Method for preparing gamma-valerolactone by liquid-phase hydrogenation and catalyst used by same

A liquid-phase hydrogenation, valerolactone technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of high production process risks and production costs. high selectivity, simple operation and high catalytic activity

Inactive Publication Date: 2015-06-10
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Among the methods proposed in the above-mentioned prior art, the catalytic reaction process for preparing γ-valerolactone from α-angelica lactone as a starting material needs to be carried out under harsh conditions such as high temperature or high pressure, which consumes a lot of energy.
Moreover, the existing method is complex in process, difficult to operate, and highly dangerous in the production process; its high hydrogen-to-oil ratio or high pressure means that the reaction requires a large amount of hydrogen to participate in the reaction, making the production cost higher

Method used

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  • Method for preparing gamma-valerolactone by liquid-phase hydrogenation and catalyst used by same
  • Method for preparing gamma-valerolactone by liquid-phase hydrogenation and catalyst used by same

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Experimental program
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Effect test

Embodiment 1

[0030] The preparation of embodiment 1 supported palladium catalyst:

[0031] Take PdCl proportionally 2 Add the solution into the titanium oxide aqueous solution (Pd: titanium oxide = 1:19, weight ratio), stir evenly at room temperature and adjust the pH to Pd 2+ After the precipitation was complete, sodium borohydride (Pd:sodium borohydride=1:10, molar ratio) was added and stirring was continued for 2 hours. The obtained solution is filtered and dried to prepare a supported palladium catalyst, and palladium metal nanoparticles are evenly distributed on the carrier.

[0032] Titanium oxide is used in this embodiment. In other embodiments, common oxides such as silicon oxide, aluminum oxide, and nickel oxide, and activated carbon can also be used to achieve the same effect.

[0033] In this embodiment, PdCl is used 2 . In other embodiments it can also be Pd(NO 3 ) 2 or Pd(Ac) 2 , all achieve the same effect.

[0034] Sodium borohydride is used as reducing agent in thi...

Embodiment 2

[0036] The preparation of embodiment 2 supported palladium-nickel alloy catalysts:

[0037] Take PdCl proportionally 2 and Ni(NO 3 ) 2Add the solution into the aqueous solution of silicon oxide (Pd:Ni:SiO2=0.001:0.4:0.59 weight ratio), stir well at room temperature and adjust the pH to Pd 2+ and Ni 2+ Precipitation is complete, add sodium borohydride (Pd:NaBH 4 =1:10, molar ratio) and continued to stir for 2 hours. The resulting solution was filtered and dried to prepare a supported palladium-nickel catalyst.

[0038] Silicon oxide is used in this embodiment. In other embodiments, common oxides such as titanium oxide and aluminum oxide and activated carbon can also be used to achieve the same effect.

[0039] In this embodiment, PdCl is used 2 . In other embodiments it can also be Pd(NO 3 ) 2 or Pd(Ac) 2 , all achieve the same effect.

[0040] In this example, Ni(NO 3 ) 2 . In other embodiments it can also be NiCl 2 or Ni(Ac) 2 , all achieve the same effect. ...

Embodiment 3

[0043] Example 3 α-angelica lactone hydrogenation reaction

[0044] Use the Pd / TiO that embodiment 1 prepares 2 Catalyst is carried out to prepare gamma-valerolactone by liquid-phase hydrogenation of alpha-angelica lactone, in round bottom flask, load catalyst, consumption is about 10% (accounting for alpha-angelica lactone mass percentage), solvent (water) dilution ratio About 50:1 (water: α-angelica lactone, volume ratio), the reaction temperature is 25 ℃, under the pressure of hydrogen balloon (0.1MPa) for 1 hour, α-angelica lactone 100%, γ-amyloid The lactone selectivity is 100%.

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Abstract

The invention discloses a method for preparing gamma-valerolactone by liquid-phase hydrogenation, which comprises the following step: under the conditions of low temperature and low pressure, carrying out high-selectivity hydrogenation on alpha-angelica lactone by using a supported catalyst to obtain the gamma-valerolactone. The invention also discloses the supported catalyst and a preparation method thereof, and application of the supported catalyst in the method for preparing gamma-valerolactone by liquid-phase hydrogenation. The method has the advantages of mild reaction conditions, high catalytic activity, high selectivity of the product gamma-valerolactone and the like.

Description

technical field [0001] The present invention relates to a liquid-phase hydrogenation method for directly producing high-purity γ-valerolactone from α-angelica lactone, and the supported catalyst used in the process and its liquid-phase hydrogenation method from α-angelica lactone Application in the preparation of γ-valerolactone. Background technique [0002] γ-valerolactone, also known as 4-methylbutyrolactone, is recognized as a widely used organic compound, which can be used in food flavors, preparation of liquid fuels, synthesis of organic intermediates and polymer polyester monomers, as Medicines and adhesives etc. As far as it is concerned, its natural fruit flavor is widely used in food additives; it also has the characteristics of low melting point (-31°C), high boiling point (207°C), flash point (96°C) and partial miscibility with water , so that it also has a good application as a green solvent. [0003] At present, levulinic acid is generally used as raw materi...

Claims

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Application Information

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IPC IPC(8): C07D307/33B01J23/44B01J23/89
CPCB01J23/44B01J23/892C07D307/33
Inventor 关业军张沛袁庆庆
Owner EAST CHINA NORMAL UNIV
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