Method for preparing small spherical Pd catalyst

A catalyst and pellet technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of troublesome catalyst separation, unstable product hydrogenation degree, etc. Hydrogen characteristics and effects of stability control

Inactive Publication Date: 2008-05-28
上海中远化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these carriers that can be used to load Pd are all in powder form, so they can only be used in ebullating bed and ta

Method used

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  • Method for preparing small spherical Pd catalyst

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Example Embodiment

[0029] Example 1

[0030] (1) After vacuum drying, the finished large-pored silica gel pellets are put into a buffer solution composed of CP grade glacial acetic acid, CP grade ammonium acetate and pure water for pore expansion. The pH value of the buffer solution is equal to 4.9-5.1, and the buffer solution and The volume ratio of silica gel beads is 2:1. Under nitrogen bubbling, keep the temperature at 45°C, after 72 hours, wash the silica gel pellets with deionized water to neutrality, filter out the silica gel pellets, and vacuum dry. (2) Immerse the dried silica gel pellets in the palladium dichloride-hydrochloric acid solution. The solution is mixed with C.P grade concentrated hydrochloric acid and C.P grade palladium dichloride, and their weight ratio is 20:1. After the palladium dichloride is completely dissolved, it is diluted with 2M hydrochloric acid to 100:1. Place it at room temperature and pressure for 70 hours, and stir once an hour to filter out the pellets. (3) Pu...

Example Embodiment

[0031] Example 2

[0032] Except that the palladium dichloride is completely dissolved in step (2), and then diluted to 300:1 with 2M hydrochloric acid, other conditions are the same as in Example 1. The resulting small spherical Pd catalyst has physical and chemical indicators: Pd weight %: 0.1, specific surface area 160-190m 2 / g, the pore volume is 0.546cm 3 / g, the most acceptable aperture D is equal to 112.5 , Particle size 4.5-5.8mm, internal pressure strength (average) ≥ 6kg / particle.

Example Embodiment

[0033] Example 3

[0034] The fixed bed reactor synthesizes 1,4-butanediol. Device as attached figure 1 As shown, the fixed-bed reactor [3] is composed of a stainless steel tube (1Cr18Ni9Ti) with a length of Ф32mm, a length of 300mm, and a wall thickness of 3mm. After the outer jacket, it flows out from the cooling water outlet [4]. After the prepared small spherical Pd catalyst is filled, it can be used. (Design pressure is 1.6MPa)

[0035] The hydrogenation raw material 1,4-butynediol is fed into the quantitative pump [1] from the A end, heated by the pipe wall, and injected into the bottom B end of the reactor [3]. Hydrogen enters the bottom B end of the reactor [3] from the hydrogen inlet [2], and after mixing with 1,4-butynediol, hydrogenation is carried out under the catalysis of 30 g of the small spherical Pd catalyst prepared under the conditions of Example 1. During the reaction, the generated 1,4-butanediol overflows from the C end of the top of the reactor [3], is coole...

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Abstract

The invention relates to a preparation method of a globule shaped palladium catalyst for hydrogenation reactions. The load palladium-charcoal catalyst for hydrogenation reactions has the advantages of low reaction pressure, low reaction temperature, high activity and stable character of the catalyst. However, powder load palladium-charcoal usually can only be used in fluidized beds and tank stirred reactors. The globule shaped palladium catalyst takes large pore globule silica gel as the carrier, and absorbs palladium on the surface of and in the inner pores of the silica gel, thus the characteristics of original powder load palladium-charcoal catalyst are saved and the globule shape is fabricated to be applied to solid bed reactors, so that hydrogenation reactions can perform in a continuous state, thus greatly enhancing the stability of hydrogenation stability.

Description

technical field [0001] The invention relates to a preparation method of a Pd catalyst in a chemical reaction, in particular to a preparation method of a small spherical Pd catalyst used in a hydrogenation reaction. Background technique [0002] Supported Pd catalysts are widely used in the hydrogenation of various organic compounds, such as: hydrogenation of alkynes to alkenes, hydroalkylation of alkenes, hydrogenation of nitrobenzene to aniline, hydrogenation of aromatic ketones to aromatic alcohols, etc. . [0003] Usually, Pd for various hydrogenation is supported on activated carbon, alumina, PVP, titania, etc. However, these supports that can be used to load Pd are all in powder form, so they can only be used in ebullating bed and tank-type gap reactors, which brings troubles in catalyst separation and instability in the degree of hydrogenation of products. Contents of the invention [0004] The purpose of the present invention is to aim at the deficiencies in the p...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J21/08B01J35/08B01J35/04
Inventor 陈唐
Owner 上海中远化工有限公司
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