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Catalyst for preparing 1, 3-butanediol by hydrogenating 3-hydroxybutyraldehyde as well as preparation method and application of catalyst

A hydroxybutyraldehyde and catalyst technology, applied in the field of 3-hydroxybutyraldehyde hydrogenation preparation 1, 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 the effect of reducing the amount of catalyst, excellent activity, conversion rate and high selectivity

Active Publication Date: 2021-03-09
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional Raney nickel catalyst has low activity and requires a higher reaction temperature (above 100°C)
Although there is a patent report that metal nickel can be loaded to increase the reactivity, the alumina catalyst used is acidic, which easily causes the dehydration or even polymerization of 3-hydroxybutyraldehyde, which seriously affects the yield and purity of the product and increases the product yield. Difficulty in separating and refining

Method used

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  • Catalyst for preparing 1, 3-butanediol by hydrogenating 3-hydroxybutyraldehyde as well as preparation method and application of catalyst
  • Catalyst for preparing 1, 3-butanediol by hydrogenating 3-hydroxybutyraldehyde as well as preparation method and application of catalyst
  • Catalyst for preparing 1, 3-butanediol by hydrogenating 3-hydroxybutyraldehyde as well as preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0048] A Pt / CeO 2 The preparation method of catalyst comprises the following steps:

[0049] (1) Dissolve cerous nitrate hexahydrate in deionized water, add urea and stir to dissolve. The solid-liquid ratio of the cerous nitrate hexahydrate to deionized water is 8-9g / 30mL, and the mass ratio of the cerous nitrate hexahydrate to urea is 8-9:0.2.

[0050] (2) Add citric acid solution (150-250 mg / L) into the solution obtained in step (1), and stir evenly; the volume ratio of the solution obtained in step (1) to the citric acid solution is 25-35:2.

[0051] (3) Adjust the pH of the solution obtained in step (2) to 9.5-10.5, and stir for 20-40 min.

[0052] (4) Put the solution obtained in step (3) into the reaction device, seal it and react at 150-160°C for 20-30h, cool to room temperature after the reaction, centrifuge the precipitate, wash with water until neutral, 50-70 ℃ dry.

[0053] (5) Calcinate the precipitate obtained in step (4) in the air at 400-600°C for 2-4h to ob...

Embodiment 1

[0061] 8.68g cerous nitrate hexahydrate (Ce(NO 3 ) 3 ·6H 2 O) was dissolved in 60mL of deionized water, and 0.2g of urea (CO(NH 2 ) 2 ), stir and dissolve; then add 2mL citric acid solution (200mg / L), stir evenly, add ammonia water dropwise, adjust the pH to 10, and continue stirring for 30min; react in an oven at 155°C for 24h; Centrifuge, wash with water until neutral, and dry at 60°C; Grind the obtained precipitate and calcinate in air at a heating rate of 5°C / min to 500°C for 3 hours to obtain a cerium oxide carrier; weigh CeO 2 Carrier 1g, add 2mL water. Stir for 30min, ultrasonic for 30min. Add 0.5 ml of chloroplatinic acid solution containing 0.1 g / mL of platinum, and stir for 1 h. Dry in an oven at 80°C; 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 reduction at 250°C for 1 h in / Ar atmosphere 2 catalyst.

[0062] Get the catalyst 0.1g prepared by the above method and disperse in 10mL of 30% 3-hydr...

Embodiment 2

[0067] With reference to the same catalyst preparation and reaction steps in Example 1, the difference is that the volume of chloroplatinic acid solution containing platinum 0.1g / mL is 0.2-0.8ml, and the reaction time is 1.5h to obtain the catalysts with different platinum loads. 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 rate 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 deep hydrogenation of part of the product 1,3-butanediol.

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Abstract

The invention relates to the technical field of catalytic hydrogenation, and discloses a catalyst for preparing 1, 3-butanediol by hydrogenating 3-hydroxybutyraldehyde, a preparation method and application thereof, and a Pt / CeO2The catalyst can be used for preparing the 1, 3-butanediol by hydrogenating the 3-hydroxybutyraldehyde, has the characteristics of high reaction activity, high selectivityand good stability, and can be used for efficiently hydrogenating the 3-hydroxybutyraldehyde into the 1, 3-butanediol by using a reaction kettle in a hydrogen atmosphere at a lower temperature. The CeO2 carrier is prepared by adopting a solvothermal method, and then Pt is impregnated and loaded, so that the catalyst is prepared, and the preparation method is simple. In addition, by optimizing thehydrogenation process, the 1, 3-butanediol can be prepared with high conversion rate and high selectivity.

Description

technical field [0001] The invention relates to the technical field of catalytic hydrogenation, in particular to a catalyst for preparing 1,3-butanediol by hydrogenating 3-hydroxybutyraldehyde, a preparation method and application thereof. Background technique [0002] 1,3-Butanediol (1,3-BDO) has good hygroscopicity and water solubility, and is odorless and low-toxic. It can be used as a moisturizer, antibacterial agent, and used in the production of cosmetics and pharmaceuticals. At the same time, 1,3-butanediol can also be used to produce unsaturated polyester resins, plasticizers, moisturizers and softeners, etc., and has a wide range of applications in industrial production. [0003] At present, there are two main methods for synthesizing 1,3-butanediol: biological method and chemical synthesis method. Although the biological method has mild production conditions, high selectivity, and less waste discharge, the yield is low and it is difficult to achieve large-scale pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/63B01J35/08C07C29/141C07C31/20
CPCB01J23/63C07C29/141B01J35/51C07C31/207Y02P20/584
Inventor 赵怀远刘皓岚姜媛媛周茹茹叶恒舒郑丽萍杜玮辰侯昭胤
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD