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Preparation process of 1, 1-dichloro-3, 3, 3-trifluoropropene

A preparation process, a technology of trifluoropropene, which is applied in the preparation of halogenated hydrocarbons, catalyst activation/preparation, organic chemistry, etc., and can solve the problems of low conversion rate of reaction raw materials

Active Publication Date: 2020-10-23
ZHEJIANG RES INST OF CHEM IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has a reaction temperature of 350-550°C and a reaction time of 30 seconds, but the conversion rate of the reaction raw materials is very low, only about 10%.

Method used

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  • Preparation process of 1, 1-dichloro-3, 3, 3-trifluoropropene

Examples

Experimental program
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Embodiment 1

[0050] Embodiment 1: (catalytic system: 15wt%Ru / 85%Cr 2 o 3 ;3wt%Sm 2 o 3 , 2wt% SmCl 3 , 4wt% ZnO, wherein the mass of the main catalyst is 100%)

[0051] The main catalyst is prepared by impregnation method: the nitrate of the active component Ru is stirred and dissolved in deionized water to obtain a metal salt solution, that is, the impregnation solution; the dried multi-level micro / mesoporous Cr 2 o 3 The carrier was impregnated in the impregnating solution for 4 hours at room temperature, then filtered, and dried in a drying oven at 110°C for 9 hours to obtain a precursor. Finally, the obtained precursor was calcined under an inert gas argon atmosphere, and calcined at 500°C for 5 hours to obtain the main catalyst. Among them, the multi-level micro / mesoporous Cr 2 o 3 The specific surface area of ​​the carrier is 65.5m 2 / g, the average pore diameter is 8.5nm, 65.5% of the pore diameter is 0.2-2nm, and 12.7% of the pore diameter is 15-50nm.

[0052] By physicall...

Embodiment 2

[0054] Embodiment 2: (catalytic system: 15wt%Pd / 85%Cr 2 o 3 ;3wt% La 2 o 3 , 2wt% LaCl 3 , 4wt% ZnO, wherein the mass of the main catalyst is 100%)

[0055] The main catalyst is prepared by impregnation method: the nitrate of the active component Pd is stirred and dissolved in deionized water to obtain a metal salt solution, that is, the impregnation solution; the dried multi-level micro / mesoporous Cr 2 o 3 The carrier was impregnated in the impregnating solution for 4 hours at room temperature, then filtered, and dried in a drying oven at 110°C for 9 hours to obtain a precursor. Finally, the obtained precursor was calcined under an inert gas argon atmosphere, and calcined at 500°C for 5 hours to obtain the main catalyst. Among them, the multi-level micro / mesoporous Cr 2 o 3 The specific surface area of ​​the carrier is 55.8m 2 / g, the average pore diameter is 9.5nm, 55.5% of the pore diameter is 0.2-2nm, and 15.2% of the pore diameter is 15-50nm.

[0056] By physical...

Embodiment 3

[0075] Trifluoromethane raw material stream (1) and trichloroethylene raw material stream (2) are passed into the reactor respectively, and in the presence of the catalytic system of Example 1, gas phase reaction generates reaction product stream (3). The heating temperature of the reactor is 400°C, the raw material trifluoromethane is excessive, and the molar ratio of trifluoromethane and trichloroethylene is 1.5:1. In the reaction stage, a reaction-promoting gas is added, and the reaction-promoting gas is Cl with a molar ratio of 20%. 2 and 80% molar CO 2 , the molar ratio of reaction-promoting gas to trifluoromethane is 0.01:1. The reaction product stream (3) is sent to a separation system for separation to obtain the target product 1,1-dichloro-3,3,3-trifluoropropene.

[0076] Wherein, excess trifluoromethane passes through an extraction tower, is purified and circulated into the initial reactor as a reaction raw material. The extract liquid in the extraction tower is i...

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Abstract

The invention relates to a method for producing a 1, 1-dichloro-3, 3, 3-trifluoropropene with high added value by taking trifluoromethane and trichloroethylene as raw materials. According to the method, a catalytic system composed of a main catalyst and a catalytic auxiliary agent of specific types in a special proportion is adopted; wherein the active component of the main catalyst is selected from one or more of Fe, Co, Ni, Ru, Rh, Pd, Pt, Cu, Ag and Au, multi-stage micro / mesoporous Cr2O3 is adopted as a carrier, and a metal oxide and / or a rare earth auxiliary agent is adopted as a catalyticauxiliary agent, so that the selectivity on the target product 1, 1-dichloro-3, 3, 3-trifluoropropene is effectively improved. According to the method disclosed by the invention, not only the resource utilization of the byproduct trifluoromethane is promoted, but also the types of raw materials of the 1, 1-dichloro-3, 3, 3-trifluoropropene product are expanded, and remarkable economic benefits and social benefits are generated.

Description

technical field [0001] The invention relates to a preparation process of 1,1-dichloro-3,3,3-trifluoropropene, in particular to a method of reacting trifluoromethane and trichloroethylene as raw materials in the presence of a catalyst to produce Process for the preparation of value-added 1,1-dichloro-3,3,3-trifluoropropene products. Background technique [0002] With the increasing trend towards global climate change, alternative technologies for products with high ozone depletion potential (ODP) and high global warming potential (GWP) are also increasing. 1,1-dichloro-3,3,3-trifluoropropene as 3,3-dichloro-1,1,1,2,2-pentafluoropropane and 1,3-dichloro-1,1, An effective substitute for 2,2,3-pentafluoropropane, widely used in detergents, aerosols, refrigerants, blowing agents and other solvents. In the preparation process of 1,1-dichloro-3,3,3-trifluoropropene, it is particularly important to reduce the cost of raw materials and optimize the process. [0003] Trifluorometha...

Claims

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Application Information

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IPC IPC(8): C07C17/269C07C17/38C07C21/18B01J27/138B01J35/10B01J37/02B01J37/26
CPCB01J27/138B01J37/0201B01J37/26C07C17/269C07C17/38B01J35/613B01J35/615B01J35/643B01J35/695B01J35/647C07C21/18
Inventor 刘武灿王术成周飞翔张建君韩文锋
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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