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A method for directly oxidizing lignin in wood powder to prepare high value-added products and cellulose
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A high value-added, cellulose technology, applied in textiles and papermaking, fiber raw material treatment, pretreatment with oxygen compounds, etc., can solve the problems of difficult lignin and high requirements for reaction conditions, and achieve low equipment requirements and high selectivity Good, high yield effect
Active Publication Date: 2018-02-09
QILU UNIV OF TECH
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Problems solved by technology
However, in the conversion of lignin, the requirements for reaction conditions are relatively high, and it is more difficult to directly convert lignin in lignocellulosic raw materials.
Method used
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Embodiment 1
[0022] (1) Weigh 1g of poplar wood powder and 60mL of 1mol / L sodium hydroxide solution in a stainless steel autoclave, feed 10bar oxygen, heat to a reaction temperature of 80°C, and react for 0.5 hours.
[0023] (2) After the reaction, the mixture is transferred to a beaker, the cellulose is filtered, the filtrate is acidified to precipitate unreacted lignin, after filtration, the filtrate is precipitated by ethanol precipitation to hemicellulose, and the filtered filtrate is extracted with ethyl acetate.
[0024] 1mL of the extract was used for qualitative analysis of the reaction products by GC-MS, and quantitative analysis of the main reaction products by high performance liquid chromatography.
[0025] The obtained aromatic monomer and organic acid product mainly contain vanillin, vanillic acid, syringaldehyde, syringic acid, coumaric acid, vanillyl ethyl ketone, and the total concentration of the monomer product is 25.12mg / g (1g of wood powder The phenolic monomer of 25.1...
Embodiment 2
[0027] As shown in Example 1, the difference is that the reaction temperature is 160°C. The obtained aromatic monomers and organic acid products mainly include vanillin, vanillic acid, syringaldehyde, syringic acid, coumaric acid, vanillyl ethyl ketone, the total concentration of the monomer product is 47.66mg / g, organic acid, formic acid , the total concentration of acetic acid and oxalic acid was 80.51 mg / g.
Embodiment 3
[0029] As shown in Example 1, the difference is that the reaction time is 2h. The obtained aromatic monomers and organic acid products mainly include vanillin, vanillic acid, syringaldehyde, syringic acid, coumaric acid, vanillyl ethyl ketone, the total concentration of the monomer product is 31.23mg / g, organic acid, formic acid , the total concentration of acetic acid and oxalic acid was 73.51 mg / g.
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Abstract
The invention discloses a method for preparing high-added-value products and cellulose by directly oxidizing lignin in wood powder. According to the method, the wood powder and a sodium hydroxide solution are added into a high-pressure reaction kettle; oxygen is introduced; stirring and heating are performed to perform oxidization reaction; then, cellulose is filtered; filter liquid is acidified for precipitating unreacted lignin; after the filtering, semi-cellulose in the filter liquid is precipitated by an ethyl alcohol precipitating method; the filtered filter liquid is extracted by organic solvents; extraction liquid is subjected to rotary evaporation concentration, and then, the high-added-value products are obtained; the industrial popularization and application are facilitated. The lignin in the wood powder is directly oxidized; the use of a catalyst is not needed; the lignin and the high-added-value products including aromatic monomers and organic acid products can be obtained; the reaction conditions are mild; the reaction time is short; no other additives exist; the yield is high; the selectivity is high; a reaction system achieves the green and environment-friendly effect; the environment is not polluted; the industrial popularization and application are facilitated.
Description
technical field [0001] The invention relates to the technical field of utilization and treatment of agricultural and forestry biomass resources, in particular to a method for directly oxidizing lignin in wood flour to prepare high value-added products and cellulose. Background technique [0002] In recent years, with the rapid development of global industrialization, the huge energy consumption has made petrochemical resources increasingly scarce. Under this situation, biomass energy has become more and more popular due to its advantages such as renewable, wide sources, low price, abundant reserves and environmental friendliness. It is considered as a potential petrochemical alternative raw material. Woody biomass raw materials are mainly composed of three components: cellulose, hemicellulose and lignin. Among them, lignin is mainly a phenylpropane polymer formed by oxidative polymerization of three kinds of 4-hydroxy-cinnamyl alcohols with different degrees of methoxylatio...
Claims
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Application Information
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