Method for preparing acetovanillone and acetosyringone by catalytically saponifying lignin

A technology of acetosyringone and vanilla ethyl ketone, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of underutilization, transformation, and environmental pollution, and achieve heating time Short, high reaction efficiency, efficient degradation effect

Active Publication Date: 2017-10-24
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As a by-product of the wood hydrolysis industry and the paper industry, due to insufficient utilization, it has become an environment...

Method used

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  • Method for preparing acetovanillone and acetosyringone by catalytically saponifying lignin
  • Method for preparing acetovanillone and acetosyringone by catalytically saponifying lignin
  • Method for preparing acetovanillone and acetosyringone by catalytically saponifying lignin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Weigh 1 g of lignin and 16 mL of isopropanol and mix them into a reaction tank, put the reaction tank into a microwave reactor, set the microwave power to 600 W, and react for 30 min at a certain reaction temperature of 120 °C. After the reaction is complete, take out the digestion tank and let it cool down naturally. The product was filtered and washed with the solvent isopropanol, and the filtered liquid product was uniformly dissolved in isopropanol to 20 mL, and the liquid product was to be detected.

Embodiment 2

[0029] a. Weigh 2.47 g Co(NO 3 ) 2 ·6H 2 O was placed in a beaker, fully diluted with deionized water to form a solution, and an equal volume was impregnated in 10 g Al 2 o 3 support, stirred and impregnated at room temperature for 24 h. Then put into the drying box 85 ° C drying for 12 h to obtain the catalyst precursor, in the air atmosphere, the catalyst precursor was carried out in the muffle furnace for 500 ° C, calcination for 4 h. Finally, the calcined catalyst was heated in 90 mL / min of H 2 Reduction under the atmosphere for 1.5 h, the reduction temperature is 550 ° C, the catalyst 5% Co / Al can be obtained 2 o 3 .

[0030] b. Weigh 1 g of lignin, 16 mL of isopropanol, mix them into the reaction tank, and add 0.5 g of catalyst 5%Co / Al 2 o 3 Mix together in a reaction tank, put the reaction tank into a microwave reactor, set the microwave power to 600 W, and react for 30 min at a certain reaction temperature of 120 °C. After the reaction is complete, take o...

Embodiment 3~5

[0032] a. 5% Co / ZrO 2 , 5% Co / CeO 2 , 5% Co / MgO catalyst preparation process adopts a step in embodiment 2, and difference is to use different carrier ZrO respectively 2 , CeO 2 and MgO to prepare the catalyst.

[0033] b. The degradation step of lignin and catalyst in isopropanol solvent adopts the b step in Example 2, the difference is that the catalyst type added is respectively 5% Co / ZrO 2 , 5% Co / CeO 2 , 5% Co / MgO.

[0034] The liquid product was qualitatively detected by GC / MS, and the relationship between the peak areas of two high-yield products (vanillyl ethyl ketone and acetosyringone) in the liquid product was directly obtained. The effect of different catalysts on the distribution of lignin alcoholysis products is shown in figure 1 .

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PUM

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Abstract

The invention discloses a method for preparing acetovanillone and acetosyringone by catalytically saponifying lignin. The method comprises the following steps: by taking lignin as a raw material, performing microwave alcoholysis in an alcohols solvent containing a loaded metal catalyst; cooling, filtering and washing, thereby acquiring a liquid product containing acetovanillone and acetosyringone as primary components. The loaded metal catalyst is formed by active center Co and carrier. The invention provides an environment-friendly and low-cost loaded metal catalyst by modifying the traditional method for degrading lignin; two compounds in high yield, namely, acetovanillone and acetosyringone, are prepared by efficiently degrading the lignin under a microwave heating condition; the method is characterized by mild reaction condition, short heating time and higher reaction efficiency.

Description

technical field [0001] The invention relates to the technical field of lignin utilization, in particular to a method for preparing vanillyl ethyl ketone and acetosyringone by catalyzing the alcoholysis of lignin. Background technique [0002] Today, the world's energy consumption crisis, serious environmental pollution and other issues are increasingly concerned. The massive use of fossil fuels such as coal by human beings has not only caused the exhaustion of energy resources, but also seriously polluted the environment with the waste gas and wastewater discharged. Biomass energy, as an emerging energy with good development prospects, is a renewable energy in which solar energy is stored in plants in the form of chemical energy, and is known as the best renewable energy. [0003] Biomass is mainly composed of cellulose, hemicellulose and lignin. Lignin is a natural organic polymer compound, second only to cellulose in quantity. It is estimated that 150 billion tons of lig...

Claims

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Application Information

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IPC IPC(8): C07C45/51C07C49/84B01J23/83B01J23/78B01J23/75
CPCB01J23/75B01J23/78B01J23/83C07C45/51C07C49/84
Inventor 沈德魁刘娜娜
Owner SOUTHEAST UNIV
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