Iridium picolinate complex catalyst for synthesizing acetic acid by methanol carbonylation

An oxo synthesis, iridium complex technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, organic chemistry, etc., can solve the problems of separation of reaction products, inconvenient recycling, etc. , the effect of enhancing solubility

Inactive Publication Date: 2010-04-14
JIANGSU SOPO GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are a lot of reports about the rhodium catalyst supported by polymer resin used in methanol carbonylation to prepare acetic acid. Usually this type of heterogeneous catalytic system has a certain effect on the improvement of catalytic performance in some aspects, but due to gas, solid and liquid The limitation of the phase reaction system; it is inconvenient to the separation and circulation of the reaction product, especially for the direct application of the current industrial device

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 0.20mol of 2-vinylpyridine monomer and 0.1mol of methyl acrylate monomer and mix with 1.2g of azobisisobutyronitrile, add to 70ml of benzene solvent, react at 60°C for 10 hours under stirring, and cool to room temperature, and precipitated with petroleum ether to obtain the copolymer ligand.

[0023] Copolymer ligands with different proportions of 2-vinylpyridine and methyl acrylate were obtained by the above method.

Embodiment 2

[0025] Weigh 1 part by weight of the 2-vinylpyridine-methyl acrylate copolymer in Example 1 and dissolve it in 50 parts by weight of acetic acid. Stir and heat to reflux, add IrCl3 or IrI3 or Ir(OAc)3, the amount added is 3-10% of the copolymer in terms of iridium weight, after reacting for 30 minutes, cool to room temperature, precipitate with ether, and filter to obtain the copolymer iridium catalyst.

[0026]Obtain the copolymer of different 2-vinylpyridine-methyl acrylate proportioning with IrCl respectively with above-mentioned method 3 , IrI 3 , Ir(OAc) 3 copolymer iridium catalysts.

Embodiment 3

[0028] Take by weighing 1 part by weight of the copolymer in Example 1, and add it under stirring to contain [Ir(CO) 2 I] In the acetic acid solution, the addition is Ir: copolymer=0.03-0.1: 1, reacted for 20 minutes, and used Precipitate and filter ether to obtain a copolymer iridium catalyst.

[0029] Obtain the copolymers of different 2-vinylpyridine-methyl acrylate ratios with [Ir(CO) 2 I] 2 and [Ir(CO) 2 Cl] 2 catalyst.

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PUM

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Abstract

The invention discloses an iridium picolinate complex catalyst for synthesizing acetic acid by methanol carbonylation and a preparation method and an application thereof, a ligand of the catalyst is a copolymer of 2-vinyl pyridine and methyl acrylate, and a copolymer iridium complex catalyst is formed by the complexation reaction with an iridium compound. The preparation method comprises the steps of preparing the ligand of the catalyst, then dissolving 1 part by weight of the copolymer in 10-100 parts by weight of the acetic acid, stirring, heating under reflux, adding the iridium compound which accounts for 3-10% of the weight of the copolymer, carrying out reaction for 10-60min, cooling to the room temperature, using ether for precipitation, filtering and then obtaining a copolymer iridium catalyst. The 1 part by weight of the copolymer is added into the acetic acid solution containing (Ir(CO)2I)2 or (Ir(CO)2Cl)2 under stirring, the feeding is 3-10% of the weight of the copolymer calculated by the weight of iridium, the reaction is carried out for 10-30min under stirring, the ether is used for precipitation, and the copolymer iridium catalyst is obtained by filtering. The copolymer iridium catalyst is used for preparing the acetic acid by methanol carbonylation reaction and has good catalytic performance.

Description

technical field [0001] The invention belongs to the field of methanol carbonylation reaction to prepare acetic acid, and in particular relates to the catalyst and its preparation method. Background technique [0002] Methanol carbonylation reaction to prepare acetic acid is currently the most widely used and most advanced technical route in industry. From the invention of the original Monsanto Company (US3 769 329) to the high-iodine low-water reaction system (US5 001 259, EP055618) of Celanes Company, rhodium is used as the catalyst active component. Due to the high price of rhodium, the research on non-rhodium-based catalysts has always been a hot topic, the most successful of which is the application of iridium-based catalysts (EP0749948, EP0752406) in industrial production. This technology was developed by BP Chemical Company in 1996, called Catva process. Compared with rhodium-based catalysts, iridium-based catalysts have the advantages of low price and less reaction b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C53/08C07C51/12
Inventor 宋勤华袁国卿邵守言闫芳凌晨钱庆利曹宏兵郭存悦闫丰文
Owner JIANGSU SOPO GRP
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