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Preparation method of nano-chromium oxyfluoride catalyst with high specific surface area

A technology of chromium oxyfluoride catalyst and high specific surface area, which is applied in the direction of catalyst activation/preparation, nanotechnology for materials and surface science, chemical instruments and methods, etc., and can solve the problem of harsh reaction conditions, complex process, large particle size, etc. problems, to achieve the effect of mild preparation conditions, easy access to raw materials, and uniform distribution

Inactive Publication Date: 2018-05-11
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen from the above patents that the existing preparation methods of chromium-based catalysts still have the problems of complicated process, harsh reaction conditions and heavy pollution
[0004] The preparation method of the high specific surface chromium-based catalyst reported above still has at least the following problems: (1) the process is complicated, and the chromium-containing oxide precursor is obtained first, and then the catalyst is obtained through high-temperature fluorination treatment, the preparation route is long, and the product Poor batch stability; (2) The high-temperature hydrogen fluoride fluorination treatment conditions are harsh, pollution is heavy, and the high-temperature fluorination reaction is a strong exothermic process, and the process operation is difficult; (3) The hydrogen fluoride used in the gas-phase fluorination is greatly excessive, resulting in high raw material costs , and the effluent waste hydrogen fluoride has great environmental pollution; (4) the obtained fluorinated chromium-based catalyst has low fluorine content, small specific surface area, large particle size, and low activity

Method used

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  • Preparation method of nano-chromium oxyfluoride catalyst with high specific surface area
  • Preparation method of nano-chromium oxyfluoride catalyst with high specific surface area
  • Preparation method of nano-chromium oxyfluoride catalyst with high specific surface area

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: Preparation of high specific surface nano-chromium oxyfluoride catalyst

[0023] Dissolve 1.0M chromium source in 50mL polyol solvent, reflux at 30-80°C for 6 hours, then add the fluorinated reagent dropwise to the above solution with stirring, the dropping time is 30min, and then Reflux and stir at 140°C-200°C for 6 hours to obtain a suspension; then statically age at 100-160°C for more than 24 hours, then wash and filter to obtain a solid; finally roast at 200-350°C for more than 4 hours in an air atmosphere to prepare A high surface nanocrystalline chromium oxyfluoride catalyst material was obtained. The texture properties of chromium oxyfluoride prepared under different chromium sources, polyol solvents, complexing agents, fluorinating reagents, and calcination temperatures are shown in Table 1.

[0024] The physicochemical property results of the high specific surface nano-chromium oxyfluoride catalyst of Table 1 Example 1

[0025]

[0026]

Embodiment 2

[0027] Embodiment 2: Preparation of high specific surface nano-chromium oxyfluoride catalyst

[0028] Dissolve 1.0M chromium nitrate and polyethylene glycol in 50mL of ethylene glycol, reflux at 60°C for 6h, then add HF aqueous solution (40wt.%) dropwise to the above solution with stirring, and the dropping time is After the dropwise addition, reflux and stir at 160°C for 6h to obtain a suspension; then stand and age at 160°C for more than 24h, then wash and filter to obtain a solid; finally roast at 300°C for more than 4h to obtain a high Specific surface nanocrystalline chromium oxyfluoride. The textures of chromium oxyfluoride obtained with different amounts of polyethylene glycol are shown in Table 2.

[0029] Table 2 The results of the physical and chemical properties of the high specific surface nano-chromium oxyfluoride catalyst of Example 2

[0030] Numbering

Embodiment 3

[0031] Embodiment 3: Preparation of high specific surface nano-chromium oxyfluoride catalyst

[0032] Dissolve 1.0M chromium nitrate and polyethylene glycol (Cr / complexing agent mass ratio: 1:3) in 50 mL of ethylene glycol, reflux at 60°C for 6 hours, then add HF aqueous solution dropwise to In the above solution, the dropwise addition time is 30min. After the dropwise addition, reflux and stir at 160°C for 6h to obtain a suspension; then statically age at 160°C for more than 24h, then wash and filter to obtain a solid; finally at 300°C Calcined under the lower pressure for more than 4 hours, the high specific surface nanocrystalline chromium oxyfluoride was prepared. The textures of chromium oxyfluoride prepared with different HF concentrations are shown in Table 3.

[0033] The physicochemical property results of the high specific surface nano-chromium oxyfluoride catalyst of table 3 embodiment 3

[0034]

[0035]

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Abstract

The invention discloses a preparation method of a nano-chromium oxyfluoride catalyst with high specific surface area and aims to solve the problems of high raw material cost, complex synthesis process, difficult uniform mixing of chromium fluoride and oxygen elements, incapability of effectively controlling grain size and the like in existing preparation methods. The preparation method of the nano-chromium oxyfluoride catalyst comprises the following steps: (1) preparing a solution containing a chromium source precursor, a polyol solvent and a complexing agent component, and performing refluxing at 30-80 DEG C; (2) adding a fluorinating reagent to the solution obtained in (1) for fluorination, and performing refluxing and stirring at 140-200 DEG C to obtain a suspension; (3) performing aging, washing and filtering on the suspension at 100-160 DEG C to obtain a solid, and finally, performing roasting at 200-350 DEG C to obtain the nano-chromium oxyfluoride catalyst with high specific surface area.

Description

technical field [0001] The invention relates to a chromium oxyfluoride catalyst, in particular to a mild, simple and environment-friendly preparation method of a nano-chromium oxyfluoride catalyst with a high specific surface area. Background technique [0002] In the gas-phase catalytic synthesis of fluorine-containing halogenated hydrocarbons, such as the preparation of the third-generation refrigerant hydrofluorocarbons (HFCs) and the fourth-generation refrigerant hydrofluoroolefins (HFOs), strong corrosive HF or one of the reactants 1. It may be generated during the reaction, so the catalyst used must be a material that can exist stably in a high-temperature HF atmosphere. So far, fluorinated chromium oxide has been proven to be stable for a long time in the above-mentioned strong corrosive atmosphere. More importantly, the research results show that the catalytic active center for the preparation of fluorine-containing halocarbons is chromium oxyfluoride generated afte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/132B01J35/10B01J37/08B82Y30/00B82Y40/00C01G37/00
CPCB82Y30/00B82Y40/00C01G37/00B01J27/132B01J37/08B01J35/613B01J35/615
Inventor 毛伟吕剑白彦波郝志军马辉秦越王博杨志强何飞石磊徐强
Owner XIAN MODERN CHEM RES INST
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