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Preparation method of gamma-valerolactone

A technology of valerolactone and catalyst, which is applied in the application field of metal catalysts in the preparation of γ-valerolactone, which can solve the problems of reduction of catalytic active sites, agglomeration of metal nanoparticles, low catalyst activity, etc., and achieve increased recyclability The effect of frequency reduction, reduction of agglomeration and reduction of migration

Active Publication Date: 2017-06-20
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] From the above, it can be seen that in the reaction of hydrogenation of levulinic acid and its derivatives to γ-valerolactone, the catalyst activity is low and the phenomenon of easy deactivation is common, which is mainly due to the loss of active components in the recycling process, resulting in The reduction of catalytic active sites; for solid-phase catalysts, the aggregation of metal nanoparticles and by-products covering the surface of the catalyst may also lead to carbon deposition.

Method used

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  • Preparation method of gamma-valerolactone
  • Preparation method of gamma-valerolactone
  • Preparation method of gamma-valerolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] First add 0.1g RuCl 3 ·nH 2 O was dissolved in 5 g of deionized water, impregnated with 1 g of SBA-15, and dried overnight to obtain RuCl 3 / SBA-15 template; then dissolve 1.25g glucosamine hydrochloride in 5g deionized water, add 0.5ml concentrated sulfuric acid, impregnate RuCl 3 / SBA-15 template; dry at 100°C for 6 hours, and dry at 160°C for 6 hours; then dissolve 0.8g of glucosamine hydrochloride in 3g of water, add 3 drops of concentrated sulfuric acid, and impregnate RuCl again 3 / SBA-15 template; dry at 100°C for 6h, dry at 160°C for 6h; finally, under the protection of inert gas, calcine at 850°C for 3h to obtain a black powder, then remove the silicon template with 10wt% HF, and mix with water-absolute ethanol The solution was washed until neutral, and dried in vacuum at 110°C for 24 hours. The catalyst prepared by the embedding method is marked as Ru-NOMC, and the catalyst prepared in this example is marked as 5% Ru-NOMC.

[0047] The TEM image of 5% Ru-NO...

Embodiment 2

[0049] 0.1g RuCl 3 ·nH 2 O was dissolved in 5 g of deionized water, impregnated with 1 g of SBA-15, and dried overnight to obtain RuCl 3 / SBA-15 template; then dissolve 1.25g glucosamine hydrochloride in 5g deionized water, add 0.5ml concentrated sulfuric acid, impregnate RuCl 3 / SBA-15 template; dry at 100°C for 6h, 160°C for 6h; then under the protection of inert gas, calcined at 850°C for 3h to obtain a black powder, then remove the silicon template with 10wt% HF, and mix with water-absolute ethanol The solution was washed until neutral, and dried in vacuum at 110°C for 24 hours.

[0050] In the catalyst prepared in this embodiment, the average particle diameter of the Ru nanoparticles is 1.53±0.31 nm.

Embodiment 3

[0052] 0.1g RuCl 3 ·nH 2 O was dissolved in 5 g of deionized water, impregnated with 1 g of SBA-15, and dried overnight to obtain RuCl 3 / SBA-15 template; then dissolve 1.25g glucosamine hydrochloride in 5g deionized water, add 0.5ml concentrated sulfuric acid, impregnate RuCl 3 / SBA-15 template; dry at 160°C for 12h; then dissolve 0.8g of glucosamine hydrochloride in 3g of water, add 3 drops of concentrated sulfuric acid, and impregnate RuCl again 3 / SBA-15 template; dry at 160°C for 12h; finally, under the protection of inert gas, calcine at 850C for 3h to obtain a black powder, then remove the silicon template with 10wt% HF, and wash with water-absolute ethanol mixed solution until neutral, Vacuum drying at 110°C for 24 hours is enough.

[0053] In the catalyst prepared in this embodiment, the average particle diameter of the Ru nanoparticles is 1.44±0.29 nm.

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Abstract

The invention discloses a preparation method of gamma-valerolactone. The gamma-valerolactone is prepared from acetylpropionic acid through catalytic hydrogenolysis reaction; an adopted catalyst is prepared by taking nitrogen-doped mesoporous carbon as a carrier and taking transition element M as an active component through an embedding method. The invention discloses the preparation method of the gamma-valerolactone; the conversion rate of the acetylpropionic acid and the selectivity of the gamma-valerolactone can be remarkably improved when the nitrogen-doped mesoporous carbon loaded transition element catalyst prepared through the embedding method is adopted; more importantly, the catalyst has extremely high circulating stability; after the catalyst is repeatedly used for 5 times, the extremely high conversion rate and selectivity can still be kept.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to the application of a metal catalyst prepared by an embedding method in the preparation of gamma-valerolactone. Background technique [0002] Fossil energy such as coal, natural gas and oil is the foundation of human survival and development. With the depletion of fossil resources, the deterioration of the ecological environment, global warming and rapid economic development, it is urgent to find a new type of renewable energy. Replace non-renewable fossil energy. Biomass has become the main source of renewable fuels and chemicals due to its abundant reserves, wide range of sources, and low price. Among the many biomass-based chemicals, γ-valerolactone (GVL) can be used as flavor compounds, solvents, food additives and liquid fuels; it can undergo a series of reactions to generate products with added value, such as 2-methyl Tetrahydrofuran (2-MTHF), 1,4-pentanediol, 5-nonanone, ...

Claims

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Application Information

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IPC IPC(8): C07D307/33B01J27/24
CPCB01J27/24C07D307/33
Inventor 魏作君刘海燕苏传敏楼炯涛刘迎新
Owner ZHEJIANG UNIV
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