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Preparation method of Ni-SiO2/Al2O3 catalyst

A catalyst, c·min-1 technology, applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., can solve the problems of increased consumption, unsatisfactory hydrogenation effect, etc., to reduce the content and reduce the color of the product. degree, the effect of improving the utilization rate

Active Publication Date: 2012-11-21
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to carry out further hydrogenation conversion and product separation to 1,4-butanediol finished product, has increased the input of extra equipment and the consumption of energy, and the hydrogenation catalyst that it uses is general type hydrogenation catalyst, and its hydrogenation The effect is not ideal

Method used

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  • Preparation method of Ni-SiO2/Al2O3 catalyst
  • Preparation method of Ni-SiO2/Al2O3 catalyst
  • Preparation method of Ni-SiO2/Al2O3 catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take the specific surface area as 223m 2 g -1 , the pore volume is 0.62cm 3 g -1 , with an average pore diameter of 9.75nm on the alumina carrier, impregnating the ethanol solution of tetraethyl orthosilicate on the alumina carrier, drying, and calcining to obtain SiO with a silicon mass fraction of 0.5%. 2 / Al 2 o 3 Carrier: Weigh 50.0g nickel chloride and 25.3g urea to prepare 100ml nickel salt solution; take 90ml prepared nickel salt solution and impregnate it into 100g SiO with a silicon mass fraction of 0.5%. 2 / Al 2 o 3 In the carrier, stir well at room temperature, seal it in the container and let it stand for 14 hours; heat the sealed container with the sample in a blast oven at 90°C for 10 hours; then open the container, and dry the sample in a blast oven at 90°C Dry for 5 hours, then heat up to 120°C and dry for 4 hours; -1 Heating up to 110°C, and then at 0.5°C·min -1 Heating up to 250°C, and finally at 2°C·min -1 Raise the temperature to 450°C, kee...

Embodiment 2

[0036] Take the specific surface area as 110m 2 g -1 , the pore volume is 0.40cm 3 g -1 , with an average pore diameter of 14.08nm on the alumina support, impregnating the ethanol solution of methyl orthosilicate on the alumina support, drying, and roasting to obtain SiO with a silicon mass fraction of 1%. 2 / Al 2 o 3 Carrier: Weigh 124.4g of nickel sulfate and 14.2g of urea to prepare 100ml of nickel salt solution; take 90ml of prepared nickel salt solution and impregnate it into 100g of SiO with a silicon mass fraction of 1%. 2 / Al 2 o 3 In the carrier, stir well at room temperature, seal it in the container and let it stand for 20 hours; place the sealed container with the sample in a blast oven at 95°C and heat it for 10 hours; then open the container, and dry the sample in a blast oven at 95°C Dry for 5 hours, then heat up to 120°C and dry for 4 hours; -1 Heating up to 110°C, and then at 0.1°C·min -1 Heating up to 250°C, and finally at 5°C·min -1 Raise the tempe...

Embodiment 3

[0038] Take the specific surface area as 350m 2 g -1 , the pore volume is 1.02cm 3 g -1 , with an average pore diameter of 7.63nm on an alumina support, impregnating the ethanol solution of ammonium silicofluoride onto the alumina support, drying and calcining to obtain SiO with a silicon mass fraction of 3%. 2 / Al 2 o 3 Carrier; take 137.6g of nickel nitrate and 2.8g of urea to prepare 100ml of nickel salt solution; take 60ml of the prepared nickel salt solution and impregnate it into 50g of SiO with a silicon mass fraction of 3% above 2 / Al 2 o 3 In the carrier, stir well at room temperature, seal it in the container and let it stand for 3 hours; place the sealed container with the sample in a blast oven at 95°C and heat it for 7 hours; then open the container, and dry the sample in a blast oven at 90°C Dry for 3 hours, then heat up to 120°C and dry for 12 hours; then dry in air atmosphere at 2°C·min -1 Heating up to 110°C, and then at 1°C·min -1 Heating up to 250°C...

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Abstract

The invention provides a preparation method of Ni-SiO2 / Al2O3 catalyst, which comprises the steps of: introducing auxiliaries into an alumina carrier; heating the carrier; preparing nickel salt containing urea; impregnating the solution onto the heated carrier in a manner of isometric impregnation; placing the impregnated sample in a sealed container for in-situ reaction at the temperature higher than 90 DEG C; and carrying out drying, roasting, reducing and passivating to obtain the catalyst product which contains 5 to 25% of nickel by mass fraction and 0.5 to 7% of silicon auxiliary by mass fraction and which includes the double functions of hydrolysis and hydrogenation. The catalyst is used for the secondary hydrogenation process for the preparation of 1, 4-butanediol from hydrogenated 1,4-butynediol by a two-step method, thereby accomplishing the hydrolyzed and hydrogenated conversion of chromophore cyclic acetal, reducing the chromaticity of 1,4-butanediol products and improving the product quality.

Description

technical field [0001] The present invention relates to a catalyst, specifically a kind of cyclic acetal 2-(4'-hydroxybutoxy)-tetrahydrofuran hydrolysis and hydrogenation conversion Ni in the two-stage hydrogenation process of 1,4-butynediol -SiO 2 / Al 2 o 3 Catalyst preparation method. Background technique [0002] The two-stage hydrogenation process of 1,4-butynediol to prepare 1,4-butanediol is a complex system containing multiple components and accompanied by many side reactions. In this system, containing 1,4-butynediol, 1,4-butenediol, 4-hydroxybutyraldehyde, hemiacetal and acetal 2-(4'-hydroxybutoxy)-tetrahydrofuran and other unsaturated carbonyl compounds. There are the following chemical changes between them: [0003] HO-CH 2 -C≡C-CH 2 -OH+H 2 →HO-CH 2 -CH=CH-CH 2 -OH+154.8KJ / mol (1) [0004] 1,4-butynediol 1,4-butenediol [0005] HO-CH 2 -CH=CH-CH 2 -OH+H 2 →HO-CH 2 -CH 2 -CH 2 -CH 2 -OH+96.3KJ / mol (2) [0006] 1,4-butenediol 1,4-butanediol ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755C07C31/20C07C29/141C07C29/88
Inventor 赵永祥李海涛宋美婷秦晓琴
Owner SHANXI UNIV
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