A shrinkage-reducing polycarboxylate water reducer and its preparation method
A technology of polycarboxylic acid and water reducing agent, applied in the field of building admixtures, can solve the problems of small plastic shrinkage, insufficient reduction range, increase early shrinkage and total shrinkage of high-strength concrete, and achieve good dispersion performance and improve dispersion performance. Effect
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Embodiment 1
[0032] (1) Preparation of polyphosphate: under the protection of nitrogen, add 10mol trimethylolpropane to the first reaction device, cool in an ice-water bath for 1h, add 500ml triethylamine, and drop 100ml dichlorophosphoric acid under rapid stirring The dichloromethane solution of ethyl ester (solution concentration: 100mol / L), the dropwise addition time is 1h, after the dropwise addition is completed, the temperature is slowly raised to 45°C for 24h reaction. After standing for 12 hours, filter with suction, collect the filtrate, and distill off the solvent to obtain polyphosphate.
[0033] (2) Preparation of shrinkage-reducing functional macromonomer: Polyethylene glycol monomethyl ether, 4.1g maleic anhydride, 19g polyphosphate prepared in step (1), 0.5g SnCl with 100g molecular weight of 2400 2 2H 2 O and 0.6 g of o-tert-butylphenol were added to the second reaction device, and under the protection of nitrogen, they were reacted at a constant temperature of 90° C. for ...
Embodiment 2
[0037] (1) Preparation of polyphosphate: under the protection of nitrogen, add 10mol trimethylolpropane to the first reaction device, cool in an ice-water bath for 1h, add 500ml triethylamine, and drop 100ml dichlorophosphoric acid under rapid stirring The dichloromethane solution of ethyl ester (solution concentration: 100mol / L), the dropwise addition time is 1h, after the dropwise addition is completed, the temperature is slowly raised to 45°C for 24h reaction. After standing for 12 hours, filter with suction, collect the filtrate, and distill off the solvent to obtain polyphosphate.
[0038] (2) Preparation of shrinkage functional macromonomer: 100g of polyethylene glycol monomethyl ether with a molecular weight of 3000, 3.3g of maleic anhydride, 25g of polyphosphate prepared in step (1), 1g of NaHSO 4 ·H 2 O and 0.8 g of phenothiazine were added to the second reaction device, and under the protection of nitrogen, they were reacted at a constant temperature of 100° C. for ...
Embodiment 3
[0042] (1) Preparation of polyphosphate: under the protection of nitrogen, add 10mol trimethylolpropane to the first reaction device, cool in an ice-water bath for 1h, add 500ml triethylamine, and drop 100ml dichlorophosphoric acid under rapid stirring The dichloromethane solution of ethyl ester (solution concentration: 100mol / L), the dropwise addition time is 1h, after the dropwise addition is completed, the temperature is slowly raised to 45°C for 24h reaction. After standing for 12 hours, filter with suction, collect the filtrate, and distill off the solvent to obtain polyphosphate.
[0043] (2) Preparation of shrinkage-reducing functional macromonomer: 100 g of polyethylene glycol monomethyl ether with a molecular weight of 4000, 2.45 g of maleic anhydride, 15 g of polyphosphate prepared in step (1), 1.2 g of FeCl 3 ·6H 2 O and 1.0 g of phenothiazine were added to the second reaction device, and under the protection of nitrogen, they were reacted at a constant temperature...
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