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Preparation method of Cu nanoparticles-embedded ordered mesoporous carbon catalyst

A technology of catalyst and mesoporous carbon, which is applied in the field of ordered mesoporous carbon catalyst and its preparation, can solve the problems of reduced catalytic activity, high reactivity, and good dispersion of the catalyst, and achieve uniform and orderly pores, high reactivity, Good dispersion effect

Inactive Publication Date: 2016-04-27
CHINA UNIV OF MINING & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the above-mentioned problems in the prior art, the present invention provides an ordered mesoporous carbon catalyst embedded with nano-Cu particles and its preparation method and application, which effectively solves the problem that the catalytic activity of the catalyst decreases with the progress of the reaction , the chlorine-free copper-based catalyst prepared by the present invention is nano-scale, and copper particles of 5-25 nm are inlaid in the pores and surfaces of ordered mesoporous carbon, and have good dispersion, and are not easy to migrate and agglomerate during the reaction process. Continuous Fixed-bed Gas-Phase Oxidative Carbonylation of Methanol to Synthesis of Dimethyl Carbonate with High Reactivity and Good Stability at Atmospheric Pressure

Method used

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  • Preparation method of Cu nanoparticles-embedded ordered mesoporous carbon catalyst
  • Preparation method of Cu nanoparticles-embedded ordered mesoporous carbon catalyst
  • Preparation method of Cu nanoparticles-embedded ordered mesoporous carbon catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Add 1g of mesoporous silicon material SBA-15 to a mixed solution containing 1.25g of sucrose, 0.14g of concentrated sulfuric acid and 5ml of deionized water, and ultrasonically disperse the mixture in an ultrasonic oscillator for 20min; then place it in an electric blast drying oven Dry at 80°C for 6 hours. After drying, adjust the temperature to 160°C to pre-carbonize sucrose in the pores of SBA-15 for 6 hours. Weigh 0.8g sucrose, 0.09g sulfuric acid, 0.1g copper nitrate trihydrate and 5ml deionized water to make a solution, add this solution to the composite sample of SBA-15 and sucrose semipolymer prepared in the previous step, and ultrasonically disperse for 20min , followed by drying at 80°C for 6h and pre-carbonization at 160°C for 6h. The obtained sample was placed in a nitrogen-protected tube furnace, and the temperature was raised to 400°C at a rate of 2°C / min, then to 900°C at a rate of 1°C / min, and kept at a constant temperature for 4h. Finally, the complex ...

Embodiment 2

[0035] Add 1 g of mesoporous silicon material SBA-15 to a mixed solution containing 1.25 g of sucrose, 0.14 g of concentrated sulfuric acid, 0.1 g of copper nitrate trihydrate and 5 ml of deionized water, and ultrasonically disperse the mixture in an ultrasonic oscillator for 20 min; The sample was dried in an electric blast drying oven at 100°C for 6 hours. After drying, the temperature was adjusted to 160°C to prepolymerize sucrose in the pores of SBA-15 for 6 hours. Weigh 0.8g sucrose, 0.09g sulfuric acid and 5ml deionized water to make a solution, add this solution to the composite sample of SBA-15 and sucrose semipolymer prepared in the previous step, ultrasonically disperse for 20min, and then dry at 100°C 6h, pre-carbonization at 160°C for 6h. The obtained sample was placed in a nitrogen-protected tube furnace, and the temperature was raised to 400°C at a rate of 2°C / min, then to 900°C at a rate of 1°C / min, and kept at a constant temperature for 4h. Finally, the composi...

Embodiment 3

[0038] Add 1g of mesoporous silicon material SBA-15 to a mixed solution containing 1.25g of sucrose, 0.14g of concentrated sulfuric acid, 0.05g of copper acetate monohydrate and 5ml of deionized water, and ultrasonically disperse the mixture in an ultrasonic oscillator for 20min; The samples were dried in an electric blast drying oven at 100°C for 6 hours. After drying, the temperature was adjusted to 160°C to pre-carbonize the sucrose in the pores of SBA-15 for 6 hours. Weigh 0.8g sucrose, 0.09g sulfuric acid, 0.03g copper acetate monohydrate and 5ml deionized water to make a solution, add this solution to the composite sample of SBA-15 and sucrose semipolymer prepared in the previous step, and ultrasonically disperse for 20min , followed by drying at 100°C for 6h and pre-carbonization at 160°C for 6h. The obtained sample was placed in a nitrogen-protected tube furnace, and the temperature was raised to 400°C at a rate of 2°C / min, then to 850°C at a rate of 1°C / min, and kept ...

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Abstract

The invention discloses a preparation method of a Cu nanoparticles-embedded ordered mesoporous carbon catalyst and belongs to the field of chemical heterogeneous catalysis. The preparation method comprises the following steps: Step 1, template mesoporous silica material SBA-15 filling-rolling over; Step 2, carbonization; and Step 3, silica removal. The process of template mesoporous silica material SBA-15 filling-rolling over comprises impregnation, dispersion, drying, pre-carbonization and single repetitive operation. The problem that catalytic activity of a catalyst will decrease with the reaction process is solved. The prepared chloride-free copper-based catalyst of the invention is a nanoscale catalyst with 5-25nm copper particles embedded in pores of and on the surface of the ordered mesoporous carbon. Dispersity is good, and migration and agglomeration are not easy to occur in the reaction process. The catalyst has high reaction activity and good stability when used in an atmospheric continuous fixed bed for methanol gaseous oxidative carbonylation for synthesis of dimethyl carbonate.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalysis in chemistry and chemical engineering, and more specifically relates to an ordered mesoporous carbon catalyst embedded with nano-Cu particles and its preparation method and application. Background technique [0002] Dimethyl carbonate (DMC) is a widely used green chemical, known as the "new cornerstone" of organic synthesis. Among the many methods of synthesizing DMC, CO, O 2 The oxidative carbonylation route with methanol as a raw material is thermodynamically very favorable, and the atomic utilization rate is as high as 80%, which is one of the most promising synthetic routes for industrial application. Activated carbon supported copper chloride catalyst (CuCl 2 / AC) and Wacker-type catalysts (CuCl 2 -PdCl 2 / AC) There are catalyst deactivation and equipment corrosion problems caused by the loss of chloride ions during the reaction process. Although adding additives or improving the pr...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07C68/00C07C69/96
CPCB01J21/18B01J23/72C07C68/01C07C69/96
Inventor 王瑞玉梁华根刘玲曹红霞
Owner CHINA UNIV OF MINING & TECH
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