CN117681296A - Pretreatment and superfine method for wood and bamboo raw materials - Google Patents

Pretreatment and superfine method for wood and bamboo raw materials Download PDF

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Publication number
CN117681296A
CN117681296A CN202410143885.4A CN202410143885A CN117681296A CN 117681296 A CN117681296 A CN 117681296A CN 202410143885 A CN202410143885 A CN 202410143885A CN 117681296 A CN117681296 A CN 117681296A
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wood
bamboo
temperature
superfine
steam explosion
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CN117681296B (en
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张景杰
段培高
刘畅
杜雨菡
高志杰
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Shandong Alpa Powder Technology Co ltd
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Shandong Alpa Powder Technology Co ltd
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Abstract

The invention discloses a wood-bamboo raw material pretreatment and superfine method, and belongs to the technical field of biomass energy and biomass environmental protection. The method disclosed by the invention adopts hydrogen peroxide solution to dissolve the raw material of the wood and bamboo, destroys the lignin structure in the raw material of the wood and bamboo, and utilizes CO 2 Weak acid H with water 2 CO 3 Promoting hemicellulose in the wood bamboo raw material to degrade; and (3) carrying out steam explosion treatment subsequently, penetrating water molecules into the cell wall structure of the wood and bamboo at high temperature and high pressure, then rapidly decompressing to cause certain mechanical fracture of the cellulose fiber structure, and finally further refining by using an ultrafine grinder to obtain the wood and bamboo powder with the required granularity. The invention adopts the raw materials which are green, environment-friendly, low in price and easy to obtain, and the technical process is nontoxic and harmless.

