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A method for preparing guaiacol and phenol by microwave-assisted depolymerization of lignin

A microwave-assisted, guaiacol technology, applied in the fields of biomass energy and chemicals, can solve the problems of low controllability of product components, high cost input, low yield of conversion products, etc., and achieves utilization value and economy. Good effect, reduce side reactions, improve heat transfer efficiency

Active Publication Date: 2022-06-07
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A certain degree of degradation of lignin can be achieved by means of thermochemical conversion. However, at present, there are problems such as low degradation efficiency, serious charring phenomenon, low conversion product yield, and difficult product collection, which seriously restrict lignin. Efficient transformation and utilization of nutrients
[0004] At present, most researches realize the degradation of lignin under high pressure, high temperature and a large amount of hydrogen atmosphere, but the high cost input and low controllability of product components restrict the development of technology, and the liquid oil obtained by pyrolysis is often as high as above There are hundreds of species, which have caused great obstacles to the purification and application of its high-value components

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 3g glycine and 15g Fe (NO 3 ) 3 ·7H 2 O was dissolved in 1000 mL of a mixture of ethanol and water (the volume ratio of ethanol and water was 1:2), hydrothermally reacted at 150 °C for 12 hours, cooled to room temperature, washed three times with ethanol and distilled water, and then dried at 50 °C Dry in the box for 8 hours to obtain Fe 2 O 3 Nanospheres; dissolve 1 g of alkali lignin in 1000 mL of tetrahydrofuran, then add 2 g of Fe obtained above 2 O 3 Nanospheres, after fully stirring for 3 hours, placed in a dialysis bag with a molecular weight cut-off of 8000, put the dialysis bag into deionized water, and slowly stirred and dialyzed in a fume hood for 24 hours to obtain core-shell Fe 2 O 3 @Lignin was washed 4 times with absolute ethanol and dried at 100 °C for 12 h to obtain dry core-shell Fe 2 O 3 @Lignin; add 1g ammonium molybdate and 5g thiourea to 150mL deionized water and mix well, stir at 60°C for 6 hours, add oxalic acid, adjust pH to 2, take the ...

Embodiment 2

[0041] 3g glycine and 30g Fe (NO 3 ) 3 ·7H 2 O was dissolved in 500 mL of a mixture of ethanol and water (the volume ratio of ethanol and water was 1:2), hydrothermally reacted at 180 °C for 12 hours, cooled to room temperature, washed with ethanol and distilled water for 4 times, and then dried at 80 °C Dry in the box for 6 hours to obtain Fe 2 O 3 Nanospheres; dissolve 1 g of solvent lignin in 200 mL of tetrahydrofuran, then add 0.5 g of Fe obtained above 2 O 3 Nanospheres, after fully stirring for 3 hours, placed in a dialysis bag with a molecular weight cut-off of 14,000, put the dialysis bag into deionized water, and slowly stirred and dialyzed in a fume hood for 36 hours to obtain core-shell Fe 2 O 3 @Lignin was washed 6 times with absolute ethanol and dried at 80 °C for 12 h to obtain dry core-shell Fe 2 O 3 @Lignin; add 1 g of ammonium molybdate and 2 g of thiourea into 80 mL of deionized water and mix well, stir at 50°C for 6 hours, add oxalic acid, adjust the...

Embodiment 3

[0043] 3g glycine and 24g Fe (NO 3 ) 3 ·7H 2 O was dissolved in 750 mL of a mixture of ethanol and water (the volume ratio of ethanol and water was 1:2), hydrothermally reacted at 200 °C for 12 hours, cooled to room temperature, washed with ethanol and distilled water for 5 times, and then dried at 60 °C Dry in the box for 7 hours to obtain Fe 2 O 3 Nanospheres; 1 g of sulfated lignin was dissolved in 500 mL of tetrahydrofuran, and then 1 g of Fe obtained above was added 2 O 3 Nanospheres, after fully stirring for 3 hours, placed in a dialysis bag with a molecular weight cut-off of 10,000, put the dialysis bag into deionized water, and slowly stirred and dialyzed in a fume hood for 48 hours to obtain core-shell Fe 2 O 3 @Lignin was washed 5 times with absolute ethanol and dried at 90 °C for 12 h to obtain dry core-shell Fe 2 O 3 @Lignin; add 1g ammonium molybdate and 3g thiourea to 100mL deionized water and mix well, stir at 40°C for 6 hours, add oxalic acid, adjust pH...

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Abstract

The invention discloses a method for preparing guaiacol and phenol by microwave-assisted depolymerization of lignin. By compounding microwave absorption medium, lignin and catalyst, a microwave reactant with a "sandwich" structure is designed, which has a great It increases the contact area between lignin, catalyst and microwave absorbing medium, reduces the generation of side reactions, and has positive significance for the directional regulation mechanism control of lignin conversion into high-value guaiacol and phenol.

Description

technical field [0001] The invention belongs to the technical field of biomass energy and chemicals, in particular to a method for preparing guaiacol and phenol by microwave-assisted depolymerization of lignin. Background technique [0002] Lignin is one of the important components of biomass and the second most abundant biopolymer on earth after cellulose. In addition to its huge reserves in nature, lignin is also a major by-product of the pulp and paper industry, and the pulp and paper industry produces about 50 million tons of lignin each year, but only about 2% of the lignin is separated for use in various products, Most are discarded as waste, or burned to recover heat and generate electricity, resulting in a huge waste of resources. For this reason, it is imperative to find new high value-added applications of lignin. [0003] Lignin has both carbon chains and aromatic rings in its structure, and is connected with a methoxy group (-OCH). 3 ), hydroxyl (-OH), carboxy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/00C07C41/01C07C43/23C07C39/04B01J27/051
CPCC07C41/01C07C37/004C07C37/005B01J27/0515C07C43/23C07C39/04Y02P20/52
Inventor 王文亮黄佳乐马振浩薛白亮游翔宇段超李金宝李新平
Owner SHAANXI UNIV OF SCI & TECH
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