Preparation method of hydroxytetrahydrofuran compound
A technology of hydroxytetrahydrofuran and compound, which is applied in the chemical industry, can solve the problems of low process conversion rate, expensive reaction conditions of catalysts, harsh reaction conditions, etc., and achieves the effects of lowering reaction temperature, being beneficial to large-scale industrial production, and being inexpensive.
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Embodiment 1
[0045] 10%Ru-SnOx-CeO 2 Catalyst preparation
[0046] To 600mL the concentration is 1mol / L Ce(NO 3 ) 3 The concentration is 0.5mol / L KOH drop by drop, keep the drop solution temperature at 35°C until the pH of the slurry reaches 13, retest after stirring for 1 hour, if the alkalinity decreases, you can add a little lye until the pH is constant at 13.
[0047] The obtained sol system was aged at 65° C. for 24 hours, filtered and washed until the TDS detection value of the filtrate was less than 20 ppm.
[0048] The obtained suction filtration gel was dispersed in 800ml 95% ethanol, and 30g SnCl 4 Add, continue to drop KOH lye until the pH reaches 12, the resulting slurry is centrifugally washed until the pH of the centrifuge is less than 8, and the resulting precipitate is vacuum-dried at 80 to obtain SnOx-CeO 2 .
[0049] The calculated amount of RuCl 3 Make it into an aqueous solution, use the aforementioned deposition and precipitation method to immobilize it on the ca...
Embodiment 2
[0057] 10%Ru-SnOx-CeO 2 -SiO 2 Catalyst preparation
[0058] The preparation process of catalyst is the same as embodiment 1, and difference is that 1mol / L Ce(NO 3 ) 3 Disperse in 500ml of 20% silica sol and then add KOH solution dropwise. The target catalyst is 10% Ru-SnOx-CeO 2 -SiO 2 .
[0059] Synthesis of 3-Hydroxytetrahydrofuran
[0060] Load 15g Amberlyst-35 as acid catalyst I on a 8mm×400mm fixed bed reaction tube, pass 3,4-epoxytetrahydrofuran and methanol (molar ratio 1:3) through the catalyst bed preheated to 80°C, and control the liquid material The airspeed is 1.0h- 1 , while N 2 The purge flow rate is 80ml / min, and the discharge liquid is directly pumped into the 30g 10% Ru-SnOx-CeO 2 -SiO 2 The catalyst is used as the reaction tube of hydrogenolysis catalyst II, and hydrogen gas is introduced into the reaction tube, and then the system back pressure is 6MPa, and the reaction is carried out at 130°C, and the liquid space velocity is kept at 0.6h- 1 Af...
Embodiment 3
[0062] The specific implementation process is the same as in Example 2, except that ZSM-5 (purchased from Nankai University Catalyst Factory, with a silicon-aluminum ratio of 25) is used as the acid catalyst 1, and the yield of 3-hydroxytetrahydrofuran reaches 76.2%.
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