CN112624085A - Preparation method of cellulose-based all-carbon aerogel - Google Patents
Preparation method of cellulose-based all-carbon aerogel Download PDFInfo
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- CN112624085A CN112624085A CN202011583132.3A CN202011583132A CN112624085A CN 112624085 A CN112624085 A CN 112624085A CN 202011583132 A CN202011583132 A CN 202011583132A CN 112624085 A CN112624085 A CN 112624085A
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- 239000001913 cellulose Substances 0.000 title claims abstract description 71
- 229920002678 cellulose Polymers 0.000 title claims abstract description 71
- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 48
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 239000004743 Polypropylene Substances 0.000 claims abstract description 24
- 229920001155 polypropylene Polymers 0.000 claims abstract description 24
- 238000003763 carbonization Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000032683 aging Effects 0.000 claims abstract description 17
- -1 polypropylene Polymers 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000013329 compounding Methods 0.000 claims abstract description 4
- 235000010980 cellulose Nutrition 0.000 claims description 64
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000011159 matrix material Substances 0.000 claims description 21
- 239000011240 wet gel Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 10
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 10
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 10
- 238000011282 treatment Methods 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 7
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 7
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000003349 gelling agent Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 239000000499 gel Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000000352 supercritical drying Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 10
- 230000002209 hydrophobic effect Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000005539 carbonized material Substances 0.000 abstract description 2
- 230000015271 coagulation Effects 0.000 description 4
- 238000005345 coagulation Methods 0.000 description 4
- 238000001879 gelation Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000004964 aerogel Substances 0.000 description 2
- 230000004931 aggregating effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a preparation method of cellulose-based all-carbon aerogel, and relates to a preparation method of carbon aerogel. A preparation method of cellulose-based all-carbon aerogel comprises the following steps: (1) preparing cellulose sol; (2) compounding the cellulose sol and the fiber felt; (3) aging of the composite material; (4) drying the composite material; (5) and preparing the carbon aerogel by a carbonization process. The cellulose-based all-carbon aerogel prepared by the method has the following beneficial effects: (1) compared with the water absorption of the polypropylene fiber to water before carbonization, the carbonized material has excellent hydrophobic property and high oil absorption property. (2) The cellulose-based carbon aerogel has low production cost, simple process and short production period, and is expected to be applied in large scale.
Description
Technical Field
The invention discloses a preparation method of cellulose-based all-carbon aerogel, and relates to a preparation method of carbon aerogel.
Background
The aerogel is a nano porous network structure formed by aggregating nano particles, has the characteristics of low thermal conductivity, high porosity, high specific surface area and the like, and has wide application prospects in the fields of heat insulation, adsorption and the like. The polypropylene fiber has good performances of tensile strength, impact strength, rigidity, wear resistance, chemical resistance, surface hardness and the like, but the polypropylene fiber has low oil absorption rate and limits the application of the polypropylene fiber, cellulose aerogel is compounded in the polypropylene fiber, and the hydrophobic carbon aerogel is obtained by combining a carbonization process, so that the oil absorption efficiency of the material can be effectively increased. However, there is no good method for preparing the carbon aerogel, so a new preparation method needs to be designed to meet the actual demand.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a cellulose-based all-carbon aerogel, which can quickly and well prepare the cellulose-based all-carbon aerogel.
A preparation method of cellulose-based all-carbon aerogel comprises the following steps:
(1) preparation of cellulose sols
Weighing a proper amount of lithium hydroxide monohydrate, urea and deionized water, mixing to obtain a mixed solution, dispersing a proper amount of microcrystalline cellulose powder into the prepared mixed solution, stirring for a specified time, performing ultrasonic dispersion treatment, sealing, and freezing in a freezer; then taking out and mechanically stirring, and centrifuging to obtain cellulose sol;
(2) compounding of cellulose sol and fiber felt
Placing a fiber matrix in a container, pouring the cellulose sol obtained in the step (1) into the container, taking the cellulose sol submerged in the fiber matrix as a standard, placing a gelling agent into the container, and waiting for gelling;
(3) ageing of composite materials
After the gel is formed in the step (2), peeling the wet gel outside the fiber substrate, soaking the wet gel in an aging solution, and aging for a period of time under a preset condition;
(4) drying of composite materials
Drying the aged composite material obtained in the step (3) to obtain a cellulose aerogel-polypropylene fiber composite material;
(5) preparation of carbon aerogel by carbonization process
And (4) carbonizing the composite material obtained in the step (4) to obtain the cellulose-based all-carbon aerogel.
