Catalyst for cyclohexene hydration and preparation method thereof, and preparation method of cyclohexanol
A catalyst, cyclohexanol technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of slow reaction speed, low yield of cyclohexanol, etc. problem, to achieve the effect of easy separation, excellent thermal stability, and high repeatability
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preparation example Construction
[0019] The preparation method of described catalyst provided by the invention comprises the following steps:
[0020] (1) Trimethylamine, 1,4-butane sultone and HZSM-5 are first contacted in an organic solvent, and the organic solvent in the first contact product is removed; the conditions of the first contact include the first The temperature of the first contact is 20-70°C, the time of the first contact is 8-72 hours, and the molar ratio of 1,4-butane sultone to trimethylamine is 0.8-1.2:1;
[0021] (2) at -5°C to 10°C, the product obtained in step (1) is subjected to a second contact with phosphoric acid, the conditions of the second contact include that the temperature of the second contact is 40-90°C, the second contact The time is 3-10 hours, and the molar ratio of phosphoric acid to trimethylamine in step (1) is 0.7-1.2:1.
[0022] The present invention is not particularly limited to the amount of HZSM-5 described in step (1), as long as it can cooperate with the compo...
preparation example 1
[0045] This preparation example is used to illustrate the preparation of the catalyst for preparing cyclohexanol from cyclohexene hydration provided by the present invention.
[0046] (1) 1 mol of trimethylamine, 1 mol of 1,4-butane sultone and 1000 g of HZSM-5 were contacted in 1 L of ethyl acetate, and reacted at 50° C. for 48 hours to obtain the first contact product. After the first contact product was taken out, the organic solvent was distilled off under reduced pressure to obtain a white solid. The solid was washed successively with ethanol, toluene and anhydrous ether, and then dried in vacuum at 80°C to constant weight;
[0047] (2) At 5° C., the product obtained in step (1) was contacted with 1 mol of phosphoric acid, and the temperature was raised to 60° C. for 6 hours to obtain the second contact product. The second contact product was washed with deionized water, and then vacuum-dried at 80° C. to constant weight to obtain catalyst C1.
[0048] 1 H NMR (deutera...
preparation example 2
[0051] This preparation example is used to illustrate the preparation of the catalyst for preparing cyclohexanol from cyclohexene hydration provided by the present invention.
[0052] (1) 1 mol of trimethylamine, 0.8 mol of 1,4-butane sultone and 200 g of HZSM-5 were contacted in 1 L of ethyl acetate, and reacted at 20° C. for 72 hours to obtain the first contact product. After the first contact product was taken out, the organic solvent was distilled off under reduced pressure to obtain a white solid. The solid was washed successively with ethanol, toluene and anhydrous ether, and then dried in vacuum at 80°C to constant weight;
[0053] (2) At -5°C, the product obtained in step (1) was contacted with 0.7 mol of phosphoric acid, and the temperature was raised to 90°C for 3 hours to obtain the second contact product. The second contact product was washed with deionized water, and then vacuum-dried at 80° C. to constant weight to obtain catalyst C2. Characterized by NMR, the ...
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