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Iridium-based catalyst supported by acid-treated carbon carrier, and preparation method and application thereof

A catalyst and acid treatment technology, applied in physical/chemical process catalysts, carbon monoxide or formate reaction preparation, chemical instruments and methods, etc., can solve the problems of low selectivity, low space-time yield, and deactivation of molecular sieve carbon deposits. , to achieve the effect of high selectivity, low methane content and reduced selectivity

Active Publication Date: 2017-12-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
First of all, although the system has a high methyl acetate selectivity at a lower conversion rate, its selectivity still needs to be improved when the conversion rate reaches more than 90%; unfavorable for industrialization

Method used

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  • Iridium-based catalyst supported by acid-treated carbon carrier, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Weigh 8g of activated carbon, add 50ml of 1mol / L dilute nitric acid, cook at 60°C for 3 hours, wash with deionized water until neutral, and dry in an oven at 120°C to obtain acid-treated activated carbon. Weigh 3mL concentrated HCl and add 0.0128gLa 2 o 3 Stir until dissolved, then add 2.1ml of HCl with a concentration of 0.019g / mL to 3mL of hydrochloric acid solution 2 IrCl 6 ·6H 2 O aqueous solution, and then impregnated 1.5 g of the above-mentioned acid-treated coconut shell charcoal. Evaporate the solvent in a water bath at 80°C, dry in an oven at 120°C for 10 hours, and roast at 350°C under nitrogen protection for 4 hours to obtain an acid-treated iridium-based catalyst supported on a carbon carrier.

Embodiment 2

[0029] Weigh 8g of activated carbon, add 50ml of 1mol / L dilute nitric acid, cook at 60°C for 3 hours, wash with deionized water until neutral, and dry in an oven at 120°C to obtain acid-treated activated carbon. Then take 4.5g of the activated carbon from the previous step and react with 50ml of concentrated sulfuric acid at 180°C for 10h, wash with hot deionized water until neutral and free of sulfate ions, and oven-dry at 120°C to obtain sulfonic acid-treated activated carbon. Weigh 4mL concentrated HCl and add 0.0298gLa 2 o 3 Stir until dissolved, then add 4.943ml of HCl with a concentration of 0.019g / mL to 4mL of hydrochloric acid solution 2 IrCl 6 ·6H 2 O aqueous solution, and then impregnated 4 g of the above acid-treated activated carbon. Evaporate the solvent in a water bath at 80°C, dry in an oven at 120°C for 10 hours, and roast at 350°C under nitrogen protection for 4 hours to obtain an acid-treated activated carbon-supported iridium-based catalyst.

Embodiment 3

[0031] Weigh 4g of activated carbon and 50ml of concentrated sulfuric acid to react at 180°C for 10h, wash with deheated deionized water until neutral and free of sulfate ions, and dry in an oven at 120°C to obtain sulfonic acid-treated activated carbon. Weigh 3mL concentrated HCl and add 0.0213gLa 2 o 3 Stir until dissolved, then add 3.467ml of HCl with a concentration of 0.019g / mL to 3mL of hydrochloric acid solution 2 IrCl 6 ·6H 2O aqueous solution, then impregnated 2.5 g of the above acid-treated coconut shell charcoal. Evaporate the solvent in a water bath at 80°C, dry in an oven at 120°C for 10 hours, and roast at 350°C under nitrogen protection for 4 hours to obtain an acid-treated activated carbon-supported iridium-based catalyst

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Abstract

The invention a catalyst supported by an acid-treated carbon carrier and used for preparation of methyl acetate from methanol through carbonylation, and a preparation method thereof. The catalyst is composed of main active components and a carrier, wherein the main active components are iridium and transition metal or an oxide aid thereof, and the contents of iridium and transition metal or the oxide aid thereof account for 0.01-5.0% and 0.1-30% of the weight of the catalyst, respectively; and the carrier is the acid-treated carbon carrier including acid-treated coconut shell carbon or apricot shell carbon and other acid-treated carbonized carriers. The purpose of acid treatment is to increase methyl acetate selectivity and reduce methane. According to the invention, the Ir-based catalyst is formed by loading metal on the acid-treated carrier through an impregnation method. In a fixed-bed reactor, high-activity high-selectivity conversion of CH3OH / CO into methyl acetate and reduction in methane selectivity can be realized at a certain temperature and pressure and under the action of the catalyst.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalytic carbonylation, and specifically relates to an iridium-based catalyst supported by an acid-treated carbon carrier, a preparation method thereof, and an application thereof in the reaction of producing methyl acetate through heterogeneous carbonylation of methanol. 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 dehyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18B01J35/10B01J23/46B01J23/63B01J27/02B01J27/10B01J27/18B01J27/24C07C67/36C07C69/14
CPCC07C67/36B01J21/18B01J23/468B01J23/63B01J27/02B01J27/10B01J27/18B01J27/24B01J35/617B01J35/618B01J35/647B01J35/651C07C69/14
Inventor 丁云杰任周宋宪根吕元陈维苗
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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