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Supported catalyst, preparation method and application thereof

A supported catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, oxime preparation, etc., can solve the problem that it is difficult to stabilize the selectivity of cyclohexanone oxime, it cannot be widely used, and the product needs to be separated, etc. problems, achieve the effects of reducing solid and liquid waste discharge, environmental friendliness, and reducing production and operation costs

Active Publication Date: 2021-04-06
方晓亮
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  • Description
  • Claims
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Problems solved by technology

However, the supported Pd catalyst used for hydrogenation under this technology requires the presence of lead(II) oxide, and the reaction process needs to be carried out under high pressure
Because oxide lead salt is extremely unfriendly to environment, and the yield of cyclohexanone oxime of this process is only 70%, so the route of hydrogenation nitrocyclohexane to prepare cyclohexanone oxime has not been widely used
In addition, the patent (CN102125840A) provides a supported Pt catalyst with carbon nanotubes as the carrier, and exhibits good hydrogenation activity, but it is difficult for the catalyst to stabilize the selectivity of cyclohexanone oxime in the actual application process. Ketoxime is prone to deep hydrogenation to form cyclohexane hydroxylamine and cyclohexylamine, which makes the product need subsequent separation, which virtually increases the production cost

Method used

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  • Supported catalyst, preparation method and application thereof
  • Supported catalyst, preparation method and application thereof
  • Supported catalyst, preparation method and application thereof

Examples

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preparation example Construction

[0031] The invention provides a preparation method of a supported catalyst, comprising the following steps:

[0032] 1) placing the carrier in deionized water, dispersing and stirring evenly to obtain an aqueous solution dispersed with the carrier;

[0033] 2) dissolving the Pt precursor in deionized water, and adding it to the aqueous solution dispersed with the carrier obtained in step 1), fully stirring, impregnating, separating, washing, vacuum drying, and calcining in a hydrogen atmosphere for 2-6 hours, Prepare the first catalyst.

[0034] 3) Soak the first catalyst prepared in step 2) in indium nitrate aqueous solution or tin tetrachloride aqueous solution for 1-3 hours, centrifuge, vacuum-dry, and calcinate in a hydrogen atmosphere for 2-6 hours to obtain the catalyst containing Pt-In 2 o 3-x or Pt-SnO 2-x Supported catalysts with structural units.

[0035] figure 2 Contains Pt-In for the present invention 2 o 3-x The Raman test spectrum of the supported cataly...

Embodiment 1

[0044] 1-1 Preparation of Pt-In 2 o 3-x / Al 2 o 3 catalyst

[0045] 1) Weigh 1g Al 2 o 3 The solid powder was dispersed in deionized water, ultrasonically dispersed for 30 minutes, placed on a 400r / min magnetic stirrer, fully stirred evenly, and an aqueous solution dispersed with carriers was obtained;

[0046] 2) Weigh 200mg H 2 PtCl 6 Dissolve in 10mL of deionized water, drop by drop into the aqueous solution dispersed with the carrier, fully stir and impregnate overnight, centrifuge, wash with deionized water for 3 times, dry in vacuum, and calcinate at 180°C for 2-6h under hydrogen atmosphere , to prepare 1wt%Pt / Al 2 o 3 catalyst;

[0047] 3) 1wt%Pt / Al 2 o 3 The catalyst is soaked in 1mol / L indium nitrate aqueous solution for 1-3 hours, centrifuged, dried in vacuum, and calcined in a hydrogen atmosphere at 180°C for 2-6 hours to obtain 1wt% Pt-In 2 o 3-x / Al 2 o 3 Catalyst, wherein the molar ratio of Pt and In is (1:2).

[0048] 1-2 Catalytic hydrogenation...

Embodiment 2

[0051] Compared with Example 1, the difference is that the H weighed in step 1-1 2 PtCl 6 The mass is 100mg, and the Pt loading in the prepared catalyst is 0.5wt%, and other experimental conditions are the same as in Example 1.

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Abstract

The present invention provides a supported catalyst, a preparation method and applications thereof. The supported catalyst comprises two parts such as an active component and a carrier, wherein the active component is a Pt-based catalyst containing a Pt-In2O3-x or Pt-SnO2-x structure unit, and the supported catalyst is used for catalyzing nitro cyclohexane hydrogenation to prepare cyclohexanone-oxime. According to the invention, the catalyst containing Pt-In2O3-x and Pt-SnO2-x structural units has ideal nitrocyclohexane hydrogenation activity and selectivity, the preparation process of the catalyst is simple, side reactions possibly introduced can be reduced, the production and operation cost is effectively reduced, the complex degree of cyclohexanone-oxime production and the emission of solid-liquid wastes can be reduced, and the used active components are environment-friendly and pollution-free.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a catalyst containing Pt-In 2 o 3-x or Pt-SnO 2-x Supported catalyst of structural unit and its preparation method and application. Background technique [0002] Oxime is a valuable organic intermediate, which is widely used in polymers, perfumes, coatings and other fields. Typical examples include cyclohexanone oxime, an important precursor for the production of caprolactam and nylon-6, and its annual demand is as high as 3 million tons. The current commercial production of cyclohexanone oxime is mainly through the ammoxidation process of cyclohexanone. In this process, the catalytic oxidation of cyclohexane to cyclohexanone is the core technology, but the process efficiency is extremely low, and the highest single-cycle yield is only 8-10%. In addition, this process will also produce a large amount of by-product ammonium sulfate, so this approach is very uneconomical and...

Claims

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Application Information

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IPC IPC(8): B01J23/62C07C249/10C07C251/44
CPCB01J23/62B01J23/626C07C249/10C07C2601/14C07C251/44
Inventor 郑南峰周文挺刘圣杰陈洁
Owner 方晓亮
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