Method for preparing high-molecular-weight polybutylene glycol carbonate under catalysis of organic alkali synergistic Ti/Si composite material
A polybutylene glycol and composite material technology is applied in the field of organic base synergistic Ti/Si composite material to catalyze the preparation of high molecular weight polybutylene glycol carbonate, which can solve the problems of harsh reaction conditions, low APC molecular weight, and high catalyst dosage, and achieves Easy preparation, good dispersibility, high molecular weight effect
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specific Embodiment approach 1
[0034] Specific embodiment one: a kind of organic base synergistic Ti / Si composite material of this embodiment catalyzes the method for preparing high molecular weight polytetramethylene glycol carbonate according to the following steps:
[0035] 1. Prepolymerization: In an argon atmosphere, add 1,4-butanediol (18g, 0.2mol), dimethyl carbonate (45g, 2.5equiv, 0.5mol), DMAP (0.049g) into the reactor , carry out the transesterification prepolymerization reaction, control the temperature of the distillation head during the reaction process to be 64 ° C, the stirring speed is 400 rpm, and the prepolymerization ends after 3 hours to obtain low molecular weight polytetramethylene carbonate terminated by hydroxyl and methoxy groups;
[0036] 2. Polycondensation: Add 0.116g of Ti / Si catalyst to the reactor after step 1, and after polycondensation reaction at 170°C for 1 hour, reduce the vacuum degree of the reaction system to 4000Pa, react for 1 hour, and continue to reduce the vacuum ...
specific Embodiment approach 2
[0041] Specific embodiment two: a kind of organic base synergy Ti / Si composite material catalyzes the method for preparing high molecular weight polytetramethylene glycol carbonate of the present embodiment according to the following steps:
[0042] 1. Prepolymerization: In an argon atmosphere, 1,4-butanediol (18g, 0.2mol), dimethyl carbonate (36g, 2equiv, 0.4mol), and MTBD (0.306g) were added to the reactor, Carry out the transesterification prepolymerization reaction, control the temperature of the distillation head during the reaction to be 64° C., the stirring speed is 400 rpm, and the prepolymerization ends after 2 hours to obtain low molecular weight polytetramethylene carbonate terminated by hydroxyl and methoxy groups;
[0043] 2. Polycondensation: Add 0.116g of Ti / Si catalyst to the reactor after step 1. After polycondensation reaction at 170°C for 2 hours, reduce the vacuum degree of the reaction system to 1100Pa, react for 1h, and continue to reduce the vacuum degree...
specific Embodiment approach 3
[0048] Specific embodiment three: a kind of organic base synergy Ti / Si composite material of this embodiment catalyzes the method for preparing high molecular weight polytetramethylene glycol carbonate to carry out as follows:
[0049] 1. Prepolymerization: In an argon atmosphere, add 1,4-butanediol (18g, 0.2mol), dimethyl carbonate (45g, 2.5equiv, 0.5mol), and DABCO (0.224g) into the reactor , carry out the transesterification prepolymerization reaction, control the temperature of the distillation head during the reaction to be 62°C, the stirring speed is 400rpm, and the prepolymerization ends after 3.5h, to obtain low molecular weight polytetramethylene carbonate terminated by hydroxyl and methoxy groups;
[0050] 2. Polycondensation: Add 0.116g of Ti / Si catalyst to the reactor after step 1, and after polycondensation reaction at 130°C for 3 hours, reduce the vacuum degree of the reaction system to 10000Pa, react for 1h, and continue to reduce the vacuum degree to 100Pa, Aft...
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