Star-shaped polycarboxylate superplasticizer with controllable molecular structure and preparation method thereof
A technology of star-shaped polycarboxylic acid and molecular structure is applied in the field of concrete admixtures, which can solve the problems of insufficient initial dispersion performance and high concrete viscosity.
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Embodiment 1
[0060] Step 1) Add 60.0g of ethylenediamine and 452.6g of 2-(phenylthioformylthio)propionic acid into the reactor, under the protection of nitrogen, heat up to 60°C, add 0.26g of concentrated sulfuric acid, and continue to heat up to At 80°C, keep the temperature for 6 hours, then cool down to obtain the acylated product C.
[0061] Step 2) In a glass reactor equipped with a thermometer, a stirrer, a dropping funnel and a nitrogen inlet tube, add 51.2g of acylated product C, 14.4g of acrylic acid, 19.6g of hydroxyethyl acrylate phosphate, 200g of polyethylene glycol Monomethyl ether acrylate (Mn=500g / mol), 1.43g of azobisisobutylamidine hydrochloride, and 190.2g of water were mixed, stirred to form a uniform monomer aqueous solution, and N 2 O in the solution 2 discharge, the N 2 A reversible addition-fragmentation chain transfer polymerization reaction was carried out under protection at a reaction temperature of 50°C for 12 hours to obtain a star-shaped polycarboxylate wat...
Embodiment 2
[0063] Step 1) Add 51.5g of diethylenetriamine and 698.5g of 4-cyano-4-(phenylthioformylthio)valeric acid into the reactor, raise the temperature to 60°C under the protection of nitrogen, and add 7.5g Benzenesulfonic acid, continue to heat up to 110°C, keep the temperature constant for 3h, and cool down to obtain the acylated product C.
[0064] Step 2) In a glass reactor equipped with a thermometer, a stirrer, a dropping funnel and a nitrogen inlet tube, add 47.1g of acylated product C, 17.2g of methacrylic acid, 39.2g of hydroxyethyl acrylate phosphate, 200g of polyethylene Glycol monomethyl ether methacrylate (Mn=1000g / mol), 3.03g of 4,4'-azobis(4-cyanovaleric acid), and 303.5g of water were mixed and stirred to form a uniform monomer aqueous solution. Access to N 2 O in the solution 2 discharge, the N 2 The reversible addition-fragmentation chain transfer polymerization reaction was carried out under protection, the reaction temperature was 60°C, and the polymerization ...
Embodiment 3
[0066] Step 1) Add 51.5g of diethylenetriamine and 838.1g of 4-cyano-4-(phenylthioformylthio)pentanoic acid into the reactor, raise the temperature to 60°C under the protection of nitrogen, and add 17.8g For 4-dimethylaminopyridine, continue to heat up to 90° C., keep the temperature constant for 5 hours, and cool down to obtain the acylated product C.
[0067] Step 2) In a glass reactor equipped with a thermometer, a stirrer, a dropping funnel and a nitrogen inlet tube, add 47.1g of acylated product C, 20.0g of dimethacrylic acid, 21.0g of hydroxyethyl methacrylate phosphate, Mix 200g ethoxylated polypropylene glycol polytetramethylene glycol monomethacrylate (Mn=2000g / mol), 5.76g azobisisobutylamidine hydrochloride, and 288.1g water, and stir to make a uniform aqueous monomer solution , into N 2 O in the solution 2 discharge, the N 2 The reversible addition-fragmentation chain transfer polymerization reaction was carried out under protection, the reaction temperature was ...
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