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Preparation method of hydroformylation homogeneous complex catalyst

A hydroformylation catalyst, olefin hydroformyl technology, applied in the direction of organic compound/hydride/coordination complex catalyst, carbon monoxide reaction preparation, physical/chemical process catalyst, etc., can solve unfavorable industrial promotion and application, process steps cumbersome and other problems, to achieve the effect of wide application range, simplified process flow and mild process conditions

Active Publication Date: 2012-03-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above two methods have their own beneficial aspects, but the problem is that the process steps are too complicated, which is not conducive to industrial promotion and application.

Method used

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Examples

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Effect test

Embodiment 1

[0043] The used catalyst waste liquid is the deactivated catalyst in the process of producing butyraldehyde in the hydroformylation reaction of propylene with carbon monoxide and hydrogen, and its activity is reduced to below 30% of the fresh catalyst. The catalyst waste liquid was concentrated on a scraped thin film evaporation device. The concentration of rhodium in the gained concentrated waste liquid is 4900ppm.

[0044] Add 8.08 g of the above-mentioned concentrated catalyst waste liquid and 50 ml of absolute ethanol into a 500 ml three-neck flask, stir to fully dissolve them, then add 50 ml of 1mol / L ethanol solution of nitric acid, and mix well. Add 2ml of hydrogen peroxide to the flask, slowly heat to 70°C, and react for 5h. Then 50 ml of an ethanol solution containing 2.5 g of NaOH was added. Feed synthesis gas into the reaction system, and after staying for 30 minutes, add 50 ml of ethanol solution containing 1.00 g of triphenylphosphine, raise the temperature to 8...

Embodiment 2

[0046] In a 500ml three-necked flask, add 9.04g of concentrated catalyst waste liquid and 50ml absolute ethanol in Example 1, stir to make it fully dissolve, then add the ethanol solution of 50ml 1mol / L nitric acid, and mix homogeneously. Air is passed into the mixed solution in the flask, and the air is bubbled through the bottom of the liquid through an immersion tube, so that the oxygen and the catalyst waste liquid are fully contacted and reacted, and the flow rate of the air is 100ml / min. Stir and slowly raise the temperature to 90°C, stop feeding air after 20 hours of reaction. Then 50 ml of ethanol solution containing 2.5 g of NaOH was added and the temperature was lowered to 80°C. Feed synthesis gas into the reaction system, and after staying for 30 minutes, add 50 ml of ethanol solution containing 1.00 g of triphenylphosphine, and continue to stir and react for 30 minutes. Then 50 ml of an ethanol solution containing 1.40 g of NaOH and 0.91 g of sodium borohydride we...

Embodiment 3

[0048] In a 500ml three-necked flask, add 8.55g of concentrated catalyst waste liquid and 50ml of absolute ethanol in Example 1, stir to make it fully dissolved, then add 50ml of 1mol / L ethanol solution of sulfuric acid, and mix well. Air is introduced into the mixed solution in the flask, and the air is bubbled through the bottom of the liquid through an immersion tube, so that the oxygen and the catalyst waste liquid can fully contact and react, and the flow rate of the air is 100ml / min. Stir and slowly raise the temperature to 90°C, stop feeding air after 20 hours of reaction. Then 50 ml of ethanol solution containing 2.5 g of NaOH was added and the temperature was lowered to 80°C. Feed synthesis gas into the reaction system, and after staying for 30 minutes, add 50 ml of ethanol solution containing 1.00 g of triphenylphosphine, and continue to stir and react for 30 minutes. Then 50 ml of an ethanol solution containing 1.40 g of NaOH and 0.90 g of sodium borohydride were a...

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Abstract

The invention discloses a preparation method of a hydroformylation homogeneous complex catalyst and aims at directly preparing hydridocarbonyl tri(triphenylphosphine) rhodium by taking hydroformylation catalyst waste liquid containing a phosphine rhodium complex as an initial raw material. The preparation method comprises the following steps of: taking the hydroformylation catalyst waste liquid containing the phosphine rhodium complex as the initial raw material, when the concentration of rhodium in the waste liquid is 1000-2,0000ppm, firstly, carrying out oxidation treatment on the catalyst waste liquid under the acid condition to break through a rhodium cluster; secondly, synthesizing the hydridocarbonyl tri(triphenylphosphine) rhodium in the atmosphere of synthetic gas; and thirdly, filtering an ethanol solution as a precipitation prepared in the second step when the precipitation is hot and washing and drying the obtained precipitation to obtain a product of the hydridocarbonyl tri(triphenylphosphine) rhodium. The preparation method has the advantages of high yield, simple process flow and mild conditions.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of a homogeneous complex catalyst for olefin hydroformylation. The catalyst waste liquid containing deactivated rhodium phosphine complex is used as a raw material to directly prepare a homogeneous complex catalyst for olefin hydroformylation. A method for phase complexing catalyst tris(triphenylphosphine)carbonyl hydrogen rhodium. Background technique [0002] Tris(triphenylphosphine)hydrogen rhodium carbonyl RhH(CO)(TPP) 3 are α-olefins and syngas (CO and H 2 A good catalyst for the hydroformylation reaction to generate normal and isomeric aldehydes. For example, propylene and syngas in RhH(CO)(TPP) 3 In the presence of a homogeneous catalyst, n-butyraldehyde and isobutyraldehyde are produced. [0003] The document J.Amer.Chem.Soc.V85, p3500, 1963, reported for the first time that trans-RhCl(CO)(TPP) 2 As the starting material, RhH(CO)(TPP) was syn...

Claims

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Application Information

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IPC IPC(8): C07F15/00B01J31/24C07C45/50C07C47/02
Inventor 李彤王世亮吕顺丰刘博秦燕璜
Owner CHINA PETROLEUM & CHEM CORP
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