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Pd/SiO2 catalyst and preparation method and application thereof

A catalyst and co-catalyst technology, applied in the direction of physical/chemical process catalysts, carbon-based compound preparation, chemical instruments and methods, etc., can solve problems such as difficult to obtain, high reactivity, etc., to reduce residence time, improve selectivity, Overcoming the effect of intermittent liquid phase hydrogenation process production operation

Active Publication Date: 2014-02-12
SHANDONG NHU PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Activated carbon is mainly composed of micropores, and the number of mesopores is small. Therefore, when activated carbon is used as a carrier, it is difficult to obtain high reactivity; at the same time, the "restricted reaction" of FA in the smaller catalyst particle pores may make PA Easier to overhydrogenate to by-product alcohols

Method used

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  • Pd/SiO2 catalyst and preparation method and application thereof
  • Pd/SiO2 catalyst and preparation method and application thereof
  • Pd/SiO2 catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 0.52ml of palladium chloride-hydrochloric acid solution (palladium chloride concentration of 0.08g / ml) to 50ml of deionized water, then add 1.5g of citric acid, wait for it to dissolve, and mix with the palladium chloride-hydrochloric acid solution. Pour 25g of 6-8 mesh spherical silica gel particles into it and soak for 2 hours. The above mixture was dried on a rotary evaporator at 50°C and 0.09MPa for 3 hours, and then at 80°C and 0.09MPa for 2 hours. The dried catalyst was calcined in a muffle furnace at 400° C. for 3 hours to obtain catalyst A. The weight content of metal Pd is 0.1%, and the rest is silica gel support; the obtained catalyst is spherical particles of 6-8 mesh, the average particle strength is 8.3Kg / particle; its specific surface area is 213.5m 2 / g, the most probable pore diameter is 19.6nm, and the pore volume is 1.01ml / g.

Embodiment 2

[0042] The preparation method of catalyst B is the same as that of Example 1, but the carrier used is 6-8 mesh block silica gel particles. The weight content of the metal Pd is 0.1%, and the rest is silica gel support; the obtained catalyst is 6-8 mesh block particles, the average particle strength is 3.1Kg / particle; its specific surface area is 166.2m 2 / g, the most probable pore size is 23.4nm, and the pore volume is 0.98ml / g.

Embodiment 3

[0044] Add 1.56ml of palladium chloride-hydrochloric acid solution (palladium chloride concentration of 0.08g / ml) to 50ml of deionized water, then add 1.5g of ethylenediamine, wait for it to dissolve, and mix with the palladium chloride-hydrochloric acid solution, Pour 25g of 6-8 mesh lumpy silica gel particles into it and soak for 2 hours. The above mixture was dried on a rotary evaporator at 50°C and 0.09MPa for 1 hour, and then at 80°C and 0.09MPa for 2 hours. The dried catalyst was calcined in a muffle furnace at 400°C for 3 hours to obtain catalyst C. The weight content of metal Pd is 0.5%, and the rest is silica gel support; the obtained catalyst is spherical particles of 6-8 mesh, the average particle strength is 4.0Kg / particle; its specific surface area is 220.1m 2 / g, the most probable pore diameter is 18.6nm, and the pore volume is 0.97ml / g.

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Abstract

The invention discloses a Pd / SiO2 catalyst and a preparation method and application thereof. The Pd / SiO2 catalyst comprises the following components: 98-99.99% of silicon dioxide carrier, 0.01-1% of palladium metal component, and 0-1% of promoter, wherein the silicon dioxide carrier is a spheroidal or block silica gel particle, the specific surface area is 150-300m<2> / g, the most probable pore diameter is 15-30nm, the pore volume is 0.8-1.2ml / g, the particle size is 4-18 mesh, the average value of particle strength is greater than 1kg per particle, and the promoter is selected from one or a few of alkali metal, alkaline-earth metal, transition metal and rear earth metal. The catalyst not only has high catalytic activity, but also can be used for solving the problem of excessive hydrogenation of the reaction product caused by internal diffusion limitation, and is especially suitable for continuous liquid phase selective hydrogenation of 6,10,14-trimethyl-13-alkene-2-pentadecanone with large molecular weight in a fixed bed reactor.

Description

Technical field [0001] The invention belongs to the field of catalytic hydrogenation, and specifically relates to a Pd / SiO 2 Catalyst and its preparation method and application. Background technique [0002] Hexahydrofarnesyl acetone (6,10,14-trimethyl-2-pentadecanone, PA) is slightly sweet and smooth. It is an important chemical for the preparation of plant alcohols and isophytol, and then vitamin E Intermediate. At present, several PA synthetic routes in the industry need to go through the selective catalytic hydrogenation process of 6,10,14-trimethyl-13-en-2-pentadecanone (FA-4H) to obtain PA (The reaction process is like figure 1 Shown). [0003] by figure 1 It can be seen that the C=C double bond in FA-4H undergoes selective hydrogenation to form the product PA, while the C=O double bond in PA is hydrogenated, that is, the reaction (2) produces by-product 6,10,14-trimethyl 2-pentadecanol (PA-alcohol); a small amount of the C=O double bond in FA-4H will also be hydrogenated ...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/63C07C49/04C07C45/62
Inventor 江大好张群峰梁秋霞李小年陈为超李雷益梁百安
Owner SHANDONG NHU PHARMA
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