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A kind of supported imidazolium ionic liquid catalyst and its application in catalytic oxidation of cyclohexane to prepare cyclohexanone and cyclohexanol

An imidazole ionic liquid and technology of ionic liquid, which are applied to the supported imidazole ionic liquid catalyst and the application field in the catalytic oxidation of cyclohexane to prepare cyclohexanone and cyclohexanol, can solve the problem of low catalyst activity, harsh operating conditions, etc. Problems such as low reaction selectivity, to achieve the effect of good stability, simple reaction system and good reaction selectivity

Active Publication Date: 2020-08-04
重庆市化工研究院有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have more or less problems such as low catalyst activity, low reaction selectivity, harsh operating conditions, and complicated processes.

Method used

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  • A kind of supported imidazolium ionic liquid catalyst and its application in catalytic oxidation of cyclohexane to prepare cyclohexanone and cyclohexanol
  • A kind of supported imidazolium ionic liquid catalyst and its application in catalytic oxidation of cyclohexane to prepare cyclohexanone and cyclohexanol
  • A kind of supported imidazolium ionic liquid catalyst and its application in catalytic oxidation of cyclohexane to prepare cyclohexanone and cyclohexanol

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preparation example Construction

[0030] The preparation method of the transition metal doped SBA-16 mesoporous molecular sieve supported type imidazolium ionic liquid catalyst of one embodiment, comprises the following steps:

[0031] (1) N-methylimidazole (0.5mol), 3-chloropropyltriethoxysilane (0.5mol) and toluene (800mL) were reacted at 110°C for 24 hours, the solvent was recovered, and vacuum-dried at 70°C for 6 hours to obtain intermediate Body 1;

[0032] (2) Intermediate 1 (8g), metal-doped mesoporous molecular sieve M-SBA-16 (10g) and toluene (200mL) were reacted at 100°C for 24 hours, filtered, and vacuum-dried at 70°C for 8 hours to obtain ionic liquid 2;

[0033] (3) Ionic liquid 2 (0.01mol) continued to react with ferric chloride (0.01mol), copper chloride (0.01mol), or chromium chloride (0.01mol) in acetonitrile (80mL) at 70°C for 24 hours and then filtered , acetonitrile, and dried to obtain M-SBA-16 mesoporous molecular sieve-loaded imidazolium ferric chloride salt ionic liquid, M-SBA-16 mesop...

Embodiment 1

[0037] In a stainless steel reaction kettle, add cyclohexane 10mL, 0.2g Mn-SBA-16@IL[FeCl 4 ], filled with 1.2MPa oxygen, stirred and reacted at 110°C for 4 hours. Cool to room temperature, filter and recover the catalyst. GC-MS analysis results showed that the conversion rate of cyclohexane was 10.7%, and the total selectivity of cyclohexanol and cyclohexanone was 89.2%, wherein the selectivity of cyclohexanol was 39.8%, and the selectivity of cyclohexanone was 49.4%. .

Embodiment 2

[0039] In a stainless steel reaction kettle, add cyclohexane 10mL, 0.2g Mn-SBA-16@IL[CuCl 3 ], filled with 1.2MPa oxygen, stirred and reacted at 110°C for 4 hours. Cool to room temperature, filter and recover the catalyst. GC-MS analysis results showed that the conversion rate of cyclohexane was 10.3%, the total selectivity of cyclohexanol and cyclohexanone was 90.3%, and the selectivity of cyclohexanol was 42.5%.

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Abstract

The invention discloses a loaded imidazole ionic liquid catalyst and application thereof in preparation of cyclohexanone and cyclohexanol by catalytic oxidation of cyclohexane. The method uses cyclohexane as the reactant, adopts oxygen as the oxidant, and employs a transition metal doped SBA-16 mesoporous molecular sieve loaded ionic liquid as the catalyst, no organic solvent or additive is neededin the reaction process, and high selective oxidation reaction is carried out to prepare cyclohexanol and cyclohexanone. At the end of the reaction, separation of the catalyst and the product can beachieved by simple filtration, and the catalyst can be recycled well. The catalyst provided by the invention is easy to prepare, and has the advantages of small dosage, high catalytic efficiency, highreaction selectivity and simple operation, and is an efficient and environment-friendly synthetic method.

Description

technical field [0001] The invention relates to a method for preparing cyclohexanol and cyclohexanone by using cyclohexane as a raw material to catalyze the selective oxidation of molecular oxygen, and a novel transition metal-doped mesoporous molecular sieve-supported ionic liquid catalyst and a preparation method for the catalyst. [0002] technical background [0003] Cyclohexanol and cyclohexanone are important chemical raw materials, widely used in the production of pharmaceutical and pesticide intermediates, polymer materials, industrial coatings and other compounds. At present, the main method of producing cyclohexanol and cyclohexanone at home and abroad is cyclohexane oxidation method, mainly including cyclohexane catalytic oxidation method and cyclohexane non-catalytic oxidation method, among which cyclohexane catalytic oxidation method is the industrial production of cyclohexane Hexanol and cyclohexanone are the most important methods. At present, cobalt salts or ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07F7/08C07C49/403C07C45/33C07C35/08C07C29/50
CPCB01J31/0295B01J2231/72C07C29/50C07C45/33C07F7/0836C07C49/403C07C35/08Y02P20/54Y02P20/584
Inventor 胡玉林陈刚高川巩珣
Owner 重庆市化工研究院有限公司