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Ruthenium-palladium/carbon catalyst and preparation method thereof

A carbon catalyst and catalyst technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve problems such as uneconomical production and high hydrogenation operating pressure, Achieve the effects of no three wastes discharge, improve surface properties, and increase oxygen-containing functional groups

Inactive Publication Date: 2014-05-07
JIANGSU GOLD BRIDGE SALT & CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Patents US3334149, US3334149, and CN1099382 applied by U.S. Eastman Corporation all describe the method for preparing 1,4-cyclohexanedicarboxylate as raw material with dimethyl terephthalate, and the palladium / alumina catalyst used ( Palladium loading 0.5-1%) is constantly improving, but the pressure used is greater than 6.0MPa, and the higher operating pressure of hydrogenation is uneconomical in production

Method used

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  • Ruthenium-palladium/carbon catalyst and preparation method thereof
  • Ruthenium-palladium/carbon catalyst and preparation method thereof
  • Ruthenium-palladium/carbon catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Take 20g of self-made mesoporous carbon as the carrier material, place it in 80ml of 5mol / L nitric acid aqueous solution, immerse in a water bath at 80℃ for 12h, cool, filter, wash until neutral, and dry; at 120℃, vacuum conditions Lower degassing treatment for 2h;

[0046] (2) According to the active component ruthenium loading of 5.00% and palladium loading of 0.05%, respectively configure a 3mol / L ruthenium chloride solution and a 1.0mol / L palladium chloride solution;

[0047] (3) The acid-treated mesoporous carbon is impregnated with a ruthenium solution for 4 hours, dried at 80°C for 4 hours, and dried at 120°C for 6 hours by the vacuum equal amount impregnation method; the same method is used to impregnate the palladium solution, and then stand in a water bath at 80°C for 4 hours, at 80°C. Dry for 4 hours to obtain a ruthenium palladium-carbon catalyst precursor;

[0048] (4) Use a 10wt% NaOH aqueous solution to adjust the pH value to 11-12, precipitate for 2 hours,...

Embodiment 2

[0053] The ruthenium palladium / carbon catalysts with 8.0% and 1.0% ruthenium and palladium loadings were prepared by the same method as in Example 1. The catalyst number was CAT-2 / MC.

Embodiment 3

[0055] The ruthenium and palladium loadings were 3.0% and 0.1% ruthenium palladium / carbon catalysts prepared by the same method as in Example 1; the catalyst number was CAT-3 / MC.

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Abstract

The invention discloses a ruthenium-palladium / carbon catalyst and a preparation method thereof. A catalyst carrier is a carbon material, and active ingredients are Ru and Pd nanoparticles, wherein the load capacity of Ru is 0.5%-8.0%, the load capacity of Pd is 0.1%-2.0%, and the dispersity of ruthenium-palladium can achieve 30%-80%. The carrier is subjected to acid-base oxidization pretreatment, so that surface oxygen-containing functional groups can be increased, the property of ruthenium-palladium on the surface of the carbon material can be improved, the dispersity of ruthenium-palladium can be improved, the active ingredients can be firmly adsorbed on the functional groups, and the catalyst can show high activity in the reaction process. The prepared catalyst is applied to DMT (dimethyltryptamine) hydrogenation to prepare DMCD (dimethyl 1,4-cyclohexanedicarboxylate). The activity of the catalyst is not reduced after the catalyst is used for 20 times in an autoclave of 5000ml, the conversion rate of DMT can achieve 99.3%-100%, and the selectivity of DMCD can achieve 95.5%-96.4%. The purity of DMCD, which is simply distilled and purified, is greater than 99.5%. The preparation method has the advantages of being mild in technological conditions, simple in equipment, free from emission of three wastes, economic in investment, low in energy consumption, and feasible for industrialization.

Description

Technical field [0001] The invention relates to a high-activity and high-stability ruthenium-palladium / carbon catalyst for preparing DMCD by hydrogenation of DMT, a preparation method and application thereof, and belongs to the technical field of catalytic hydrogenation. Background technique [0002] Dimethyl terephthalate, abbreviated as DMT (Dimethyl terephthalate), is white needle-like crystals with a melting point of 140.7°C and a boiling point of 284°C. It is easy to sublime. Mainly used to synthesize polyester fiber, resin, film, polyester paint and engineering plastics. The one-step hydrogenation product of DMT is dimethyl 1,4-cyclohexanedicarboxylate (DMCD), and the two-step hydrogenation product is 1,4-cyclohexanedimethanol (CHDM). [0003] DMCD is an important type of organic intermediates and green chemicals. It can be used as a modified material for polymers and an important raw material for the production of CHDM. The high-performance polyester and other materials sy...

Claims

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Application Information

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IPC IPC(8): B01J23/46C07C69/75C07C67/303
Inventor 臧涵宋金文沈俭一申卫卫夏志朱天松
Owner JIANGSU GOLD BRIDGE SALT & CHEM GRP
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