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A kind of method and its application of using oxygen to catalyze ethanol to prepare nanometer lignin

A technology of lignin and ethanol, which is applied in the direction of fermentation, etc., can solve the problems of inability to produce autocatalytic effect, high cooking temperature and operating pressure, and limit the scope of application, so as to improve the safety of process operation, low molecular weight, and wide application range Effect

Active Publication Date: 2021-03-23
ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the acetyl group content in the hemicellulose of softwood raw materials is very small, it cannot produce autocatalytic effect
[0006] 2) The cooking temperature is too high and the operating pressure is too high
The pressure of 65% ethanol aqueous solution at 195°C can reach 2.3MPa, which obviously brings great operational risks
However, in this technical scheme, the lignin separated from the waste liquid contains sulfur by using the alkali method or the kraft method for pulping, which limits its scope of application; aqueous or organic solvent, and then precipitate it with an anti-solvent
Due to the use of corrosive or organic reagents in this process, such as dioxane and tetrahydrofuran, the preparation process has potential environmental hazards

Method used

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  • A kind of method and its application of using oxygen to catalyze ethanol to prepare nanometer lignin
  • A kind of method and its application of using oxygen to catalyze ethanol to prepare nanometer lignin
  • A kind of method and its application of using oxygen to catalyze ethanol to prepare nanometer lignin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] S1: Crushing the straw. Shorten the wheat straw to about 5 cm, put it into a pulverizer, run it for 30 seconds to obtain powdery straw, and dry it at 105°C for 4 hours to obtain dry powdery straw.

[0048]S2: Accurately weigh 10 g of absolute dry powdery straw, and place it in a 250 mL reaction kettle. Prepare an aqueous ethanol solution with a mass concentration of 70% with distilled water, and add it to the reaction kettle according to the ratio of material to liquid 1:10.

[0049] S3: Start the stirring rotor to stir, seal the reaction kettle, open the gas inlet and outlet valves, pass oxygen into the reaction kettle for 5 minutes, judge according to experience and common sense that the air above the material is completely replaced by oxygen, and then close the gas outlet valve.

[0050] S4: Start the reactor, heat it to 70°C, and keep it warm for 2 hours to react. During the reaction, keep oxygen flowing. When the pressure in the reactor reaches about 0.8-1.3Mpa, t...

Embodiment 2

[0059] S1: Crushing the straw. Shorten the wheat straw to about 5 cm, put it into a pulverizer, run it for 30 seconds to obtain powdery straw, and dry it at 105°C for 4 hours to obtain dry powdery straw.

[0060] S2: Accurately weigh 10 g of absolute dry powdery straw, and place it in a 250 mL reaction kettle. Prepare an aqueous ethanol solution with a mass concentration of 80% with distilled water, and add it to the reaction kettle according to the ratio of material to liquid 1:20.

[0061] S3: Start the stirring rotor to stir, seal the reaction kettle, open the gas inlet and outlet valves, pass oxygen into the reaction kettle for 5 minutes, judge according to experience and common sense that the air above the material is completely replaced by oxygen, and then close the gas outlet valve.

[0062] S4: Start the reactor, heat it to 80°C, and keep it warm for 3 hours to react. During the reaction, keep oxygen flowing. When the pressure in the reactor reaches about 0.8-1.3Mpa, ...

Embodiment 3

[0071] S1: Crushing the straw. Shorten the wheat straw to about 5 cm, put it into a pulverizer, run it for 30 seconds to obtain powdery straw, and dry it at 105°C for 4 hours to obtain dry powdery straw.

[0072] S2: Accurately weigh 5 g of dry powdered straw and place it in a 250 mL reaction kettle. Prepare an aqueous ethanol solution with a mass concentration of 80% with distilled water, and add it to the reaction kettle according to the ratio of material to liquid 1:30.

[0073] S3: Start the stirring rotor to stir, seal the reaction kettle, open the gas inlet and outlet valves, pass oxygen into the reaction kettle for 5 minutes, judge according to experience and common sense that the air above the material is completely replaced by oxygen, and then close the gas outlet valve.

[0074] S4: Start the reactor, heat it to 90°C, and keep it warm for 2 hours to react. During the reaction, keep oxygen flowing. When the pressure in the reactor reaches about 0.8-1.3Mpa, the pressu...

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Abstract

The invention belongs to the technical field of resource regeneration and utilization and particularly relates to a method for preparing nano lignin by using oxygen catalytic ethanol and application of the method. Under a low-temperature low-pressure condition, lignin is extracted by using oxygen catalytic ethanol, and compared with a conventional catalytic ethanol pulping technique, the method issafe in pulping process and high in lignin yield. The method is technically characterized by comprising the following steps: putting crushed straw into a reaction kettle, and adding an ethanol solution; introducing oxygen into the reaction kettle, after air above a material is completely substituted by the oxygen, sealing the reaction kettle; heating, and keeping the temperature to implement reactions; after the reactions end, opening the valve of the reaction kettle, and releasing the pressure; after pressure release is completed, filtering immediately, and separating the straw from a liquid; distilling the liquid, and removing ethanol so as to obtain a lignin mixture; hydrolyzing the lignin mixture, performing retrogradation precipitation on the lignin, centrifuging, and performing freeze drying on precipitate of a lower layer, thereby obtaining lignin.

Description

technical field [0001] The invention belongs to the technical field of resource regeneration and utilization, and in particular relates to a method for preparing nanometer lignin by catalyzing ethanol with oxygen and its application. Background technique [0002] There are about 1 billion tons of agricultural waste in my country every year, mainly wheat straw and rice straw, etc. Most of the wheat straw and rice straw are still at the level of rough processing or unprocessed. Straws such as wheat straw contain about 60% to 80% of cellulose and about 15% to 25% of lignin. If wheat straw or rice straw is burned directly, it will not only aggravate the severity of smog, but also cause agricultural waste. massive waste of biomass resources. [0003] At present, the effective utilization of agricultural waste is mainly to use wheat straw to make paper, and the more mature method is alkaline pulping. However, the high silicon content in non-wood biomass raw materials such as whe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H7/00C12P1/00
CPCC08H6/00C12P1/00C12P2201/00
Inventor 李静罗江浩章沈翀
Owner ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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