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Low-content supported ruthenium-palladium bimetal hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst, supported technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of high usage, high cost of catalyst materials, single metal It can improve and improve the catalytic selective hydrogenation performance of materials, reduce the cost of materials, and reduce the consumption of precious metals.

Inactive Publication Date: 2013-06-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the actual industrial production process, the selective hydrogenation of dimethyl terephthalate (DMT) to dimethyl 1,4-cyclohexanedicarboxylate mainly uses monometallic noble metal catalyst materials, in which noble metal The amount of the catalyst used is as high as 2% to 10%, which makes the cost of the catalyst material higher. At the same time, due to the small force of the single metal on the carrier, it is very prone to shedding and poisoning during use.

Method used

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  • Low-content supported ruthenium-palladium bimetal hydrogenation catalyst and preparation method thereof
  • Low-content supported ruthenium-palladium bimetal hydrogenation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Measure 5.4g of spherical θ-Al with a volume of 11ml and a particle size of 20-40 mesh 2 o 3 , placed in 12ml of a mixed solution of ruthenium nitrate and palladium nitrate, the mass ratio of ruthenium nitrate and palladium nitrate is 1:1, the total concentration of metal ions is 0.013mol / L, ultrasonic treatment at 25°C for 12h, and then cooling, After washing and filtering, drying at 70°C for 6h, and then calcining at 450°C for 8h to obtain a low-content supported ruthenium-palladium bimetallic nanocatalyst Ru-Pd / Al 2 o 3 , the mass ratio of active metal ruthenium and palladium in the catalyst measured by inductively coupled plasma emission spectroscopy is 19:21, and the total content is 0.28wt%.

[0025] Based on the liquid phase reactor evaluation device, weigh 0.5g Ru-Pd / Al 2 o 3 , placed in 10ml of deionized water, adding sodium hydroxide to adjust the pH to 10; adding 10 drops of fresh sodium borohydride aqueous solution, the concentration of sodium borohydrid...

Embodiment 2

[0028] Measure 8.5g volume and be 17ml particle size be 40-60 purpose clover-shaped η-Al 2 o 3 , placed in 16ml of ruthenium chloride solution with a concentration of 0.005mol / L, ultrasonically treated at 45°C for 24h, then cooled, washed and filtered, then dried at 40°C for 12h, and then the obtained dry solid Place in 16ml of palladium nitrate solution with a concentration of 0.01mol / L, ultrasonically treat at 45°C for 24h, then cool, wash and filter, dry at 40°C for 12h, and finally at 500°C Calcination treatment for 6h to obtain low-content supported ruthenium-palladium bimetallic nanocatalyst Ru-Pd / Al 2 o 3 , the mass ratio of active metal ruthenium and palladium in the catalyst measured by inductively coupled plasma emission spectrometry is 19:39, and the total content is 0.29wt%.

[0029] Based on the liquid phase reactor evaluation device, weigh 0.4gRu-Pd / Al 2 o 3 , put in 5ml deionized water, add sodium hydroxide to adjust the pH to 8; add dropwise 5 drops of fre...

Embodiment 3

[0032] Measure 12.5g volume of 25ml flake δ-Al with a particle size of 10-30 mesh 2 o 3 , placed in a mixed solution of 24ml of ruthenium chloride and palladium chloride, wherein the mass ratio of ruthenium chloride and palladium chloride is 2:1, the total molar concentration of metal is 0.01mol / L, ultrasonic treatment at 30°C 12h, after cooling, washing and filtering, drying at 50°C for 10h, and finally calcining at 400°C for 6h to obtain a low-content supported ruthenium-palladium bimetallic nanocatalyst RuPd / Al 2 o 3 , the mass ratio of active metal ruthenium and palladium in the catalyst was measured by inductively coupled plasma emission spectrometry to be 40:19, and the total content was 0.19wt%.

[0033] Based on the liquid phase reactor evaluation device, weigh 0.5g RuPd / Al 2 o 3 , put in 15ml deionized water, add sodium hydroxide to adjust the pH to 11; add dropwise 12 drops of fresh sodium borohydride aqueous solution (concentration: 800g / L), stir for 50min, afte...

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Abstract

The invention belongs to the technical field of catalysts and particularly relates to a low-content supported ruthenium-palladium bimetal hydrogenation catalyst and a preparation method thereof. The preparation method of the catalyst comprises the following steps: preparing a ruthenium monometal solution and a palladium monometal solution; under ultrasonic conditions, supporting the two active components (ruthenium and palladium) of the metal catalyst on the surface of an aluminum oxide carrier by respectively adopting a co-impregnation method and a fractional impregnation method; and washing, drying, roasting, and performing other treatment processes to finally obtain the low-content supported ruthenium-palladium bimetal hydrogenation catalyst. According to the invention, the method is low in cost; and the prepared bimetal hydrogenation catalyst has high selective hydrogenation activity, and shows excellent catalytic activity, favorable catalytic stability and high 1,4-cyclohexanedicarboxylic acid dimethyl ester (CHDM) yield when being used in the reaction process of preparing CHDM through selective hydrogenation of dimethyl terephthalate.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a low-content supported ruthenium-palladium bimetallic hydrogenation catalyst and a preparation method thereof, which is applied to catalyze the selective hydrogenation synthesis of dimethyl phthalate (DMT). The reaction of dimethyl 4-cyclohexanedicarboxylate (DMCD). Background technique [0002] As an important catalyst material, supported catalysts are widely used in petrochemical processes, especially in the selective hydrogenation and oxidation of hydrocarbons such as olefins and aromatics, due to their excellent heat and mass transfer properties and their suitability for continuous reactions. It has been widely used in important reaction processes such as catalysis, and its usage accounts for more than 70% of the total amount of catalysts. [0003] In the petrochemical process, the common supported metal catalysts are mostly monometallic catalysts, whose main ...

Claims

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Application Information

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IPC IPC(8): B01J23/46C07C69/75C07C67/303
Inventor 张法智陈加利郭莉
Owner BEIJING UNIV OF CHEM TECH
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