Catalyst for fluorinating of chloropenta fluoroethane to convert into hexafluoroethane, a preparation method and application in purifying pentafluoroethane

A technology of pentafluorochloroethane and hexafluoroethane, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, and preparation of halogenated hydrocarbons, and can solve the problems of unsuitable treatment, extremely high equipment requirements, and liquid phase reactions High pressure and other problems, to avoid the loss of active component antimony, strong catalytic activity, high fluorine and chlorine exchange capacity

Active Publication Date: 2017-10-13
SHANDONG DONGYUE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the product yield is high and the reaction temperature is low, the liquid phase reaction pressure is high, and antimony fluoride has extremely high requirements on equipment, and it is not suitable for handling a small amount of pentafluorochloroethane in pentafluoroethane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation method of the catalyst for the fluorination conversion of pentafluoro-chloroethane to hexafluoroethane, the specific steps are as follows:

[0037] Fully mix antimony pentoxide and aluminum oxide at a mass ratio of 1:10, grind them into a fine powder in a mortar, sieve to get a powder of <5 microns, add 5% pure water of the powder weight, and shake Spherical particles of 3-7 mm are made in the granulator. Dry in an oven at 100° C. for 24 hours, and then bake at 360° C. for 6 hours to obtain a catalyst precursor. Fill 100g of catalyst precursor into a 500mm-long DN25 carbon steel reaction tube, pass hydrogen fluoride gas at a rate of 0.75mol / h at 180°C to activate the catalyst precursor, and keep it for 36h to obtain a new antimony-aluminum catalyst.

[0038] The obtained catalyst was analyzed by element, and the atomic mass percentage of each element was: antimony: 6.6%, aluminum: 46.56%, oxygen: 26.14%, fluorine: 20.7%.

[0039] The specific method of...

Embodiment 2

[0043] The preparation method of the catalyst for the fluorination conversion of pentafluoro-chloroethane to hexafluoroethane, the specific steps are as follows:

[0044] Fully mix antimony pentoxide and aluminum oxide at a mass ratio of 1:7, grind them into a fine powder in a mortar, sieve to get a powder of <5 microns, add 5% pure water of the powder weight, and shake Spherical particles of 3-7 mm are made in the granulator. Dry at 100° C. for 24 hours in an oven, and then bake at 380° C. for 6 hours to obtain a catalyst precursor. Fill 100g of catalyst precursor into a 500mm-long DN25 carbon steel reaction tube, pass hydrogen fluoride gas at a rate of 0.75mol / h at 180°C to activate the catalyst precursor, and keep it for 36h to obtain a new antimony-aluminum catalyst.

[0045] The obtained catalyst was analyzed by element, and the atomic mass percentage of each element was: antimony: 9.1%, aluminum: 44.83%, oxygen: 25.66%, fluorine: 20.41%.

[0046] The specific method of...

Embodiment 3

[0050] The preparation method of the catalyst for the fluorination conversion of pentafluoro-chloroethane to hexafluoroethane, the specific steps are as follows:

[0051] Fully mix antimony pentoxide and aluminum oxide at a mass ratio of 1:4, grind them into a fine powder in a mortar, sieve to get a powder of <5 microns, add 5% pure water by weight of the powder, and shake Spherical particles of 3-7 mm are made in the granulator. Dry in an oven at 100° C. for 24 hours, and then bake at 340° C. for 6 hours to obtain a catalyst precursor. Fill 100g of catalyst precursor into a 500mm-long DN25 carbon steel reaction tube, pass hydrogen fluoride gas at a rate of 0.75mol / h at 180°C to activate the catalyst precursor, and keep it for 36h to obtain a new antimony-aluminum catalyst.

[0052] The obtained catalyst was analyzed by element, and the atomic mass percentage of each element was: antimony: 14.5%, aluminum: 41.04%, oxygen: 24.68%, fluorine: 19.78%.

[0053] The specific metho...

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Abstract

The invention relates to a catalyst for fluorinating of chloropenta fluoroethane to convert into hexafluoroethane, a preparation method and application in purifying pentafluoroethane. The preparation method comprises the following steps of using antimony pentoxide and aluminium oxide as raw materials, mixing, grinding, enabling the antimony pentoxide and the aluminium oxide to fully mix and touch, and roasting, so as to obtain a precursor; leading hydrogen fluoride gas to fluorinate the precursor, and enabling antimony (V) and aluminum to easily form an antimony (V)-fluorine-aluminum bonding structure. The preparation method has the advantages that by adopting the bonding structure, the fluorine and chloride compounds of the antimony (V) can be effectively fixed and uniformly distributed at the surface of aluminum oxide and aluminum fluoride, so that the dispersivity of the active component (antimony) is improved, the loss of the active component (antimony) is avoided, the high-efficiency utilization of the antimony as the solid catalyst for gas-phase catalyzing is guaranteed, and the antimony can effectively play functions; the fluorine and chloride exchange ability of the antimony is further improved by the high acidity of the aluminum, so that the obtained antimony-aluminum catalyst has high fluorine and chloride exchange ability and strong catalysis activity.

Description

technical field [0001] The invention relates to a catalyst for the fluorination of pentafluoro-chloroethane to hexafluoroethane, a preparation method and an application in purifying pentafluoroethane, belonging to the field of catalyst materials. Background technique [0002] Pentafluoroethane is a good low-temperature refrigerant and one of the raw materials of R410. At present, the known industrial production methods of pentafluoroethane include the chloroethylene method and the tetrafluoroethylene method, among which the production cost of the tetrachloroethylene method is relatively low, and is currently the mainstream production process. However, in the production process of the tetrachlorethylene method, pentafluorochloroethane will inevitably be produced. The reason is that the intermediate product trifluorodichloroethane is easily disproportionated to obtain by-product pentafluorochloroethane under high temperature production conditions. , due to the azeotropic situ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/125C07C17/20C07C19/08C07C17/395
CPCB01J27/125C07C17/206C07C17/395C07C19/08
Inventor 王伟王鑫丁晨孙森都荣礼韩春华徐强张星全
Owner SHANDONG DONGYUE CHEM
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