Preparation method of hydrogenation catalyst

A hydrogenation catalyst and catalyst technology are applied in the preparation of organic compounds, chemical instruments and methods, preparation of hydroxyl compounds, etc., which can solve the problems of large influence of catalyst activity, poor stability, and influence on product quality, etc., to improve the reaction Effects of activity and selectivity as well as stability, uniform grain size, and non-collapse

Active Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst prepared by this method has low selectivity and poor stability
During the reaction process, catalyst activity is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0035] Example 1

[0036] (1) At 20℃, it will contain 125 grams of Cu(NO 3 ) 2 .3H 2 O and 313.2 grams of Zn(NO 3 ) 2 .6H 2 1000ml of O mixed solution and precipitant ammonia (molar concentration of 4.41mol / L) are co-precipitated in parallel, and the pH of the precipitation system is maintained at 5.4. After the addition, continue constant temperature stirring for 50 minutes;

[0037] (2) Add 131.7 grams of Cu(NO) to the precipitate obtained in step (1) 3 ) 2 .3H 2 O and 204.4 g Al(NO 3 ) 3 9H 2 O, 48.5 g Mn (NO 3 ) 2 1000ml of soluble salt mixed solution (50ml of polyoxyethylene polyoxypropylene pentaerythritol ether is added) and precipitant ammonium carbonate (molar concentration of 1.7mol / L) are co-precipitated in parallel, while the temperature of the system is increased to 50°C , And maintain the pH value of the precipitation system at 6.6, after the co-current dripping, stir at constant temperature for 100 minutes;

[0038] (3) Filter the product obtained in step (2...

Example Embodiment

[0040] Example 2

[0041] (1) Put 125 grams of Cu(NO 3 ) 2 .3H 2 O and 99.32 g (NH 4 ) 6 H 2 W 12 O 40 .45H 2 O was dissolved in 1000mL deionized water, and then the precipitation agent ammonium carbonate (molar concentration of 5.0mol / L) was added dropwise for co-precipitation, and the pH of the precipitation system was maintained at 5.0. After the addition, the constant temperature stirring was continued for 60 minutes;

[0042] (2) Add 131 grams of Cu(NO) to the precipitate obtained in step (1) 3 ) 2 .3H 2 O and 145.44 grams of Al(NO 3 ) 3 9H 2 O, 38.4 grams of Ti(NO 3 ) 4 1000mL of soluble salt mixed solution and precipitating agent ammonia (molar concentration of 1.5mol / L, which contains 30mL of polyoxyethylene polyoxypropanolamine ether) are co-precipitated in parallel, while the temperature of the system is increased to 60 ℃, and Keep the pH of the precipitation system at 7.0, and after the co-current dripping is finished, stir at constant temperature for 90 minutes;

...

Example Embodiment

[0045] Example 3

[0046] (1) At 40℃, it will contain 155 grams of Cu(NO 3 ) 2 .3H 2 O and 161.7 grams of Mo(NO 3 ) 6 .5H 2 1000mL of O mixed solution and precipitating agent ammonia (molar concentration 5.0mol / L) are co-precipitated in parallel, and the pH of the precipitation system is maintained at 6.2. After the addition, continue constant temperature stirring for 60 minutes;

[0047] (2) First add 25 mL of polyoxypropylene oxide ethylene glycerol ether to the precipitate obtained in step (1), stir well and add 170 g of Cu(NO 3 ) 2 .3H 2 O and 187.0 g Al(NO 3 ) 3 9H 2 O, 70.9 g Zr(NO 3 ) 4 .5H 2 O soluble salt mixed solution 1000mL and precipitation agent ammonium bicarbonate (molar concentration of 2.0mol.L -1 ) Co-precipitation is added dropwise while the temperature of the system is increased to 70°C and the pH of the precipitation system is maintained at 7.5. After the dropwise addition is completed, constant temperature stirring is performed for 120 minutes;

[0048] ...

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Abstract

The invention discloses a preparation method of a hydrogenation catalyst. The catalyst has a formula of Cu-Al-A-B-O, wherein the A represents one or more components selected from Zn, Mo, and W, and the B represents one or more components selected from Ba, Mn, Mg, Ti, Ce, and Zr. The preparation method comprises the following steps: subjecting part of Cu and A to a parallel-flow precipitation treatment, and then subjecting the rest Cu, Al and B to a parallel-flow precipitation treatment; wherein the two parallel-flow precipitation treatments are carried out under different conditions and the second parallel-flow precipitation treatment is carried out on the basis of the first parallel-flow precipitation treatment so as to form a stable frame structure of the catalyst, and moreover, a supercritical drying technology is adopted so as to enable the prepared catalyst to have a larger specific surface area and more concentrated pore distribution; furthermore, metal nano particles do not agglomerate during the drying process, and thus the prepared catalyst has the advantages of uniform particle size and concentrated pore distribution. The catalyst is used during a hydrogenation method for preparing 1,4-butanediol from dialkyl maleate and/or dialkyl succinate. The reaction activity, reaction selectivity, and stability of the catalyst are all improved.

Description

technical field [0001] The invention relates to a method for preparing a hydrogenation catalyst, in particular, using dialkyl maleate and / or dialkyl succinate as raw materials to produce 1,4-butanediol by gas-phase hydrogenation and A method for preparing a hydrogenation catalyst for the co-production of tetrahydrofuran and gamma-butyrolactone. Background technique [0002] 1,4-Butanediol is an important basic organic chemical raw material, mainly used in the production of tetrahydrofuran, polybutylene terephthalate (PBT), γ-butyrolactone and polyurethane (PU). In recent years, due to the rapid growth in the demand for thermoplastic elastic fibers and elastomers, the demand for PTMEG (polytetramethylene ether glycol) and PTMG (polytetrahydrofuran ether) as monomers is strong, making the upstream raw material 1,4-butanedi The demand for alcohol is also growing rapidly, and major 1,4-butanediol producers in the world, such as BASF and DUPON, have expanded their production c...

Claims

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Application Information

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IPC IPC(8): B01J23/889B01J23/888B01J23/885C07C29/149C07C31/20C07D307/08C07D307/33
Inventor 张艳侠高鹏付秋红袁胜华张皓段日包洪洲乔凯
Owner CHINA PETROLEUM & CHEM CORP
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