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Method for extracting hydrogenated lignin from paper making black liquor by adopting electrolytic hydrogenation process

A paper-making black liquor and lignin technology, which is applied in the direction of lignin derivatives, chemical instruments and methods, electrolysis process, etc., can solve the problems of difficulty in controlling the degree of hydrogenation, high cost and energy consumption, and high price, and achieve hydrogenation Conditions are easy to control, quality is improved, and equipment is simple

Inactive Publication Date: 2003-09-17
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrogen-donating solvent used in the solvent hydrogenation process, such as tetrahydroquinoline, is expensive, with high cost and energy consumption, which affects its industrial application
Hydrogenated anthracene oil can be used as an alternative solvent. However, steps such as separation and rehydrogenation of anthracene oil are added to the process, and a huge auxiliary system is required.
The problem in the catalytic hydrogenation process is that the degree of hydrogenation is difficult to control, and the catalyst particles mixed with lignin are difficult to remove, which directly affects the quality of hydrogenated lignin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In an isolated electrolyzer, metal platinum is used as the anode, foamed lead is used as the cathode, and a saturated calomel electrode is used as the reference electrode, and 3.7mol / L of N,N dimethylformamide, 1.1mol / L of ethanol, 10.4 mol / L of water, 0.06mol / L of tetrabutylammonium bromide, and 28g / L of lignin, in the process of electrolysis, nitrogen gas is passed through for slow bubbling protection, and the cathode potential is controlled at 2.2v (vs.SCE), The electrolysis temperature is 20°C, after electrolysis for 8 hours, the electrolysis product is taken out, separated by a centrifuge at 3000r / min for 5 minutes and filtered to obtain hydrogenated lignin, then washed with distilled water, dried at 80°C for 5 hours, and the hydrogenated lignin The carbon ratio increased by 0.11, and the softening point decreased by 11°C.

Embodiment 2

[0021] In an isolated electrolytic cell, platinum is used as the anode, lead foam is used as the cathode, and a saturated calomel electrode is used as the reference electrode. Add 4.9mol / L of N, N dimethylformamide, 2.9mol / L of ethanol, 15.4mol / L of water, 0.11mol / L of tetrabutylammonium bromide and 46g / L of lignin, in the process of electrolysis, feed nitrogen gas for slow bubbling protection, control the cathode potential at 2.2v (vs.SCE), and the electrolysis temperature After 12 hours of electrolysis at 30°C, the electrolysis product hydrogenated lignin was taken out, separated by a centrifuge at 3000r / min for 5 minutes and filtered to obtain hydrogenated lignin, then washed with distilled water, and dried at 80°C for 5 hours, the hydrogen-carbon ratio of the hydrogenated lignin Increased by 0.17, and the softening point decreased by 22°C.

Embodiment 3

[0023] In an isolated electrolytic cell, platinum is used as the anode, lead foam is used as the cathode, and a saturated calomel electrode is used as the reference electrode. Add 5.8mol / L of N, N dimethylformamide, 4.3mol / L of ethanol, 19.4mol / L of water, 0.17mol / L of tetrabutylammonium bromide and 64g / L of lignin, in the process of electrolysis, nitrogen gas is slowly bubbled for protection, the cathode potential is controlled at 2.2v (vs. SCE), and the electrolysis temperature is 40 ℃, after 16 hours of electrolysis, take out the electrolyzed product, separate it by a centrifuge at 3000r / min for 5 minutes and filter to obtain hydrogenated lignin, then wash it with distilled water and dry it at 80℃ for 5 hours, the hydrogen-carbon ratio of the hydrogenated lignin increases by 0.19, The softening point dropped by 25°C.

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Abstract

The invention relates to a method for preparing hydrogenated lignin by using an electrolytic hydrogenation process. The method uses foamed Pb as cathode, Pt as anode, saturated calomel electrode as reference electrode, N,N dimethylformamide and ethanol as electrolytic solvent and water as hydrogen-donating solvent in an isolated electrolytic cell. Butylammonium bromide is used as a supporting electrolyte for electrolytic hydrogenation of lignin. The process has mild operating conditions, no catalyst, water as the hydrogen supply solvent, no pollution, easy control of the hydrogenation process, simple equipment, and low cost. After hydrogenation, the softening point of hydrogenated lignin decreases and the hydrogen-to-carbon ratio increases.

Description

technical field [0001] The invention relates to an electrolytic hydrogenation technology for lignin in papermaking black liquor, in particular to a method for preparing hydrogenated lignin from papermaking black liquor by using the electrolytic hydrogenation process. Background technique [0002] Lignin, cellulose and hemicellulose are the main components of the plant skeleton, and they are relatively abundant renewable resources in nature. Lignin produces alkali lignin in the paper pulping process and dissolves in black liquor. After it is discharged into rivers, it not only pollutes the environment, but also wastes a lot of lignin resources. more and more people's attention. [0003] Lignin is a by-product of the paper industry. It has abundant sources and high carbon content. Compared with other raw materials, lignin has greater advantages in terms of economic cost. From the perspective of the structure of lignin, it is an amorphous polymer with a ne...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F1/44C25B3/25
Inventor 张建安张小勇韩润林李佐虎
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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