Catalyst for preparing 1,3-butanediol by hydrogenation of 3-hydroxybutyraldehyde, preparation method and application thereof
A technology of hydroxybutyraldehyde and catalyst, which is applied in the field of 3-hydroxybutyraldehyde hydrogenation preparation 1, which can solve the problems of increasing the difficulty of product separation and refining, dehydration or even polymerization of 3-hydroxybutyraldehyde, affecting product yield and purity, etc. , to achieve high stability, long service life, and prevent agglomeration
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[0048] A Pt / CeO 2 The preparation method of catalyst comprises the following steps:
[0049] (1) Dissolve cerium nitrate hexahydrate in deionized water, add urea and stir to dissolve. The solid-liquid ratio of the cerium nitrate hexahydrate to deionized water is 8-9 g / 30mL, and the mass ratio of the cerium nitrate hexahydrate to the urea is 8-9:0.2.
[0050] (2) adding the citric acid solution (150-250 mg / L) to the solution obtained in step (1), and stirring evenly; the volume ratio of the solution obtained in step (1) to the citric acid solution is 25-35:2.
[0051] (3) Adjust pH=9.5-10.5 of the solution obtained in step (2), and stir for 20-40 min.
[0052] (4) Load the solution obtained in step (3) into a reaction device, seal and react at 150-160° C. for 20-30 hours, cool down to room temperature after the reaction, centrifuge the precipitate, wash with water until neutral, 50-70 °C drying.
[0053] (5) calcining the precipitate obtained in step (4) at 400-600 ° C for ...
Embodiment 1
[0061] 8.68g of cerium nitrate hexahydrate (Ce(NO 3 ) 3 ·6H 2 O) was dissolved in 60 mL of deionized water, and 0.2 g of urea (CO (NH) was added. 2 ) 2 ), stir and dissolve; then add 2mL citric acid solution (200mg / L), stir evenly, add ammonia water dropwise, adjust pH to 10, continue stirring for 30min; react in 155℃ oven for 24h; Centrifugal separation, washed with water to neutrality, and dried at 60 °C; the obtained precipitate was ground and then calcined in air, the heating rate was 5 °C / min, raised to 500 °C, and calcined for 3 h to obtain a cerium oxide carrier; Weigh CeO 2 1 g of carrier, 2 mL of water was added. Stir for 30 min and sonicate for 30 min. Add 0.5 ml of a chloroplatinic acid solution containing 0.1 g / mL of platinum, and stir for 1 h. Put it into an oven at 80 °C to dry; grind the dried sample, put it into a reduction furnace, and put it in a 5% H 2 5%Pt / CeO can be obtained by reducing at 250℃ for 1h in / Ar atmosphere 2 catalyst.
[0062] Dispers...
Embodiment 2
[0067] With reference to the same catalyst preparation and reaction steps in Example 1, the difference is that the volume of 0.1g / mL chloroplatinic acid solution containing platinum is added to be 0.2-0.8ml, and the reaction time is 1.5h to obtain catalysts with different platinum loadings. The conversion rate of 3-hydroxybutyraldehyde and the yield of 1,3-butanediol are shown in Table 2.
[0068] Table 2. Pt / CeO with different platinum loadings 2 The conversion of 3-hydroxybutyraldehyde and the yield of 1,3-butanediol obtained under
[0069] catalyst 2%Pt / CeO 2
[0070] The results in Table 2 show that on the ceria support, the most suitable Pt loading is 5% (weight ratio), and excess Pt may lead to the deep hydrogenation of part of the product 1,3-butanediol.
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