Preferably, the mass ratio of the lithium hydroxide monohydrate, the urea, the water and the cellulose in the step (1) is 7: 12: 81: 2-5.
Preferably, in step (2), the fiber matrix is polypropylene fiber, and the gelling agent is methanol.
Preferably, the aging solution in the step (3) is a mixed solution of ethanol and water.
Preferably, the drying method in step (4) is freeze drying or CO2And (5) supercritical drying.
Preferably, the carbonization process in the step (5) is carried out at a carbonization temperature of 500-.
And (2) carrying out ultrasonic dispersion treatment after stirring for a specified time in the step (1) by using an ultrasonic disperser.
The cellulose-based all-carbon aerogel prepared by the method has the following beneficial effects:
(1) compared with the water absorption of the polypropylene fiber to water before carbonization, the carbonized material has excellent hydrophobic property and high oil absorption property.
(2) The cellulose-based carbon aerogel has low production cost, simple process and short production period, and is expected to be applied in large scale.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention.
Fig. 2 is a schematic representation of the hydrophobicity of cellulose-based carbon aerogels.
Detailed Description
The invention will be further illustrated with reference to the following examples, without however limiting the scope of protection thereto, with reference to the attached figures 1-2.
A preparation method of cellulose-based all-carbon aerogel comprises the following steps:
(1) preparation of cellulose sols
Weighing a proper amount of lithium hydroxide monohydrate, urea and deionized water, mixing to obtain a mixed solution, dispersing a proper amount of microcrystalline cellulose powder into the prepared mixed solution, stirring for a specified time, performing ultrasonic dispersion treatment, sealing, and freezing in a freezer; then taking out and mechanically stirring, and centrifuging to obtain cellulose sol;
(2) compounding of cellulose sol and fiber felt
Placing a fiber matrix in a container, pouring the cellulose sol obtained in the step (1) into the container, taking the cellulose sol submerged in the fiber matrix as a standard, placing a gelling agent into the container, and waiting for gelling;
(3) ageing of composite materials
After the gel is formed in the step (2), peeling the wet gel outside the fiber substrate, soaking the wet gel in an aging solution, and aging for a period of time under a preset condition;
(4) drying of composite materials
Drying the aged composite material obtained in the step (3) to obtain a cellulose aerogel-polypropylene fiber composite material;
(5) preparation of carbon aerogel by carbonization process
And (4) carbonizing the composite material obtained in the step (4) to obtain the cellulose-based all-carbon aerogel.
Preferably, the mass ratio of the lithium hydroxide monohydrate, the urea, the water and the cellulose in the step (1) is 7: 12: 81: 2-5.
Preferably, in step (2), the fiber matrix is polypropylene fiber, and the gelling agent is methanol.
Preferably, the aging solution in the step (3) is a mixed solution of ethanol and water.
Preferably, the drying method in step (4) is freeze drying or CO2And (5) supercritical drying.
Preferably, the carbonization process in the step (5) is carried out at a carbonization temperature of 500-.
Example 1
Into a beaker was added 81mL of deionized water, 7 g of lithium hydroxide monohydrate and 12g of urea, and 2g of microcrystalline cellulose was added. After 5 minutes of ultrasonic dispersion, the mixed solution was frozen in a refrigerator for 12 hours, taken out, mechanically stirred and centrifuged to obtain a cellulose sol. Placing a polypropylene fiber matrix in a container, pouring the prepared cellulose sol into the container, placing the container in a methanol coagulation bath until the cellulose sol submerges the fiber matrix, and placing the container in an environment temperature of 20 ℃ for gelation. After gelling, peeling the wet gel outside the fiber matrix, soaking the wet gel in a mixed solution of ethanol and water, aging the wet gel at 20 ℃ for 5 days, and carrying out freeze drying treatment on the aged composite material to obtain the cellulose aerogel-polypropylene fiber composite material. And then placing the cellulose aerogel-polypropylene fiber composite material in a tubular furnace for carbonization for 1 hour, wherein the carbonization temperature is 500 ℃ (the heating rate is 2 ℃/min), and the cellulose-based carbon aerogel is prepared, the hydrophobic angle is 129 ℃, and the oil absorption rate is 14 g/g.
