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Ruthenium-based catalyst as well as preparation method and application thereof

A ruthenium-based catalyst and catalyst technology, applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of dependence on alkaline additives, harsh reaction conditions, and easy deactivation, and achieve easy industrialization Application, high selectivity, and the effect of less by-product formation

Inactive Publication Date: 2021-04-27
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, the catalyst system in the prior art has the disadvantages of low activity, easy deactivation, harsh reaction conditions, and the need to rely on alkaline additives.

Method used

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  • Ruthenium-based catalyst as well as preparation method and application thereof
  • Ruthenium-based catalyst as well as preparation method and application thereof
  • Ruthenium-based catalyst as well as preparation method and application thereof

Examples

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preparation example Construction

[0024] As another aspect of the present invention, also provide a kind of preparation method as above-mentioned ruthenium-based catalyst, this preparation method comprises the steps:

[0025] Step 1: impregnating carbon nitride with an aqueous solution containing a ruthenium source to obtain a catalyst precursor mixed suspension;

[0026] Step 2: adding a reducing agent to the mixed suspension of the catalyst precursor, and performing a reduction and activation reaction on the ruthenium ions supported on the carbon nitride to obtain a ruthenium-based catalyst.

[0027] In some embodiments of the present invention, in step 1, the ruthenium source includes a water-soluble ruthenium salt;

[0028] Wherein the source of ruthenium can be but not limited to ruthenium trichloride;

[0029] Wherein the concentration of the ruthenium source in the aqueous solution containing the ruthenium source is 0.1 g / L-10 g / L.

[0030] In some embodiments of the present invention, in step 1, the ...

Embodiment 1

[0038] The ruthenium-based catalyst supported by carbon nitride is prepared by impregnation method, and the specific operation steps are as follows:

[0039] (1) At room temperature, put 55 g of urea in a crucible with a lid, place it in a muffle furnace for calcination at 600°C for 4 hours, rinse it with deionized water and ethanol three times, and dry it in an oven at 80°C overnight.

[0040] (2) 0.2gRuCl 3 Dissolve in 100mL deionized water, add 1.9g of carbon nitride obtained in step (1) under stirring, continue stirring for 10min, and ultrasonically immerse for 30min to obtain a mixed suspension;

[0041] (3) Add 0.22 g of sodium borohydride to the mixed suspension obtained in step (2), continue ultrasonication for 30 min, take it out, and stir for 12 h.

[0042] (4) Centrifuge the suspension described in step (3), wash and filter the obtained precipitate with deionized water and ethanol, and dry at 100° C. for 12 hours to obtain a solid catalyst.

[0043] Performance te...

Embodiment 2

[0047] This example adopts the preparation method of the ruthenium-based catalyst in Example 1, the difference is that the carbon nitride precursor urea is replaced by melamine in the catalyst preparation step (1), and other conditions are exactly the same as those in Example 1.

[0048] The performance test conditions of the catalyst obtained in this embodiment are exactly the same as those in Example 1.

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Abstract

The invention discloses a ruthenium-based catalyst as well as a preparation method and application thereof. The ruthenium-based catalyst comprises an active component metal ruthenium and a carrier carbon nitride, wherein the metal ruthenium accounts for 0.1%-30% of the total mass of the ruthenium-based catalyst. Compared with the prior art, the ruthenium-based catalyst prepared by the invention is used for preparing 1,4-cyclohexanediamine by selective hydrogenation of p-phenylenediamine, an alkali metal additive does not need to be introduced, p-phenylenediamine can be converted into 1,4-cyclohexanediamine with high activity and high selectivity, and the side reaction of deamination is effectively inhibited.

Description

technical field [0001] The invention relates to the field of catalyst preparation, in particular to a ruthenium-based catalyst, a preparation method and an application thereof. Background technique [0002] 1,4-Cyclohexanediamine (CHDA), as an aromatic amine compound, can be used as a raw material for fuels and pharmaceutical intermediates, and can also be used to prepare chemical products such as polyamide resins. In addition, it can be used in the polyurethane industry to prepare 1 , 4-cyclohexane diisocyanate is an important fine chemical intermediate in the chemical industry. Therefore, the development of 1,4-cyclohexanediamine production has important industrial value. [0003] In the reported research so far, Ru is loaded on Al 2 o 3 As a catalyst, at a temperature of 160°C to 200°C and a hydrogen circulation pressure of 4MPa to 8MPa, with 1,4-dioxane as a solvent, p-phenylenediamine undergoes a hydrogenation reaction in a fixed-bed reactor to obtain The target pro...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J23/46B01J35/10C07C209/72C07C211/36
CPCB01J27/24B01J23/462C07C209/72C07C2601/14B01J35/613B01J35/615C07C211/36
Inventor 王利国韩风刚李会泉贺鹏曹妍陈家强徐爽
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI