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Homogeneous catalytic preparation method of gamma-valerolactone

A homogeneous catalysis and valerolactone technology, which is applied in the direction of organic chemistry, can solve the problems of harsh reaction conditions of γ-valerolactone, difficulty in large-scale production, and large amount of catalyst, so that the amount of catalyst can be recycled and the reaction conditions Mild, low-catalyst effect

Active Publication Date: 2015-06-17
UNIV OF SCI & TECH OF CHINA
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  • Claims
  • Application Information

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Problems solved by technology

Patent application CN102558108A discloses a method for preparing γ-valerolactone catalyzed by an iridium-pincer ligand complex, with mild conditions and high yield and selectivity, but the reaction system needs to use an organic solvent, and the catalyst Poor tolerance to acid, need to add a large amount of inorganic base to neutralize levulinic acid raw material
[0004] Therefore, in general, the preparation of gamma-valerolactone by the existing technology has the problems of harsh reaction conditions (high temperature and high pressure) and a large amount of catalyst, resulting in high production costs, difficulty in large-scale production, and environmental pollution problems

Method used

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Experimental program
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Effect test

Embodiment 1-8

[0045] Add 4mL of pre-prepared levulinic acid aqueous solution (1.25mmol / mL) and 1mL of the above-mentioned catalyst 1-8 aqueous solution (500μmol / L) into the reaction kettle respectively, and replace the inside of the reaction kettle with hydrogen gas for 3 times and reduce the hydrogen pressure Adjusted to 1MPa, stirred and reacted at 120°C for 4h. After the reaction was completed, the reaction system was cooled to room temperature, and then the reaction solution was sampled and diluted with methanol, and the yield of the product γ-valerolactone was detected by GC. The catalyst used in the reaction and its molar amount relative to the raw material levulinic acid, the type and amount of the hydrogen source raw material, and the yield results of the reaction are shown in Examples 1-8 in Table 1.

[0046] Finally, the prepared product can be easily obtained, for example, by extractive isolation using ethyl acetate.

Embodiment 9

[0048] Add 4mL of pre-prepared levulinic acid aqueous solution (1.25mmol / mL) and 1mL of the above-prepared catalyst 6 aqueous solution (50μmol / L) into the reactor, and replace the inside of the reactor with hydrogen for 3 times, then adjust the hydrogen pressure to 1MPa , The reaction was stirred at 120°C for 36h. After the reaction was completed, the reaction system was cooled to room temperature, and then the reaction solution was sampled and diluted with methanol, and the yield of the product γ-valerolactone was detected by GC. The catalyst used in the reaction and its molar amount relative to the raw material levulinic acid, the type and amount of the hydrogen source raw material, and the reaction yield results are shown in Example 9 in Table 1.

[0049] Finally, the prepared product can be easily obtained, for example, by extractive isolation using toluene.

Embodiment 10-13

[0051] Add 4 mL of pre-prepared levulinic acid aqueous solution (1.25 mmol / mL), 1 mL of the above-prepared catalyst 6 aqueous solution (500 μmol / L) and 7.5 mmol of formic acid into the reaction kettle, and stir the reaction at 120 ° C for 4 h (wherein Example The reaction time in 13 is 6h). After the reaction was completed, the system was cooled to room temperature, the reaction solution was sampled and diluted with methanol, and the yield of the product γ-valerolactone was detected by GC. For the catalyst used in the reaction and its molar amount relative to the raw material levulinic acid, the type and amount of the hydrogen source raw material, and the reaction yield results, refer to Examples 10-13 in Table 1.

[0052] Finally, the prepared product can be easily obtained, for example, by extractive isolation using benzene.

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Abstract

The invention relates to a homogeneous catalytic preparation method of gamma-valerolactone. The method comprises the step of reacting an acetylpropionic acid raw material with a hydrogen source raw material to obtain the product of gamma-valerolactone by using water as a solvent and with the existence of a water soluble iridium catalyst. By adopting the method disclosed by the invention, the defect that the existing preparation method of the gamma-valerolactone needs harsh reaction conditions of high temperature, high pressure, a lot of organic acid, a lot of organic base, and a lot of organic solvent is conquered, the economical efficiency and safety of the preparation method are improved, reaction is simple, catalyst is small in dose and can be repeatedly used, and the product is high in yield, easy to separate, and is quite high in industrial application value.

Description

technical field [0001] The invention relates to the preparation of chemicals, in particular to a preparation method of gamma-valerolactone. Background technique [0002] At present, the energy and chemicals needed for the survival and development of human society mainly come from traditional fossil raw materials, such as coal, oil, and natural gas. With the gradual depletion of these fossil raw materials, it is necessary to start looking for new alternative resources. Biomass can be used both as an energy source and as a source of organic carbon for the production of chemicals and materials, so it is considered to be the new resource most likely to replace fossil raw materials. γ-valerolactone is a biomass platform molecule with high potential application value, which can be used not only as a new type of fuel, but also as a source of organic carbon for the synthesis of high value-added chemicals. [0003] At present, the preparation of γ-valerolactone is mainly obtained f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33
Inventor 傅尧王琰邓晋郭庆祥
Owner UNIV OF SCI & TECH OF CHINA
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