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Method for preparation of aromatic aldehyde by means of waste biomass pretreated with dilute acid and through acetylation

A technology for pretreatment of biomass and acetylation, applied in the fields of environmental protection and new energy, can solve the problems of low utilization efficiency of non-fibrous compounds, and achieve the effect of improving application potential and simple process

Inactive Publication Date: 2016-09-07
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Plant biomass is an important part of biological resources, among which cellulose and hemicellulose are the raw materials for the production of fuel ethanol, while lignin is less efficient as a non-fibrous compound

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Pretreatment step: dry the waste rice straw, shear and grind it to a size of 180 mesh, mix and stir 5g of biomass powder and 25mL of phosphoric acid solution with a mass fraction of 0.5% to make a slurry, pour it into a 250mL closed autoclave, and While stirring, the temperature was raised to 50°C, maintained for 0 min, passed through tap water to cool to room temperature, and the reaction mixture was poured out. The reaction mixture was filtered with suction, the solid phase was collected and dried. Weigh 3 g of the solid phase after pretreatment with phosphoric acid, acetic acid / acetic anhydride (18ml / 18ml), and 4wt% sulfuric acid, mix them thoroughly, and add them into a three-necked flask. Raise the temperature to 60°C, react for 4 hours, and cool to room temperature after the reaction. Pour the reacted mixture into a centrifuge tube, centrifuge in a centrifuge, separate the supernatant from the precipitate, and discard the supernatant. The resulting precipitate is...

Embodiment 2

[0025] Pretreatment steps: dry the discarded pine branches, cut and grind them to a size of 120 mesh, take 10g of biomass powder and 100mL of 3% phosphoric acid solution, mix and stir to make a slurry, pour it into a 250mL closed autoclave, and While stirring, the temperature was raised to 100°C and kept for 150 min, passed through tap water to cool to room temperature, and the reaction mixture was poured out. The reaction mixture was filtered with suction, the solid phase was collected and dried. Weigh 1 g of the solid phase after pretreatment with phosphoric acid, acetic acid / acetic anhydride (10ml / 10ml), and 0.5wt% sulfuric acid, mix them thoroughly, and add them into a three-necked flask. Raise the temperature to 10°C, react for 1 h, and cool to room temperature after the reaction is complete. Pour the reacted mixture into a centrifuge tube, centrifuge in a centrifuge, separate the supernatant from the precipitate, and discard the supernatant. The resulting precipitate is...

Embodiment 3

[0028] Pretreatment steps: dry the green waste willow leaves, cut and grind them to the size of 80 mesh, take 15g of biomass powder and 60mL of 8% acetic acid solution, mix and stir to make a slurry, and pour it into a 250mL closed autoclave , heated to 150°C while stirring, kept for 300min, passed tap water to cool to room temperature, and poured out the reaction mixture. The reaction mixture was filtered with suction, the solid phase was collected and dried. Weigh 5 g of the solid phase after pretreatment with acetic acid, acetic acid / acetic anhydride (30ml / 30ml), and 6wt% sulfuric acid, mix them thoroughly, and add them into a three-necked flask. Raise the temperature to 90°C, react for 8 hours, and cool to room temperature after the reaction. Pour the reacted mixture into a centrifuge tube, centrifuge in a centrifuge, separate the supernatant from the precipitate, and discard the supernatant. The resulting precipitate is the solid phase after acetylation treatment, and it...

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Abstract

The invention relates to a method for oxidation preparation of aromatic aldehyde by means of waste biomass pretreated with dilute acid and through acetylation. Washed waste biomass is dried and smashed to obtain 40-180-mesh powder, and solid phase is collected and drying is conducted after dilute acid treatment; then acetylation treatment is conducted on the solid phase subjected to dilute acid treatment, and suction filtration is conducted on reactant to obtain a solid phase serving as the raw material for oxidation preparation of aromatic aldehyde; cellulose acetate solid phase and 20-200 mL sodium hydroxide solution of 0.2-2 mol / L are added into a high pressure reactor, stirring is conducted, then CuSO4 is added, the high pressure reactor is sealed, oxygen is introduced till gage pressure is 0.5-2 MPa, and reaction is conducted for 30-120 min at 120-200 DEG C; reaction liquid is cooled and acidized with hydrochloric acid till ph value is 3.0-4.0, filtration is conducted, then chloroform extraction is conducted on filtrate, and rotary evaporation is conducted on extract liquor to obtain the aromatic aldehyde. The process is simple, and the application potential of waste biomass is improved greatly.

Description

technical field [0001] The invention belongs to the technical field of environmental protection and new energy, and in particular relates to a method for preparing aromatic aldehydes by using dilute acid and acetylated pretreated biomass. Background technique [0002] With the shortage of petroleum resources, the use of renewable biomass to produce fuels and chemicals has become a current research hotspot. Plant biomass is an important part of biological resources, among which cellulose and hemicellulose are the raw materials for the preparation of fuel ethanol, while lignin, as a non-fibrous compound, has low utilization efficiency. Generally, lignin is considered to be a complex compound with phenylpropane structure as the unit, and there are three basic structures (non-condensed structures): guaiacyl structure, syringyl structure and p-hydroxyphenyl structure. Therefore, under alkaline conditions, the degradation of lignin by molecular oxygen wet oxidation can yield vani...

Claims

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Application Information

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IPC IPC(8): C07C45/32C07C47/52
CPCC07C45/32
Inventor 张士成曹磊昌陈建民
Owner FUDAN UNIV
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