Method for hydrodeoxidation upon lignin by using ruthenium-based catalyst under deep eutectic solvent condition

A low eutectic solvent, ruthenium-based catalyst technology, applied in molecular sieve catalysts, lignin derivatives, chemical instruments and methods, etc., can solve the problems of water consumption, large organic solvent consumption, difficulty in direct utilization, etc., and achieve wider application. The effect of surface, large pore size, and large specific surface area

Active Publication Date: 2020-01-17
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Lignocellulosic biomass is mainly composed of three major components: lignin, cellulose and hemicellulose. Lignin is the only renewable natural polymer resource with aromatic structure. Therefore, lignin is used in the production of fuel, Biomass-based materials and phenolic compounds from fossil sources have great potential, but due to the complex chemical bond connections between lignin, cellulose and hemicellulose, it is difficult to use them directly, so certain methods need to be adopted Separation of lignin from three major components
In recent years, the lignin used for hydrodeoxygenation is mostly organic solvent lignin. The extraction process of organic solvent lignin requires a large amount of organic solvent, and finally requires water precipitation, which also consumes a large amount of water.

Method used

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  • Method for hydrodeoxidation upon lignin by using ruthenium-based catalyst under deep eutectic solvent condition
  • Method for hydrodeoxidation upon lignin by using ruthenium-based catalyst under deep eutectic solvent condition
  • Method for hydrodeoxidation upon lignin by using ruthenium-based catalyst under deep eutectic solvent condition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0024] Weigh a certain amount of ChCl and acetic acid (the molar ratio of the two substances is 1:2), add it into a beaker, stir and heat in an oil bath at 80°C for 2h, and obtain a clear and transparent solution after cooling, which is the prepared ChCl: Acetic acid DES.

[0025] Add eucalyptus wood powder and deionized water (reaction solid-to-liquid ratio 1:12g / ml) into a high-pressure reactor, and react at 170°C for 1 hour under a nitrogen atmosphere. After the reaction, cool to room temperature, filter under reduced pressure, and filter the residue Dry at 105°C for 12h to obtain a hydrothermal residue.

[0026] Weigh 2g of hydrothermal residue and 40g of ChCl: acetic acid DES, add them to the Erlenmeyer flask, and react at 120°C for 4h. , the filter residue was dried at 105°C for 12 hours, weighed after cooling to room temperature, and the mass of lignin dissolved in the DES filtrate was obtained according to the subtraction method. The volume is 50ml.

[0027] Add 100...

Embodiment 5

[0028] The adsorption-desorption curve and pore size distribution figure of the catalyst used in embodiment 5 are as follows figure 1 shown. according to figure 1 It can be seen that the catalyst has a V-type isotherm and a H3-type hysteresis loop. From the pore size distribution diagram, it can be seen that the pore size of the catalyst belongs to mesopores, the pore size distribution is narrow, and the pore size is large. It has better catalytic activity, and the yield of liquid products and phenolic products is higher.

[0029] Table 1 Effect of different catalysts on lignin hydrodeoxygenation

[0030]

Embodiment 6-11

[0032] With reference to Example 5, the Ru / γ-Al of 100mg 2 o 3 The catalyst and 50ml of DES filtrate were added to the high-pressure reaction kettle, and the gas was repeatedly replaced by hydrogen for 3 times, and 1MPa H was filled after removing all the air. 2 ,React at 120-280°C for 4 hours. After the reaction, quickly cool down the reactor with cold water, collect the gas, filter it under reduced pressure, and extract it with ethyl acetate. See Table 2 for the yield of liquid products and phenols.

[0033] Table 2 Effect of temperature on lignin hydrodeoxygenation

[0034]

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Abstract

The invention discloses a method for hydrodeoxidation upon lignin by using a ruthenium-based catalyst under a deep eutectic solvent (DES) condition. The method comprises the following steps: putting hydrothermal residues and a DES into a conical bottle, performing a reaction for 3-4 hours at 100-120 DEG C, and performing vacuum suction filtration so as to obtain DES filtrate of dissolved lignin, wherein the ratio of the hydrothermal residues to the DES is 1:20g/g; and in a hydrogen atmosphere, putting the deep eutectic solvent of the dissolved lignin and 50-300mg of a catalyst into a high-pressure reactor, and performing a reaction for 2-15 hours at 120-280 DEG C, wherein the catalyst is Ru/Nb2O5, Ru/ZSM-5, Ru/HY, Ru/gamma-Al2O3 or Ru/C. At a lower pressure and pressure and under short reaction conditions, operation of depolymerizing lignin to prepare phenolic compounds is achieved.

Description

technical field [0001] The invention belongs to the field of hydrodeoxygenation of lignin, and in particular relates to a method for hydrodeoxygenating lignin with a ruthenium-based catalyst under the condition of deep eutectic solvent. Background technique [0002] Lignocellulosic biomass is mainly composed of three major components: lignin, cellulose and hemicellulose. Lignin is the only renewable natural polymer resource with aromatic structure. Therefore, lignin is used in the production of fuel, Biomass-based materials and phenolic compounds from fossil sources have great potential, but due to the complex chemical bond connections between lignin, cellulose and hemicellulose, it is difficult to use them directly, so certain methods need to be adopted Lignin is separated from three major components. In recent years, most of the lignin used for hydrodeoxygenation is organic solvent lignin. The extraction process of organic solvent lignin requires a large amount of organic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J23/648B01J29/12B01J29/44C07C37/00C07G1/00C07C39/00
CPCB01J23/462B01J23/6484B01J29/126B01J29/44B01J2229/18C07C37/004C07G1/00C07C39/00
Inventor 常杰张淑迪付严黄晴雯
Owner SOUTH CHINA UNIV OF TECH
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