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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 a fluorination catalyst activation method, which comprises: 1) drying, wherein a catalyst precursor is subjected to step-by-step drying at a temperature of 100-400 DEG C undera diluent gas flow; and 2) activating, wherein the activating is performed in three stages, the initial control stage a comprises that the temperature is adjusted to 100-300 DEG C after the drying, hydrogen fluoride is introduced under a diluent gas flow, and the reaction heat [delta]T does not exceed 40 DEG C during the introducing, the step-by-step activation stage b comprises that the mass flow of the hydrogen fluoride is adjusted after the reaction heat [delta]T is stable, a mass flow ratio of the diluent to the hydrogen fluoride is controlled within a certain rang, and step-by-step activation is performed, and the deep activation stage C is performed. According to the present invention, with the fluorination catalyst activation method, the damage of the sharp heat release on the structure of the catalyst can be avoided during the activating, the activated catalyst has the high fluorine content and the high specific surface area so as to provide the high catalytic activity, and the selectivity of R125 is up to more than 68% when the activated catalyst is used for the catalytic preparation of R125.

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
CPCB01J23/002B01J23/26B01J35/1019B01J37/08B01J37/26B01J2523/00C07C17/206B01J2523/22B01J2523/27B01J2523/31B01J2523/67C07C19/08
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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