Description

Pretreatment and superfine method for wood and bamboo raw materials
Technical Field
The invention belongs to the technical field of biomass energy and biomass environmental protection, and particularly relates to a wood-bamboo raw material pretreatment and superfine method.
Background
The wood-bamboo industry is an indispensable civil industry for improving the life quality of people, and the wood-bamboo is a natural polymer composite material composed of cellulose, hemicellulose and lignin, has the advantages of environmental protection, high strength-weight ratio, beautiful texture and the like, and is widely applied to the field of building and housing. However, in some application scenarios, it is difficult to directly use the bamboo, and a treatment method is necessary to refine the bamboo.
The existing pretreatment method of the wood and bamboo mainly uses chemical reagents such as strong acid, strong alkali and the like to destroy the structure so as to achieve the aim of pretreatment. However, the chemical pretreatment methods such as strong acid and strong alkali not only consume a large amount of chemical reagents, but also have strong corrosiveness to equipment; meanwhile, a large amount of waste residues and waste liquid are generated after the reaction, the environment is seriously polluted, and the sustainable development strategic requirements cannot be met.
Therefore, the development of an environment-friendly and efficient wood-bamboo refining treatment method has important value.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a wood-bamboo raw material pretreatment and superfine method, which is used for solving the technical problems of serious environmental pollution, low efficiency and the like of the existing wood-bamboo raw material pretreatment and superfine method.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the invention discloses a wood-bamboo raw material pretreatment and superfine method, which comprises the following steps:
s1: putting the raw materials of the wood and bamboo into hydrogen peroxide solution, stirring and filtering to obtain filter residues; drying the filter residues to constant weight to obtain dried wood-bamboo powder;
s2: mixing the dried wood bamboo powder with water, and adding CO 2 After high-temperature and high-pressure reaction is carried out in the atmosphere, collecting liquid components and solid residues after the high-temperature and high-pressure reaction, and sequentially carrying out water washing and drying treatment on the solid residues to obtain pretreated wood-bamboo powder;
s3: performing steam explosion treatment on the pretreated wood-bamboo powder to obtain a steam explosion product; and crushing the steam explosion product to obtain the superfine wood-bamboo powder.
Further, in S1, the dosage ratio of the wood and bamboo raw material to the hydrogen peroxide solution is (300-500) g: (2-3) L.
Further, in S1, the mass percentage of the hydrogen peroxide solution is 6% -10%.
Further, in S1, the temperature during stirring is 50-80 ℃, the stirring rotating speed is 500-600 r/min, and the stirring time is 30-60 min.
In S1, the temperature of the drying treatment is 100-105 ℃.
Further, the dosage ratio of the wood-bamboo raw material in S1 to the water in S2 is (300-500 g): (200-300) mL;
s2, the high-temperature high-pressure reaction is carried out in a closed space and CO 2 The process is carried out under an atmosphere.
Further, the temperature of the high-temperature high-pressure reaction is 100-200 ℃, and the time of the high-temperature high-pressure reaction is 15-200 min.
Further, the CO 2 The pressure of the atmosphere is 1-7 MPa.
Further, in S3, the temperature of the steam explosion treatment is 200-300 ℃, the pressure of the steam explosion treatment is 2.0-2.5 MPa, and the pressure maintaining time in the steam explosion treatment process is 30-50S.
Further, the granularity of the pretreated wood-bamboo powder is 1000-2000 meshes; the granularity of the superfine wood-bamboo powder is 4000-10000 meshes.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a pretreatment and superfine method of wood and bamboo raw materials, which adopts hydrogen peroxide solution to dissolve the wood and bamboo raw materials, destroy lignin structure in the wood and bamboo raw materials, and uses OH - Impair the saponification of the ester bonds between the internal molecules of the cellulose and hemicellulose and the xylan hemicellulose and other components; then high-temperature high-pressure reaction is carried out, and under the condition of high temperature and high pressure, the wood, bamboo and CO are reacted 2 By reaction with CO 2 And the action of water, i.e. CO 2 Weak acid H with water 2 CO 3 Promoting the raw wood and bambooHemicellulose in the material is degraded, so that a dense structure of three components of the plant fiber raw material is broken, and the hydrolysis rate of the wood fiber raw material is increased; subsequently, steam explosion treatment is carried out, water molecules penetrate through the cell wall structure of the wood bamboo under high temperature and high pressure, then pressure is quickly reduced, a certain mechanical fracture is caused to the cellulose fiber structure, and huge blasting force, friction force and collision force are generated when the contained water is flashed, so that the fiber raw material is crushed; meanwhile, the high temperature and the high pressure aggravate the damage of hydrogen bonds and the change of ordered structures in cellulose, so that new hydroxyl groups are released, the adsorption capacity of the cellulose is improved, and the hydrolysis of hemicellulose and the conversion of lignin are promoted; further carrying out final refinement to obtain wood-bamboo powder with required granularity; the invention adopts the raw materials which are green, environment-friendly, low in price and easy to obtain, and the technical process is nontoxic and harmless.
Drawings
FIG. 1 is a schematic process flow diagram of the pretreatment and superfine method of the wood-bamboo raw material of the invention.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
As shown in FIG. 1, the invention provides a method for pretreating and superfine wood and bamboo raw materials, which comprises the following steps:
step 1: pouring 300-500 g of wood and bamboo raw materials into a beaker containing 2-3L of hydrogen peroxide solution with the mass percentage of 6% -10%, and then placing the beaker into a constant-temperature magnetic stirrer for stirring and filtering to obtain filter residues; washing filter residues with deionized water for 3-5 times, transferring the washed filter residues into an oven, and drying at 100-105 ℃ until the weight is constant to obtain dried wood-bamboo powder; the dried wood-bamboo powder is 500-1000 meshes;
step 2: mixing the dried wood and bamboo powder with ultrapure water, transferring into a high-temperature high-pressure reaction kettle, sealing, and introducing a certain amount of CO 2 Stirring is started to perform high-temperature high-pressure reaction, after the high-temperature high-pressure reaction is finished, the mixture is rapidly cooled to room temperature, and then residual CO is released 2 Collecting liquid components and solid residues, and sequentially performing water washing and drying treatment on the solid residues to obtain pretreated wood-bamboo powder; the pretreated wood-bamboo powder is 1000-2000 meshes;
step 3: pouring the pretreated wood-bamboo powder into a steam explosion device, performing steam explosion treatment under certain steam, pressure and dwell time, opening a steam explosion cabin door after the steam explosion treatment is finished, collecting materials from a material bin, and drying for later use to obtain a steam explosion product; at this time, the steam explosion product is 3000-4000 meshes;
step 4: transferring the steam explosion product into an ultrafine grinder for grinding to obtain ultrafine wood bamboo powder with required granularity; at this time, the superfine wood-bamboo powder is 4000-10000 meshes.
Preferably, the method of the invention refines 1000-2000 meshes of pretreated wood-bamboo powder into 4000-10000 meshes.
Preferably, in the step 1, the temperature during stirring is 50-80 ℃, the stirring rotating speed is 500-600 r/min, and the stirring time is 30-60 min; more preferably, the temperature during stirring is 75deg.C, the stirring speed is 600r/min, and the stirring time is 60min.
Preferably, in the step 2, the temperature of the high-temperature high-pressure reaction is 100-200 ℃, the time of the high-temperature high-pressure reaction is 15-200 min, and CO 2 The pressure of the atmosphere is 1-7 MPa; more preferably, the high temperature and high pressure reaction temperature is 150deg.C, the high temperature and high pressure reaction time is 100min, and CO 2 The pressure of the atmosphere was 4MPa.
Preferably, in the step 3, the temperature of the steam explosion treatment is 200-300 ℃, the pressure of the steam explosion treatment is 2.0-2.5 MPa, and the pressure maintaining time in the steam explosion treatment process is 30-50 s.