Example 2
Into a beaker was added 81mL of deionized water, 7 g of lithium hydroxide monohydrate and 12g of urea, and 3 g of microcrystalline cellulose was added. After 5 minutes of ultrasonic dispersion, the mixed solution was frozen in a refrigerator for 12 hours, taken out, mechanically stirred and centrifuged to obtain a cellulose sol. Placing a polypropylene fiber matrix in a container, pouring the prepared cellulose sol into the container, placing the container in a methanol coagulation bath until the cellulose sol submerges the fiber matrix, and placing the container in an environment temperature of 20 ℃ for gelation. After gelling, peeling the wet gel outside the fiber matrix, soaking the wet gel in a mixed solution of ethanol and water, aging the wet gel at 20 ℃ for 5 days, and carrying out freeze drying treatment on the aged composite material to obtain the cellulose aerogel-polypropylene fiber composite material. And then placing the cellulose aerogel-polypropylene fiber composite material in a tubular furnace for carbonization for 2 hours at the carbonization temperature of 600 ℃ (the heating rate is 2 ℃/min), so as to prepare the cellulose-based carbon aerogel, wherein the hydrophobic angle is 137 ℃, and the oil absorption rate is 20 g/g.
Example 3
Into a beaker was added 81mL of deionized water, 7 g of lithium hydroxide monohydrate and 12g of urea, and 4 g of microcrystalline cellulose was added. After 5 minutes of ultrasonic dispersion, the mixed solution was frozen in a refrigerator for 12 hours, taken out, mechanically stirred and centrifuged to obtain a cellulose sol. Placing a polypropylene fiber matrix in a container, pouring the prepared cellulose sol into the container, placing the container in a methanol coagulation bath until the cellulose sol submerges the fiber matrix, and placing the container in an environment temperature of 20 ℃ for gelation. After gelling, peeling the wet gel outside the fiber matrix, soaking the wet gel in a mixed solution of ethanol and water, aging the wet gel at 20 ℃ for 5 days, and carrying out freeze drying treatment on the aged composite material to obtain the cellulose aerogel-polypropylene fiber composite material. And then placing the cellulose aerogel-polypropylene fiber composite material in a tubular furnace for carbonization for 3 hours at the carbonization temperature of 600 ℃ (the heating rate is 2 ℃/min), so as to prepare the cellulose-based carbon aerogel, wherein the hydrophobic angle is 138 ℃, and the oil absorption rate is 18 g/g.
Example 4
Into a beaker was added 81mL of deionized water, 7 g of lithium hydroxide monohydrate and 12g of urea, and 5 g of microcrystalline cellulose was added. After 5 minutes of ultrasonic dispersion, the mixed solution was frozen in a refrigerator for 12 hours, taken out, mechanically stirred and centrifuged to obtain a cellulose sol. Placing a polypropylene fiber matrix in a container, pouring the prepared cellulose sol into the container, placing the container in a methanol coagulation bath until the cellulose sol submerges the fiber matrix, and placing the container in an environment temperature of 20 ℃ for gelation. After gelling, peeling the wet gel outside the fiber matrix, soaking the wet gel in a mixed solution of ethanol and water, aging the wet gel at 20 ℃ for 5 days, and carrying out freeze drying treatment on the aged composite material to obtain the cellulose aerogel-polypropylene fiber composite material. And then placing the cellulose aerogel-polypropylene fiber composite material in a tubular furnace for carbonization for 4 hours at the carbonization temperature of 700 ℃ (the heating rate is 2 ℃/min), so as to prepare the cellulose-based carbon aerogel, wherein the hydrophobic angle is 135 ℃, and the oil absorption rate is 15 g/g.
