Preparation method of multi-phase catalyst for synthesizing dimethoxy bisphenol bimethyl carbonate
A technology of dimethoxycarbonic acid bisphenol diester and heterogeneous catalyst, which is applied in the preparation of organic carbonate, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., can solve the difficulty of product and catalyst. Separation and other problems, to achieve the effect of reduced preparation cost, easy availability of raw materials, and simple preparation method
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[0016] The invention provides a kind of preparation method (abbreviation method) of the heterogeneous catalyst of synthesizing bisphenol dimethoxycarbonate diester, it is characterized in that the method comprises the following steps:
[0017] (1) dissolving polyvinylpyrrolidone in deionized water, stirring to make it fully dissolved, to obtain solution A; the mass fraction of polyvinylpyrrolidone in solution A is 2% to 6%;
[0018] The molecular weight of polyvinylpyrrolidone is 40000-1300000;
[0019] (2) Add the lithium source and the titanium source successively or simultaneously into solution A, stir and sonicate for 30-60 minutes, and then stir for 6-12 hours to obtain solution B; the molar ratio of the lithium source and the titanium source is 1:1-1 :10;
[0020] (3) Move solution B into the autoclave, place the autoclave in an oven at 150-180°C, and react under pressure for 3-6 hours; take out the autoclave, cool to room temperature, open the autoclave, and use rotary...
Embodiment 1
[0028] Weigh 2g of polyvinylpyrrolidone (K90) and dissolve it in 100g of water, stir for 1h to fully dissolve; then add LiNO 3 , etc. LiNO 3 Add TiO after complete dissolution 2 (The molar ratio of Ti / Li is 2:1), after stirring continuously for 12 hours, move the solution into a high-pressure reactor with a polytetrafluoroethylene liner at 150°C for 4 hours, evaporate the water after cooling, and dry it at 120°C Calcined at 300°C for 4h in a muffle furnace.
[0029] Mix 1g of catalyst with 5.6g of bisphenol A, raise the temperature to 180°C, then add 34ml of dimethyl carbonate, control the temperature of the system at 160-180°C, the by-product methanol produced by the reaction will be removed by distillation, and will be removed by the reaction distillation column The temperature of the distillate is controlled at 50-65°C, and the unreacted dimethyl carbonate is refluxed into the reaction system. After 10 hours of reaction, it is filtered to obtain bisphenol dimethoxycarbona...
Embodiment 2
[0031] The catalyst preparation method is the same as in Example 1, except that the titanium source is changed to titanium tetrachloride, the molar ratio of Ti / Li is 6:1, and the calcination temperature is 400°C.
[0032] Mix 1g of catalyst with 5.6g of bisphenol A, raise the temperature to 180°C, then add 34ml of dimethyl carbonate, control the temperature of the system at 160-180°C, the by-product methanol produced by the reaction will be removed by distillation, and will be removed by the reaction distillation column The temperature of the distillate was controlled at 50-65°C, and the unreacted dimethyl carbonate was refluxed into the reaction system. After 10 hours of reaction, it was filtered to obtain bisphenol dimethoxycarbonate, and the yield reached 93.6%, while bisphenol A The conversion rate reached 46.7%.
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