Catalyst for preparing gamma-butyrolactone by normal-pressure gas-phase dehydrogenation of 1,4-butanediol and preparation method thereof
A technology of butanediol and catalyst, applied in the field of catalyst preparation, can solve the problems of high price of 1,4-butanediol, increase the difficulty of manufacturing process, etc., improve the skeleton structure and pore structure, reduce the low and high shrinkage rate active effect
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Embodiment 1
[0025] Take 1000ml of deionized water, add 152g of copper nitrate, 91.4g of zinc nitrate, 117.7g of aluminum nitrate in turn, fully dissolve and heat up to 65°C, add 250g of polyethylene glycol-800, stir well, and then add SiO 2 30g of silica gel with a content of 30%, stir well to make it evenly mixed, control the temperature of the mixed liquid at 55-65°C, lubricating oil precipitant 1.5M Na 2 CO 3 Solution, the pH value of the control liquid terminal system is 8.0, under stirring, the temperature of the mixed system is raised to 85 ° C, sinking for 5 hours, filtered, washed, and dried at 110 ° C for 15 hours, the dried product is in the Calcined at 545-555° C. for 4.5 hours, and when it was naturally cooled to room temperature, 1.5% graphite was added as a lubricant to prepare a molded Φ5×5mm catalyst sample.
[0026] Take 10ml of the above sample catalyst with a particle size of 20-40 mesh, put it into the isothermal section of a Φ12×600mm fixed-bed reactor, and start hea...
Embodiment 2
[0028] Take 800ml of deionized water, add 116.7g of copper nitrate, 127.9g of zinc nitrate, and 95.6g of aluminum nitrate in turn, fully dissolve and heat up to 70-80°C, add 200g of polyethylene glycol-1000, mix well, and add SiO 2 65g of silica sol with a content of 20%. After stirring evenly, control the temperature of the mixing system at 65-75°C, and add 1.5M NaHCO 3 Precipitating agent in the mixed system, control the end point pH value to 7.5, settle at 80°C for 8 hours, filter, wash with deionized water, dry at 110-120°C for 12 hours, bake at 450°C for 6 hours, cool down to room temperature naturally, add 1.5% graphite was used as a lubricant to prepare a molded Φ5×5mm catalyst sample.
[0029] The catalyst activation conditions are the same as Example 1, the reaction temperature is 240°C, the hydrogen-alcohol ratio is 10, and the liquid hourly pore velocity is 2.0h -1 , The conversion rate of the catalyst to 1,4-butanediol is 99.1%, and the selectivity of 1,4-butaned...
Embodiment 3
[0031] Take 800ml of deionized water, add 167g of copper nitrate, 73.5g of zinc nitrate, and 75g of aluminum nitrate in sequence. After fully dissolving, heat up to 80-90°C, add 130g of polyethyl alcohol-1500, mix well, and add SiO 2 100g of silica sol with a content of 15%, stir well, mix evenly, control the temperature of the mixture at 75-85°C, add 1.5M Na 2 CO 3 and NaHCO 3 Composite precipitant (Na 2 CO 3 : NaHCO 3 =1:1 molar ratio), control the pH value of the precipitation end point to 7.5, sink at 90°C for 4 hours, filter, wash, and dry the filter cake at 100-110°C for 18 hours, and the dried product is at 645-655°C Roast for 4 hours, cool down to room temperature naturally, add 1.5% graphite as a lubricant, and prepare a molded Φ5×5mm catalyst sample.
[0032] The catalyst activation conditions are the same as in Example 1, the reaction temperature is 300°C, and the liquid hourly pore velocity is 2.75h -1 , the ratio of hydrogen to alcohol is 8, the conversion r...
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