Claims (6)
1. A preparation method of cellulose-based all-carbon aerogel is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of cellulose sols
Weighing a proper amount of lithium hydroxide monohydrate, urea and deionized water, mixing to obtain a mixed solution, dispersing a proper amount of microcrystalline cellulose powder into the prepared mixed solution, stirring for a specified time, performing ultrasonic dispersion treatment, sealing, and freezing in a freezer; then taking out and mechanically stirring, and centrifuging to obtain cellulose sol;
(2) compounding of cellulose sol and fiber felt
Placing a fiber matrix in a container, pouring the cellulose sol obtained in the step (1) into the container, taking the cellulose sol submerged in the fiber matrix as a standard, placing a gelling agent into the container, and waiting for gelling;
(3) ageing of composite materials
After the gel is formed in the step (2), peeling the wet gel outside the fiber substrate, soaking the wet gel in an aging solution, and aging for a period of time under a preset condition;
(4) drying of composite materials
Drying the aged composite material obtained in the step (3) to obtain a cellulose aerogel-polypropylene fiber composite material;
(5) preparation of carbon aerogel by carbonization process
And (4) carbonizing the composite material obtained in the step (4) to obtain the cellulose-based all-carbon aerogel.
2. The method of preparing a cellulose-based all-carbon aerogel according to claim 1, wherein: in the step (1), the mass ratio of the lithium hydroxide monohydrate to the urea to the water to the cellulose is 7: 12: 81: 2-5.
3. The method of preparing a cellulose-based all-carbon aerogel according to claim 1, wherein: in the step (2), the fiber matrix is polypropylene fiber, and the gelling agent is methanol.
4. The method of preparing a cellulose-based all-carbon aerogel according to claim 1, wherein: the aging liquid in the step (3) is a mixed solution of ethanol and water.
5. The method of preparing a cellulose-based all-carbon aerogel according to claim 1, wherein: the drying method in the step (4) is freeze drying or CO2And (5) supercritical drying.
6. The method of preparing a cellulose-based all-carbon aerogel according to claim 1, wherein: the carbonization process in the step (5) is carried out at the carbonization temperature of 500-.
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|---|---|---|---|---|
| WO2006025148A1 (en) * | 2004-08-30 | 2006-03-09 | Univ Nihon | Lithium ion conductive material utilizing bacterial cellulose organogel, lithium ion battery utilizing the same and bacterial cellulose aerogel |
| CN105017555A (en) * | 2014-04-29 | 2015-11-04 | 中国科学院化学研究所 | Cellulose aerogel and preparation method for hybrid aerogel thereof |
| CN105820372A (en) * | 2016-03-30 | 2016-08-03 | 青岛大学 | Conductive aerogel and preparation method thereof |
| CN105970193A (en) * | 2016-05-24 | 2016-09-28 | 中国工程物理研究院激光聚变研究中心 | Metal aerogel with high specific surface area and preparation method thereof |
| CN108314000A (en) * | 2018-02-12 | 2018-07-24 | 浙江大学 | A kind of preparation method of high stretchable full carbon aerogels |
| CN111591972A (en) * | 2020-05-18 | 2020-08-28 | 华东交通大学 | Super-elastic hydrophilic all-carbon aerogel and preparation method thereof |
-
2020
- 2020-12-28 CN CN202011583132.3A patent/CN112624085B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006025148A1 (en) * | 2004-08-30 | 2006-03-09 | Univ Nihon | Lithium ion conductive material utilizing bacterial cellulose organogel, lithium ion battery utilizing the same and bacterial cellulose aerogel |
| CN105017555A (en) * | 2014-04-29 | 2015-11-04 | 中国科学院化学研究所 | Cellulose aerogel and preparation method for hybrid aerogel thereof |
| CN105820372A (en) * | 2016-03-30 | 2016-08-03 | 青岛大学 | Conductive aerogel and preparation method thereof |
| CN105970193A (en) * | 2016-05-24 | 2016-09-28 | 中国工程物理研究院激光聚变研究中心 | Metal aerogel with high specific surface area and preparation method thereof |
| CN108314000A (en) * | 2018-02-12 | 2018-07-24 | 浙江大学 | A kind of preparation method of high stretchable full carbon aerogels |
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