Catalyst for hydration of cyclohexene, preparation method thereof, and preparation method of cyclohexanol
A cyclohexene hydration and catalyst technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of low activity, low surface area, poor hydrothermal stability It can achieve the effect of high catalytic activity, simple preparation method and low corrosiveness.
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[0020] On the other hand, the present invention provides a kind of preparation method of cyclohexene hydration catalyst, the method comprises the following steps:
[0021] (1) Trimethylamine, 1,4-butane sultone and rod-shaped SBA-15 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 contact temperature is 20-70°C, the first contact time is 8-72 hours, the molar ratio of 1,4-butane sultone to trimethylamine is 0.8-1.2:1, the ratio of rod-shaped SBA-15 to trimethylamine The weight ratio is 3.5-45:1;
[0022] (2) at -5 DEG C to 10 DEG C, the product that step (1) obtains is carried out second contact with phosphoric acid, and the condition of second contact comprises that the temperature of second contact is 40-90 DEG C, the time of second contact is 3-10 hours, the molar ratio of phosphoric acid to trimethylamine in step (1) is 0.7-1.2:1.
[0023] According to the...
Embodiment
[0036] The following examples will further illustrate the present invention, but do not limit the present invention thereby.
[0037] In the following examples and comparative examples:
[0038] In the catalyst prepared by the following preparation examples, the content of the rod-shaped SBA-15=the weight of the added rod-shaped SBA-15 / the weight of the catalyst×100%, the content of the compound with the structure shown in formula (I)=100% - Content of stick SBA-15.
[0039] Rod-shaped SBA-15 was purchased from Changchun Jilin University High-Tech Co., Ltd.; PEG-400 was purchased from Haian Petrochemical Plant in Jiangsu Province.
[0040] In the present invention, adopt gas chromatograph (purchased in Shanghai Precision Scientific Instrument Co., Ltd., model is GC128) to carry out the analysis of each composition in the system, carry out quantification by calibration normalization method, all can refer to prior art to carry out, on this basis Calculate the conversion rate o...
preparation example 1
[0049] This preparation example is used to illustrate the preparation of the catalyst for preparing cyclohexanol from cyclohexene hydration provided by the present invention.
[0050] (1) Under nitrogen protection, the rod-shaped SBA-15 (the most probable pore diameter is 6.2 nanometers, the pore volume is 1.0 ml / g, the specific surface area is 646 square meters / g, and the length of the rod is in the range of 30-100 microns ) calcined at 400°C for 10 hours to remove hydroxyl groups and residual moisture, thereby obtaining heat-activated rod-shaped SBA-15;
[0051] (2) 1mol trimethylamine, 1mol 1,4-butane sultone and 1000 grams of thermally activated rod-shaped SBA-15 were contacted in 1L 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 ethe...
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