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A kind of activation method of fluorination catalyst

A technology of fluorination catalyst and activation method, which is applied in the field of preparation of fluorination catalyst, can solve the problems of destroying the internal structure of the catalyst, affecting the catalytic activity of the catalyst, and not considering the exothermic catalyst of the reaction, so as to avoid damage and achieve high catalytic activity Effect

Active Publication Date: 2020-12-22
RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the above-mentioned activation methods do not take into account the influence of reaction heat and temperature changes on the internal structure of the catalyst. Since the catalyst will undergo a violent heat release when it first contacts hydrogen fluoride, a sharp temperature rise may also occur during the activation process, and these mutations will be damaged to varying degrees. The internal structure of the catalyst affects the catalytic activity of the catalyst

Method used

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  • A kind of activation method of fluorination catalyst

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Effect test

Embodiment 1

[0065] Drying: Take 80g, about 100mL of catalyst precursor A (composed of chromium oxide, aluminum oxide, magnesium oxide and zinc oxide), fill it into a fixed bed reactor, the whole heating rate is 8°C / min, under nitrogen mass flow In 60g / h atmosphere, dry at 200°C, 300°C and 350°C for 2 hours respectively;

[0066] Initial control: After drying, adjust the mass flow rate of hydrogen fluoride to 36g / h at 240°C and 60g / h nitrogen atmosphere to ensure that △T does not exceed 20°C. If it exceeds 20°C, cut off hydrogen fluoride, and continue to feed when the temperature returns to 240°C Fluorination until hydrogen fluoride can be fed continuously and ΔT does not exceed 20°C;

[0067] Step-by-step activation: 1. Adjust the mass flow rate of hydrogen fluoride to 88g / h and keep it constant, the temperature is 240°C, adjust the mass flow ratio of nitrogen and hydrogen fluoride to 0.8:1 and activate for 2h; 2. Adjust the temperature to 280°C, adjust nitrogen and hydrogen fluoride Act...

Embodiment 2

[0070] Drying: Take 80g, about 100mL of catalyst precursor A (composed of chromium oxide, aluminum oxide, magnesium oxide and zinc oxide), fill it into a fixed bed reactor, the whole heating rate is 8°C / min, under nitrogen mass flow In 60g / h atmosphere, dry at 200°C, 300°C and 350°C for 2 hours respectively;

[0071] Initial control: After drying, adjust the mass flow rate of hydrogen fluoride to 36g / h at 240°C and 60g / h nitrogen atmosphere to ensure that △T does not exceed 20°C. If it exceeds 20°C, cut off hydrogen fluoride, and continue to feed when the temperature returns to 240°C Fluorination until hydrogen fluoride can be fed continuously and ΔT does not exceed 20°C;

[0072] Step-by-step activation: 1. Adjust the mass flow rate of hydrogen fluoride to 88g / h and keep it constant, the temperature is 240°C, adjust the ratio of mass flow rate of nitrogen and hydrogen fluoride to 0.8:1 and activate for 2h; 3. Adjust the temperature to 360°C, adjust the mass flow ratio of nit...

Embodiment 3

[0075] Drying: Take 80g, about 100mL of catalyst precursor A (composed of chromium oxide, aluminum oxide, magnesium oxide and zinc oxide), fill it into a fixed bed reactor, the whole heating rate is 8°C / min, under nitrogen mass flow In 60g / h atmosphere, dry at 200°C, 300°C and 350°C for 2 hours respectively;

[0076] Initial control: After drying, adjust the mass flow rate of hydrogen fluoride to 36g / h at 240°C and 60g / h nitrogen atmosphere to ensure that △T does not exceed 20°C. If it exceeds 20°C, cut off hydrogen fluoride, and continue to feed when the temperature returns to 240°C Fluorination until hydrogen fluoride can be fed continuously and ΔT does not exceed 20°C;

[0077] Step-by-step activation: 1. Adjust the mass flow rate of hydrogen fluoride to 40g / h and keep it constant, the temperature is 240°C, adjust the mass flow ratio of nitrogen and hydrogen fluoride to 0.8:1 and activate for 2h; 2. Adjust the temperature to 280°C, adjust nitrogen and hydrogen fluoride Act...

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Abstract

The invention relates to an activation method of a fluorination catalyst, which includes: 1) Drying: step-by-step drying of the catalyst precursor at 100-400°C under diluent gas flow; 2) Activation: carried out in three stages: a. Initial control : After drying, adjust the temperature to 100-300°C, and introduce hydrogen fluoride under the diluent gas flow. During the introduction process, the reaction heat △T does not exceed 40°C; b. Step-by-step activation: After the reaction heat △T becomes stable, Adjust the mass flow of hydrogen fluoride, and control the mass flow ratio of diluent to hydrogen fluoride within a certain range to perform step-by-step activation; c. Deep activation. The activation method of the fluorination catalyst provided by the invention can avoid rapid heat generation from damaging the structure of the catalyst during the activation process. The activated catalyst has higher fluorine content and specific surface area, thereby having higher catalytic activity and is used in When R125 is catalytically prepared, the selectivity of R125 is as high as over 68%.

Description

technical field [0001] The invention relates to the technical field of preparation of fluorination catalysts, in particular to a method for activating the fluorination catalyst used in the gas-phase fluorination reaction of halogenated hydrocarbons and hydrogen fluoride. Background technique [0002] In the field of fluorine chemical industry, since the ozone depletion potential (ODP) of hydrofluorocarbons (HFCs) is 0, the global warming potential (GWP) is small, and the refrigeration performance is similar to that of chlorofluorocarbons (CFCs), it is an ideal choice for CFCs. Substitutes are widely used in large commercial refrigerants, blowing agents, fire extinguishing agents, etc. Gas-phase fluorine-chlorine exchange reaction is the key reaction for the selective synthesis of fluorine-containing compounds. It has been widely used in the industrial production process of hydrofluorocarbons because of its simplicity, economy and practicality, less pollution and easy operati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/26B01J35/10B01J37/08B01J37/26C07C17/20C07C19/08
CPCC07C17/206B01J23/002B01J23/26B01J37/08B01J37/26B01J2523/00B01J35/615B01J2523/22B01J2523/27B01J2523/31B01J2523/67C07C19/08
Inventor 李义涛胡为晴唐火强孙明刚邓龙辉张宏清
Owner RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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