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Ruthenium/aluminum oxide catalyst, as well as preparing method and application thereof

A catalyst and alumina technology, applied in physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve uneconomical production, increase operating costs, high-pressure reaction device costs, etc. problems, to achieve the effect of no three wastes discharge, long service life and low energy consumption

Inactive Publication Date: 2014-04-02
JIANGSU GOLD BRIDGE SALT & CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Obviously, the use of higher hydrotreating operating pressure is not economical in production, because of the increased operating costs and the cost of the required high-pressure reaction equipment

Method used

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  • Ruthenium/aluminum oxide catalyst, as well as preparing method and application thereof
  • Ruthenium/aluminum oxide catalyst, as well as preparing method and application thereof
  • Ruthenium/aluminum oxide catalyst, as well as preparing method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Macroporous water-thin pseudobauxite (Na 2 O≤0.1%, Fe 2 O 3 ≤0.02%) Calcination at 550℃ for 8h, heating rate 10℃ / min, to obtain γ-Al 2 O 3 Carrier, spare

[0044] (2) Prepare ruthenium solution based on 5% ruthenium loading, with a concentration of 1.0mol / L;

[0045] (3) Slowly add the solution prepared in (2) dropwise to alumina, immerse in vacuum for 6 hours, and let stand for 1 hour;

[0046] (4) Use 10% NaOH aqueous solution to adjust the pH value of the solution at 80°C to 11-12, precipitate for 3 hours, and let stand for 1 hour;

[0047] (5) Reduce the above solution with 37wt% formaldehyde, the amount used is 130% of the theoretical amount, and then stand for 2h after reduction for 2h;

[0048] (6) Filtration, washing, no Cl detected by silver nitrate solution - ; Keep it wet for later use.

[0049] The catalyst number is CAT-1. The pore size distribution of the catalyst is shown in figure 2 , The catalyst is used for DMT hydrogenation to prepare DMCD product distribu...

Embodiment 2

[0051] Change the ruthenium loading in step (2) in Example 1 to 3%, and the other steps are the same as in Example 1. The catalyst number is CAT-2.

Embodiment 3

[0053] Change the ruthenium loading in step (2) in Example 1 to 6%, and the other steps are the same as in Example 1. The catalyst number is CAT-3.

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Abstract

The invention discloses a ruthenium / aluminum oxide catalyst, as well as a preparing method and application thereof. The carrier of the catalyst is Al2O3, and Ru is used as an active ingredient of the catalyst, wherein the loading capacity of the Ru is 3.0% to 8.0%, and the grain diameter of the Ru is 1nm to 5nm. The catalyst has a specific surface area of 100-500m<2> / g, a pore volume of 0.8-1.2ml / g and a pore diameter of 2-50nm. Macro-porous aluminum oxide is used as a carrier precursor, water in micro-pores is effectively removed through baking pre-processing, the surface potential of hydrogen distribution and the pore diameter distribution are changed, and the dispersion degree of the ruthenium is improved. The prepared catalyst is used for the hydrogenation of dimethyl terephthalate (DMT) to prepare dimethyl cyclohexanedicarboxylates (DMCD). The activity of the catalyst is not reduced after being used in a 5000ml autoclave for 20 times. The conversion rate of the DMT is 99.3% to 100%, and the selectivity of the DMCD is 95.5% to 96.4%. Through simple distillation and purification, the purity of the DMCD is bigger than 99.5%. The preparing method has the advantages of mild technical conditions, simple equipment, no emission of three wastes, investment saving, low energy consumption and easy realization of industrialization.

Description

Technical field [0001] The invention relates to a ruthenium / alumina catalyst for preparing DMCD (dimethyl 1,4-cyclohexanedicarboxylate) by hydrogenation of DMT (dimethyl terephthalate) with high activity and stability, and a preparation method thereof. It 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 DMCD, and the two-step hydrogenation product is CHDM (1,4-cyclohexane dimethanol). [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 materia...

Claims

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Application Information

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IPC IPC(8): B01J23/46C07C69/75C07C67/303
Inventor 宋金文臧涵沈俭一夏志申卫卫朱成杰
Owner JIANGSU GOLD BRIDGE SALT & CHEM GRP
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