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Method for improving selectivity of citronellol synthesized through citronellal hydrogenation

A technology for citronellol and citronellal, which is applied in the field of improving the selectivity of citronellal hydrogenation to synthesize citronellol, can solve the problems of cumbersome process and low selectivity, and achieves improved selectivity, mild catalytic conditions, high efficiency and high efficiency. high yield effect

Active Publication Date: 2018-10-02
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional preparation methods often have problems such as cumbersome process and low selectivity.

Method used

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  • Method for improving selectivity of citronellol synthesized through citronellal hydrogenation
  • Method for improving selectivity of citronellol synthesized through citronellal hydrogenation
  • Method for improving selectivity of citronellol synthesized through citronellal hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of Pt@ZIF-67 catalyst

[0035] Under normal temperature and pressure, 32.84mg 2-methylimidazole, 58.205mg Co(NO 3 ) 2 ·6H 2 O and 0.3 mL pvp-dispersed methanol solution of Pt nanoparticles of about 3 nm were mixed at room temperature for 24 h, and the resulting precipitate was washed, centrifuged, and dried to obtain Pt@ZIF-67. Among them, pvp dispersed about Pt nanoparticles such as figure 1 As shown, the XRD pattern of Pt@ZIF-67 is as follows figure 2 As shown, the TEM image of the TEM image of Pt@ZIF-67 is shown in image 3 shown.

[0036] Pt@ZIF-67 as catalyst for catalytic reaction

[0037] The Pt@ZIF-67 catalyst was weighed and activated in a vacuum oven at 120°C for 10 hours, and 15 mg of the activated Pt@ZIF-67 catalyst was placed in a polytetrafluoroethylene lining, 15 mL of methanol was added as a solvent, and the catalyst was dispersed by ultrasonication for 10 minutes. uniform; then add 100 μL citronellal and a magnetic stirrer, assemble...

Embodiment 2

[0039] Preparation of Pd@ZIF-67 Catalyst

[0040] The preparation method of the Pd@ZIF-67 catalyst is the same as in Example 1, only the Pt nanoparticles are replaced with Pd nanoparticles.

[0041] The Pt@ZIF-67 catalyst was weighed and activated in a vacuum oven at 100°C for 12 hours, and 15 mg of the activated Pd@ZIF-67 catalyst was weighed in a polytetrafluoroethylene lining, and 15 mL of methanol was added as a solvent. The catalyst was evenly dispersed; then 100 μL of citronellal and a magnetic stirrer were added to assemble the autoclave and hydrogen gas was introduced. The reaction conditions were set as follows: hydrogen pressure 0.1MPa, temperature 150°C, stirring speed 800rpm, reaction time 10h. Using GC to detect citronellal and its hydrogenation products, the results are: the conversion rate is about 85%, and the selectivity of the main product citronellol is >90%.

Embodiment 3

[0043] Preparation of Pt@ZIF-8 catalyst

[0044] Under normal temperature and pressure, 15mL 2-methylimidazole (25mM), 15mL Co(NO 3 ) 2 ·6H 2 O (25 mM) and 1 mL pvp-dispersed Pt nanoparticles methanol solution of about 1 nm were mixed at room temperature for 24 h, and the resulting precipitate was washed, centrifuged, and dried to obtain Pt@ZIF-8.

[0045] Among them, the SEM image of Pt@ZIF-8 is as follows Figure 4 As shown, the TEM image of Pt@ZIF-8 is as follows Figure 5 As shown, it can be seen from the data that Pt is uniformly wrapped into MOFs, and different kinds of catalysts with good performance are obtained.

[0046] Pt@ZIF-8 as catalyst for catalytic reaction

[0047] The Pt@ZIF-8 catalyst was weighed and activated in a vacuum oven at 110°C for 11 hours in a vacuum. Weighed 15 mg of the activated Pt@ZIF-8 catalyst into a polytetrafluoroethylene lining, added 15 mL of methanol as a solvent, and ultrasonicated for 10 minutes. The catalyst was evenly dispersed;...

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Abstract

The invention discloses a method for improving selectivity of citronellol synthesized through citronellal hydrogenation. The method comprises the following steps: taking metal nano-particle @MOFs as acatalyst, performing activating treatment, and catalyzing selective hydrogenation of citronellal to produce citronellol accompanying with stirring and heating under the conditions of a hydrogen atmosphere and a pressure of 0.1-1MPa. Compared with the traditional catalytic reaction process, the method disclosed by the invention is mild in catalytic conditions and high in efficiency and yield, andhas high selectivity of the principal product citronellol. Moreover, according to the method, the nanoscale metal nano-particles are coated in the MOFs, and due to a protective effect of the MOFs structure, the metal nano-particles do not agglomerate and re-grow in the reaction process, so that the continuous high efficiency and stability of the catalyst are ensured.

Description

technical field [0001] The invention relates to the technical field of MOFs composite materials and catalysts, in particular to a method for improving the selectivity of citronellal hydrogenation to synthesize citronellol. Background technique [0002] Citronellal is a very important raw material for the preparation of various fine chemicals. The carbonyl group in the citronellal structure is selectively hydrogenated to generate the unsaturated alcohol-citronellol, which is widely used in perfume. Citronellol has a wide range of uses. It is a very important spice with a fresh rose aroma. It is usually blended with floral fragrances such as geraniol and phenylethyl alcohol, and can be used to manufacture hydroxydihydrocitronellol, hydroxy The raw material of dihydrocitronellal; it is also used in the preparation of soaps, room fresheners, etc.; citronellol can also be used in food flavors, such as soft drinks, baked goods, sugar, jelly and pudding. Citronellol, one of the r...

Claims

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Application Information

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IPC IPC(8): C07C29/141C07C33/025B01J31/22
CPCC07C29/141B01J31/1691B01J31/1815B01J31/2239B01J2531/845B01J2531/26B01J2231/645B01J35/396B01J35/393C07C33/025
Inventor 霍峰蔚张伟娜张文垒姬文兰褚慧敏张所瀛房传真孟凡辰
Owner NANJING UNIV OF TECH
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