Method for preparing monophenol compound through catalyzing degradation of lignin by using ammino-complex

A technology of ammonia complexes and lignin, which is applied in the field of preparing monophenolic compounds by using ammonia complexes to catalyze the degradation of lignin, can solve the problems of complicated product purification operations, poor selectivity of degradation products, and low product yields, and achieve improved Effect of product selectivity, increased contact sites, high degradation rate

Active Publication Date: 2017-07-14
GUANGXI ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has the advantages of mild conditions, high yield, and short reaction time. However, the above-mentioned process still has many side reactions, poor selectivity of degradation products, complex purification operations of products after reactions, and low product yields.

Method used

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  • Method for preparing monophenol compound through catalyzing degradation of lignin by using ammino-complex
  • Method for preparing monophenol compound through catalyzing degradation of lignin by using ammino-complex
  • Method for preparing monophenol compound through catalyzing degradation of lignin by using ammino-complex

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) In parts by weight, 5 parts of bagasse lignin, 0.5 parts of sodium hydroxide, 8 parts of hydrogen peroxide aqueous solution with a mass fraction of 4:1 in a weight ratio of 30% and a mass fraction of 5% The mixture of zinc chlorate aqueous solution, 0.15 parts of zinc acetate, 4 parts of ammonia solution with a mass fraction of 25% and 100 parts of deionized water are mixed, poured into a high-pressure reactor, quickly sealed and stirred evenly at a speed of 300 r / min. Forms a clear solution;

[0035] (2) Continue to maintain a stirring speed of 300r / min, heat the high-pressure reactor to 150°C, stop the reaction after 120min of reaction, and naturally cool to room temperature to obtain a primary degradation product;

[0036](3) Adjust the pH value of the primary degradation product to 2 with an aqueous sulfuric acid solution with an acid mass fraction of 10%, seal the high-pressure reactor, heat to 120° C., stop the reaction after reacting for 10 minutes, and natur...

Embodiment 2

[0044] (1) In parts by weight, 1 part of eucalyptus lignin, 0.5 part of potassium hydroxide, 0.5 part of hydrogen peroxide aqueous solution with a mass fraction of 3:1 in a weight ratio of 30% and a mass fraction of 5% The mixture of zinc chlorate aqueous solution, 0.1 part of zinc oxide, 1 part of ammonia solution with a mass fraction of 5% ammonia solution and 100 parts of deionized water are mixed, poured into a high-pressure reactor, quickly sealed and stirred at a speed of 300r / min Uniform, forming a clear solution;

[0045] (2) Continue to maintain a stirring speed of 300r / min, heat the high-pressure reactor to 120°C, stop the reaction after 100min of reaction, and naturally cool to room temperature to obtain a primary degradation product;

[0046] (3) After adjusting the pH value of the primary degradation product to 2 with a sulfuric acid aqueous solution with a mass fraction of 10%, seal the high-pressure reactor, heat to 100° C., stop the reaction after 10 minutes of...

Embodiment 3

[0050] (1) In parts by weight, 2 parts of bagasse lignin, 0.8 parts of sodium hydroxide, 4 parts of hydrogen peroxide aqueous solution with a mass fraction of 2:1 in a weight ratio of 30% and a mass fraction of 5% The mixture of zinc chlorate aqueous solution, 0.15 parts of zinc sulfate, 2 parts of ammonia solution with a mass fraction of 15% of ammonia solution and 100 parts of deionized water are mixed, poured into a high pressure reactor, quickly sealed and stirred at a speed of 300r / min Uniform, forming a clear solution;

[0051] (2) Continue to maintain a stirring speed of 300r / min, heat the high-pressure reactor to 135°C, stop the reaction after 150min of reaction, and naturally cool to room temperature to obtain a primary degradation product;

[0052] (3) After adjusting the pH value of the primary degradation product to 2.5 with an aqueous sulfuric acid solution with an acid mass fraction of 11%, seal the high-pressure reactor, heat to 105° C., stop the reaction after ...

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Abstract

The invention discloses a method for preparing a monophenol compound through catalyzing degradation of lignin by using an ammino-complex. The method comprises the steps: adding the lignin, a metal salt, ammonia water, a peroxidant, an alkali and deionized water into a high-pressure reaction vessel, and carrying out stirring to form a uniform solution; carrying out a reaction for 100 to 240 minutes at the temperature of 120 DEG C to 180 DEG C, and carrying out cooling; and adjusting the pH value of a reaction solution to 2 to 3 with an acid, then, carrying out a reaction for 10 to 20 minutes at the temperature of 100 DEG C to 120 DEG C, carrying out cooling, then, carrying out filtration to collect filtrate, carrying out extraction on the filtrate with dichloromethane, separating an organic phase, and carrying out drying with anhydrous calcium chloride, thereby obtaining a monophenol compound mixed solution. According to the method, a stable ammino-complex solution is formed by using the metal salt and the ammonia water under alkaline conditions, so that the number of sites of contact between a catalyst and the lignin can be effectively increased compared with that in the conventional lignin oxidative degradation method; the degradation of the lignin can be efficiently catalyzed in an aqueous solution under moderate reaction conditions; and the method has the characteristics of high efficiency and low cost and is applicable to large-scale industrial production.

Description

[0001] 【Technical field】 [0002] The invention relates to the field of comprehensive utilization of biomass, in particular to a method for preparing monophenolic compounds by catalyzing lignin degradation with ammonia complexes. [0003] 【Background technique】 [0004] With the dwindling of fossil energy sources, obtaining energy, fuels and chemicals from woody biomass has become crucial. Woody biomass has the characteristics of being renewable and extremely rich in resources. Lignin is one of the important components of woody biomass. The content of lignin in woody plants accounts for about 20-35%, and that of herbaceous plants is 14-25%. Its annual output is as high as 150 billion tons. In the structure of lignin, there are both carbon chains and benzene rings. There are hydroxyl groups, aldehyde groups, ketone groups, carboxyl groups or ethylenic bonds on the carbon chains, and hydroxyl groups and methoxy groups on the benzene rings. It is an extremely complex non-crystall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/54C07C39/04C07C45/00C07C45/51C07C47/565C07C47/575C07C49/825C07C49/84B01J31/18
CPCB01J31/1805C07C37/004C07C37/54C07C45/00C07C45/51C07C39/04C07C47/565C07C47/575C07C49/825C07C49/84Y02P20/52
Inventor 黎演明杜芳黎李秉正冼学权陈东
Owner GUANGXI ACAD OF SCI
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