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Catalyst for hydrofluorination reaction of acetylene to prepare vinyl fluoride and 1,1-difluoroethane, and preparation method and application thereof

The technology of difluoroethane and catalyst is applied in the field of catalyst for acetylene hydrofluorination reaction and its preparation field, and can solve the problems of carbon deposition, short service life, complicated preparation process and the like

Inactive Publication Date: 2014-07-16
SINOCHEM LANTIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to provide a catalyst with low cost, high activity, long service life and simple preparation process and its preparation method, which is used for the synthesis of vinyl fluoride and 1,1-difluoroethane by the gas phase method of acetylene, and solves the problem that currently used for acetylene Aluminum-based catalysts for hydrofluorination reactions have problems such as serious carbon deposition, short service life, and complicated preparation processes.

Method used

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  • Catalyst for hydrofluorination reaction of acetylene to prepare vinyl fluoride and 1,1-difluoroethane, and preparation method and application thereof
  • Catalyst for hydrofluorination reaction of acetylene to prepare vinyl fluoride and 1,1-difluoroethane, and preparation method and application thereof
  • Catalyst for hydrofluorination reaction of acetylene to prepare vinyl fluoride and 1,1-difluoroethane, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] La 2 o 3 , B 2 o 3 They were respectively treated under air atmosphere at 100°C for 6 hours, and mixed at a mass ratio of 1:1 to obtain modified component A. AlF 3 , modified component A, and bentonite were mixed according to the mass percentage composition of 95%, 4%, and 1%, and were blended by ball milling, extruded by wet mixing extrusion, and dried at 105°C for 18 hours to obtain a catalyst precursor . Take 300g of the catalyst precursor and put it into a φ30*1200 carbon steel reaction tube. 2Roast at 200°C for 6 hours under protection, and then pass HF:N 2 The mixture of = 1:12 was fluorinated at 150°C for 2 hours, heated to 400°C for 2 hours, and then gradually increased the concentration of HF until pure HF was fluorinated for 4 hours to obtain the catalyst of the present invention, marked as Cat.1-1.

Embodiment 2

[0033] La(NO 3 ) 3 Calcined at 400° C. for 16 hours under a nitrogen atmosphere to obtain modified component A. AlF 3 , modified component A, and graphite are mixed according to the mass percentage of 85%, 10%, and 5%. After ball milling and blending, they are extruded by wet mixing extrusion and dried at 105 ° C for 24 hours to obtain a catalyst precursor. . Take 300g of the catalyst precursor and put it into a ф30*1200 carbon steel reaction tube. 2 Roast at 200°C for 16 hours under protection, and then pass HF:N 2 The mixture of =1:1 was fluorinated at 200°C for 2 hours, raised to 320°C for 2 hours, and then gradually increased the concentration of HF until pure HF was fluorinated for 4 hours to obtain the catalyst of the present invention, marked as Cat.2-1.

Embodiment 3

[0040] La(OH) 3 Calcined at 400° C. for 6 hours in an air atmosphere to obtain modified component A. AlF 3 , modified component A, and silicon carbide were mixed according to the mass percentage of 85%, 10%, and 5%, and were blended by ball milling, extruded by wet mixing extrusion, and dried at 120°C for 24 hours to obtain a catalyst precursor body. Get 10g of the catalyst precursor and pack it into a carbon steel reaction tube with a diameter of 14mm and a length of 600mm. 2 Roast at 200°C for 6 hours under protection, and then pass HF:N 2 The mixture of = 1:12 was fluorinated at 150°C for 2 hours, heated to 350°C for 2 hours, and then gradually increased the concentration of HF until pure HF was fluorinated for 4 hours to obtain the catalyst of the present invention, marked as Cat.3.

[0041] Catalyst Cat.3 that this embodiment makes is applied in acetylene hydrofluorination reaction, HF / C 2 h 2 The molar ratio of 1.4:1, its C 2 h 2 The reactivity and selectivity of...

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Abstract

The invention discloses a catalyst for a hydrofluorination reaction of acetylene to prepare vinyl fluoride and 1,1-difluoroethane. A catalyst precursor is formed by an aluminum-containing compound, a modified component A and a modified component B, and then the catalyst is obtained by baking and carrying out fluorination treatment of the catalyst precursor, wherein the modified component A is a combination of one, two, three or more selected from compounds of lanthanide metals, group IIIA metals, group IVB metals and group VA metals, and the modified component B is a combination of one, two, three or more selected from compounds of bentonite, graphite, silicon carbide, pseudo-boehmite and a sesbania powder. The catalyst provided by the invention is low in cost, high in activity, long in service life, and simple in preparation process, and can overcome the defects that a commonly used aluminum-based catalyst is severe in carbon deposition, short in service life, complicated in preparation process and the like.

Description

technical field [0001] The invention relates to a fluorination catalyst, in particular to a catalyst for acetylene hydrofluorination and a preparation method thereof. Background technique [0002] Vinyl fluoride (VF) is an important fluorine-containing monomer, which can be used to prepare polyvinyl fluoride (PVF) and fluorine-containing fine chemicals. Among them, PVF is the one with the lowest fluorine content and the smallest density among fluororesins. It has excellent chemical corrosion resistance, hydrophobicity, abrasion resistance, aging resistance and non-stickiness. It has been widely used in the protective layer of building materials. , the packaging of aviation industry and solar cells, the inner wall coating of packaging containers, the anticorrosion of oil pipelines in oil fields, etc. [0003] 1,1-Difluoroethane (HFC-152a) is an excellent substitute for ozone-depleting substances and an intermediate in the production of polyvinylidene fluoride resin. DuPont ...

Claims

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Application Information

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IPC IPC(8): B01J23/10B01J27/224B01J23/08B01J23/18B01J21/16C07C17/08C07C21/18C07C19/08
Inventor 张迪林胜达郭荔王术成陈淼赵翀
Owner SINOCHEM LANTIAN
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