Regeneration method for inactivated rh-p (rhodium-phosphine) complex catalyst for carbonylation reaction

A technology of carbonylation reaction and complexes, which is applied in the field of regeneration of deactivated rhodium-phosphine complex catalysts in carbonylation reactions, to achieve the effects of easy industrialization, reduced dosage, and improved catalyst activity

Active Publication Date: 2013-03-06
CHINA PETROLEUM & CHEM CORP
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Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide a kind of catalyst regeneration method that is easy to industrially implement for the dea

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  • Regeneration method for inactivated rh-p (rhodium-phosphine) complex catalyst for carbonylation reaction

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Embodiment 1～6 and comparative example 7

[0035] In the butyraldehyde reaction liquid produced by the industrial butanol unit, the activity of the rhodium catalyst has been reduced from 100% to about 25% of the fresh catalyst. After removing part of the butyraldehyde, the rhodium content is about 1100mg / kg, and the triphenylphosphine content is about 10%. . Add 50 g of the reaction solution containing the partially deactivated catalyst into a 100 ml reactor, purging the reactor with nitrogen, and then adding acetylenic alcohols or esters containing 3 to 6 carbon atoms in different proportions as shown in Table 1 React with carboxylic acid, add 10% triethanolamine aqueous solution into the reactor after the reaction, neutralize unreacted carboxylic acid or halide, and generate water-soluble salt.

[0036] After the neutralization reaction is finished, two distinct liquid phases are formed by static settling, which are separated to obtain an organic phase containing an aqueous phase and a rhodium complex catalyst. The ...

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Abstract

The invention relates to a regeneration method for inactivated rh-p (rhodium-phosphine) complex catalyst for carbonylation reaction, which comprises the following steps of: firstly, carrying out hybrid reaction on inactivated rh complex catalyst reaction liquid with 3-6 carbon atom containing alkynol or ester and a carboxylic acid; then, adding a tertiary alkanolamine aqueous solution into the obtained reaction liquid, so that unreacted carboxylic acids or halides are neutralized, and then a water soluble salt is generated; carrying out settling separation on the water soluble salt so as to obtain a rh-p complex catalyst containing organic phase; and washing the separated organic phase with water so as to obtain a rh complex catalyst containing solution which has higher catalytic activity in comparison with the inactivated rh complex catalyst. According to the regeneration method provided by the invention, the application amount of an expensive-price and large-toxicity regenerated reaction reagent (3-6 carbon atom containing alkynol or ester) can be greatly reduced; the reaction conditions are moderate, so that the online regeneration of catalysts can be performed under the condition of not stopping the continuous carbonylation reaction; and the technological process is simple, and the activity of the catalyst subjected to regeneration is high, thereby solving the problem that the regeneration cost of the catalyst is high.

Description

technical field [0001] The invention belongs to the technical field of catalyst regeneration, in particular to a method for regeneration of a carbonylation reaction deactivated rhodium-phosphine complex catalyst. Background technique [0002] The "OXO" reaction is the oxo synthesis reaction, also known as the hydroformyl reaction or hydroformylation reaction. In the low-pressure carbonylation process of aldehydes, the catalyst used in the reaction process is a rhodium-phosphine catalyst system. Using this catalyst, the reaction pressure is low and side reactions are few, which are well known in the art. However, as the continuous oxo reaction proceeds, the rhodium-phosphine catalyst loses or partially deactivates even in the substantial absence of exogenous catalyst poisons. The comprehensive effect of reaction process conditions such as reaction temperature, reactant partial pressure, phosphine ligand / rhodium molar ratio, rhodium concentration, etc., can lead to the forma...

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Application Information

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IPC IPC(8): B01J31/40B01J31/24
Inventor 菅秀君王申军潘清刘淑芝何宗华马瑞杰
Owner CHINA PETROLEUM & CHEM CORP
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