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Catalyst system used for synthesizing acetic acid and acetic anhydride and application thereof

A catalyst, acetic anhydride technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, preparation of carboxylic acid anhydride, etc., can solve the problem of catalytic activity, unsatisfactory stability, no catalytic activity, There are no problems such as catalytic activity, and the catalytic process is simple and easy, the formation is simple and rapid, and the preparation cost is reduced.

Inactive Publication Date: 2010-10-27
YANKUANG LUNAN CHEM FERTILIZER PLANT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But 2-aminobendazole mentioned in it, 2-amino-4-picoline etc., are easy to form chelated rhodium compound structure with transition metal rhodium compound, and this chelate has no catalytic activity, needs If you want to turn it into a catalyst with high activity, you must carry out a long and complex treatment of the ligand to be active. The unmodified ligand and rhodium compound complexes not only do not have catalytic activity, but actually make the The rhodium in the original active catalyst is poisoned and deactivated due to the re-formation of inactive chelates, and there are problems of unsatisfactory catalytic activity and stability

Method used

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  • Catalyst system used for synthesizing acetic acid and acetic anhydride and application thereof

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Embodiment 1

[0017] Embodiment 1: the preparation of bonding type rhodium ion complex: the steps are as follows:

[0018] (1) Quaternization of caffeine: Add caffeine to the quaternary methyl iodide reagent, the molar ratio of caffeine and methyl iodide is 1:0.5, then add benzene to dilute, leave to react for 12 hours, and obtain part of the quaternization Ligand caffeine.

[0019] (2) Synthesis of the caffeine-bonded rhodium ion complex: the caffeine ligand after the quaternization of the above gained and dicarbonyl diiodide dirhodium [Rh 2 (CO) 2 I 2 ] Proportioning according to the mass ratio of 10:1, adding to benzene, stirring and reacting for 4 hours at room temperature and under the protection of argon, naturally drying, and drying under reduced pressure to obtain the product, which is a brown-yellow crystalline powder.

Embodiment 2

[0020] Embodiment 2: the preparation of bonding type rhodium ion complex: the steps are as follows:

[0021] (1) Quaternization of caffeine: Add caffeine to the quaternary methyl iodide reagent, the molar ratio of caffeine and methyl iodide is 1:0.8, then add ethanol to dilute, leave to react for 14 hours, and obtain part of the quaternization Ligand caffeine.

[0022] (2) Synthesis of the caffeine-bonded rhodium ion complex: the caffeine ligand after the quaternization of the above gained and dicarbonyl dichlorodirhodium [Rh 2 (CO) 2 Cl 2 ] Proportioning according to the ratio of mass ratio 20:1, adding it to ethanol, stirring and reacting for 5 hours at room temperature and under the protection of argon, drying naturally, and drying under reduced pressure to obtain the product, which is a yellow crystalline powder.

Embodiment 3

[0023] Embodiment 3: in 250ml zirconium autoclave, add dicarbonyl dichlorodirhodium [Rh 2 (CO) 2 Cl 2 ] Catalyst 0.144g, caffeine 1.0g, methyl acetate 111g, methyl iodide 31.24g, acetic acid 12g, acetic anhydride 15.3g and lithium acetate 3.9g, fill CO to remove the air in the kettle, simultaneously feed into the system H 2 Heat up to 140°C, by volume H 2 :CO=1:30, keep the kettle pressure at 4.0Mpa, stir at 500 rpm, react for 20min, the increment of acetic anhydride is 114.8g, and the space-time yield of acetic anhydride is 13.5mol / L-h.

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Abstract

The present invention discloses a catalyst system used for acetic acid and acetic anhydride synthesis and the application. Halide of rhodium is used for active specie of a catalyst and alkyl halide, alkali metal iodine and organic solvent are used as the catalyst. Caffeine is used as a ligand. The mass proportion of the caffeine and the halide of the rhodium is one till thirty to one. The catalyst system provided by the present invention has the advantage of good compatibility. The hard removing problems of the wall attachment, the falling to the bottom and the coking of the catalyst are not easy to happen in carbonylation reaction equipment. And the present invention has the advantages of high catalytic activity, high selectivity, high thermal stability and strong anti-coking performance. Any complex pretreatment before the catalysis is not needed. The formation of the catalyst system is simple and rapid. The catalyst process is simple and easy to be implemented. And the present invention also has the advantages of high catalytic activity, high stability, good compatibility, low cost, etc.

Description

technical field [0001] The invention relates to a catalyst system for synthesizing acetic acid and acetic anhydride with caffeine as a ligand and its application in synthesizing acetic acid and acetic anhydride. Background technique [0002] Acetic anhydride, also known as acetic anhydride, referred to as acetic anhydride, is a colorless liquid that flows easily, is flammable, and decomposes into acetic acid when it meets water. Soluble in organic solvents such as ethanol, ether, benzene and chloroform. Acetic anhydride is an important organic chemical raw material. It is mainly used as an acetylating agent, and can also be used as a dehydrating agent and a material for making high-grade photosensitive films. Acetic anhydride is also widely used in medicine, dyestuff, pesticide, light industry, textile and other industries. It is the raw material for the production of dozens of commonly used medicines such as aspirin, vitamin E, cortisone acetate, and chloramphenicol. It is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/30C07C53/12C07C51/56
Inventor 吕运江吴永国李胜果陶美玲孙清涛张雷
Owner YANKUANG LUNAN CHEM FERTILIZER PLANT
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