The first aspect of the invention provides a pretreatment method of wood-bamboo raw materials, which comprises the following steps: reacting hydrogen peroxide solution with wood and bamboo raw materials; then using high-temperature high-pressure reaction kettle to make CO 2 High-temperature high-pressure reaction is carried out under the condition.
Wherein, the mass percentage of the hydrogen peroxide solution is 6% -10%, preferably 7% -9%, more preferably 8%.
The second aspect of the invention provides a method for ultrafine grinding of wood and bamboo raw materials, which comprises the steps of steam explosion treatment by a steam explosion device and grinding by an ultrafine grinding device.
In some preferred embodiments of the invention, the conditions of the steam explosion treatment include:
preferably, the temperature of the steam explosion treatment is 220-250 ℃, the pressure of the steam explosion treatment is 2.0-2.3 MPa, and the pressure maintaining time in the steam explosion treatment process is 35-40 s.
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1
A wood-bamboo raw material pretreatment and superfine method comprises the following steps:
s1: pouring 300g of wood bamboo raw material into a beaker containing 2L of hydrogen peroxide solution with the mass percentage of 8%, placing the beaker into a constant-temperature magnetic stirrer for stirring, wherein the stirring temperature is 75 ℃, the stirring rotating speed is 600r/min, the stirring time is 60min, and filtering after the stirring is finished to obtain filter residues; washing the filter residue with deionized water for 5 times, transferring the washed filter residue into an oven, and drying at 105 ℃ until the weight is constant to obtain dried wood-bamboo powder;
s2: mixing the dried wood bamboo powder with 200mL of ultrapure water, transferring into a high-temperature high-pressure reaction kettle, sealing, and introducing 4MPa of CO 2 Stirring, heating to 150deg.C, performing high-temperature high-pressure reaction for 100min, rapidly cooling to room temperature after the high-temperature high-pressure reaction, and releasing residual CO 2 Collecting liquid components and solid residues, and sequentially performing water washing and drying treatment on the solid residues to obtain pretreated wood-bamboo powder;
s3: pouring the pretreated wood-bamboo powder into a steam explosion device for steam explosion treatment; the temperature of the steam explosion treatment is 250 ℃, the pressure of the steam explosion treatment is 2.3MPa, and the pressure maintaining time in the steam explosion treatment process is 40s; after the steam explosion treatment is finished, opening a steam explosion cabin door, collecting materials from a material bin, and drying for later use to obtain a steam explosion product; and (3) transferring the steam explosion product into an ultrafine grinder of Shandong Er powder science and technology Co., ltd, and grinding to obtain 4000-10000-mesh ultrafine wood-bamboo powder.
Example 2
A wood-bamboo raw material pretreatment and superfine method comprises the following steps:
s1: pouring 300g of bamboo into a beaker containing 2L of alkaline hydrogen peroxide solution with the mass fraction of 7%, placing the beaker into a constant-temperature magnetic stirrer for stirring at the temperature of 75 ℃, the stirring speed of 550r/min, the stirring time of 50min, and filtering after the stirring is finished to obtain filter residues; washing filter residues with deionized water for 4 times, transferring the washed filter residues into an oven, and drying at 105 ℃ until the weight is constant to obtain dried wood-bamboo powder;
s2: mixing the dried wood bamboo powder with 200mL of ultrapure water, transferring into a high-temperature high-pressure reaction kettle, sealing, and introducing CO of 2MPa 2 Stirring is started, the temperature is raised to 120 ℃ to carry out high-temperature high-pressure reaction for 50min, the reaction is cooled to room temperature rapidly after the reaction is finished, and then residual CO is released 2 Collecting liquid components and solid residues, and sequentially performing water washing and drying treatment on the solid residues to obtain pretreated wood-bamboo powder;
s3: pouring the pretreated wood-bamboo powder into a steam explosion device for steam explosion treatment; the temperature of the steam explosion treatment is 250 ℃, the pressure of the steam explosion treatment is 2.0MPa, and the pressure maintaining time in the steam explosion treatment process is 35s; after the steam explosion treatment is finished, opening a steam explosion cabin door, collecting materials from a material bin, and drying for later use to obtain a steam explosion product; and (3) transferring the steam explosion product into an ultrafine grinder of Shandong Er powder science and technology Co., ltd, and grinding to obtain 4000-10000-mesh ultrafine wood-bamboo powder.
Example 3
A wood-bamboo raw material pretreatment and superfine method comprises the following steps:
s1: pouring 300g of bamboo into a beaker containing 3L of alkaline hydrogen peroxide solution with the mass fraction of 9%, placing the beaker into a constant-temperature magnetic stirrer for stirring, wherein the stirring temperature is 80 ℃, the stirring rotating speed is 600r/min, the stirring time is 60min, and filtering after the stirring is finished to obtain filter residues; washing filter residues with deionized water for 3 times, transferring the washed filter residues into an oven, and drying at 105 ℃ until the weight is constant to obtain dried wood-bamboo powder;
s2: mixing the dried wood bamboo powder with 200mL of ultrapure water, transferring into a high-temperature high-pressure reaction kettle, sealing, and introducing CO of 5MPa 2 Stirring, heating to 200deg.C, performing high temperature and high pressure reaction for 150min, rapidly cooling to room temperature after the high temperature and high pressure reaction, and releasing residual CO 2 Collecting liquid components and solid residues, and sequentially performing water washing and drying treatment on the solid residues to obtain pretreated wood-bamboo powder;
s3: pouring the pretreated wood-bamboo powder into a steam explosion device for steam explosion treatment; the temperature of the steam explosion treatment is 250 ℃, the pressure of the steam explosion treatment is 2.3MPa, and the pressure maintaining time in the steam explosion treatment process is 40s; after the steam explosion treatment is finished, opening a steam explosion cabin door, collecting materials from a material bin, and drying for later use to obtain a steam explosion product; and (3) transferring the steam explosion product into an ultrafine grinder of Shandong Er powder science and technology Co., ltd, and grinding to obtain 4000-10000-mesh ultrafine wood-bamboo powder.
Example 4
A wood-bamboo raw material pretreatment and superfine method comprises the following steps:
s1: pouring 500g of bamboo into a beaker containing 2L of alkaline hydrogen peroxide solution with the mass fraction of 6%, placing the beaker into a constant-temperature magnetic stirrer for stirring at the temperature of 75 ℃ at the stirring speed of 500r/min for 30min, and filtering after stirring to obtain filter residues; washing the filter residue with deionized water for 5 times, transferring the washed filter residue into an oven, and drying at 100 ℃ until the weight is constant to obtain dried wood-bamboo powder;
s2: mixing the dried wood bamboo powder with 300mL of ultrapure water, transferring into a high-temperature high-pressure reaction kettle, sealing, and introducing CO of 1MPa 2 Stirring, heating to 100deg.C, reacting at high temperature and high pressure for 15min, cooling to room temperature, and releasing residual CO 2 Collecting liquid components and solid residues, and sequentially performing water washing and drying treatment on the solid residues to obtain pretreated wood-bamboo powder;
s3: pouring the pretreated wood-bamboo powder into a steam explosion device for steam explosion treatment; the temperature of the steam explosion treatment is 200 ℃, the pressure of the steam explosion treatment is 2.5MPa, and the pressure maintaining time in the steam explosion treatment process is 30s; after the steam explosion treatment is finished, opening a steam explosion cabin door, collecting materials from a material bin, and drying for later use to obtain a steam explosion product; and (3) transferring the steam explosion product into an ultrafine grinder of Shandong Er powder science and technology Co., ltd, and grinding to obtain 4000-10000-mesh ultrafine wood-bamboo powder.
By analyzing the examples 1 to 4, the wood-bamboo powder finally obtained by the method of the invention meets the requirements, which shows that the invention can well destroy the structure of the wood-bamboo by pretreatment and ultrafining.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (10)

