action of 0.01mol potassium persulfate, 0.03mol sodium sulfite and 0.01mol mercaptopropanol, keep at 50°C for free radical polymerization for 5 hours to obtain a carbonyl-containing polycarboxylate superplasticizer prepolymer;
[0028] 2) Preparation of fluorine-containing shrinkage-reducing polycarboxylate superplasticizer: mix 1 mol of carbonyl-containing polycarboxylate superplasticizer prepolymer with 4 mol of Prakash reagent (TMSCF 3 ) for nucleophilic substitution reaction for 20 minutes, after the reaction was completed, the pH value was adjusted to 5.5 with potassium hydroxide, and water was added to obtain a shrinkage-reducing polycarboxylate-based water-reducer with a mass concentration of 15%.
Embodiment 3
[0030] 1) Preparation of carbonyl-containing polycarboxylate superplasticizer prepolymer: 0.3mol 3-buten-2-one, 4mol fumaric acid and 1mol 3-methyl-3-butene-1-polyethylene glycol (4000g / mol) under the action of 0.05mol hydrogen peroxide, 0.1mol ferrous pyrophosphate and 0.05mol mercaptoacetic acid, keep at 30°C for free radical polymerization for 3 hours to obtain a carbonyl-containing polycarboxylate superplasticizer prepolymer ;
[0031] 2) Preparation of fluorine-containing shrinkage-reducing polycarboxylate superplasticizer: 1 mol polycarboxylate superplasticizer prepolymer containing carbonyl, and 0.01mol Prakash reagent (TMSCF 3 ) for 30 minutes of nucleophilic substitution reaction, after the reaction was completed, the pH value was adjusted to 5.5 with sodium hydroxide, and water was added to obtain a shrinkage-reducing polycarboxylate water reducer with a mass concentration of 35%.
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