Inorganic membrane catalyst and preparation method and application thereof

An inorganic membrane and catalyst technology, applied in the preparation of organic compounds, the preparation of amino compounds, chemical instruments and methods, etc., can solve the problems of low efficiency and conversion rate, difficult separation of products and catalyst impurities, and achieve uniform loading and strong acidity. , the effect of rapid coordination

Active Publication Date: 2021-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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Problems solved by technology

[0006] Aiming at the problems of low efficiency and conversion rate of amination reaction in the prior art and difficult separation of product and catalyst impurities, the present invention provides an inorganic membrane catalyst and its preparation method, and applies the catalyst to the reaction of polyether polyols and liquid ammonia In the preparation of polyether amine, methyl tert-butyl ether and hydrocyanic acid react to prepare tert-butylamine and other amination reactions, the catalyst activity and stability are good, the reaction efficiency and reaction conversion rate are high, the product selectivity is high, and good results have been obtained. The response effect

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  • Inorganic membrane catalyst and preparation method and application thereof

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preparation example Construction

[0030] The following specifically introduces the preparation process of the inorganic membrane catalyst of the present invention: one, 200~250g zirconium n-butoxide (Zr(OBui) 4 ) was dissolved in 250mL ethanol to prepare a zirconium n-butoxide ethanol solution with a molar concentration of 2-4mol / L. Two, be that the nitric acid aqueous solution of 5~8mol / L is added dropwise the zirconium n-butoxide ethanolic solution that step one obtains with molar concentration, obtain transparent sol, then add polyvinyl alcohol and polyethylene glycol of 4~8g respectively, continue to stir, A sol with a certain viscosity is further obtained. Third, the α-Al 2 o 3 Immerse the ceramic tube vertically into the sol obtained in step 2 for 1 to 2 minutes, then pull it out at a pulling speed of 10 to 15 cm / min, then heat-treat it at 100°C for 5 to 10 minutes, repeat the above dipping and pulling and heat treatment for 3 to 5 times, and then calcined at 1000 to 1200° C. for 3 to 6 hours. 4. Seq...

Embodiment 1

[0034] In this example, an inorganic membrane catalyst was prepared and applied to the amination reaction of methyl tert-butyl ether and hydrocyanic acid to prepare tert-butylamine:

[0035] Preparation of inorganic membrane catalysts:

[0036] (1) Dissolve 200 grams of zirconium n-butoxide in 250 mL of ethanol to prepare a solution of zirconium n-butoxide in ethanol, and add an aqueous solution of nitric acid with a molar concentration of 5 mol / L to the above solution dropwise to obtain a transparent sol, and then add 5 g of Continue to stir polyvinyl alcohol and 4g polyethylene glycol to further obtain a sol with a certain viscosity, the stirring temperature is 40°C, and the stirring speed is 200r / min;

[0037] (2) Add α-Al 2 o 3 Immerse the ceramic tube vertically into the sol obtained in step (1) for 2 minutes, pull it out at a pulling speed of 10cm / min, and then heat-treat it at 100°C for 10 minutes, repeat the above steps of dipping, pulling and heat treatment 5 times...

Embodiment 2

[0042] In this example, an inorganic membrane catalyst was prepared and applied to the amination reaction of methyl tert-butyl ether and hydrocyanic acid to prepare tert-butylamine:

[0043] Preparation of inorganic membrane catalysts:

[0044] (1) Dissolve 200 grams of zirconium n-butoxide in 250 mL of ethanol to prepare a solution of zirconium n-butoxide in ethanol; add an aqueous solution of nitric acid with a molar concentration of 6 mol / L to the above solution dropwise to obtain a transparent sol, and then add 5 g of Continue stirring polyvinyl alcohol and 5g polyethylene glycol to further obtain a sol with a certain viscosity, the stirring temperature is 40°C, and the stirring speed is 200r / min;

[0045] (2) Add α-Al 2 o 3 Immerse the ceramic tube vertically into the sol obtained in step (1) for 1 minute, pull it out at a pulling speed of 13 cm / min, and then heat-treat it at 100°C for 8 minutes, repeat the above steps of dipping, pulling and heat treatment 5 times, an...

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Abstract

The invention provides a preparation method of an inorganic membrane catalyst. The preparation method comprises the following steps: mixing an acidic ethanol solution of zirconium n-butoxide with PVA and PEG to obtain sol, dipping an inert carrier into the sol, preparing a gel-state membrane by a dip-coating method, drying and roasting, and sequentially impregnating the coated inert carrier by using a silver nitrate sulfuric acid solution and one solutions elected from a palladium nitrate sulfuric acid solution, a platinum nitrate sulfuric acid solution and a rhodium nitrate sulfuric acid solution to obtain the inorganic membrane catalyst which is used in amination reaction. According to the inorganic membrane catalyst, the ZrO2 membrane is used as a carrier, different metal solutions are respectively impregnated according to a certain sequence under the conditions of pressure reduction, ultrasonic vibration and a certain impregnation temperature, and the impregnation solution is continuously boiled, so that active components of the catalyst are uniformly loaded and have high dispersity, SO4<2-> and metal ions on the surface of oxide are rapidly and uniformly coordinated, and the catalyst has relatively strong acidity, relatively high activity and relatively good stability.

Description

technical field [0001] The present invention relates to a kind of inorganic membrane catalyst and its preparation method and application, especially relate to ZrO 2 The membrane is an inorganic membrane catalyst whose carrier supports active components, and its application in amination reaction. Background technique [0002] Conventional catalysts are prepared by uniformly dispersing active components and cocatalysts, and loading them on selected carriers by means of impregnation and chemical deposition. Usually, the catalyst supports are particles of different materials, shapes and sizes, with a certain specific surface area and suitable pore structure, which greatly reduces the sintering and aggregation of active components and enhances the mechanical strength of the catalyst. The carrier can sometimes provide additional active centers, which can have different activities through the overflow and interaction between the active component and the carrier. The membrane cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/66C07C209/00C07C211/07C08G65/325
CPCB01J23/66B01J23/002B01J35/0066C07C209/00C08G65/3255C07C211/07Y02P20/584
Inventor 刘野赵亮王岩于庆志党雷
Owner CHINA PETROLEUM & CHEM CORP
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