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Preparation method of hydroxymethylated lignin

A technology for hydroxymethylation and lignin is applied in the field of microwave-assisted hydroxymethylation modified lignin preparation, and can solve the problems of low lignin activity and slow hydroxymethylation efficiency.

Inactive Publication Date: 2017-04-05
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Technical problem to be solved: In order to solve the shortcomings of low lignin activity and slow hydroxymethylation efficiency, the invention provides a preparation method of microwave-assisted hydroxymethylation modified lignin

Method used

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  • Preparation method of hydroxymethylated lignin

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Experimental program
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Effect test

Embodiment 1

[0017] Dissolve 10g of biomass butanol lignin in 40mL of 2% NaOH solution, adjust the pH to 9 with 40% NaOH solution while stirring, add 8g of 37% formaldehyde solution and stir evenly, place the mixed solution in a microwave reactor, and React at 70°C for 15min, 30min, 45min, 60min, take samples respectively, cool to room temperature, take a small part to measure the content of free aldehyde, add acid to precipitate the rest, filter, wash and dry to obtain hydroxymethylated lignin. The amount of formaldehyde consumed measured at four times was 41.15mmol / 100gLignin, 60.06mmol / 100gLignin, 83.07mmol / 100gLignin, and 105.85mmol / 100gLignin.

Embodiment 2

[0019] Dissolve 10g of biomass butanol lignin in 40mL of 2% NaOH solution, adjust the pH to 10.5 with 40% NaOH solution while stirring, add 10g of 37% formaldehyde solution and stir evenly, put the mixed solution in a microwave reactor, React at ℃ for 15min, 30min, 45min, 60min, take samples respectively, cool to room temperature, take a small part to measure the content of free aldehyde, add acid to precipitate the rest, filter, wash and dry to obtain hydroxymethylated lignin. The amount of formaldehyde consumed measured at four times was 150.01mmol / 100gLignin, 203.54mmol / 100gLignin, 213.97mmol / 100gLignin, and 223.42mmol / 100gLignin.

Embodiment 3

[0021] Dissolve 10g of biomass butanol lignin in 40mL of 2% NaOH solution, adjust the pH to 12 with 40% NaOH solution while stirring, add 15g of 37% formaldehyde solution and stir evenly, put the mixed solution in a microwave reactor, and React at 70°C for 15min, 30min, 45min, 60min, take samples respectively, cool to room temperature, take a small part to measure the content of free aldehyde, add acid to precipitate the rest, filter, wash and dry to obtain hydroxymethylated lignin. The amount of formaldehyde consumed measured at four times was 292.20mmol / 100gLignin, 330.29mmol / 100gLignin, 347.59mmol / 100gLignin, 347.36mmol / l00gLignin.

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Abstract

The invention discloses a preparation method of hydroxymethylated lignin with microwave assist. The method comprises the following steps: dissolving lignin in an alkaline solution, adjusting pH to be 9-12, adding a certain amount of a formaldehyde solution while performing uniform stirring, putting the obtained mixed solution in a microwave reactor, carrying out a reaction at a certain temperature in a range of 70-90 DEG C for 15-45 min, performing cooling to the room temperature, adding acid for precipitation, and performing filtration, washing and drying to obtain hydroxymethylated lignin. The hydroxymethylated lignin is prepared through microwave-assisted heating. The method is short in reaction time, low in energy, and increased in hydroxyl group content of lignin. The method is beneficial for further application of lignin and has bright application prospects.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to the preparation of microwave-assisted hydroxymethylation modified lignin. Background technique [0002] Lignin is the most abundant renewable polyphenolic compound in nature. However, due to its complex molecular structure and few active sites, lignin has low reactivity and is difficult to be utilized. In order to improve its activity, a large number of scholars have carried out research on the modification of lignin. The hydroxymethylation of lignin is one of the commonly used methods for lignin modification. In the patent 201310197577.1, conventional heating is used, and the hydroxymethylation modification is completed after 1-2 hours of reaction at 60-90°C. However, the reaction Long time and low efficiency limit the application of lignin. [0003] Microwave heating technology is widely used in the synthesis and extraction of substances due to its high heat...

Claims

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Application Information

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IPC IPC(8): C08H7/00
Inventor 许玉芝夏成龙高士帅王春鹏储富祥
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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