Catalyst for compounding fluorine-containing halohydrocarbon and preparation method of catalyst

A technology of catalysts and halogenated hydrocarbons, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as complex processes, high energy consumption, and complicated process flows, and achieve mild preparation conditions, The effect of simple operation and easy-to-obtain raw materials

Active Publication Date: 2016-01-20
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] Above-mentioned report prepares the catalyzer that fluorine-containing halogenated hydrocarbon is used, still exists following problem at least: (1) anhydrous sol-gel fluorination method is that the organic solvent of metal source and anhydrous HF is fluorine with expensive organometallic source, and this method must be operated under anhydrous conditions, the process is complicated, and it is difficult to apply to industrial production. At the same time, the metal fluorides obtained are all amorphous structures, unstable at high temperatures, and will quickly crystallize into low specific surface

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  • Catalyst for compounding fluorine-containing halohydrocarbon and preparation method of catalyst
  • Catalyst for compounding fluorine-containing halohydrocarbon and preparation method of catalyst
  • Catalyst for compounding fluorine-containing halohydrocarbon and preparation method of catalyst

Examples

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Example Embodiment

[0052] Example 1: Preparation of large specific surface area, mesoporous aluminum fluoride

[0053] A mixture of 15.0g of large specific surface area, mesoporous alumina, and 15.0g of organic polymer additives was dissolved in 100mL of water. The suspension was refluxed for 12h under stirring at 60℃, and then the aqueous solution of fluorinated reagent was slowly dropped under stirring. Add to the above suspension, the dripping time is 2h, the fluorination temperature is controlled at 90℃, after the dripping is completed, stir for 6h, then statically age at 50℃ for 12h, and then wash, filter, and dry to obtain a large ratio Surface area, mesoporous aluminum fluoride. Table 1 shows the specific surface area and pore size distribution of aluminum fluoride prepared under different alumina specific surface areas, pore structures, organic polymer additives, and fluorinating reagents.

[0054] Table 1 Physicochemical properties of aluminum fluoride in Example 1

[0055]

[0056]

Example Embodiment

[0057] Example 2: Preparation of large specific surface area, mesoporous zirconium fluoride

[0058] A mixture of 15.0g of large specific surface area, mesoporous alumina, and 30.0g of organic polymer additives was dissolved in 100mL of water. The suspension was refluxed for 12h under stirring at 80℃, and then the aqueous solution of fluorinated reagent was slowly dropped under stirring. Add to the above suspension, the dripping time is 4h, the fluorination temperature is controlled at 60℃, after the dripping is completed, stir for 8h, and then statically age at 50℃ for 12h, and then wash, filter and dry to obtain a large ratio Surface area, mesoporous aluminum fluoride. Table 2 shows the specific surface area and pore size distribution of zirconium fluoride prepared under different zirconia specific surface area, pore structure, organic polymer additives, and fluorinating reagent.

[0059] Table 2 Physicochemical properties of zirconium fluoride in Example 2

[0060]

[0061]

Example Embodiment

[0062] Example 3: Preparation of large specific surface area, mesoporous magnesium fluoride

[0063] A mixture of 15.0g of large specific surface area, mesoporous magnesium oxide, and 45.0g of organic polymer additives was dissolved in 100mL of water. The suspension was refluxed for 12h under stirring at 30°C, and then the fluorinated reagent aqueous solution was slowly dropped under stirring. Add to the above suspension, the dripping time is 3h, the fluorination temperature is controlled at 30℃, after the dripping is completed, stir for 8h, then static aging at 50℃ for 12h, and then wash, filter, and dry to obtain a large ratio Surface area, mesoporous aluminum fluoride. Table 3 shows the specific surface area and pore size distribution of magnesium fluoride prepared under different magnesium oxide specific surface areas, pore structures, organic polymer additives, and fluorinating reagents.

[0064] Table 3 Physicochemical properties of magnesium fluoride in Example 3

[0065]

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Abstract

The invention discloses a catalyst for compounding fluorine-containing halohydrocarbon and a preparation method of the catalyst and aims at solving problems that the specific surface area is small, the hole channel size is non-adjustable, an existing preparation method is expensive and complex, and the like in an existing preparation process. According to the catalyst disclosed by the invention, an active component comprises one or more of II group elements, VIII group elements, Cr or Cu; and a metal fluoride active carrier comprises one or more of aluminum fluoride, zirconium fluoride or magnesium fluoride. The preparation method of the metal fluoride-based catalyst which is large in specific surface area and has a mesoporous structure comprises the following steps: (1) preparing a turbid liquid solution of a metallic oxide which is large in specific surface area and has the mesoporous structure, and an organic polymeric additive, and backflowing at 0-100 DEG C; (2), dropwise adding an aqueous solution of a fluorinated reagent into the turbid liquid solution obtained in the step (1) for fluorination; and (3) dipping an aqueous solution of the active component into a metal fluoride base body obtained in the step (2), and roasting at 350-400 DEG C to obtain the catalyst.

Description

technical field [0001] The invention belongs to the field of refrigerants and relates to a metal fluoride catalyst, in particular to a large specific surface area and mesoporous metal fluoride catalyst used for synthesizing fluorine-containing halogenated hydrocarbons and a mild and simple preparation method thereof. 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, metal fluorides are the only substances that can exist stably in the above-mentioned strong corrosive atmosphere for a long time. However, metal fluorides must have a large specific surface area to obtain con...

Claims

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Application Information

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IPC IPC(8): B01J27/125B01J27/135B01J27/12B01J27/132B01J27/128B01J27/13B01J27/138B01J35/10B01J37/26
Inventor 毛伟吕剑徐强白彦波王伟亢建平王博马辉郝志军张伟
Owner XIAN MODERN CHEM RES INST
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