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Method for preparing gamma-valerolactone by acetylpropionic acid catalytic hydrogenation

A technology of levulinic acid and valerolactone, applied in chemical instruments and methods, molecular sieve catalysts, physical/chemical process catalysts, etc., can solve the problems of difficulty in adapting to large-scale industrial production, harsh catalyst reaction conditions, and rapid decline in catalyst activity, etc. problems, achieve high industrial application value, improve economy and safety, and achieve high yield

Active Publication Date: 2016-02-03
SYNFUELS CHINA TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] To sum up, there are problems in the preparation of GVL by the current process, such as high cost of microbial reduction method, harsh catalyst preparation and reaction conditions in the patent of catalytic hydrogenation method, difficult recovery of catalyst, or large loading of precious metals, making it difficult to adapt to large-scale industrial production. Production
In addition, the use of non-precious metal patented methods, due to the acidity of the raw material levulinic acid itself, causes the problem of rapid decline in catalyst activity and the problem of corrosion to the reactor in gas-phase hydrogenation, which ultimately leads to higher production costs, poor efficiency, and safety. Low sex

Method used

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  • Method for preparing gamma-valerolactone by acetylpropionic acid catalytic hydrogenation
  • Method for preparing gamma-valerolactone by acetylpropionic acid catalytic hydrogenation
  • Method for preparing gamma-valerolactone by acetylpropionic acid catalytic hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] (1) Preparation of catalyst

[0048] Weigh 0.05g RuCl into a 100mL beaker 3 ·3H 2 O, dissolved with 8g of secondary water, shake well, add carrier γ-Al to the solution 2 o 3 6g, mixed evenly, soaked at room temperature for 8h, dried at 80°C for 12h, calcined at 300°C in an air atmosphere, and then reduced in a hydrogen atmosphere kettle at 130°C for 2h to obtain the ruthenium-based catalyst provided by the present invention (the Ru loading capacity is 0.32%).

[0049] (2) Catalytic performance test

[0050] Add 10g of water as a solvent, 8g of levulinic acid and 0.10g of the above catalyst in the autoclave, seal the autoclave, fill it with 4MPa hydrogen, react at 130°C for 3h, cool to room temperature after the reaction, and slowly depressurize to the atmosphere Pressure, open the autoclave to sample, GC detection, LA conversion rate 30.5%, GVL selectivity 99.9%.

[0051] Wherein, the structure of the resulting product γ-valerolactone (GVL) is confirmed by GC-MS da...

Embodiment 2

[0053] (1) Preparation of catalyst

[0054] Weigh 0.05g RuCl into a 100mL beaker 3 ·3H 2 O, dissolve with 8g of secondary water, shake well, add carrier ZSM-56g to the solution, mix evenly, impregnate at room temperature for 8h, dry at 80°C for 12h, roast at 300°C in an air atmosphere, and then reduce in a hydrogen atmosphere kettle at 130°C for 2h , the ruthenium-based catalyst provided by the present invention (Ru loading is 0.32%) can be obtained.

[0055] (2) Catalytic performance test

[0056] Add 10g of water as a solvent, 8g of levulinic acid and 0.10g of the above catalyst in the autoclave, seal the autoclave, fill it with 4MPa hydrogen, react at 130°C for 3h, cool to room temperature after the reaction, and slowly depressurize to the atmosphere Pressure, open the autoclave to sample, GC detection, LA conversion rate 45.5%, GVL selectivity 99.9%.

Embodiment 3

[0058] (1) Preparation of catalyst

[0059] Weigh 0.05g RuCl into a 100mL beaker 3 ·3H 2 O, dissolve with 8g of secondary water, shake well, add 6g of carrier activated carbon to the solution, mix evenly, impregnate at room temperature for 8h, dry at 80°C for 12h, and reduce in a hydrogen atmosphere kettle at 130°C for 2h to obtain the ruthenium provided by the invention based catalyst (0.32% Ru loading).

[0060] (2) Catalytic performance test

[0061] Add 10g of water as a solvent, 8g of levulinic acid and 0.10g of the above catalyst in the autoclave, seal the autoclave, fill it with 4MPa hydrogen, react at 130°C for 2h, cool to room temperature after the reaction, and slowly depressurize to the atmosphere Pressure, open the autoclave to sample, GC detection, LA conversion rate 90.5%, GVL selectivity 99.9%.

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Abstract

The invention discloses a method for preparing gamma-valerolactone by acetylpropionic acid catalytic hydrogenation. Through high efficiency catalysis of levulinic acid hydrogenation based on a loaded ruthenium catalyst under mild conditions, gamma-valerolactone is prepared. The method has a levulinic acid conversion rate of 100% and gamma-valerolactone selectivity of 99.9%. The loaded ruthenium catalyst has a low active metal load capacity (less than 1.5w.t.%) and high activity (TOF, 7676h<1>), has good water and acid resistance and is suitable for an intermittent reactor and a continuous fixed bed reactor. The method solves the problem that the existing gamma-valerolactone preparation method needs a high temperature and high pressure and utilizes organic acids and bases and an organic solvent, improves preparation method economy and safety, utilizes a small amount of a catalyst, realizes catalyst recycle, has a high product yield and product separation easiness, and has a latent industrial application value.

Description

technical field [0001] The invention belongs to the technical field of biomass conversion, and relates to a method for preparing gamma-valerolactone by catalyzing the hydrogenation of levulinic acid. Background technique [0002] Resource shortage and environmental pollution have become two prominent problems in the development of human society. The key to the sustainable development of human beings is to provide enough energy, food and chemicals for the ever-increasing population without endangering the earth environment on which we live. Crude oil, natural gas and coal are important energy and chemical raw materials. They can be converted into fuels and chemicals needed by people through a series of chemical reactions, but they cannot be regenerated. Among renewable energy and resources, solar energy, water energy, wind energy, geothermal energy, ocean energy, etc. can be efficiently converted into electricity or hydrogen energy, promising to solve energy problems, but th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J29/44C07D307/33
CPCY02P20/50Y02P20/584
Inventor 谭静静崔静磊朱玉雷陈林峰杨勇李永旺
Owner SYNFUELS CHINA TECH CO LTD
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