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Method for preparing bio-based phenol compounds through catalytic liquefaction on rice straw

A bio-based phenol and catalytic liquefaction technology, applied in the fields of environmental protection and bio-based chemicals, can solve problems such as hydrothermal liquefaction treatment that does not involve straw

Active Publication Date: 2015-11-11
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But above processing method does not relate to the method for carrying out hydrothermal liquefaction treatment of rice straw

Method used

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  • Method for preparing bio-based phenol compounds through catalytic liquefaction on rice straw
  • Method for preparing bio-based phenol compounds through catalytic liquefaction on rice straw
  • Method for preparing bio-based phenol compounds through catalytic liquefaction on rice straw

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Using straw as raw material, first crush the straw, take 15g of straw powder and pour it into a 250mL high-pressure reactor, add 150mL of deionized water and 2g of activated copper-zinc-aluminum catalyst, stir to make a slurry, and fill the reactor with 1.2MPaH 2 , heated to 260°C while stirring, kept for 30min, passed tap water to cool to room temperature, and poured out the reaction mixture. After the solid-liquid separation of the product, the solid phase product was extracted with 100 mL of ethyl acetate, extracted and filtered; 10 mL of the aqueous phase product was extracted with 20 mL of ethyl acetate, extracted and separated. The extracted phases were diluted and quantified respectively, and the extracted phases obtained by liquid separation were qualitatively and quantitatively analyzed for phenolic compounds by gas chromatography-mass spectrometry (GC-MS). The yield of phenolic compounds was 13.83% ( relative to the quality of lignin in wood straw). The solid...

Embodiment 2

[0018] Using straw as raw material, first crush the straw, take 15g of straw powder and pour it into a 250mL high-pressure reactor, add 75mL of deionized water, 75mL of ethanol and 2g of activated copper-zinc-aluminum catalyst, stir to make a slurry, and fill the reactor with into 1.2MPaH 2 , heated to 300°C while stirring, kept for 30min, passed tap water to cool to room temperature, and poured out the reaction mixture. After the solid-liquid separation of the product, the solid phase product was extracted with 100 mL of ethyl acetate, extracted and filtered; 10 mL of the aqueous phase product was extracted with 20 mL of ethyl acetate, extracted and separated. The obtained extract phases were diluted and quantified respectively, and the extract phases obtained by liquid separation were qualitatively and quantitatively analyzed for phenolic compounds by gas chromatography-mass spectrometry (GC-MS). The yield of phenolic compounds was 28% ( relative to the quality of lignin in...

Embodiment 3

[0020] The solid residue obtained by the reaction was dried at 105°C, and the dried residue was put into a tube-type atmosphere furnace under air, 500 o C roasting for 1h; reactivate the roasted residue, use hydrogen to remove the air in the tube first, the activation temperature is 300°C, the heating rate is 1°C / min, the hydrogen flow rate is kept at 60mL / min, and the activation time is 2h. After the activation process is completed, wait for the temperature to cool down to room temperature and take it out. Using straw as raw material, first crush the straw, take 15g of rice straw powder and pour it into a 250mL autoclave, add 75mL of deionized water, 75mL of ethanol and the solid residue after the activation of the above-mentioned roasting, stir to make a slurry, and fill the reaction kettle with 1.2MPaH 2 , heated to 300°C while stirring, kept for 30min, passed tap water to cool to room temperature, and poured out the reaction mixture. After the solid-liquid separation of ...

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Abstract

The present invention belongs to the technical field of environmental protection and bio-based chemicals, and specifically relates to a method for preparing bio-based phenol compounds through catalytic liquefaction on rice straw. The method comprises: crushing collected rice straw, grinding, carrying out other simple treatments, directly pouring into a high pressure reaction kettle according to a certain solid liquid ratio, introducing hydrogen with a certain pressure into the reaction kettle, selecting industrial copper-zinc-aluminum as a catalyst, carrying out stirring heating to a temperature of 200-340 DEG C, maintaining the temperature for 5-120 min, rapidly cooling to a room temperature, collecting, filtering the reaction mixture, respectively extracting the water phase and the solid phase with an organic solvent, and carrying out qualitative analysis and quantitative phenol compound analysis on the extraction phase obtained through the liquid separation by using a gas chromatography mass spectrometry (GC-MS). According to the method of the present invention, the rice straw is adopted as the raw material, the method can be used to carry out the liquefaction treatment on the rice straw in the large-scale and direct manner while the high added value phenol chemicals are obtained, such that the resource utilization of the rice straw is achieved while the environmental problem and the society problem caused by burning of a lot of the rice straw are reduced.

Description

technical field [0001] The invention belongs to the technical field of environmental protection and bio-based chemicals, and in particular relates to a method for preparing phenolic compounds by hydrothermally catalyzing liquefaction of rice straw. Background technique [0002] Rice, an annual grass plant, likes high temperature, humidity, and short sunshine, and has no strict requirements on soil. Nearly half of the world's population feeds on rice. The northernmost limit of rice growth is Huma, Heilongjiang Province, China. The main growing areas are southern China, Taiwan, Japan, the Korean Peninsula, Southeast Asia, South Asia, the Mediterranean coast, and the southeastern United States. Rice is also grown in parts of Central America, Oceania and Africa, and along rivers in northern China. Rice is grown almost everywhere except Antarctica. As the crop with the largest planting area and the highest yield in China, a lot of rice straw (rice straw) is produced every year....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/00C07C39/00
CPCC07C37/004C07C39/00
Inventor 张士成周超朱向东郝诗来陈建民
Owner FUDAN UNIV