CN112626903A - Method for extracting lignin from urea-assisted low-temperature alkali liquor - Google Patents

Method for extracting lignin from urea-assisted low-temperature alkali liquor Download PDF

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Publication number
CN112626903A
CN112626903A CN202011504577.8A CN202011504577A CN112626903A CN 112626903 A CN112626903 A CN 112626903A CN 202011504577 A CN202011504577 A CN 202011504577A CN 112626903 A CN112626903 A CN 112626903A
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China
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urea
lignin
alkali liquor
liquor
temperature
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徐建
王标
汪伟
李新龙
耿樊辉
张海诚
邱华伟
张楷
徐霞
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Anhui University of Technology AHUT
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Anhui University of Technology AHUT
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00Pulping cellulose-containing materials
    • D21C3/02Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes

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  • Inorganic Chemistry (AREA)
  • Compounds Of Unknown Constitution (AREA)

Abstract

The invention discloses a method for extracting lignin by using urea-assisted low-temperature alkali liquor, which belongs to the technical field of high-value conversion and utilization of agricultural wastes and comprises the following steps: (1) crushing, sieving, washing and drying corn straws to obtain corn straw powder; (2) adding urea into an alkali liquor to obtain a mixed liquor, then adding corn straw powder into the mixed liquor, carrying out lignin extraction operation treatment, and obtaining a slurry after the reaction is finished; (3) carrying out reduced pressure suction filtration separation on the slurry to obtain filtrate and filter residue, washing the residue with distilled water to obtain washing liquid, combining the washing liquid and the filtrate, regulating the pH value to 2 after reduced pressure concentration, standing for 2-3h, then carrying out centrifugal separation to obtain a precipitate, and drying the precipitate to obtain lignin; according to the invention, the dissolution of lignin in the corn straw in the low-temperature alkali liquor is promoted by using the additive urea and the good swelling effect of the urea, so that the production efficiency of the lignin is improved, and the production cost is reduced.

Description

Method for extracting lignin from urea-assisted low-temperature alkali liquor
Technical Field
The invention relates to the technical field of high-valued conversion and utilization of agricultural wastes, in particular to a method for extracting lignin from urea-assisted low-temperature alkali liquor.
Background
With the rapid development of social economy, the annual consumption of non-renewable resources such as petroleum and coal by human beings is rapidly increased, which leads to the increasing exhaustion of petrochemical resources on the earth. Meanwhile, when the traditional energy sources are developed and utilized, serious environmental problems (such as air pollution, greenhouse effect, ozone layer holes, acid rain and the like) can be caused, and the production and the life of human beings are adversely affected. With the excessive consumption of non-renewable energy sources such as petroleum and the like and the improvement of human environmental awareness, the development of renewable resources to replace traditional petrochemical resources becomes a research hotspot of energy researchers in all countries in the world. China is a big agricultural country and can generate a large amount of straws every year, and the treatment mode of the straws is mainly direct burning or smashing and backfilling in the past. Straw is used as a lignocellulose material and mainly comprises three components of cellulose, hemicellulose and lignin, and the extensive treatment (direct burning or crushing and backfilling) of the straw not only causes the waste of resources, but also can bring huge damage to the natural environment. In recent years, with the improvement of environmental protection requirements, the outdoor straw burning is controlled to a certain extent, but the research on high-value conversion and utilization of the straw needs to be strengthened.
The lignin in the straw is a natural aromatic compound polymer, and has great potential for replacing or partially replacing fossil resources as raw materials for producing aromatic compounds. However, in the straw, the connection between lignin and cellulose and hemicellulose is very complicated, which brings great difficulty to the separation and extraction of lignin. In the prior art, the common lignin separation and extraction method requires higher temperature and pressure, and such extraction conditions put higher requirements on the reaction vessel.
Therefore, a method for extracting lignin by using urea-assisted low-temperature alkali liquor is provided to solve the problems.
Disclosure of Invention
The invention aims to provide a method for extracting lignin by using urea-assisted low-temperature alkali liquor, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following scheme to realize the following steps:
the invention provides a method for extracting lignin by urea-assisted low-temperature alkali liquor, which specifically comprises the following steps:
(1) crushing, sieving, washing and drying corn straws to obtain corn straw powder;
(2) adding urea into an alkali liquor to obtain a mixed liquor, then adding corn straw powder into the mixed liquor, carrying out lignin extraction operation treatment, and obtaining a slurry after the reaction is finished;
(3) and carrying out reduced pressure suction filtration separation on the slurry to obtain filtrate and filter residue, washing the residue with distilled water to obtain washing liquid, combining the washing liquid and the filtrate, regulating the pH value to 2 after reduced pressure concentration, standing for 2-3h, then carrying out centrifugal separation to obtain a precipitate, and drying the precipitate to obtain the lignin.
Preferably, in the step (1), the particle size of the corn stalk powder is 10-100 meshes.
Preferably, in the step (2), the alkali solution is any one of sodium hydroxide solution and potassium hydroxide.
Preferably, in the step (2), the mass concentration of the alkali liquor is 1-5%.
Preferably, in the step (2), the addition amount of the urea is 1-10% of the total mass of the mixed solution.
Preferably, in the step (2), the solid-to-liquid ratio of the corn stalk powder to the mixed solution is 1 (10-20), and the solid-to-liquid ratio is a mass-to-volume ratio (g/ml).
Preferably, in the step (2), the reaction temperature is 40 ℃ and the reaction time is 1-5 h.
The invention has the beneficial effects that:
the invention has the advantages that:
1. the lignin separation and extraction conditions are mild, and the operation is convenient;
2. the temperature is low during treatment, and the requirement on equipment is low;
3. the additive urea is a cheap and reproducible chemical, and the good swelling effect of the urea is utilized to promote the dissolution of lignin in the corn straws in low-temperature alkali liquor, so that the production efficiency of the lignin is improved, and the production cost is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for extracting lignin by urea-assisted low-temperature alkali liquor comprises the following steps:
(1) crushing, sieving, washing and drying corn straws to obtain corn straw powder;
(2) adding urea into an alkali liquor to obtain a mixed liquor, then adding 15g of corn straw powder into 150ml of the mixed liquor, carrying out lignin extraction operation treatment, and reacting for 2 hours at 40 ℃ to obtain a slurry;
(3) and carrying out reduced pressure suction filtration separation on the slurry to obtain filtrate and filter residue, washing the residue with distilled water to obtain washing liquid, combining the washing liquid and the filtrate, regulating the pH value to 2 after reduced pressure concentration, standing for 3 hours, then carrying out centrifugal separation to obtain a precipitate, and drying the precipitate to obtain the lignin.
In the step (1), the grain diameter of the corn straw powder is 10-100 meshes; in the step (2), the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. In the step (2), the addition amount of urea accounts for 5% of the total mass of the mixed solution.
Through analysis, the dissolution rate of the lignin reaches 68.82%, and compared with that of the lignin without urea (only 5% NaOH solution is adopted), the dissolution rate of the lignin is improved by 7.12%.
Example 2
A method for extracting lignin by urea-assisted low-temperature alkali liquor comprises the following steps:
(1) crushing, sieving, washing and drying corn straws to obtain corn straw powder;
(2) adding urea into an alkali liquor to obtain a mixed liquor, then adding 15g of corn straw powder into 150ml of the mixed liquor, carrying out lignin extraction operation treatment, and reacting for 3 hours at 40 ℃ to obtain a slurry;
(3) and carrying out reduced pressure suction filtration separation on the slurry to obtain filtrate and filter residue, washing the residue with distilled water to obtain washing liquid, combining the washing liquid and the filtrate, regulating the pH value to 2 after reduced pressure concentration, standing for 3 hours, then carrying out centrifugal separation to obtain a precipitate, and drying the precipitate to obtain the lignin.
In the step (1), the grain diameter of the corn straw powder is 10-100 meshes; in the step (2), the alkali liquor is a sodium hydroxide solution with the mass concentration of 5%. In the step (2), the addition amount of urea accounts for 5% of the total mass of the mixed solution.
Analysis shows that under the condition, the dissolution rate of lignin in the corn straws reaches 76.92 percent, and the data is similar to that of the corn straws treated by 5 percent NaOH alone (without urea) for 5 hours (the dissolution rate is 77.94 percent).
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not exhaustive. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (7)