1. The wood and bamboo raw material pretreatment and superfine method is characterized by comprising the following steps:
s1: putting the raw materials of the wood and bamboo into hydrogen peroxide solution, stirring and filtering to obtain filter residues; drying the filter residues to constant weight to obtain dried wood-bamboo powder;
s2: mixing the dried wood bamboo powder with water, and adding CO 2 After high-temperature and high-pressure reaction is carried out in the atmosphere, collecting liquid components and solid residues after the high-temperature and high-pressure reaction, and sequentially carrying out water washing and drying treatment on the solid residues to obtain pretreated wood-bamboo powder;
s3: performing steam explosion treatment on the pretreated wood-bamboo powder to obtain a steam explosion product; and crushing the steam explosion product to obtain the superfine wood-bamboo powder.
2. The method for pretreating and superfine wood-bamboo raw materials according to claim 1, wherein in S1, the ratio of the wood-bamboo raw materials to the hydrogen peroxide solution is (300-500) g: (2-3) L.
3. The method for pretreating and superfine wood and bamboo raw materials according to claim 1, wherein in S1, the mass percentage of the hydrogen peroxide solution is 6% -10%.
4. The method for pretreating and superfine wood and bamboo materials according to claim 1, wherein in the step S1, the stirring temperature is 50-80 ℃, the stirring speed is 500-600 r/min, and the stirring time is 30-60 min.
5. The method for pretreating and superfine wood-bamboo raw materials according to claim 1, wherein in S1, the temperature of the drying treatment is 100-105 ℃.
6. The method for pretreating and superfine wood-bamboo raw materials according to claim 1, wherein the ratio of the wood-bamboo raw materials in S1 to the water in S2 is (300-500) g: (200-300) mL;
s2, the high-temperature high-pressure reaction is carried out in a closed space and CO 2 The process is carried out under an atmosphere.
7. The method for pretreating and superfine wood and bamboo materials according to claim 6, wherein the high temperature and high pressure reaction temperature is 100-200 ℃, and the high temperature and high pressure reaction time is 15-200 min.
8. The method for pretreating and superfine wood-bamboo raw materials according to claim 7, wherein the CO 2 The pressure of the atmosphere is 1-7 MPa.
9. The method for pretreating and superfine wood and bamboo materials according to claim 1, wherein in the step S3, the temperature of the steam explosion treatment is 200-300 ℃, the pressure of the steam explosion treatment is 2.0-2.5 MPa, and the pressure maintaining time in the steam explosion treatment process is 30-50S.
10. The method for pretreating and superfine wood-bamboo raw materials according to claim 1, wherein the particle size of the pretreated wood-bamboo powder is 1000-2000 meshes; the granularity of the superfine wood-bamboo powder is 4000-10000 meshes.
CN202410143885.4A 2024-02-01 Pretreatment and superfine method for wood and bamboo raw materials Active CN117681296B (en)

