Preparation method of butanediol secondary hydrogenation catalyst by butynediol two-step hydrogenation

A technology for butynediol and butanediol production, which is applied in the fields of hydrogenation preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., and can solve the problem of poor catalyst stability, affecting normal operation, and parking accidents and other problems, to achieve high catalytic activity and selectivity, and long catalyst service life

Active Publication Date: 2008-11-19
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the pulverization of silica gel under the high pressure of the second stage reaction, the fine particles produced will cause the pressure fluctuation of the reactor, resulting in the occurrence of parking accidents
The poor stability of the catalyst greatly affects the normal production

Method used

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  • Preparation method of butanediol secondary hydrogenation catalyst by butynediol two-step hydrogenation

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take an alumina carrier, impregnate it with a conventional soluble magnesium salt, dry it, and calcine it to obtain a carrier containing 4w% magnesium; take 100 g of the carrier and treat it at 150°C under 0.1mm Hg pressure for 10 minutes, or directly heat it in a blast oven at 150°C 3h, then lowered to room temperature for later use; weigh 59.4g nickel nitrate hexahydrate, 50.8g nickel acetate tetrahydrate and 1g polyethylene glycol 4000 to prepare 200mL mixed nickel salt solution; take 200mL prepared mixed nickel salt solution and dip into In 100g of the treated carrier, let it stand at room temperature for 2h; filter off the excess solution, dry at 120°C for 8h, heat up to 450°C and roast for 8h to decompose the salt, and then in H 2 Reduction treatment was carried out at 350° C. for 30 h in a stream, and after cooling down to room temperature, it was deactivated by oxygen to obtain Catalyst No. 1.

Embodiment 2

[0024] An alumina carrier was taken, impregnated with a conventional soluble copper salt, dried, and calcined to obtain a carrier containing 3w% copper; the rest of the steps were the same as in Example 1 to obtain Catalyst No. 2.

Embodiment 3

[0026] An alumina carrier was taken, impregnated with a conventional soluble molybdenum salt, dried, and calcined to obtain a carrier containing 4w% molybdenum; the rest of the steps were the same as in Example 1 to obtain catalyst No. 3.

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Abstract

The invention provides a method for preparing a butanediol secondary hydrogenation catalyst through adopting the butynediol two-step hydrotreation, and the method comprises the following steps: an accelerant is introduced into an alumina carrier; the carrier is heated; mixed nickel complex solution containing organic nickel salt, inorganic nickel salt and surfactant is prepared; the mixed nickel salt solution is dipped on the heated carrier, and the catalyst product with the nickel content of 5-25 w% and the accelerant content of 0.001-6 w% can be obtained by drying, baking, deoxidizing and passivating. The catalyst can be used in the process of preparing the butanediol secondary hydrogenation by adopting the butynediol two-step hydrotreation, the carbonyl can be reduced to be lower than 0.2 mg (KOH)*g<-1>, and the contents of acetal and butylene glycol are enabled to be reduced to the lowest level. Through the subsequent rectification, the butylene glycol product with the purity more than or equal to 99.5 percent and the chromaticity lower than or equal to 10 AHPA can be produced.

Description

technical field [0001] The invention relates to a two-stage hydrogenation catalyst, in particular to a preparation method of a two-stage hydrogenation catalyst for 1,4-butynediol hydrogenation to 1,4-butanediol. Background technique [0002] The two-step hydrogenation of 1,4-butynediol to 1,4-butanediol involves the following process: the first step (also known as one-stage hydrogenation) generally adopts a suspended bed (or bubbling slurry bed), using Raney-nickel catalyst, low-pressure hydrogenation at 50-80°C, 1-3MPa hydrogen pressure, hydrogenation of 1,4-butynediol to 1,4-butanediol, while the solution contains butanol , unsaturated hydrogenation product butene diol, butene diol isomerization product 4-hydroxybutyraldehyde and acetal obtained by condensation reaction of aldehyde and alcohol; because 4-hydroxybutyraldehyde and acetal cannot pass rectification method to remove, the presence in the product affects the purity and quality of the product, and further high-pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78B01J23/755B01J23/883C07C29/17C07C31/20
Inventor 赵永祥李海涛杨学英孙自瑾张鸿喜梁小元刘滇生张因盖媛媛
Owner SHANXI UNIV
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