Selective hydrogenation catalyst and preparation method and application thereof
A hydrogenation catalyst and catalyst technology, applied in hydrogenation preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc., can solve problems such as increasing the amount of active components and reducing catalyst activity
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example 1
[0013] Catalyst preparation: 105 g PdCl 2 (Pd content 59.5%), add 150 milliliters of 37% hydrochloric acid, 1600 milliliters of water, after heating and dissolving, adjust pH=4-5 with 30% sodium hydroxide solution for later use. In a 50-liter reactor, add 6300 grams of calcium carbonate and 22 liters of water, stir and heat until the temperature reaches 70°C, then add the pre-prepared palladium chloride solution dropwise. Finish dripping in 3 hours and keep for 30 minutes. Then add 600 ml of 0.7 mol / L sodium formate solution, and react at 75° C. for 1 hour. Cool down and filter, the filter cake is washed six times, each 1000 ml, and discharged. The wet product was put into an enamel tray and baked in an oven at 140° C. for 10 hours to obtain a finished catalyst with a palladium content of 1%.
example 2
[0017] Catalyst preparation: 100 g PdCl 2 (Pd content 59.5%), add 150 milliliters of 37% hydrochloric acid, 2000 milliliters of water, after heating and dissolving, adjust pH=4-5 with 30% sodium hydroxide solution for later use. In a 50-liter reactor, add 6,500 grams of barium sulfate and 25 liters of water, stir and heat to 70°C, then add the pre-prepared palladium chloride solution dropwise. Finish dripping in 3 hours and keep for 30 minutes. Then add 630 ml of 0.7 mol / L sodium formate solution, and react at 75° C. for 1 hour. Cool down and filter, the filter cake is washed six times, each 1000 ml, and discharged. The wet product was placed in an enamel tray in an oven at 140°C for 8 hours. The palladium content of the catalyst was 0.91%.
[0018] Application example: Add 2.5 kg of the above catalyst, 750 kg of 1,4-butynediol and 250 kg of water into a 2000-liter autoclave. The autoclave was replaced with nitrogen and hydrogen 4 times successively. Continuously feed hy...
example 3
[0021] The preparation of the catalyst was the same as in Example 1, and the palladium content was adjusted to be 0.8%.
[0022] Application example: Add 3 kg of the above catalyst, 700 kg of 1,4-butynediol and 300 kg of water into a 2000-liter autoclave. The autoclave was replaced with nitrogen and hydrogen 4 times successively. Continuously feed hydrogen and keep the hydrogen pressure at 0.4Mpa, and control the reaction temperature at 95-105°C until no hydrogen is absorbed as the end point of the reaction. The temperature is lowered, and the catalyst is separated by filtration and returned to the autoclave for recycling. Filtrate obtains 704 kilograms of products through vacuum dehydration, and through analysis (analysis method is the same as above), wherein 1,4-butenediol content is 98.2% (wherein cis content is 96.3%, trans content is 1.9%), 1,4- Butynediol content is 0.12%, 1,4-butanediol content is 0.35%.
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