Nuclear-shell-type catalyst, synthesis method thereof, and method for preparing gamma-valerolactone through catalyzing of levulinic acid by nuclear-shell-type catalyst

A technology of levulinic acid and catalyst, which is applied in the field of preparing γ-valerolactone by hydrogenation of levulinic acid, can solve the problems of poor catalyst stability, poor catalyst reuse performance, easy agglomeration and loss of active material metals, and prevents sintering. or bleed, optimum conversion and selectivity, inhibition of sintering and bleed

Inactive Publication Date: 2019-12-10
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the catalysts for the hydrogenation of levulinic acid to synthesize γ-valerolactone mainly include noble metal Ru, Rh, Pt, Pd, Au-based catalysts and non-noble metal Ni, Cu, Co-based catalysts. U.S. Patent US20030055270 discloses a supported noble metal catalyst to catalyze Heating levulinic acid to prepare 5-methylbutyrolactone (also known as 5-valerolactone or γ-valerolactone), the metal catalyst is supported on the catalyst carrier, and the catalyst carrier is selected from carbon, SiO 2 or Al 2 o 3 , the most preferred catalyst support is oxidation stable carbon; Chinese patent CN109651304A adopts Ag / ZrO 2 As a catalyst, it catalyzes the hydrogenation of levulinic acid to prepare gamma-valerolactone. The above-mentioned catalysts are all supported catalysts. Although they improve the yield of gamma-valerolactone to a certain extent, the stability of the catalyst itself is relatively poor. The active material metal is easy to agglomerate and lose during the reaction, and the reusability of the catalyst is poor

Method used

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  • Nuclear-shell-type catalyst, synthesis method thereof, and method for preparing gamma-valerolactone through catalyzing of levulinic acid by nuclear-shell-type catalyst
  • Nuclear-shell-type catalyst, synthesis method thereof, and method for preparing gamma-valerolactone through catalyzing of levulinic acid by nuclear-shell-type catalyst
  • Nuclear-shell-type catalyst, synthesis method thereof, and method for preparing gamma-valerolactone through catalyzing of levulinic acid by nuclear-shell-type catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Core-shell catalyst Pd@mSiO 2 One-pot synthetic method for

[0031] S 1 1. Mix 0.12g CTAB and 45mL deionized water in a 150mL three-necked flask, stir and heat at room temperature to 80°C, and keep it for 30min, then add 5mL 0.02mol / L K 2 PdCl 4 solution, after continuing to stir for 10min, the solution changed from colorless and transparent to orange-red, and NaBH was added dropwise 4 Aqueous solution, continue to stir for 30min, obtain metal Pd colloidal solution;

[0032] S 2 1. Add 0.5mol / L NaOH solution to the metal Pd colloidal solution, adjust the pH value of the solution to 10, then dropwise add 0.2mLTEOS and 1.8mL methanol mixed solution to initiate the polymerization reaction of silica gel, and centrifuge to obtain Pd@SiO 2 product and dried overnight at 60 °C;

[0033] S 3 , the dried Pd@SiO 2 Roasting in a muffle furnace, the temperature was raised to 500°C at a rate of 5°C / min during firing, and the firing time at 500°C was 6h, and then 60...

Embodiment 2

[0036] Example 2 Core-shell catalyst Rh@mSiO 2 One-pot synthetic method for

[0037] S 1 , Mix 0.12g CTAB and 45mL deionized water in a 150mL three-neck flask, stir and heat at room temperature to 80°C, and keep it for 30min, then add 5mL0.02mol / L Na 2 RhCl 4 solution, after continuing to stir for 10min, the solution changed from colorless and transparent to orange-red, and NaBH was added dropwise 4 Aqueous solution, continue to stir for 30min, obtain metallic Rh colloidal solution;

[0038] S 2 1. Add 0.5mol / L NaOH solution to the metallic Rh colloidal solution, adjust the pH value of the solution to 11, then dropwise add a mixed solution of 0.2mLTEOS and 1.8mL methanol to initiate the polymerization reaction of silica gel, and centrifuge to obtain Rh@SiO 2 product and dried overnight at 60 °C;

[0039] S 3 , the dried Rh@SiO 2 Roasting in a muffle furnace, the temperature was raised to 500°C at a rate of 5°C / min during firing, and the firing time at 500°C was 6h, and...

Embodiment 3

[0040] Example 3 Core-shell catalyst Pt@mSiO 2 One-pot synthetic method for

[0041] S 1 1. Mix 0.12g CTAB and 45mL deionized water in a 150mL three-neck flask, stir and heat at room temperature to 80°C, and keep it for 30min, then add 5mL0.02mol / L K 2 PtCl 4 solution, after continuing to stir for 10min, the solution changed from colorless and transparent to orange-red, and NaBH was added dropwise 4 Aqueous solution, continue to stir for 30min, obtain metal Pt colloidal solution;

[0042] S 2 1. Add 0.5mol / L NaOH solution to the metal Pt colloidal solution, adjust the pH value of the solution to 10, then dropwise add 0.2mLTEOS and 1.8mL methanol mixed solution to initiate the polymerization reaction of silica gel, and centrifuge to obtain Pt@SiO 2 product and dried overnight at 60 °C;

[0043] S 3 , the dried Pt@SiO 2 Roasting in a muffle furnace, the temperature was raised to 500°C at a rate of 5°C / min during firing, and the firing time at 500°C was 6h, and then 60mL / ...

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Abstract

The invention relates to the technical field of hydrogenation preparation of gamma-valerolactone through levulinic acid, and discloses a nuclear-shell-type catalyst, a synthesis method thereof, and amethod for preparing gamma-valerolactone through catalyzing of levulinic acid by the nuclear-shell-type catalyst. According to the prepared nuclear-shell-type catalyst M@mSiO2, the core is metal, a shell is of a mesoporous SiO2 structure, and the catalyst can catalyze the levulinic acid to conduct hydrogenation preparation to obtain the gamma-valerolactone. The nuclear-shell-type catalyst M@mSiO2synthetized through the method catalyzes the evulinic acid to prepare the gamma-valerolactone, and the high catalyst stability, catalytic activity and reusability are achieved.

Description

technical field [0001] The present invention relates to hydrogenation of levulinic acid to prepare gamma-valerolactone, in particular to a core-shell catalyst, a synthesis method thereof, and a method for preparing gamma-valerolactone by catalyzing levulinic acid. Background technique [0002] Environmental protection and efficient use of natural resources are currently sustainable options for transforming our society into a greener future. The utilization of biomass or biological products is becoming crucial not only for the development of efficient and environmentally sound technologies, but also for the utilization of agricultural and forestry wastes. Levulinic acid is considered an important bio-based platform chemical that can be easily and inexpensively produced by simple hydrolysis of lignocellulose. A series of valuable chemical substances can be obtained by hydrogenation of levulinic acid, such as γ-valerolactone, valeric acid and 2-methyltetrahydrofuran, among whi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/46B01J23/42B01J35/08C07D307/33
CPCB01J23/42B01J23/44B01J23/464B01J35/0013B01J35/006B01J35/0086B01J35/08C07D307/33Y02P20/584
Inventor 刘悦吕明鑫于世涛刘仕伟李露解从霞于海龙吴琼刘毓翔
Owner QINGDAO UNIV OF SCI & TECH
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