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Resin-based immobilized rhodium-phosphine complex catalyst as well as preparation method and application of catalyst

A technology of rhodium complexes and catalysts, which is applied in the field of resin-based immobilized rhodium-phosphine complex catalysts and their preparation, can solve the problems of poor catalytic effect, low activity, gaps, etc., achieve high selectivity, improve catalytic activity, reduce Effects of rhodium loss

Inactive Publication Date: 2017-05-10
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Yasan He et al. (Journal of Porous Mater, 2009, 16: 721-729) used MCM-41 as the carrier, modified the surface of the carrier with phosphine-containing and nitrogen-containing silicone coupling reagents, and impregnated RhCl 3 , with styrene as the substrate, in order to achieve higher reactivity and selectivity of branched-chain aldehydes, additional triphenylphosphine needs to be added, but due to the reducibility of the ligand, Rh(III) is partially reduced to a lower activity oxidation state, so the catalytic effect is poor
[0007] Ki-Chang Song et al. (Catalysis Today, 2011, 164:561-565) modified the surface of the carrier with a phosphine ligand after amination of SBA-15, and encapsulated the rhodium complex in SBA-15. Due to the phosphine ligand The coordination effect of rhodium can be specifically fixed inside and on the surface of the mesopore, so it has high selectivity and no loss of rhodium, but compared with the homogeneous catalytic effect, there is still a big gap

Method used

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  • Resin-based immobilized rhodium-phosphine complex catalyst as well as preparation method and application of catalyst
  • Resin-based immobilized rhodium-phosphine complex catalyst as well as preparation method and application of catalyst
  • Resin-based immobilized rhodium-phosphine complex catalyst as well as preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Synthesis of phenolic resin

[0030] 1) Weigh 2.44g of phenol, melt it at 40-42°C, add 0.52g of 20wt% NaOH solution under stirring conditions, then add 4.2g of formaldehyde (37wt% formaldehyde solution) dropwise at 50°C, and then React at ℃ for 1 hour, adjust the pH to 7.0 with 0.6M HCl solution, and remove water by evaporation at 50℃;

[0031] 2) Weigh 3.2g of F127 and dissolve it in 20mL of ethanol, stir at 40°C for 1 hour to obtain a clear solution, add the phenolic oligomer obtained in step 1), stir at 40°C for 1 hour, and filter to remove the precipitated salt in the solution;

[0032] 3) Pour the solution obtained in step 2) into a flat plate, place it in an oven at 40°C overnight to remove ethanol by evaporation, then solidify it at 100°C for 24 hours, take it out and grind it into powder;

[0033] 4) Put the obtained powder into a tube furnace, pass N 2 , and raised the temperature to 350°C at a rate of 1°C / min, and roasted at a constant temperature for 3 h...

Embodiment 2

[0043] Synthesis of Phosphorus-Containing Phenolic Resin

[0044] 1) Weigh 2.44g of phenol, melt it at 40-42°C, add 0.52g of 20wt% NaOH solution under stirring conditions, then add 4.2g of formaldehyde (37wt% formaldehyde solution) dropwise at 50°C, and then React at ℃ for 1h, adjust the pH to ~7.0 with 0.6M HCl solution, and evaporate the water at 50℃;

[0045] 2) Dissolve 3.2g of F127 in 20.0mL of ethanol, stir at 40°C for 1 hour to obtain a clear solution, then add 4mL of distilled water and 4mL of 0.6mol / L HCl, then add 0.72g of phosphoric acid and the phenolic formaldehyde obtained in step 1) For the oligomer, after stirring for 1 hour, pour it into a flat plate, evaporate the moisture at room temperature, and then cure it in an oven at 100°C for 24 hours;

[0046] 3) Put the obtained solid into a tube furnace, pass N 2 , and raised the temperature to 350°C at a rate of 1°C / min, and roasted at a constant temperature for 3 hours. The obtained solid was taken out after na...

Embodiment 3

[0049] Synthesis of Resorcinol Resin

[0050] 1) Weigh 0.55g resorcinol, 0.35g HMTA, 1.00g F127 and 0.20g 1,3,5-trimethylbenzene, dissolve them in 18g water, stir vigorously at room temperature for 2h, and dissolve the obtained homogeneous Pour the solution into a 100mL autoclave, react at 100°C for 12h, filter to obtain orange-red polymer particles, wash and dry in the air;

[0051] 2) Put the obtained polymer pellets into a tube furnace and pass N 2 , and the temperature was raised to 350°C at a rate of 1°C per minute, and after constant temperature roasting for 3 hours, the obtained solid was naturally cooled and taken out, stored in a desiccator, and recorded as RS.

[0052] The preparation operation of the catalyst is the same as in Example 1 except that the carrier is resorcinol resin (RS).

[0053] Measure respectively the catalytic effect of the rhodium-phosphine complex catalyst obtained in Examples 1-3 to the hydroformylation of 1-octene, and its measurement operat...

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Abstract

The invention discloses a resin-based immobilized rhodium-phosphine complex catalyst as well as a preparation method and an application of the catalyst. A resin polymer is taken as a carrier and modified with a phosphine ligand and bonded with a rhodium complex, and the immobilized rhodium-phosphine complex catalyst is synthesized. According to the catalyst, the rhodium-phosphine complex is immobilized on the surface of carrier resin through oxygen bridged bonds, accordingly, a rhodium-phosphine coordination catalytic active center with higher catalytic activity and selectivity is formed on the surface of the carrier, so that the catalyst has the characteristics of mild reaction condition, good selectivity, stable catalytic performance, easiness in separation, recyclability and the like and can be used for catalysis of a 1-octene hydroformylation reaction.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a resin-based immobilized rhodium-phosphine complex catalyst and a preparation method and application thereof. Background technique [0002] The hydroformylation reaction was discovered by Otto Roelen (1897-1993) in 1938, and it is the homogeneous catalytic process with the largest production capacity today. Intermediates, with an annual output of nearly 100 million tons. So far, homogeneous Rh and Co are mostly used as catalysts in the industry. The reaction conditions are relatively harsh and are only suitable for low-carbon chain olefins. After the reaction, the catalyst is difficult to separate from the product. Therefore, heterogeneous rhodium is synthesized. Phosphine complex catalysts have become a hot research topic nowadays. [0003] At present, the heterogeneous methods of homogeneous metal complex catalysts mainly include the following two categories: ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/10C07C45/50C07C47/02
CPCC07C45/505B01J31/1845B01J2231/321B01J2531/822B01J35/633B01J35/615C07C47/02
Inventor 吴丹陈静钱子隆李凯丽郑辉东
Owner FUZHOU UNIV
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