Method for regenerating ruthenium hydrogenation catalyst

A hydrogenation catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve fine chemical industry and partial hydrogenation catalyst regeneration inappropriate, Unable to deal with catalyst high boilers, limitations, and insufficient effects, etc., to achieve beneficial effects for maintenance and operation, performance recovery, and obvious effects

Active Publication Date: 2014-05-28
WANHUA CHEM GRP CO LTD +1
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has strong limitations and is only suitable for hydrogenation catalytic systems where water inhibits the activity of the catalyst. Causes catalyst deactivation, especially due to high boiler attachment, has little effect
[0008] In the past technology involving catalyst regeneration, the use of oxygen or air oxidation at high temperature is the most commonly used method. The high operating temperature of this method is generally above 300°C, which can easily cause metal sintering on the surface of the catalyst, which will accelerate the deactivation of the catalyst.
Therefore, the traditional high-temperature oxidation method for removing carbon deposits is not suitable for most fine chemicals and partial hydrogenation catalyst regeneration.
However, the currently reported ruthenium catalyst regeneration method has potential safety hazards in operation, and cannot deal with high boilers on the surface of the catalyst, which has the disadvantages of applicable limitations and insufficient effect.

Method used

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  • Method for regenerating ruthenium hydrogenation catalyst
  • Method for regenerating ruthenium hydrogenation catalyst
  • Method for regenerating ruthenium hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0032] MDA (p-diaminodiphenylmethane) hydrogenation to PACM (p-diaminodicyclohexylmethane) catalyst regeneration evaluation, the hydrogenation reaction process is as follows:

[0033] In a high-pressure reactor with a volume of 2L, add ruthenium / activated carbon (the content of metal ruthenium is 5wt%, based on the total weight of the catalyst) catalyst 12.5g, feed MDA 250g and methanol 250g each time, airtightly replace the air, and fill with hydrogen , at a temperature of 160°C and a pressure of 60 bar, start the hydrogenation reaction and calculate the reaction time, and stop the reaction when the reaction no longer absorbs hydrogen. The product was sampled and analyzed by capillary gas chromatography, and except for the solvent, the composition of other main components is shown in Table 1.

[0034] The quantitative analysis of the MDA hydrogenation product uses an instrument for gas chromatography, and the analysis conditions are:

[0035] The initial temperature is 50°...

Embodiment 2

[0063] MDA hydrogenation to PACM, deactivated Ru / TiO 2 (The content of metal ruthenium is 5wt%, based on the total weight of the catalyst) Catalyst regeneration evaluation, MDA hydrogenation reaction with reference to Example 1.

[0064] Before the regeneration operation of the catalyst, 40 batches have been applied mechanically, the reaction time is prolonged by 200%, and the by-product of high boilers (polyamines containing four rings or more than four rings) is 17%. The catalyst regeneration method is as follows:

[0065] a) In an ultrasonic cleaner with a volume of 2L, add deactivated ruthenium / TiO 2 (5wt%) catalyst 12.5g, add 500g methanol, under the protection of nitrogen at 150°C, pressure 0.5MPa, ultrasonic frequency 100KHz, power 300w, after ultrasonic 2h, filter to remove the solvent.

[0066] b) adding pH to the ultrasonic cleaning machine is 20wt% (NH 4 ) 2 RuCl 6 (Bailingwei, GR grade, 99%) aqueous solution 500g, at 150°C, 0.5MPa, keep the ultrasonic frequenc...

Embodiment 3

[0072] Catalyst regeneration evaluation for hydrogenation of aniline to cyclohexylamine, the hydrogenation reaction is as follows:

[0073] In a 2L autoclave, add Ru / Al 2 o 3 Catalyst (the content of metal ruthenium is 3wt%, based on the total weight of the catalyst) 6g, 500g of aniline is fed each time, the air is replaced after airtight, and hydrogen is charged. At a temperature of 140°C and a pressure of 50bar, the hydrogenation reaction is started and Calculate the reaction time, and the reaction stops when the reaction no longer absorbs hydrogen. The product was sampled and analyzed by capillary gas chromatography, and except for the solvent, other key components were found in the table below, expressed in weight percentage.

[0074] The instrument used for quantitative analysis of aniline hydrogenation reaction product is gas chromatography, and the analysis conditions are:

[0075]

[0076] The initial temperature is 50°C, kept for 2 minutes, then raised to 80°C...

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Abstract

The invention discloses a method for regenerating a ruthenium hydrogenation catalyst. The method comprises the following steps: (a) inactivated load ruthenium hydrogenation catalyst is ultrasonically cleaned in ultrasonic equipment under the protection of inert gas in presence of a solvent; (b) the catalyst treated in the step (a) is oxidized and regenerated in liquid phase in presence of an oxidant; (c) the catalyst treated in the step (b) is dried and reduced. The method for regenerating the ruthenium hydrogenation catalyst can effectively remove high-boiling organic matters attached on the surface of the catalyst, can supplement load active components lost in the catalyst, can effectively recover the activity and selectivity of the catalyst, can prolong the service life of the catalyst, and can reduce the production cost.

Description

technical field [0001] The invention relates to a method for regenerating a ruthenium hydrogenation catalyst, in particular to a method for prolonging the service life of the ruthenium hydrogenation catalyst through regeneration operation. Background technique [0002] Hydrogenation reaction is one of the cores of today's chemical industry, and almost all hydrogenation processes require the use of catalysts. For catalysts, there is a certain service life. During the normal operation of the catalyst, it can be divided into induction period, stable period and deactivation period according to the time. Catalyst deactivation does not mean that the activity of the catalyst is completely lost, but that the activity and selectivity of the catalyst gradually decrease compared to the stable period. [0003] Catalyst deactivation is a rather complex physical and chemical process. Generally, deactivation can be divided into the following two situations: one is irreversible deactivat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/96
Inventor 张聪颖陈浩李鑫高山刘振国王伟嘉唐磊刘志鹏黎源丁晧
Owner WANHUA CHEM GRP CO LTD
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