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Organic phosphine-containing polymer carrier loaded Rh-based catalyst, preparation and applications thereof

A carrier-supported, catalyst technology, applied in the direction of organic compound/hydride/coordination complex catalyst, catalyst activation/preparation, physical/chemical process catalyst, etc., can solve the problems of cumbersome synthesis steps and low specific surface area of ​​forming materials

Inactive Publication Date: 2020-05-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, porous polymers formed by chiral monomers are very rare, and their development is mainly limited by the low specific surface area of ​​the formed materials and the cumbersome synthesis steps, which are difficult for practical application. Professor Copper uses the method of external crosslinking, one-step F-C alkane A super-crosslinked polymer with chiral binaphthol monomers was directly formed. Experiments show that chiral binaphthol monomers have a higher specific surface area than naphthol-based monomers. At the same time, it can absorb carbon dioxide also show great potential for development

Method used

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  • Organic phosphine-containing polymer carrier loaded Rh-based catalyst, preparation and applications thereof
  • Organic phosphine-containing polymer carrier loaded Rh-based catalyst, preparation and applications thereof
  • Organic phosphine-containing polymer carrier loaded Rh-based catalyst, preparation and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] at 298K and N 2 Under a protective atmosphere, dissolve 5g of tris(4-vinylphenyl)phosphine ethyl iodide and 5g of tris(4-vinylphenyl)phosphine methyl iodide as monomers in 100.0ml of tetrahydrofuran solvent, and add 0.25 g of azobisisobutyronitrile free radical initiator, stirred for 2 hours. The stirred solution was transferred to a hydrothermal kettle, and solvothermally polymerized for 24 hours at 373K and nitrogen gas protection atmosphere. After the above polymerized solution is cooled to room temperature, the solvent is vacuumed out at room temperature to obtain an organic polymer carrier with a large surface area and a hierarchical porous structure. Then, at 298K and N 2 Under protective atmosphere, 0.0285g Rh 2 (CO) 4 Cl 2 Dissolve in 50ml of dichloromethane, then add 5g of the above polymer into it, stir at room temperature for 24h, wash with dichloromethane and suction filter, then vacuum the solvent to obtain a Rh-based catalyst supported by an organic p...

Embodiment 2

[0040] at 298K and N 2 Under a protective atmosphere, 5 g of tris (4-vinylphenyl) phosphine ethyl iodide and 5 g of tris (4-vinyl phenyl) phosphine methyl iodide as monomers were dissolved in 100.0 ml of CH 2 Cl 2 In the solvent, 0.25 g of azobisisobutyronitrile radical initiator was added to the above solution, and stirred for 2 hours. The stirred solution was transferred to a hydrothermal kettle, and solvothermally polymerized for 24 hours at 373K and nitrogen gas protection atmosphere. After the above polymerized solution is cooled to room temperature, the solvent is vacuumed out at room temperature to obtain an organic polymer carrier with a large surface area and a hierarchical porous structure. Then, at 298K and N 2 Under protective atmosphere, 0.050g RhCl 3 Dissolve in 50ml of tetrahydrofuran, then add 5g of the above polymer into it, stir at room temperature for 24h, wash with tetrahydrofuran and suction filter, and vacuum the solvent to obtain a Rh-based catalyst ...

Embodiment 3

[0043] at 298K and N 2 Under a protective atmosphere, 10.0 g of tris(4-vinylphenyl)phosphine methyl iodide was dissolved in 100.0 ml of dimethylformamide solvent as a monomer, and 0.25 g of azobisisoheptanonitrile radical was added to the above solution Initiator, stirred for 2 hours. The stirred solution was transferred to a hydrothermal kettle, and solvothermally polymerized for 24 hours at 373K and nitrogen gas protection atmosphere. After the above polymerized solution is cooled to room temperature, the solvent is vacuumed out at room temperature to obtain an organic polymer carrier with a large surface area and a hierarchical porous structure. Then, at 298K and N 2 Under protective atmosphere, 0.0285g Rh 2 (CO) 4 Cl 2 Dissolve in 50ml CH 2 Cl 2 , and then 5 g of the above polymer was added therein, stirred at room temperature for 24 h, washed with dichloromethane and suction filtered, and vacuumed to remove the solvent to obtain a Rh-based catalyst supported by an ...

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Abstract

The invention provides a large-surface-area hierarchical-pore-structure organic phosphine-containing polymer loaded Rh-based catalyst for preparing ethyl propionate and propionic acid through ethanolheterogeneous carbonylation, and a preparation method thereof. The catalyst is mainly composed of a main active component and a carrier, wherein the main active component is an Rh metal complex, the content of the Rh metal complex is 0.01-5.0% of the weight of the catalyst, the organic phosphine-containing polymer carrier is generated by selecting an organic salt monomer containing vinyl phosphineand adopting a solvothermal method through self-polymerization or mixed polymerization. Through strong ionic bond action between a metal complex and the quaternary phosphonium salt in a polymer carrier skeleton, an Rh metal component is highly dispersed in the polymer carrier in a monatomic form, and in a fixed bed reactor, CH3CH2OH / CO can be converted into ethyl propionate with high activity andhigh selectivity at a certain temperature and pressure under the action of the catalyst and an iodoethane cocatalyst.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalytic carbonylation, and in particular relates to a Rh-based catalyst supported by an organic phosphine-containing polymer carrier and its application in the reaction of producing ethyl propionate and propionic acid through heterogeneous carbonylation of ethanol. Background technique [0002] Propionic acid is one of the three widely used edible preservatives, and is recognized as the most economical, safe and effective edible preservative in the world; propionic acid is also an important fine chemical raw material, widely used in rubber, plastic, paint , spices, medicine, pesticides, printing and other fields. The development of my country's propionic acid industry is relatively late compared to other countries, and the consumption of propionic acid is far behind that of the United States and Europe. With the development of propionic acid industry, the demand for propionic acid in my c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J35/10B01J37/10C07C67/36C07C69/24
CPCB01J31/069B01J37/10C07C67/36B01J35/638B01J35/643B01J35/651B01J35/695B01J35/635B01J35/633B01J35/647C07C69/24
Inventor 丁云杰任周吕元
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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