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Organic nitrogen-containing polymer carrier Rh-loading catalyst as well as preparation and application thereof

A carrier loading and catalyst technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of low space-time yield, immaturity, and high separation cost

Active Publication Date: 2019-03-12
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

(2) Dimethyl ether is synthesized by carbonylation on the H-MOR molecular sieve catalyst, but the molecular sieve is seriously deactivated by carbon deposition, and the space-time yield is low
(3) When methanol carbonylation prepares acetic acid, methyl acetate exists as a by-product, but the selectivity is low and the separation cost is high
In fact, the Acetica process mentioned above is to immobilize Rh on the catalyst through the ionic bond of pyridine resin, and apply it to the heterogeneous carbonylation process, while the application of other polymers in methanol carbonylation is still relatively small. little, immature

Method used

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  • Organic nitrogen-containing polymer carrier Rh-loading catalyst as well as preparation and application thereof
  • Organic nitrogen-containing polymer carrier Rh-loading catalyst as well as preparation and application thereof
  • Organic nitrogen-containing polymer carrier Rh-loading catalyst as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] at 298K and N 2 Under a protective atmosphere, 10.0g of 3,3-divinyl-2,2-bipyridine was dissolved as a monomer in 100.0ml of dimethylformamide solvent, and 0.25g of a free radical initiator was added to the above solution. Azodiisobutyronitrile, stirred for 2 hours. The stirred solution was transferred to a hydrothermal kettle, and polymerized by solvothermal polymerization at 373K under a nitrogen atmosphere for 24 hours. After the above-mentioned polymerized solution is cooled to room temperature, the solvent is removed under vacuum at room temperature to obtain a large-surface-area hierarchically porous structure organic ligand polymer carrier formed by the polymerization of 3,3-divinyl-2,2-bipyridine. Then, at 298K and N 2 Under protective atmosphere, 0.0285g Rh 2 (CO) 4 Cl 2 Dissolved in 50ml of dichloromethane, then added 5g of 3,3-divinyl-2,2-bipyridine polymer into it, stirred at room temperature for 24h, washed with dichloromethane and suction filtered, vac...

Embodiment 2

[0031] at 298K and N 2 Under a protective atmosphere, 10.0g of 4,4-divinyl-2,2-bipyridine was dissolved as a monomer in 100.0ml of dimethylformamide solvent, and 0.25g of a free radical initiator was added to the above solution. Azodiisobutyronitrile, stirred for 2 hours. The stirred solution was transferred to a hydrothermal kettle, and polymerized by solvothermal polymerization at 373K under a nitrogen atmosphere for 24 hours. After the above-mentioned polymerized solution is cooled to room temperature, the solvent is removed under vacuum at room temperature to obtain a large-surface-area hierarchical porous structure organic ligand polymer carrier formed by the polymerization of 4,4-divinyl-2,2-bipyridine. 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 4,4-divinyl-2,2-bipyridine polymer into it, stir at room temperature for 24h, wash and filter with tetrahydrofuran, vacuum the solvent to o...

Embodiment 3

[0034] at 298K and N 2 Under a protective atmosphere, dissolve 10.0g of 5,5-divinyl-2,2-bipyridine as a monomer in 100.0ml of tetrahydrofuran solvent, and add 0.25g of azobisisoheptyl as a free radical initiator to the above solution Nitrile, stirred for 2 hours. The stirred solution was transferred to a hydrothermal kettle, and polymerized by solvothermal polymerization at 373K under a nitrogen atmosphere for 24 hours. After the above-mentioned polymerized solution is cooled to room temperature, the solvent is vacuumed out at room temperature to obtain a large-surface-area hierarchical porous structure organic ligand polymer carrier formed by self-polymerization. Then, at 298K and N 2 Under protective atmosphere, the 0.0285gRh (PPh 3 ) 3 Cl was dissolved in 50 ml of tetrahydrofuran, and 5 g of the above polymer was added thereto, stirred at room temperature for 24 hours, washed with tetrahydrofuran and filtered, and vacuumed to remove the solvent to obtain a rhodium-based...

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Abstract

The invention provides an organic nitrogen-containing polymer carrier Rh-loading catalyst as well as a preparation method and application thereof. The catalyst mainly consists of two parts, i.e. a main active component and a carrier. The main active component is rhodium metal, and the content of the main active component is 0.01 to 5.0 percent of the weight of the catalyst; and the organic nitrogen-containing polymer carrier is generated by selecting N vinyl-based organic ligands or salts, performing self-polymerization or co-polymerization by adopting a solvent thermal polymerization method and initiating the polymeric reaction by adopting an initiator. The large-surface-area multilevel porous structure organic ligand polymer can be used as the carrier for loading the metal catalyst to load the active metal component; and the metal components have relatively high coordination bond effect or hyamine ion bond effect with ligands in a polymer carrier skeleton. In a fixed bed reactor, under certain temperature and pressure, and in the presence of the catalyst, CH3OH / CO can be high actively and high selectively converted into methyl acetate.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalytic carbonylation, and in particular relates to an Rh-based catalyst loaded on an organic nitrogen-containing polymer carrier and its preparation and application. Background technique [0002] Methyl acetate is gradually replacing acetone, methyl ethyl ketone, ethyl acetate, cyclopentane, etc. internationally. Because it does not belong to the emission of organic pollutants that are restricted in use, it can meet the new environmental protection standards for paint, ink, resin, and adhesive factories. The hydrogenation of methyl acetate to ethanol is also one of the main ways to produce ethanol from coal. Its preparation methods mainly include (1) acetic acid and methanol are directly esterified with sulfuric acid as a catalyst to form a crude methyl acetate product, and then dehydrated with calcium chloride, neutralized with sodium carbonate, and fractionated to obtain a finished pro...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/10C07C67/36C07C69/14
CPCC07C67/36B01J31/1616B01J31/1815B01J35/60C07C69/14
Inventor 丁云杰任周吕元宋宪根
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI