Method for preparing phenolic chemicals by catalyzing degradation of lignin with carbon-based solid acid

A carbon-based solid acid, lignin technology, applied in chemical instruments and methods, lignin derivatives, preparation of organic compounds, etc. Difficulty in separation, etc., to achieve high-value utilization, reduce dependence on fossil resources, and be easy to recycle

Active Publication Date: 2014-12-03
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of phenolic products in the above methods is generally not high, and the use of inorganic acids and bases and hydrogen-donating solvents brings difficulties to the separat

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] (1) Preparation of carbon-based solid acid: 5g alkali lignin is placed in a three-necked flask with reflux condensing device with 250g mixed acid solution (the mass fraction of nitric acid is 5%, and the mass fraction of sulfuric acid is 64%). Protect and react in an oil bath at 80°C for 12 hours, cool and stand still, decant, filter with suction, wash with hot water until neutral, and no acid ions are detected, then dry and grind to obtain a black carbon-based solid acid catalyst.

[0012] (2) Preparation of phenolic chemicals from lignin: put 1g of alkali lignin in a stainless steel autoclave, 0.5g of the carbon-based solid acid catalyst prepared by the above-mentioned method, 50ml of deionized water, under argon pressure of 2MPa, 160 After stirring and reacting for 12 hours at the reaction temperature of ℃, cooling and standing still, the unreacted raw materials and catalyst were collected by filtration, and the reaction liquid was extracted with ethyl acetate, and th...

Embodiment 2

[0015] (1) Preparation of carbon-based solid acid: 5g alkali lignin is placed in a three-necked flask with reflux condensing device with 1000g mixed acid solution (15% nitric acid mass fraction, 47% sulfuric acid mass fraction) under nitrogen gas Protect and react in an oil bath at 160°C for 4 hours, cool and stand still, decant, filter with suction, wash with hot water until neutral, and no acid ions are detected, then dry and grind to obtain a black carbon-based solid acid catalyst.

[0016] (2) Preparation of phenolic chemicals from lignin: put 1g of organic lignin in a stainless steel autoclave, 0.1g of the carbon-based solid acid catalyst prepared by the above method, 10ml of deionized water, and put it under a helium pressure of 5MPa at 240 After stirring and reacting for 0.5 h at the reaction temperature of °C, cool and stand still, collect unreacted raw materials and catalysts by filtration, and extract the reaction liquid with ethyl acetate, and obtain phenolic chemica...

Embodiment 3

[0019] (1) Preparation of carbon-based solid acid: 5g hydrolyzed lignin is placed in a three-necked flask with reflux condensing device with 500g mixed acid solution (15% nitric acid mass fraction, 64% sulfuric acid mass fraction) under argon Protected under gas and reacted in a 60°C oil bath for 8 hours, cooled and stood still, decanted, filtered with suction, washed with hot water until neutral, and no acid ions were detected, then dried and ground to obtain a black carbon-based solid acid catalyst.

[0020] (2) Preparation of phenolic chemicals from lignin: put 1g of hydrolyzed lignin in a stainless steel autoclave, 0.4g of carbon-based solid acid catalyst prepared by the above method, 20ml of deionized water, under nitrogen pressure of 4MPa, 220°C After stirring and reacting at the reaction temperature for 2 hours, cool and stand still, collect unreacted raw materials and catalysts by filtration, and extract the reaction liquid with ethyl acetate, and obtain phenolic chemic...

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Abstract

The invention provides a method for preparing phenolic chemicals by catalyzing degradation of lignin with carbon-based solid acid. The method comprises the following steps: by taking lignin as a raw material, a carbon-based solid acid as a catalyst and a water phase as a reaction solvent, putting lignin, carbon-based solid acid and water into a high-pressure reaction kettle; and carrying out warming reaction under the protection of an inert gas, and then extracting by using ethyl acetate, and performing vacuum evaporation so as to obtain the phenolic chemicals, wherein used carbon-based solid acid is prepared by using the lignin as the raw material in an inorganic acid environment; and the lignin raw material for carbon-based solid acid is alkali lignin, organic lignin, zymolytic lignin residue or hydrolytic lignin residue. The phenol yield can be up to 53%, the relative selectivity of guaiacol aromatic products can be up to 70%, the technique disclosed by the invention is simple and environmental friendly, available in raw materials and low in demands on equipment, and does not need to use a concentrated acid with strong corrosivity, and compared with the prior art, the method has outstanding advantages.

Description

technical field [0001] The invention relates to a method for preparing phenolic chemicals by using lignin; in particular, it relates to a method for producing phenolic chemicals by using carbon-based solid acid as a catalyst to directly catalyze the degradation of lignin in an aqueous phase system. Background technique [0002] The non-renewability of fossil resources and their massive consumption lead to the shortage of energy chemicals and a series of environmental problems. The development and utilization of renewable resources has become an inevitable trend of social development. As the main component of lignocellulosic biomass, lignin is the main by-product of hydrolysis and fermentation of lignocellulosic biomass to produce ethanol and paper industry. Lignin is a natural high-molecular polymer, which is composed of phenylpropane structural units such as p-hydroxyphenylpropane, guaiacylpropane, and syringylpropane through ether bonds and carbon-carbon bonds. It has a t...

Claims

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Application Information

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IPC IPC(8): C07G1/00C07C43/23C07C41/18B01J27/20
Inventor 袁振宏谭雪松庄新姝亓伟王琼余强
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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