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Method for preparing phenolic compound by liquefaction of salix mongolica

A technology of salix salix and phenols, which is applied in the field of resource utilization of salix salix, can solve problems such as difficult treatment, high chemical oxygen demand, and restrictions on large-scale promotion of hydrothermal liquefaction, and achieves simple operation, simplified process flow, and solution Effects of water scarcity

Inactive Publication Date: 2013-06-19
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after the hydrothermal liquefaction reaction, a large amount of process water will be produced, which is a kind of wastewater containing a variety of organic substances, with high chemical oxygen demand and difficult treatment, which greatly limits the large-scale promotion of hydrothermal liquefaction.

Method used

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  • Method for preparing phenolic compound by liquefaction of salix mongolica
  • Method for preparing phenolic compound by liquefaction of salix mongolica
  • Method for preparing phenolic compound by liquefaction of salix mongolica

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Grind Salix salix, pour 30g of Salix salix powder into a 250ml high-pressure reactor and add 150ml of distilled water, stir to make a slurry, and fill the reactor with 2MPa N 2 , heated to 300°C while stirring, kept for 10min, passed tap water to cool to room temperature, poured out the reaction mixture, and cleaned the kettle cavity with tetrahydrofuran; filtered the mixture into solid and liquid phases, and the liquid phase was process water. Extract the solid phase with 150ml of tetrahydrofuran, separate and extract the extract, filter the tetrahydrofuran phase with a Buchner funnel, and then distill under reduced pressure to recover tetrahydrofuran to obtain heavy oil; extract the process water with diethyl ether, and distill the diethyl ether phase under reduced pressure to recover diethyl ether That is, medium oil is obtained, and the water phase is the return water, which is reserved for the next experiment. Heavy and medium oils are rich in phenolic compounds. ...

Embodiment 2

[0023] Salix salix is ​​crushed, 30g Salix salix powder is poured into a 250ml autoclave, the process water obtained in Example 1 is added as a medium, stirred to form a slurry, and 2MPa N 2 , heated to 300°C while stirring, kept for 10min, passed tap water to cool to room temperature, poured out the reaction mixture, and cleaned the kettle cavity with tetrahydrofuran; filtered the mixture into solid and liquid phases, and the liquid phase was process water. Extract the solid phase with 150ml of tetrahydrofuran, separate and extract the extract, filter the tetrahydrofuran phase with a Buchner funnel, and then distill under reduced pressure to recover tetrahydrofuran to obtain heavy oil. The process water is directly added to another reactor as the liquefaction medium for the next hydrothermal liquefaction reaction, and the above process is repeated once to obtain the heavy oil and process water after the process water is reused once. Finally, extract the process water with die...

Embodiment 3

[0025] Salix salix is ​​crushed, 30g Salix salix powder is poured into 250ml of high pressure and added the process water of Example 12 as a medium, stirred to form a slurry, and 2MPa N 2 , heated to 300°C while stirring, kept for 10min, passed tap water to cool to room temperature, poured out the reaction mixture, and cleaned the kettle cavity with tetrahydrofuran; filtered the mixture into solid and liquid phases, and the liquid phase was process water. Extract the solid phase with 150ml of tetrahydrofuran, separate and extract the extract, filter the tetrahydrofuran phase with a Buchner funnel, and then distill under reduced pressure to recover tetrahydrofuran to obtain heavy oil. The process water is directly added to another reactor as the liquefaction medium for the next hydrothermal liquefaction reaction, and the above process is repeated twice to obtain the heavy oil and process water after the process water is reused twice. Finally, extract the process water with diet...

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Abstract

The invention belongs to the salix mongolica resource utilization field, and concretely relates to a method for preparing a phenolic compound by directly reusing process water generated by hydro-thermal liquefaction of salix mongolica. The method comprises the following steps: dumping the crushed salix mongolica in a high pressure reaction vessel to form a mixed liquor with a certain solid-liquid mass ratio, filling inert gas with a certain pressure in a reaction vessel, stirring and heating to the temperature of 150-350 DEG C, keeping for 1-180 minutes, rapidly cooling to room temperature, collecting a reaction mixture, filtering the reaction mixture and separating to obtain a solid phase and a liquid phase, wherein the liquid phase is the process water which is directly reused as a liquefaction medium for next hydro-thermal liquefaction, and the organic compound in the organic solvent extraction process water can be used in advance, and the surplus water phase is taken as a liquefaction medium for next hydro-thermal reaction. The solid phase and the process water are extracted by an organic solvent, the organic phase is separated and filtered to remove the organic solvent to obtain bio oil. The bio oil contains abundant phenolic compound. The hydro-thermal liquefaction process water can be directly reused for simplifying the technology flow, the waste water treatment is reduced, and generation of the phenolic compound can be simultaneously promoted.

Description

technical field [0001] The invention belongs to the technical field of resource utilization of Salix salix, and specifically relates to a method of directly reusing and liquefying water in the hydrothermal liquefaction process of Salix salix to prepare phenolic compounds (mainly phenol, guaiacol, 4-ethyl-2-methoxy phenol and 2,6-dimethoxyphenol). Background technique [0002] Salix salix is ​​a kind of plant with strong growth ability and adapts to arid environment. These characteristics make them the first choice for windbreak and sand fixation, and a large area is planted in the arid regions of Northwest China. These plants need to be stubbled every once in a while, so a large number of sandy shrub branches will be produced every year, which has broad utilization prospects. [0003] Hydrothermal liquefaction treatment of biomass is a new type of treatment process, which has the advantages of wide source of raw materials, simple reaction conditions and equipment, and simp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/04C07C37/00C07C43/23C07C41/00C07C53/08C07C51/00
Inventor 张士成李长军陈忠武包红光陈建民
Owner FUDAN UNIV
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