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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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  • Summary
  • 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 tank-type gap reactors, which brings troubles in catalyst separation and instability in the degree of hydrogenation of products

Method used

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  • Method for preparing small spherical Pd catalyst

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Experimental program
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Embodiment 1

[0030] (1) Put the macroporous finished silica gel pellets into a buffer solution composed of C.P grade glacial acetic acid, C.P grade ammonium acetate and pure water after vacuum drying. The pH value of the buffer solution is equal to 4.9-5.1. The buffer solution and The volume ratio of the silica gel pellets is 2:1. Under nitrogen bubbling, keep warm at 45°C. After 72 hours, wash the silica gel pellets with deionized water until neutral, filter the silica gel pellets, and dry them in vacuum. (2) Submerge the dried silica gel pellets in 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 to 100:1 with 2M hydrochloric acid. Stand at normal temperature and pressure for 70 hours, stir once an hour, and filter out the pellets. (3) Put the filtered pellets into ammonia water with...

Embodiment 2

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

Embodiment 3

[0034] Synthesis of 1,4-butanediol in a fixed bed reactor. device attached figure 1 As shown, the fixed bed reactor [3] is composed of a stainless steel tube (1Cr18Ni9Ti) with a length of Ф32 mm, a length of 300 mm, and a wall thickness of 3 mm. Outflow from the cooling water outlet [4] behind the outer jacket. After filling the prepared small spherical Pd catalyst, 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, and after being heated by the tube wall, it is injected into the B end of the bottom of the reactor [3]. Hydrogen enters reactor [3] bottom B end by hydrogen inlet [2], and after mixing with 1,4-butynediol, hydrogenation is carried out under the catalysis of 30 grams of small spherical Pd catalysts prepared under the conditions of Example 1 Reaction, the 1,4-butanediol that generates overflows from the C end of the top of the reactor [3], and is collected at th...

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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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