A catalytic hydrogenation catalyst and its preparation and application in the selective hydrogenation of tetrahydrofarnesyl acetone

A technology for catalytic hydrogenation of farnesyl acetone, applied in the field of fixed-bed catalytic hydrogenation catalysts and their preparation and application, can solve the problems of active site reduction, catalyst activity impact, low activity, etc., to improve activity and metal utilization efficiency, and the effect of improving electronic characteristics

Active Publication Date: 2021-07-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A catalytic hydrogenation catalyst and its preparation and application in the selective hydrogenation of tetrahydrofarnesyl acetone
  • A catalytic hydrogenation catalyst and its preparation and application in the selective hydrogenation of tetrahydrofarnesyl acetone
  • A catalytic hydrogenation catalyst and its preparation and application in the selective hydrogenation of tetrahydrofarnesyl acetone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 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.

[0041] 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

[0052] 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, and the hydrogen is mixed with the gas and liquid, and then enters the tubular reactor loaded with the catalyst together. 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...

Embodiment 15～27

[0054] 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 were selected for catalyst reaction. The specific parameters are shown in Table 2.

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Abstract

The invention discloses a catalytic hydrogenation catalyst and its preparation and application in the selective hydrogenation reaction of tetrahydrofarnesyl acetone. The catalyst is composed of an activated carbon carrier coated with a modified coating and metal quantum dots loaded on the carrier; the metal is palladium, and the particle size of the metal quantum dots ranges from 3 to 6 nm; the activated carbon Irregular or shaped granular activated carbon, the size of which is not greater than 1cm; the pore structure of the activated carbon coated with the modified coating is mainly mesopores, the proportion of micropores is reduced to below 10%, and the modified coating The constituent substances are titanium dioxide, silicon dioxide and titanium silicate. The invention discloses the application of the catalytic hydrogenation catalyst in the selective catalytic hydrogenation of tetrahydrofarnesyl acetone to synthesize hexahydro farnesyl acetone. The reaction rate is fast, the stability is good, the catalyst life is long and the hydrogen can be recycled.

Description

[0001] (1) Technical field [0002] 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. [0003] (2) Technical background [0004] 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...

Claims

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Application Information

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Patent Type & Authority Patents(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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