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Naluminum fluoride base fluorating catalyst and preparation thereof

A technology based on fluorination catalyst and fluorination catalyst is applied in the field of aluminum fluoride-based fluorination catalyst and its preparation, which can solve the problems that the catalyst preparation process cannot be carried out continuously, the catalyst reproducibility cannot be guaranteed, the catalyst preparation process is complicated, and the like, To achieve the effect of shortening the preparation cycle, reducing the time of fluorination activation, and being easy to control

Active Publication Date: 2013-04-03
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to obtain a catalyst with a high specific surface area in the above-mentioned patent, Al 2 o 3 SiO 2 , using hydrogen fluoride and SiO 2 The reaction generates volatile fluorosilicon compounds to increase AlF 3 The specific surface area of ​​the carrier, but because the volatile fluorosilicon compound is easy to cool and condense, the pipeline is blocked, so that the preparation process of the catalyst cannot be carried out continuously; at the same time, the preparation process of the catalyst is complicated, the preparation period is long, and strict control of Al 2 o 3 The fluorination temperature cannot guarantee the reproducibility of the catalyst

Method used

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  • Naluminum fluoride base fluorating catalyst and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve chromium nitrate in water, react with precipitant ammonia water at 60°C, adjust the pH value of the reaction solution in the range of 7.5 to 8.5, make it fully precipitate under stirring conditions, filter the formed slurry, and use deionized Wash with water until neutral, then dry at 120°C for 12 hours to obtain Cr(OH) 3 .

[0031] Ammonium hexafluoroaluminate and the obtained Cr(OH) 3 Mix uniformly according to the mass ratio of 80:20, and press into tablets to form the catalyst precursor. The catalyst precursor was calcined in a muffle furnace at 450°C for 8 hours, then loaded into a tubular reactor, heated to 300°C, fed with hydrogen fluoride gas for fluorination for 1 hour, then raised to 350°C at a heating rate of 1°C / min, and continued After fluorination for 8 hours, an aluminum fluoride-based fluorination catalyst was obtained.

[0032] The specific surface area of ​​the catalyst was measured by BET low temperature nitrogen adsorption method to be 55...

Embodiment 2

[0036] The preparation process of the catalyst is basically the same as in Example 1, except that ammonium hexafluoroaluminate is changed to ammonium tetrafluoroaluminate.

[0037] The specific surface area of ​​the catalyst was determined by BET low temperature nitrogen adsorption method to be 45.3m 2 g -1 , the pore volume is 0.2ml·g -1 , and the proportion of pores with a diameter smaller than 2nm was 28%.

[0038] The aluminum fluoride in the calcined catalyst precursor and the fresh aluminum fluoride-based fluorination catalyst was measured by X-ray diffractometer in gamma crystal form, and chromium was in amorphous form.

[0039] In a nickel tube fixed-bed tubular reactor with an internal diameter of 38 mm, 30 ml of the aluminum fluoride-based fluorination catalyst prepared above are charged, and HF and HCFC-123 are introduced to react, and the molar ratio of HF / HCFC-123 is controlled to be 10:1, the contact time is 10 seconds, the reaction temperature is 330 ° C, aft...

Embodiment 3

[0041] The preparation process of the catalyst is basically the same as in Example 1, except that ammonium hexafluoroaluminate and Cr(OH) in the catalyst precursor 3 The mass ratio is 95:5.

[0042] The specific surface area of ​​the catalyst was measured by BET low temperature nitrogen adsorption method to be 50.4m 2 g -1 , the pore volume is 0.18ml·g -1 , and the proportion of pores with a diameter smaller than 2nm was 33%.

[0043] The aluminum fluoride in the calcined catalyst precursor and the fresh aluminum fluoride-based fluorination catalyst was measured by X-ray diffractometer in gamma crystal form, and chromium was in amorphous form.

[0044] In a nickel tube fixed bed tubular reactor with an internal diameter of 38 mm, 30 ml of the aluminum fluoride-based fluorination catalyst prepared above are loaded into it, and HF and vinylidene chloride are introduced to react, and the mol ratio of HF / vinylidene chloride is controlled to be 8:1, the contact time is 5 second...

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Abstract

The invention discloses an aluminum fluoride-based fluorinated catalyst and a preparation method thereof. The invention is to solve the problems of complicated process, long preparation cycle and poor repeatability in preparation of aluminum fluoride-based fluorinated catalyst. The precursor of the aluminum fluoride-based fluorinated catalyst contains ammonium aluminum fluoride compound and trivalent chromium compound, the mass ratio of which is 70 to 95:5 to 30, wherein, the ammonium aluminum fluoride compound is ammonium hexafluoroaluminate or ammonium tetrafluoroaluminate, and the trivalent chromium compound is chromic oxide or chromium hydroxide. The fluoride catalyst obtained through a mixing method receives calcination under 300 DEG C to 500 DEG C, and then receives fluorination by hydrogen fluoride gas under 300 DEG C to 400 DEG C to obtain the aluminum fluoride-based fluoride catalyst. The aluminum fluoride of the obtained fluorinated catalyst is Gama-A1F3 type and the chromium is amorphous. The invention is characterized by large specific surface area and pore volume, high minipore proportion, high catalytic activity and stability, simple preparation process, easiness in control, good repeatability, short fluorination activation time, etc. The catalyst is applicable to reaction for preparation of hydroflurocarbon or hydrogenous fluorochlorohydrocarbon with a plurality of types of gas-phase fluorinated halohydrocarbon.

Description

technical field [0001] The present invention relates to an aluminum fluoride-based fluorination catalyst and a preparation method thereof, in particular to an aluminum fluoride used for gas phase fluorination of halogenated hydrocarbons to prepare hydrofluorocarbons (referred to as HFCs) or hydrofluorochlorocarbons (HCFCs) Based fluorination catalyst and its preparation method. Background technique [0002] Generally, large-scale industrial production of HFCs and HCFCs adopts the method of gas-phase fluorinated halogenated hydrocarbons. This method has the advantages of simple equipment, easy continuous large-scale production, safety, and environmental protection. The fluorination catalyst plays a central role in the gas-phase fluorination of halogenated hydrocarbons. Chromium-based fluorination catalysts and aluminum fluoride-based fluorination catalysts are commonly used fluorination catalysts in the prior art. It has been proved that the specific surface area of ​​the c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/132B01J27/12B01J23/26C07C17/20
Inventor 吕剑张伟王博寇联岗石磊徐强
Owner XIAN MODERN CHEM RES INST
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