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Catalyst for preparing hexafluoroisopropanol by gas-phase catalytic hydrogenation of hexafluoroacetone hydrate, its preparation method and application

A technology for hydration of hexafluoroacetone and hexafluoroisopropanol, which is used in physical/chemical process catalysts, hydroxyl compound preparation, metal/metal oxide/metal hydroxide catalysts, etc. and other problems to achieve the effect of improving stability, reducing load and reducing production cost

Active Publication Date: 2011-12-14
中化蓝天氟材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the above reaction system is a catalytic hydrogenation reaction of fluorine-containing compounds, which inevitably produces a small amount of impurities such as HF during the reaction process. At the same time, the hexafluoroacetone hydrate system has strong acidity. These reaction characteristics are easy to cause the hydrogenation catalyst to lose live, the reaction in the patent US4467124 has only been carried out for 20h, and there is still a very large gap with the requirements of industrialization, and the document "Synthetic Research on Hexafluoroisopropanol" (Wang Yi, Ren Jiangang, Li Huili, Shaanxi Chemical Industry, 1997 (9) : 32-33) The reported product yield is less than 90%, indicating that there is still a large gap between the activity of the nickel-chromium-copper catalyst and the industrial scale-up production

Method used

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  • Catalyst for preparing hexafluoroisopropanol by gas-phase catalytic hydrogenation of hexafluoroacetone hydrate, its preparation method and application
  • Catalyst for preparing hexafluoroisopropanol by gas-phase catalytic hydrogenation of hexafluoroacetone hydrate, its preparation method and application

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Embodiment 1

[0031] The pretreatment of embodiment 1 carrier activated carbon

[0032] Configure 500ml of nitric acid solution with a mass percentage of 30% in proportion, weigh 150g of coconut shell activated carbon and add it to the nitric acid solution, heat up to 90°C, stir and reflux for 2.0h, cool down to room temperature, wash with deionized water until the pH value of the eluate Constant, vacuum drying at 100°C for 4.0h for later use.

Embodiment 2

[0033] Embodiment 2Pd-Cu-K / C catalyst preparation and activity evaluation

[0034]Take by weighing 0.1g KCl, add 10g deionized water to dissolve, add the activated carbon carrier that 10g embodiment 1 is processed in the solution, impregnate 10.0h, 90 ℃ of vacuum drying 5.0h, then weigh 6.0g chloropalladic acid aqueous solution (palladium's Mass percent content 2.55%), 1.35gCuCl 2 2H 2 O, add 4.0g deionized water to make a mixed solution, add activated carbon impregnated with K to the solution, impregnate for 10.0h, vacuum dry at 90°C for 5.0h, and then roast at 500°C for 3.0h for later use.

[0035] Weigh 3.0ml of the prepared catalyst sample and load it into a fixed-bed reactor, inject a hydrogen-nitrogen mixed gas for temperature reduction, the hydrogen ratio is 30%, the reduction temperature is 250°C, the reduction time is 2h, and the reducing gas space velocity is 500h -1 . After the reduction, the gas-phase catalytic hydrogenation reaction is carried out, the vaporiza...

Embodiment 3

[0036] Embodiment 3Pd-Cu-La / C catalyst preparation and activity evaluation

[0037] Weigh 0.31gLa(NO 3 ) 3 ·6H 2 O, 0.38gCu(NO 3 ) 3 ·3H 2 O, add 10 g of deionized water to dissolve, add the activated carbon carrier treated in Example 1 to the mixed solution, impregnate for 12.0 h, and vacuum dry at 90° C. for 5.0 h. Then take by weighing 8.0g chloropalladic acid aqueous solution (the mass percent composition of palladium 2.55%), add 2.0g deionized water and make solution, add the gac that has impregnated La before in the solution, Cu, dipping 24.0h, 90 ℃ Vacuum-dry for 5.0h, and then bake at 300°C for 5.0h for later use.

[0038] Catalyst reduction and activity evaluation methods are the same as in Example 2, wherein the proportion of hydrogen in the reducing gas is 10%, the reduction temperature is 180°C, the reduction time is 3h, and the space velocity of the reducing gas is 800h -1 . After the reduction, the gas-phase catalytic hydrogenation reaction is carried out...

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Abstract

The invention discloses a catalyst used for gas phase catalytic hydrogenation of a hexafluoroacetone hydrate for preparing hexafluoroisopropanol. The catalyst comprises a first catalyst, a second catalyst and a carrier, wherein the first catalyst consists of palladium and copper; the second catalyst is selected from one or the combination of K, La and Bi; and the catalyst is loaded on an active carbon carrier. The invention further discloses a preparation method of the catalyst and application of the catalyst to gas phase catalytic hydrogenation of the hexafluoroacetone hydrate for preparing hexafluoroisopropanol. The catalyst prepared with the method has the advantages of high catalytic hydrogenation activity, high hexafluoroisopropanol selectivity, superior catalyst stability, mild reaction condition, simple preparation process, and the like.

Description

technical field [0001] The invention belongs to a catalyst for preparing hexafluoroisopropanol by gas-phase catalytic hydrogenation of hexafluoroacetone hydrate. Background technique [0002] Hexafluoroisopropanol (HFIP) is a new type of fluorine-containing compound and a fluorine-containing alcohol with great application value. It is easily miscible with water and many organic solvents, has good thermal stability, and has good permeability to ultraviolet light. These characteristics make HFIP an ideal solvent in many polymerization systems, and it is also used as an advanced cleaning agent for the manufacture and cleaning of cutting-edge instruments and equipment. HFIP can also dissolve amino acid macromolecules very well, and the damage to protein natural fibers is far less than other solvents, so it can also be used as a spinning solvent for regenerated silk. At the same time, it is also widely used in the synthesis of anesthetics, pesticides, and medicines, such as the...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C31/38C07C29/145
Inventor 刘武灿徐卫国
Owner 中化蓝天氟材料有限公司
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