Catalytic hydrogenation catalyst as well as preparation and application thereof in tetrahydrofarnesyl acetone selective hydrogenation reaction

A catalytic hydrogenation and catalyst technology, applied in the direction of metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, carbon-based compound preparation, etc., can solve low activity, active site reduction, catalyst activity impact, etc. problem, to achieve the effect of simple preparation method, improved activity, and improved metal utilization rate

Active Publication Date: 2019-01-11
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst activity is also affected by the pore size
The pore size of the carrier is small, and the small pore size makes it difficult for large reactant molecules to enter the pores, that is, the steric hindrance effect (or the shape selection and confinement effect of the channel), and the catalytic reaction can only occur on the surface of the catalyst, and it is effective if the interior is not fully utilized. The active sites are reduced, resulting in low activity

Method used

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  • Catalytic hydrogenation catalyst as well as preparation and application thereof in tetrahydrofarnesyl acetone selective hydrogenation reaction
  • Catalytic hydrogenation catalyst as well as preparation and application thereof in tetrahydrofarnesyl acetone selective hydrogenation reaction
  • Catalytic hydrogenation catalyst as well as preparation and application thereof in tetrahydrofarnesyl acetone selective hydrogenation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Weigh 1.5g of water-soluble methyl orthosilicate and 0.05g of n-butyl titanate into the distillation flask, add 20g of activated carbon after fully stirring, then add dropwise an aqueous solution of tetramethylammonium hydroxide (containing Tetramethylammonium hydroxide (0.075g), distilled at 95°C to separate the hydrolyzate, and then heated the solid matter in the flask at 180°C for 12h.

[0036] Get the activated carbon that above-mentioned method makes (through detection mesopore ratio 70%, micropore ratio 30%, size is not more than 1cm) 1g and 15ml deionized water and 3ml methyl alcohol make mixed slurry, stir 15min, get the palladium concentration of 10mL as Drop 0.002g / mL chloropalladium acid solution into the mixture, place it under a UV lamp at 275w and 386nm for light and stir for 20min, then take out the mixed slurry, wash it with water until it is neutral, and dry it in an oven at 60°C for 24 hours . Detected SiO 2 Content 7.5%, TiO 2 The content is 0.15%, ...

Embodiment 14

[0047] The catalyst of Example 1 was loaded into a tubular reactor with an inner diameter of 20 cm, and the air was replaced with nitrogen, and then the nitrogen was replaced with hydrogen. According to tetrahydrofarnesyl acetone and methanol total volume and hydrogen volume ratio is 1:1, the ratio of tetrahydro farnesyl acetone and methyl alcohol is 2g:5ml, tetrahydro farnesyl acetone is dissolved in methanol solvent, by high pressure The liquid pump is pumped into the mixing tube in front of the reaction tube, mixed with the hydrogen, and then enters the tubular reactor loaded with the catalyst. The hydrogen pressure is set at 1MPa, the temperature is 50°C, and the liquid space velocity is 50min -1 , turn on the lighting device, set the light power to 325nm, the power to 225W, and the radiation intensity to 3820μW / cm 2 , start the reaction, after the one-way reaction, pass through the gas-liquid separation device, the unreacted hydrogen is recycled, and the liquid product is...

Embodiment 15～27

[0049] Examples 15-27 are based on the fixed-bed catalytic evaluation operation steps in Example 14. The fixed-bed catalytic hydrogenation catalysts prepared in Examples 1-13 and Comparative Examples 1-2 are selected for catalyst reaction. The specific parameters are shown in Table 2.

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Abstract

The invention discloses a catalytic hydrogenation catalyst as well as preparation and application thereof in a tetrahydrofarnesyl acetone selective hydrogenation reaction. The catalyst is composed ofan activated carbon carrier coated with a modification coating and metallic quantum dots supported onto the carrier, wherein the metal is palladium; the particle size of the metallic quantum dots ranges from 3nm to 6nm; the activated carbon is random or formed granular active carbon and has the size of not more than 1cm; the pore structure of the activated carbon coated with the modification coating mainly includes a mesoporous structure, the microporous proportion is reduced to 10% or less, and composition materials of the modification coating comprise titanium dioxide, silicon dioxide and titanium silicate. The invention discloses application of the catalytic hydrogenation catalyst in a reaction of synthesizing hexahydrofarnesyl acetone through selective hydrogenation of tetrahydrofarnesyl acetone. The application has the characteristics of being additive-free, high in conversion rate, excellent in selectivity, high in hydrogenation reaction rate, excellent in stability, long in service life and recyclable in hydrogen.

Description

(1) Technical field [0001] The invention relates to a fixed-bed catalytic hydrogenation catalyst and its preparation and application, in particular to the application of the catalyst in the fixed-bed catalytic tetrahydrofarnesyl acetone selective hydrogenation reaction. (2) Technical background [0002] 6,10,14-Trimethyl-2-pentadecanone (hexahydrofarnesylacetone, PA) is an important chemical intermediate for the preparation of vitamin E. The demand for VE has increased significantly. At present, PA is mainly prepared by 6,7-dihydrolinalool or 1,2-dehydrolinalool in industry. But in these existing several PA synthesis routes, all need finally through 6,10,14-trimethyl-13-ene-2-pentadecanone (tetrahydrofarnesyl acetone, FA-4H) Catalytic hydrogenation process can get PA, so the production of tetrahydrofarnesyl acetone also increases year by year. Therefore, it is of great significance to develop a green catalytic hydrogenation process for industrial production requirements. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J35/02B01J35/10C07C45/62C07C49/04
CPCB01J23/002B01J23/44B01J35/023B01J35/1004B01J2523/00C07C45/62B01J2523/41B01J2523/47B01J2523/824C07C49/04
Inventor 卢春山王昊朱倩文周烨彬张雪洁季豪克张群峰赵佳丰枫马磊许孝良李小年
Owner ZHEJIANG UNIV OF TECH
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