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Preparation method and application of Cu-MOF catalyst in acetylene hydrochlorination reaction

A technology of acetylene hydrochlorination and catalyst, which is applied in the direction of catalyst activation/preparation, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc. It can solve the problem of poor conversion rate of acetylene and poor catalyst stability, etc. problems, to achieve huge energy and economic benefits, good stability, and mild conditions

Pending Publication Date: 2021-08-06
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The first object of the present invention is to solve the problem of poor acetylene conversion rate and poor catalyst stability of copper catalyst in acetylene hydrochlorination reaction, and to provide a preparation method of Cu / MOF catalyst

Method used

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  • Preparation method and application of Cu-MOF catalyst in acetylene hydrochlorination reaction

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Synthesis of UIO-67: 90mg 4,4'-biphenyl dicarboxylic acid, 67mg ZrCl 4 Add 50 mL of polytetrafluoroethylene (PPL) liner, then add 15 mL of N,N-dimethylformamide (DMF) and 3 mL of acetic acid. After ultrasonic dissolution, the PPL lining was placed in a stainless steel reaction vessel, sealed and heated to 120 °C, reacted for 24 h, and cooled naturally to room temperature. The resulting precipitate was separated by centrifugation, washed with DMF several times and solvent exchanged with acetone several times, and dried at 120 °C to obtain the UIO-67 material.

[0040] (2) Preparation of catalyst Cu-UIO-67: Take 20 g of UIO-67 purified in step (1) and put it into a container. Then add 1.53g of Cu(BF 4 ) 2 Impregnated with 10ml of acetonitrile, stirred for 2 hours, centrifuged, removed the supernatant, dried in vacuum at 120°C for 10 hours, and then carried out glow discharge treatment. Use a vacuum pump with a power of 500 W to keep the system in a vacuum state, an...

Embodiment 2

[0043] (1) Same as embodiment 1.

[0044] (2) Preparation of catalyst Cu-UIO-67: Take 20 g of UIO-67 in step (1) and put it into a container. Then add 4.76g of Cu(BF 4 ) 2 Impregnated with 15ml of acetonitrile, stirred for 2 hours, centrifuged, removed the supernatant, dried in vacuum at 140°C for 10 hours, and then carried out glow discharge treatment. Use a vacuum pump with a power of 500 W to keep the system in a vacuum state, and adjust the air flow to make the plasma The pressure of the body chamber was kept at 100 Pa, and the plasma treatment intensity was adjusted by adjusting the discharge voltage value, the applied voltage was 100V, and the treatment time was 1.5h. A Cu-UIO-67 catalyst with a Cu(II) loading of 6.42wt% can be obtained.

[0045] (3) After testing, this catalyst is applied to the hydrochlorination of acetylene in a fixed-bed reactor. The reaction conditions are: temperature 120°C, reaction pressure 0.01MPa, n(HCl):n(C 2 h 2 )=1:1, acetylene space ve...

Embodiment 3

[0047] (1) Same as embodiment 1.

[0048] (2) Preparation of catalyst Cu-UIO-67: Take 20 g of UIO-67 in step (1) and put it into a container. Then add 3.45g CuCl with a concentration of 45wt% 2 THF solution, stirred for 2 hours, centrifuged, removed the supernatant, vacuum dried at 160°C for 10 hours, and then subjected to glow discharge treatment, using a vacuum pump with a power of 500 W to keep the system in a vacuum state, and adjusting the air flow to make the plasma The pressure of the chamber was kept at 100 Pa, and the plasma treatment intensity was adjusted by adjusting the discharge voltage value. The applied voltage was 120V, and the treatment time was 1.5h. A Cu-UIO-67 catalyst with a Cu(II) loading of 3.70 wt% can be obtained.

[0049] (3) After testing, this catalyst is applied to the hydrochlorination of acetylene in a fixed-bed reactor. The reaction conditions are: temperature 120°C, reaction pressure 0.01MPa, n(HCl):n(C 2 h 2 )=1:1, acetylene space velocit...

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Abstract

The invention discloses a preparation method and application of a Cu / MOF catalyst in acetylene hydrochlorination reaction. The Cu / MOF catalyst takes a metal organic framework material as a carrier, and the preparation method comprises the following steps: loading a bivalent copper-containing precursor on the carrier by a solution impregnation method, carrying out vacuum drying treatment, and then treating by a glow discharge method to finally obtain the Cu / MOF catalyst. The prepared Cu-MOF catalyst is applied to acetylene hydrochlorination reaction, high conversion rate and high selectivity of acetylene hydrochlorination reaction can be achieved, the stability is high, and the Cu-MOF catalyst has high economic applicability and industrial application value.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a preparation method and application of a supported copper catalyst for acetylene hydrochlorination. Background technique [0002] Polyvinyl chloride (PVC) is a widely used general-purpose plastic obtained by polymerizing vinyl chloride monomer (VCM). Polyvinyl chloride is widely used in important fields of the national economy such as industry, agriculture, and building materials. Vinyl chloride is mainly produced by calcium carbide acetylene method, ethylene dichloride cracking method, and petroleum ethylene method. my country's resource structure of "rich in coal, poor in oil, and low in gas" determines that the calcium carbide acetylene method will be the most important for a long time in the future. The main process for the production of vinyl chloride in my country is that mercury chloride catalyzes the reaction of acetylene and hydrogen chloride to produce vi...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/00B01J37/02B01J37/34C07C17/08C07C21/06
CPCB01J31/1691B01J31/2239B01J37/0201B01J37/349C07C17/08B01J2231/32B01J2531/16B01J2531/48B01J35/394C07C21/06
Inventor 李小年赵佳汤奇岳玉学朱文锐王婷王涛方先华
Owner ZHEJIANG UNIV OF TECH
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