Anti-cracking shrinkage-reducing type polycarboxylate superplasticizer and preparation method thereof
A technology of water reducing agent and polycarboxylic acid, which is applied in the field of anti-cracking and shrinkage polycarboxylate water reducing agent and its preparation, which can solve the problem of reducing the surface tension of the solution inside the cement slurry void, reducing the feasibility of industrial production, and lacking market competitiveness and other problems, to achieve excellent dispersion and retention effect, excellent crack resistance and shrinkage reduction performance, and safe and reliable preparation process
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Embodiment 1
[0034] 1) Preparation of anti-cracking and shrinkage-type water reducing agent prepolymerization product: 1 mol of gallic acid and 4 mol of acetic anhydride were stirred and reacted at 50°C for 3 hours under the catalytic condition of concentrated sulfuric acid (0.2 mL), washed with water, and then mixed with allyl chloride at room temperature. Reaction 24h, obtain gallic acid derivative unsaturated small monomer; Gained small monomer (0.3mol), acrylic acid (3mol) in 50mL methanol and ammonium persulfate (0.1mol), sodium bisulfite (0.1mol) and 2-mercaptopropionic acid (0.08mol) acted together, and carried out free radical polymerization at 20°C for 4 hours to obtain a prepolymerized product;
[0035] 2) Add sodium hydroxide to the obtained prepolymerization product to make the pH of the solution 7 to 8, remove the protecting group and then evaporate the solvent; continue to add terminal halogen group modified polyether (1mol, M w =1000g / mol) of 120mL acetonitrile / water (v / v=1 / ...
Embodiment 2
[0040] 1) Preparation of anti-cracking and shrinkage type water reducing agent prepolymerization product: 1 mol of gallic acid and 4 mol of acetic anhydride were stirred and reacted at 50°C for 3 hours under the catalytic condition of concentrated sulfuric acid (0.2mL), washed with water, and then mixed with allyl bromide at room temperature. Reaction 24h, obtain gallic acid derivative unsaturated small monomer; The obtained small monomer (0.3mol), methacrylic acid (3.5mol) in 50mL acetone and hydrogen peroxide (0.15mol), sodium sulfite (0.08mol) and 3- Mercaptopropionic acid (0.07mol) acted together and carried out free radical polymerization at 30°C for 3.5 hours to obtain a prepolymerized product;
[0041] 2) Add potassium hydroxide to the obtained prepolymerization product to make the pH of the solution 7 to 8, remove the protecting group and then evaporate the solvent; continue to add terminal halogen group modified polyether (1mol, M w =800g / mol) of 120mL acetonitrile / wa...
Embodiment 3
[0046]1) Preparation of anti-cracking and shrinkage-type water reducing agent prepolymerization product: 1 mol of gallic acid and 4 mol of acetic anhydride were stirred and reacted at 50°C for 3 hours under the catalytic condition of concentrated sulfuric acid (0.2 mL), washed with water, and then mixed with allyl chloride at room temperature. React for 24h to obtain unsaturated small monomers of gallic acid derivatives; the resulting small monomers (0.3mol), acrylamide (4mol) in 50mL ethanol with potassium persulfate (0.1mol), sodium pyrosulfite (0.12mol) and 2 -Mercaptopropionic acid (0.08mol) acted together, and carried out free radical polymerization at 30°C for 4.5 hours to obtain a prepolymerized product;
[0047] 2) Add triethylamine to the obtained prepolymerization product to make the pH of the solution 7 to 8, remove the protecting group and then evaporate the solvent; continue to add halogen-modified polyether (1mol, M w =3500g / mol) in 120mL of acetonitrile / water (v...
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