Technique for extracting lignin from biomass raw materials

A technology of biomass raw material and lignin, which is applied in the field of lignin extraction technology, can solve problems such as difficult separation, unsuitable lignin extraction, and affecting processing efficiency, and achieve the effects of intensified degradation and dissolution, shortened cooking time, and simple process route

Active Publication Date: 2013-04-10
JINAN SHENGQUAN GROUP SHARE HLDG
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Problems solved by technology

However, this patent also has the following disadvantages: 1. From the description in the manual, it can be seen that the process uses organic acid mixed with a catalyst represented by sulfuric acid for the first step of catalysis, and a catalyst needs to be added for catalysis during the reaction; 2. This process uses organic acid and a catalyst represented by sulfuric acid to cook biomass together. In the step of distilling organic acid, if the distillation of organic acid is not complete, the lignin cannot be completely precipitated. If the organic acid is completely distilled, add it The concentration of sulfuric acid increases, which will carbonize the lignin and affect the extraction rate of lignin; 3. Although the same organic acid is used for extracting and washing cellulose in the whole process, and the collected pretreatment liquid and washing liquid are directly used In the reaction kettle that is circulated to the first step, a large amount of lignin and pentose sugar solution dissolved therein also accumulate in the whole mixed liquor. In view of the limitation of the saturation degree of organic acid extraction, the effectiveness of the mixed black liquor to extract lignin will be reduced. Therefore, although this step is a cyclic reaction, it has little effect on the overall extraction efficiency; 4. The black liquor obtained by mixing needs to be circulated for more than 3 times before being distilled to separate the organic acid and dilute the obtained concentrated The liquid makes the lignin precipitate, which will cause a huge amount of black liquor and concentrated liquid to be processed at one time, which not only affects the treatment efficiency but also makes it difficult to realize the continuity of the process; 5. It can be seen from the manual that the lignin extraction in this process The extraction rate is only 6-16%, and the extraction rate of the whole process is relatively low
Although this method solves the problem of adding a catalyst in the process of cooking biomass, since this method is mainly used for pulp preparation, its purpose is to retain cellulose and part of hemicellulose to the greatest extent, and the entire process design is based on This is for the purpose, but the loss of lignin is not considered, and the treatment process for lignin is not given, so this process is not applicable to the process with lignin as the extraction product
[0007] "Research on Milox Solvent Method for Bleaching Bamboo Pulp" (Liang Fang, Liu Yakang, etc., Zhonghua Paper Industry, 2007, 28 (4), 40-43), shows that adopting formic acid and hydrogen peroxide as a kind of solvent pulping of cooking chemicals method to achieve the effect of dissolving or softening lignin, but the above method is a long-term steaming process at low temperature, the presence of a large amount of formic acid destroys the carbohydrates in the raw material, and because a small amount of acetic acid is produced during the hydrolysis of the raw material, The removal rate of hemicellulose in the raw material is reduced, and if you want to separate a small amount of acetic acid from formic acid in the whole process, the steps are complicated and difficult to separate. Therefore, the above method is not suitable for the extraction of lignin

Method used

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  • Technique for extracting lignin from biomass raw materials

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Embodiment 1

[0039] In this embodiment, the reeds (with a lignin content of 25.10%) are first crushed to a particle size of 2-10 cm.

[0040] The present embodiment extracts the technique of lignin from described reed, comprises the steps:

[0041] (1) After the reeds are pulverized and pretreated, use the organic acid liquid whose total acid concentration is 70% formic acid and acetic acid to cook the treated reeds. The mass ratio of acetic acid and formic acid in the organic acid liquid of the present embodiment is 1: 1, and before adding the reed raw material, add 3% hydrogen peroxide (H 2 o 2 ) as a catalyst, control the reaction temperature at 115°C, react for 55min, and have a solid-liquid mass ratio of 1:5, and carry out the first solid-liquid separation of the obtained reaction solution;

[0042] (2) adding the solid obtained from the above separation to the same acid solution as the organic acid solution described in step (1) for acid washing, wherein the amount of hydrogen pero...

Embodiment 2

[0046] In this embodiment, firstly, corn stalks (with a lignin content of 24.09%) were crushed to a particle size of 2-10 cm.

[0047] The present embodiment extracts the technology of lignin from described corn stalk, comprises the steps:

[0048] (1) After the corn stalks are pulverized and pretreated, use the organic acid liquid whose total acid concentration is 75% formic acid and acetic acid to cook the treated corn stalks, the quality of acetic acid and formic acid in the organic acid liquid of the present embodiment The ratio is 1:2, and before adding corn stalks, add 2% hydrogen peroxide (H 2 o 2 ) as a catalyst, control the reaction temperature at 90°C, react for 40min, and have a solid-liquid mass ratio of 1:15, and carry out the first solid-liquid separation of the obtained reaction solution;

[0049] (2) Add the solid obtained from the above separation into the same acid solution as the organic acid solution described in step (1) for acid washing, wherein the amo...

Embodiment 3

[0053] In this embodiment, the rice straw (19.07% lignin content) is first crushed to a particle size of 2-10 cm.

[0054] The present embodiment extracts the technique of lignin from described rice straw, comprises the steps:

[0055] (1) After the rice straw is pulverized and pretreated, the organic acid solution of formic acid and acetic acid with a total acid concentration of 80% is used to cook the treated rice straw. The mass ratio of acetic acid and formic acid in the organic acid solution of the present embodiment is 1: 6, and add before adding the straw raw material and account for 4% hydrogen peroxide (H 2 o 2 ) as a catalyst, the reaction temperature is controlled at 135° C., the reaction is 70 minutes, the solid-liquid mass ratio is 1:10, and the obtained reaction solution is subjected to solid-liquid separation for the first time;

[0056] (2) adding the solid obtained from the above separation into the same acid solution as the organic acid solution described i...

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Abstract

The invention relates to a technique for extracting lignin, in particular to a technique of utilizing organic acid to extract the lignin from biomass raw materials by a catalytic action of hydrogen peroxide. According to the method, the lignin is obtained by extracting the biomass raw materials boiled by organic acid formed by methanoic acid and acetic acid by the catalytic action of hydrogen peroxide; a whole technique route is simple; the energy consumption is lower; and an extraction ratio of the lignin reaches 80-90%.

Description

technical field [0001] The invention relates to a lignin extraction process, in particular to a process for extracting lignin from biomass raw materials by using organic acids. Background technique [0002] Lignin is a valuable chemical raw material. High-purity sulfur-free lignin can be used as polymer additives such as phenolic resins, polyurethane foams, and epoxy resins, as well as soil improvers, pesticide slow-release agents, etc. Lignin is used in These aspects can make its added value much higher than that of recovering heat after combustion as fuel. At present, lignin is mainly produced as a by-product of pulping and papermaking, such as lignosulfonate, kraft lignin, etc. However, these lignins contain sulfur and have low purity, complex components, wide molecular weight distribution, low viscosity, high dispersion, poor processability, and almost no thermoplastic properties, which greatly limit their industrial applications. Therefore, the development of a clean ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C08H8/00
Inventor 唐一林江成真刘洁刘云鹏高绍丰
Owner JINAN SHENGQUAN GROUP SHARE HLDG
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