1. A method for extracting lignin by urea-assisted low-temperature alkali liquor is characterized by comprising the following steps:
(1) crushing, sieving, washing and drying corn straws to obtain corn straw powder;
(2) adding urea into an alkali liquor to obtain a mixed liquor, then adding corn straw powder into the mixed liquor, carrying out lignin extraction operation treatment, and obtaining a slurry after the reaction is finished;
(3) and carrying out reduced pressure suction filtration separation on the slurry to obtain filtrate and filter residue, washing the residue with distilled water to obtain washing liquid, combining the washing liquid and the filtrate, regulating the pH value to 2 after reduced pressure concentration, standing for 2-3h, then carrying out centrifugal separation to obtain a precipitate, and drying the precipitate to obtain the lignin.
2. The method for extracting lignin from low-temperature alkaline liquor assisted by urea according to claim 1, wherein in the step (1), the particle size of the corn stalk powder is 10-100 meshes.
3. The method for extracting lignin with urea-assisted low-temperature alkali liquor according to claim 1, wherein in the step (2), the alkali liquor is any one of sodium hydroxide solution and potassium hydroxide.
4. The method for extracting lignin from urea-assisted low-temperature alkali liquor according to claim 1, wherein in the step (2), the mass concentration of the alkali liquor is 1-5%.
5. The method for extracting lignin with urea-assisted low-temperature alkaline liquor according to claim 1, wherein in the step (2), the addition amount of urea is 1-10% of the total mass of the mixed liquor.
6. The method for extracting lignin from urea-assisted low-temperature alkali liquor according to claim 1, wherein in the step (2), the solid-to-liquid ratio of the corn stalk powder to the mixed liquor is 1 (10-20).
7. The method for extracting lignin with urea-assisted low-temperature alkali liquor according to claim 1, wherein in the step (2), the reaction temperature is 40 ℃ and the reaction time is 1-5 h.
CN202011504577.8A 2020-12-18 2020-12-18 Method for extracting lignin from urea-assisted low-temperature alkali liquor Pending CN112626903A (en)

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CN115231958A (en) * 2022-08-17 2022-10-25 中国科学院成都生物研究所 Method for co-producing humic acid type water-soluble fertilizer and crude cellulose by using straws
CN116732800A (en) * 2023-05-08 2023-09-12 上海昶法新材料有限公司 Preparation method and application of straw pulping machine pulp and pulping waste liquid
CN116815528A (en) * 2023-04-28 2023-09-29 呼伦贝尔汇通生物科技有限公司 Lignin removing method for straw

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Publication number Priority date Publication date Assignee Title
CN115231958A (en) * 2022-08-17 2022-10-25 中国科学院成都生物研究所 Method for co-producing humic acid type water-soluble fertilizer and crude cellulose by using straws
CN116815528A (en) * 2023-04-28 2023-09-29 呼伦贝尔汇通生物科技有限公司 Lignin removing method for straw
CN116732800A (en) * 2023-05-08 2023-09-12 上海昶法新材料有限公司 Preparation method and application of straw pulping machine pulp and pulping waste liquid

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