Method for preparing gamma-valerolactone from furfural on metal/solid acid catalyst

A technology of solid acid catalyst and valerolactone, which is applied in the direction of organic chemistry, can solve the problems of high energy consumption, unfavorable large-scale production, and influence on product selectivity, and achieve low cost, easy operation, and reduced human operation loss. Effect

Active Publication Date: 2015-04-29
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

Currently, there are two main methods for preparing γ-valerolactone from furfural: one is divided into two steps (Chinese patent CN 103435577 A), that is, furfural is hydrogenated and hydrated to synthesize levulinic acid, and then separated from the hydrolyzate Levulinic acid is produced and hydrogenated to obtain γ-valerolactone. The separation of levulinic acid in this method consumes a lot of energy; another method uses 2-butanol as the hydrogen source, using B acid and Zr-Beta molecular sieve The mixture is a catalyst (Angew. Chem. Int. Ed. 2013, 52, 8022-8025), in which sulfuric acid, ion exchange resin and aluminum-containing molecular sieves are selected as the B acid catalyst, but there is a mixed catalyst in the regeneration of the catalyst in this method In addition, the hydrogenation method is transfer hydrogenation, and the 2-butanol hydrogen source used will generate by-products during the reaction process, which will affect the selectivity of the product and is not conducive to large-scale production

Method used

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  • Method for preparing gamma-valerolactone from furfural on metal/solid acid catalyst
  • Method for preparing gamma-valerolactone from furfural on metal/solid acid catalyst
  • Method for preparing gamma-valerolactone from furfural on metal/solid acid catalyst

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preparation example Construction

[0018] Catalyst preparation

[0019] Dissolve a calculated amount of metal salt solution in a small amount of water, and prepare metal / solid acid catalysts in three ways: (1) load the metal salt solution on the solid acid by impregnation method, (2) pre-coat the metal solution (3) Titrate the metal hydroxide precipitate with an alkali solution, then bake it into a metal oxide, and mechanically mix it with the solid acid. Roasted at high temperature, then reduced with hydrogen. Among them, the silicon-aluminum molecular sieve and the phosphorus-aluminum molecular sieve in the solid acid are commercial products, the metal oxide and phosphate are prepared by precipitation of corresponding metal precursors, and the metal sulfate is prepared by impregnating the corresponding metal oxide with sulfuric acid.

Embodiment 1

[0021] Add 0.15g of furfural and 5g of solvent into a batch-type high-pressure reactor with a polytetrafluoroethylene liner, and add catalysts in sequence. At the initial hydrogen pressure of 3MPa, 120 o Magnetic high-speed stirring reaction at C temperature for 6 hours; turn off hydrogen, feed nitrogen, continue to feed hydrogen after 12 hours of reaction, hydrogen pressure 3MPa, after 6 hours of reaction, separate the catalyst from the reaction solution. The reaction liquid was analyzed by gas chromatography, and the conversion rate of furfural and the yield of γ-valerolactone are shown in Table 1.

[0022] When transition metals are used as hydrogenation catalyst components, the main by-products are dark carbon deposits; when noble metals are used as catalyst hydrogenation components, the by-products are various overhydrogenation products, such as MTHF, alcohols and alkanes, etc., through Separation from the main product by means of vacuum distillation and the like.

Embodiment 2

[0023] Embodiment 2 (comparative example)

[0024] The reaction raw materials and steps are the same as in Example 1, and the catalyst used is 25wt%CoFe / ZrSO 4 , the difference is that the hydrogen pressure has been maintained at 3MPa, and nitrogen is not introduced. The conversion rate of furfural and the yield of γ-valerolactone are shown in Table 1.

[0025] Table 1 Properties of furfural to prepare γ-valerolactone over different catalysts

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Abstract

The invention discloses a method for preparing gamma-valerolactone from furfural on a metal/solid acid catalyst. On a multifunctional metal/solid acid catalyst, a hydrogenation hydrolysis product of furfural is further hydrogenated without being separated to obtain gamma-valerolactone, the reaction temperature is 80-200 DEG C, the conversion rate of furfural can reach 100%, and the selectivity of gamma-valerolactone can be equal to or higher than 80%. By adopting the technology, the fine chemical gamma-valerolactone with high added value can be synthesized from one of a renewable energy sources, namely biomass and a derivative thereof so as to reduce the relay on petrochemical materials on one hand; on the other hand, one-kettle reaction is carried out on furfural on one catalyst to prepare gamma-valerolactone, so as to avoid the separation of an intermediate product levulinic acid and save the energy source, so that the method is a green and feasible catalytic process.

Description

technical field [0001] The invention relates to the field of catalytic conversion of biomass into high value-added fine chemicals, and specifically belongs to a method for preparing gamma-valerolactone from furfural on a metal / solid acid catalyst. Background technique [0002] With the rapid growth of the world economy, fossil fuel (especially oil) resources are becoming increasingly scarce, and their use has brought a series of social and environmental problems to human society. Therefore, from one of the renewable energy sources The research on the synthesis of fuels and fine chemicals from substances and their derivatives has become one of the hotspots of scientists at home and abroad. [0003] Gamma-valerolactone melting point -30 o C, the boiling point is as high as 207 o C, which is mostly liquid, is an important solvent used in the production of fuels and a variety of chemicals. At present, γ-valerolactone is mainly produced by selective catalytic hydrogenation of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
CPCC07D307/33
Inventor 刘晓晖王艳芹丁大千卢冠忠王筠松龚学庆郭耘郭杨龙
Owner EAST CHINA UNIV OF SCI & TECH
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