Preparation method and application of catalyst for synthesizing polycarboxylate water reducer macromonomer
A technology for synthesizing polycarboxylic acid and catalyst is applied in the field of catalyst preparation for synthesizing polycarboxylic acid-series water-reducing agent macromonomers, which can solve the problems of reduced production cost, low relative molecular weight, low polymerization activity, etc. The effect of low content of by-products and improving the quality of polyether products
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Embodiment 1
[0023] Embodiment 1: Preparation of the methallyl alcohol solution of 50% methallyl-phosphazene catalyst
[0024] N 2 Under protection, put 1molPCl 5 React with 7mol 1,1,3,3-tetramethylguanidine in 4L acetonitrile solution, the temperature is controlled at -30-80°C, and the reaction time is 4 hours; after the reaction is completed, add 2L deionized water and separate the oil and water, and then separate 1L of dichloromethane was added to the aqueous phase and the oil and water were separated, and finally the solvent was removed from the separated oil phase by pressure distillation to obtain 0.92mol phosphazene chloride; then 0.92mol phosphazene chloride was added to the The mass fraction of sodium propoxide is 50% sodium methallylate-methallyl alcohol solution, the reaction temperature is 20-60°C, stirred for 3 hours, and the insoluble matter is filtered off to obtain a mass fraction of 50% methallyl Propyl-phosphazene catalyst in methallyl alcohol.
Embodiment 2
[0025] Embodiment 2: Preparation of the methallyl alcohol solution of 30% methallyl-phosphazene catalyst
[0026] N 2 Under protection, put 1mol PCl 5 React with 9mol 1,1,3,3-tetramethylguanidine in 8L tetrahydrofuran solution, the temperature is controlled at -20-90°C, and the reaction time is 7 hours; after the reaction is completed, add 6L deionized water and separate the oil and water, and then separate Add 4L chloroform to the aqueous phase and separate the oil from water, and finally remove the solvent from the separated oil phase by pressure distillation to obtain 0.94mol phosphazene chloride; then add 0.94mol phosphazene chloride to the The mass fraction of sodium is 30% sodium methallyl alcohol-methallyl alcohol solution, the reaction temperature is 30-70 ° C, stirred for 4 hours, and the insoluble matter is filtered to obtain a mass fraction of 30% methallyl - Solution of phosphazene catalyst in methallyl alcohol.
Embodiment 3
[0027] Embodiment 3: Preparation of the methallyl alcohol solution of 70% methallyl-phosphazene catalyst
[0028] N 2 Under protection, put 1mol PCl 5 React with 11mol 1,1,3,3-tetramethylguanidine in 6L nitrobenzene solution, the temperature is controlled at -20-90°C, and the reaction time is 5 hours; after the reaction is completed, add 9L deionized water and separate the oil and water, then Add 12L dichloromethane to the separated water phase and separate the oil and water, and finally remove the solvent from the separated oil phase by pressure distillation to obtain 0.96mol phosphazene chloride; then add 0.96mol phosphazene chloride to the The 70% mass fraction of potassium methallylate is potassium methallylate-methallyl alcohol solution, the reaction temperature is 40-75 ° C, stirred for 5 hours, and the insoluble matter is filtered to obtain a mass fraction of 70% formazan Allyl-phosphazene catalyst in methallyl alcohol.
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