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Nickel-phyllosilicate structure catalyst and preparation method thereof

A technology of structural catalysts and phyllosilicates, which is applied in hydrogenation preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high production costs of noble metal catalysts, environmental pollution safety risks, and reduced product selectivity. It is beneficial to low-temperature hydrogenation reaction, promotes stable adsorption and hydrogenation conversion, and improves stability and activity

Active Publication Date: 2021-03-12
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The industrial development of noble metal catalysts is limited due to high production costs and limited reserves
The Raney nickel catalyst also has problems of environmental pollution and safety risks due to its high metal content.
In the reported work, the supported Ni-based catalyst has the advantages of low cost and easy availability (CN 108097254 A), but this material also cannot achieve a good BYD direct reaction due to the problems of low activity, poor selectivity and easy deactivation. The effect of hydrogenation to prepare BDO
The reason is that in the hydrogenation process of 1,4-butynediol, it is first hydrogenated to form a transition state of 1,4-butenediol, which is very prone to C=C double bond and C- Structural isomerization of OH bonds and conversion to 2-hydroxytetrahydrofuran by-product, thereby reducing product selectivity (S.Tanielyan et al.Org.Process Res.Dev.2017,21,327-335)

Method used

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  • Nickel-phyllosilicate structure catalyst and preparation method thereof
  • Nickel-phyllosilicate structure catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take the specific surface area as 150m 2 / g, SiO with a particle size of 7-40nm 2 The aerogel was vacuum degassed at 100°C for 6 hours, and then cooled to room temperature for use; take an appropriate amount of nickel acetylacetonate and cerium nitrate to prepare a mixed aqueous solution of a metal salt with a Ni mass concentration of 5.0g / L and a Ce mass concentration of 0.5g / L; mix 10g / L degassed SiO 2 The airgel is fully dispersed in the above metal salt mixed aqueous solution, and 90 g / L of urea is continuously added and fully dissolved. Raise the temperature of the above mixed solution to 85°C, reflux and stir for 12h, centrifuge the obtained precipitate, wash with distilled water three times, dry at 105°C for 8h, raise the temperature to 550°C at a heating rate of 8°C / min and roast for 12h to make Ni- Ce-Phy catalyst precursor, catalyst precursor in H at a flow ratio of 1:2 2 :N 2 In the mixed gas, the temperature was raised to 550°C at a heating rate of 10°C...

Embodiment 2

[0035] Take the specific surface area as 100m 2 / g, SiO with a particle size of 10-35nm 2 The aerogel was vacuum degassed at 150°C for 1 hour, and then cooled to room temperature for use; take appropriate amount of nickel acetate and ammonium molybdate to prepare a mixed aqueous solution of a metal salt with a mass concentration of Ni of 1.2g / L and a mass concentration of Mo of 1.8g / L; mix 10g / L degassed SiO 2 The airgel is fully dispersed in the mixed aqueous solution of the metal salt, and 70 g / L of urea is continuously added and fully dissolved. Heat the above mixed solution to 120°C, reflux and stir for 4h, centrifuge the obtained precipitate, wash with distilled water 4 times, dry at 90°C for 10h, raise the temperature to 300°C at a heating rate of 2°C / min and roast for 2h to make Ni- Mo-Phy catalyst precursor, the catalyst precursor is in the flow ratio of 1:1 H 2 :N 2 In the mixed gas, the temperature was raised to 700°C at a heating rate of 2°C / min, and then reduc...

Embodiment 3

[0037] Take the specific surface area as 300m 2 / g, SiO with a particle size of 7-35nm 2 The aerogel was vacuum degassed at 50°C for 10 hours, and then cooled to room temperature for use; take appropriate amount of nickel acetate and cerium nitrate to prepare a mixed aqueous solution of a metal salt with a mass concentration of Ni of 0.5g / L and a mass concentration of Ce of 0.3g / L; mix 10g / L SiO after L degassing 2 The airgel is fully dispersed in the above metal salt mixed aqueous solution, and 50 g / L of urea is continuously added and fully dissolved. Heat the above mixed solution to 60°C, reflux and stir for 18h, centrifuge the obtained precipitate, wash with distilled water 4 times, dry at 125°C for 12h, raise the temperature to 400°C at a heating rate of 3°C / min and roast for 6h to make Ni- Ce-Phy catalyst precursor, the catalyst precursor is in the flow ratio of 1:1 H 2 :N 2 In the mixed gas, the temperature was raised to 650°C at a heating rate of 5°C / min, and then r...

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Abstract

The invention relates to a nickel-phyllosilicate structure catalyst and a preparation method thereof. The catalyst has low-temperature low-pressure catalytic hydrogenation activity, high selectivity and high stability. The catalyst comprises the following components in percentage by mass: 5%-40% of active metal Ni, 0.01%-15% of an auxiliary agent X and the balance of a carrier, wherein the auxiliary agent X is any one of Ce, Mg or Mo, and the carrier is metal phyllosilicate composed of the metal and the auxiliary agent. The preparation method comprises the following steps: (1) preparing a metal salt mixed aqueous solution from an active component nickel precursor and an auxiliary agent X precursor in proportion; (2) dispersing the degassed SiO2 aerogel into the metal salt mixed aqueous solution; (3) adding urea into the SiO2 aerogel-Ni-X metal salt mixed aqueous solution, heating, refluxing and stirring; (4) centrifuging, washing, drying and roasting the obtained precipitate to obtaina Ni-X-Phy catalyst precursor; and (5) carrying out reduction treatment on the catalyst precursor to obtain the Ni@X-phy catalyst.

Description

technical field [0001] The invention relates to a nickel-phyllosilicate structure catalyst and a preparation method thereof, which belongs to the low-temperature and low-pressure hydrogenation for the preparation of coal-based 1,4-butynediol and direct hydrogenation to 1,4-butanediol in one step catalyst. Background technique [0002] Hydrogenation of 1,4-butynediol (BYD) is the main method for the industrial production of 1,4-butanediol (BDO). As an important organic synthesis and fine chemical raw material, BDO's downstream products are widely used in many fields such as chemical industry, medicine, textile, automobile and daily chemical industry. But since 1,4-butynediol (OH-CH 2 -C≡C-CH 2 -OH) itself is rich in a variety of unsaturated groups, and its hydrogenation process not only involves C≡C bonds, but also involves side reactions such as C-OH bond isomerization. So far, research on catalysts for this reaction system is limited to noble metals (Pd, Pt, etc.) and R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83B01J23/755B01J23/883C07C29/17C07C31/20
CPCB01J23/83B01J23/78B01J23/883C07C29/17C07C31/207
Inventor 王长真赵永祥张因武瑞芳
Owner SHANXI UNIV
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