A kind of clay-resistant phosphonic acid-based superplasticizer and preparation method thereof
A superplasticizer and phosphonic acid-based technology, which is applied in the field of clay-resistant phosphonic acid-based superplasticizer and its preparation, can solve the problems of high production cost, unoptimistic market prospect and the like, and achieves low cost and simple synthesis process. High efficiency and low production energy consumption
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Embodiment 1
[0056] For the esterification of polyether, the synthesis initiator is methyl glycolate, the polymerization monomer is ethylene oxide, the concentration of catalyst DMC is 30 ppm, and the added amount of co-catalyst benzoic acid is 0.1% of the amount of methyl glycolate. Weigh 1 mol (90 g) of methyl glycolate, 20 mol (880 g) of ethylene oxide, 29 mg of catalyst DMC and 0.12 g of co-catalyst benzoic acid. The above-mentioned initiator methyl hydroxyacetate and the catalyst were added to the closed reaction kettle, vacuumed to -0.1MPa, fed with 20g of ethylene oxide, heated to 120°C to initiate the reaction and continued to feed the remaining ethylene oxide, kept warm. After the reaction for 1 h, the volatile substances were removed under reduced pressure, and the insoluble substances were removed by filtration to obtain the carboxylate modified polyether intermediate.
[0057] Add 1.01mol (60.7g) of ethylenediamine into the above reaction kettle containing carboxylate modified ...
Embodiment 2
[0059] Esterified polyether, the synthetic initiator is ethyl hydroxyacetate, the polymerization monomers are ethylene oxide and propylene oxide, the concentration of catalyst DMC is 40 ppm, and the amount of benzoic acid added as a co-catalyst is 0.2 of the amount of ethyl hydroxyacetate. %. Weigh 1 mol (104 g) of ethyl hydroxyacetate, 25 mol (1100 g) of ethylene oxide, 20 mol (1160 g) of propylene oxide, 95 mg of catalyst DMC and 0.24 g of co-catalyst benzoic acid. The above-mentioned initiator ethyl hydroxyacetate and the catalyst were added to the closed reaction kettle, vacuumed to -0.1MPa, fed with 20g of ethylene oxide, heated to 120°C to initiate the reaction and continued to feed the remaining ethylene oxide and ethylene oxide successively. propylene oxide, heat preservation reaction for 3h, remove volatile substances under reduced pressure, and filter to remove insoluble substances to obtain a carboxylate modified polyether intermediate.
[0060] 1.01mol (104.2g) of...
Embodiment 3
[0062] Esterified polyether, the synthesis initiator is methyl 3-hydroxypropionate, the polymerization monomers are ethylene oxide and epoxy cyclohexane, the concentration of catalyst DMC is 40ppm, and the addition amount of co-catalyst benzoic acid is 3-hydroxyl 0.3% of methyl propionate mass. Weigh 1 mol (104 g) of methyl 3-hydroxypropionate, 40 mol (1760 g) of ethylene oxide, 10 mol (981 g) of cyclohexane oxide, 114 mg of catalyst DMC and 0.36 g of co-catalyst benzoic acid. The above-mentioned starting agent methyl 3-hydroxypropionate and the catalyst were added to the closed reaction kettle, evacuated to -0.1MPa, fed with 20g of ethylene oxide, heated to 130°C to initiate the reaction and continued to feed the remaining epoxy resin successively. Ethane and epoxy cyclohexane are incubated for 3 hours, volatile substances are removed under reduced pressure, and insoluble substances are removed by filtration to obtain a carboxylate-modified polyether intermediate.
[0063] 1...
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