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Citations (3)

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Publication number Priority date Publication date Assignee Title
JP2003238969A (en) * 2002-02-19 2003-08-27 Shigeru Ito Technology for hydrolysis of impact-loaded bamboo, timber and other plant biomass using subcritical fluid or supercritical fluid
CN105482480A (en) * 2015-11-11 2016-04-13 国家林业局竹子研究开发中心 Fiber reinforced thermoplasticity plastic
CN112553269A (en) * 2020-12-24 2021-03-26 安徽工业大学 Pretreatment and enzymolysis method of corn straw

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003238969A (en) * 2002-02-19 2003-08-27 Shigeru Ito Technology for hydrolysis of impact-loaded bamboo, timber and other plant biomass using subcritical fluid or supercritical fluid
CN105482480A (en) * 2015-11-11 2016-04-13 国家林业局竹子研究开发中心 Fiber reinforced thermoplasticity plastic
CN112553269A (en) * 2020-12-24 2021-03-26 安徽工业大学 Pretreatment and enzymolysis method of corn straw

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
罗鹏: ""木质纤维素超声超临界二氧化碳预处理及其对水解效果的影响"", 《中国优秀硕士学位论文全文数据库 (工程科技Ⅰ辑)》, 31 October 2012 (2012-10-31), pages 57 - 58 *

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