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Supported MCM-41 catalyst as well as preparation method and application thereof

A technology of MCM-41 and catalyst, applied in the field of catalysis, can solve the problems of difficult reaction, high reaction temperature, poor activity, etc., and achieve the effects of low cost, simple preparation method and prevention of agglomeration

Active Publication Date: 2022-07-29
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But both are very stable substances, and it is difficult to react thermodynamically.
It was found that ZrO 2 / SO 4 2- It can activate methane and promote C-C coupling. The greater the acid strength, the easier it is to activate methane, but the specific surface area is lower and the activity is poor [New Journal of Chemistry, 2021,45(20):8978-8985]
Cu-based catalysts can effectively activate methane, but they tend to agglomerate under high temperature conditions, leading to catalyst deactivation [Applied Catalysis B: Environmental, 2017, 215:50–59]
Emad N.Al-Shafei with ZrO 2 / TiO 2 The catalyst successfully synthesized acetic acid, but the reaction temperature was too high and the yield of acetic acid was low [Chemical Engineering Journal,2021,419:129416]

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1: Preparation of modified MCM-41 molecular sieve:

[0023] Pour 5g of MCM-41 molecular sieve into 150g of 0.5mol / L gluconic acid solution, stir at 50°C for 5h, then centrifuge and dry at 80°C for 8h to obtain gluconic acid-modified MCM-41 molecular sieve.

[0024] Step 2: Preparation of modified MCM-41 molecular sieve loaded active components:

[0025] First put 1g of modified MCM-41 molecular sieve in the container, then weigh 0.1136g of FeCl 3 and 0.0227g of KCl were dissolved in ethanol, stirred until dissolved to form an ethanol solution, and then the ethanol solution was added to the gluconic acid-modified MCM-41 molecular sieve, stirred and sonicated until the mixture was uniform, allowed to stand for 5 hours, and then dried at 80 °C for 8 hours , placed it in a tube furnace to 450°C at a heating rate of 2°C / min, and calcined in an argon atmosphere for 1 h to obtain 10% FeCl 3 -2% KCl / MCM-41 catalyst.

Embodiment 2

[0027] Step 1: Preparation of modified MCM-41 molecular sieve:

[0028] Pour 5g of MCM-41 molecular sieve into 150g of 0.5mol / L gluconic acid solution, stir at 60°C for 8h, then centrifuge and dry at 100°C for 9h to obtain gluconic acid-modified MCM-41 molecular sieve.

[0029] Step 2: Preparation of modified MCM-41 molecular sieve loaded active components:

[0030] First put 1g of modified MCM-41 molecular sieve in the container, then weigh 0.1136g of CoCl 2 and 0.0227g of KCl were dissolved in ethanol, stirred until dissolved to form an ethanol solution, and then the ethanol solution was added to the gluconic acid-modified MCM-41 molecular sieve, stirred and sonicated until the mixture was uniform, left standing for 8 hours, and then dried at 90 °C for 8 hours , place it in a tube furnace and raise it to 460°C at a heating rate of 3°C / min, and bake it in a nitrogen atmosphere for 1 h to obtain 10% CoCl 2 -2% KCl / MCM-41 catalyst.

Embodiment 3

[0032] Step 1: Preparation of modified MCM-41 molecular sieve:

[0033] Pour 5g of MCM-41 molecular sieve into 150g of 0.5mol / L gluconic acid solution, stir at 70°C for 10h, then centrifuge and dry at 120°C for 10h to obtain gluconic acid-modified MCM-41 molecular sieve.

[0034] Step 2: Preparation of modified MCM-41 molecular sieve loaded active components:

[0035] First put 1g of modified MCM-41 molecular sieve in the container, then weigh 0.1136g of NiCl 2 and 0.0227g of KCl were dissolved in ethanol, stirred until dissolved to form an ethanol solution, and then the ethanol solution was added to the gluconic acid-modified MCM-41 molecular sieve, stirred and sonicated until the mixture was uniform, left standing for 10 hours, and then dried at 90 °C for 10 hours , placed it in a tube furnace to 470°C at a heating rate of 4°C / min, and calcined in a nitrogen atmosphere for 1 h to obtain 10% NiCl 2 -2% KCl / MCM-41 catalyst.

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Abstract

The invention relates to a supported MCM-41 catalyst as well as a preparation method and application thereof. The supported MCM-41 catalyst is characterized in that a gluconic acid modified MCM-41 molecular sieve is taken as a carrier, transition metal chloride is taken as a main active component, and alkali metal chloride is taken as an auxiliary active component. Wherein the transition metal chloride is one of FeCl3, CoCl2, NiCl2, CuCl2 or ZnCl2, and the alkali metal chloride is one of KCl, LiCl or NaCl; the loading mass of the transition metal chloride accounts for 10-25% of the total mass of the catalyst, and the loading mass of the alkali metal chloride accounts for 2-5% of the total mass of the catalyst. The supported MCM-41 catalyst provided by the invention has high dispersity and high activity, and can activate methane and carbon dioxide to be co-converted into acetic acid at the same time. The catalyst has the characteristics of simple preparation process, low cost, high catalytic activity and the like, and has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the field of catalysis, and relates to a supported MCM-41 catalyst and a preparation method and application thereof. The method includes the modification of the carrier and the loading of active components, and can be used to catalyze the direct synthesis of acetic acid from methane and carbon dioxide. Background technique [0002] As a bulk chemical, acetic acid is one of the important organic acids and is widely used in food, medicine, pesticides and other industries. The production of acetic acid can adopt artificial synthesis method and bacterial fermentation method, artificial synthesis method includes methanol carbonylation method, acetaldehyde oxidation method, ethylene oxidation method, etc., bacterial fermentation method includes aerobic fermentation method and anaerobic fermentation method. Among them, the production of acetic acid is mainly through the methanol carbonylation method. This method uses methanol as a ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03B01J29/04C07C51/15C07C53/08
CPCB01J29/0333B01J29/0308B01J29/044B01J29/041C07C51/15B01J2229/18C07C53/08Y02P20/52
Inventor 万辉邹鹏程王磊管国锋
Owner NANJING UNIV OF TECH
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