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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] Example 1

[0022] Pretreatment steps: dry the waste straw, shear and grind it to a size of 180 mesh, take 5g of biomass powder and 25mL of 0.5% phosphoric acid solution, mix and stir to prepare a slurry, and pour it into a 250mL airtight high-pressure reactor. While stirring, the temperature was raised to 50° C., kept for 0 min, tap water was passed to cool to room temperature, and the reaction mixture was poured out. The reaction mixture was suction filtered, and the solid phase was collected and dried. Weigh 3g of the solid phase pretreated with phosphoric acid, acetic acid / acetic anhydride (18ml / 18ml), and 4wt% sulfuric acid, mix them thoroughly and add them to a three-necked flask. The temperature was raised to 60°C, and the reaction was carried out for 4 hours. After the reaction was completed, it was cooled to room temperature. Pour the reacted mixture into a centrifuge tube, centrifuge in a centrifuge, separate the supernatant from the precipitate, discard the su...

Example Embodiment

[0024] Example 2

[0025] Pretreatment steps: dry the discarded pine branches, shear 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 prepare a slurry, and pour it into a 250mL airtight autoclave. While stirring, the temperature was raised to 100° C., kept for 150 min, tap water was passed to cool to room temperature, and the reaction mixture was poured out. The reaction mixture was suction filtered, and the solid phase was collected and dried. Weigh 1g of the solid phase pretreated with phosphoric acid, acetic acid / acetic anhydride (10ml / 10ml), and 0.5wt% sulfuric acid, and add them to a three-necked flask. Raise the temperature to 10°C, react for 1 hour, 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, discard the supernatant, and the resulting precipitate is the solid ...

Example Embodiment

[0027] Example 3

[0028] Pretreatment steps: dry greening waste willow leaves, shear and grind them to 80 mesh size, take 15g of biomass powder and 60mL of 8% acetic acid solution, mix and stir to prepare a slurry, and pour it into a 250mL airtight autoclave , While stirring, the temperature was raised to 150°C, kept for 300 minutes, and cooled to room temperature by running tap water, and the reaction mixture was poured out. The reaction mixture was suction filtered, and the solid phase was collected and dried. Weigh 5g of the solid phase pretreated with acetic acid, acetic acid / acetic anhydride (30ml / 30ml), and 6wt% sulfuric acid after fully mixing and adding them into a three-necked flask. The temperature was raised to 90°C, and the reaction was conducted for 8 hours. After the reaction was completed, it was cooled to room temperature. Pour the reacted mixture into a centrifuge tube, centrifuge in a centrifuge, separate the supernatant from the precipitate, discard the supe...

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PUM

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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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