CN112624104A - Preparation method of wood fiber-based high-conductivity carbon material - Google Patents
Preparation method of wood fiber-based high-conductivity carbon material Download PDFInfo
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- CN112624104A CN112624104A CN202110023095.9A CN202110023095A CN112624104A CN 112624104 A CN112624104 A CN 112624104A CN 202110023095 A CN202110023095 A CN 202110023095A CN 112624104 A CN112624104 A CN 112624104A
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- 229920002522 Wood fibre Polymers 0.000 title claims abstract description 25
- 239000002025 wood fiber Substances 0.000 title claims abstract description 25
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 60
- 238000005087 graphitization Methods 0.000 claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000010000 carbonizing Methods 0.000 claims abstract description 20
- 239000012467 final product Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000011068 loading method Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 238000003763 carbonization Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 14
- 238000005303 weighing Methods 0.000 description 14
- 229920002678 cellulose Polymers 0.000 description 10
- 239000001913 cellulose Substances 0.000 description 10
- 229920005610 lignin Polymers 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002006 petroleum coke Substances 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004575 stone 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
- C01B32/20—Graphite
- C01B32/205—Preparation
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a wood fiber-based high-conductivity carbon material, which comprises the steps of placing wood fiber raw materials in a closed crucible, carbonizing, and then soaking the product in a material containing a certain amount of Ni2+Overnight and dried for use. Putting the Ni-impregnated carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace for reaction for a certain time, and cooling to obtain a final product. Aiming at the problem that the wood fiber raw material is difficult to graphitize by the conventional method, the product with higher graphitization degree is successfully prepared by adopting the Ni catalytic method, has a graphite structure with more than 40 layers, and the required temperature is obviously lower than 2800 ℃ required by the conventional graphitization method. In addition, the metal used as the catalyst exists in a simple substance form, which is beneficial to improving the shielding efficiency and also avoids the risk of secondary pollution caused by concentrated acid washing. The conductivity of the obtained product can exceed 100S/cm under 20MPa, and the product has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of preparation and application of carbon materials, and mainly relates to a preparation method of a wood fiber-based high-conductivity carbon material.
Technical Field
The graphitized carbon material has the greatest characteristics of excellent conductivity and stable physicochemical properties. At present, graphitized carbon materials are usually prepared from stone raw materials such as asphalt, petroleum coke and the like under the conditions of high temperature and high pressure, which not only can be huge, but also has strict requirements on production equipment, so that the production cost is high. In contrast, lignocellulosic feedstocks not only contain high amounts of carbon. And the method has the remarkable advantages of wide sources and reproducibility, so that the preparation of the high-conductivity graphitized carbon material by using the wood fiber raw material instead of the traditional fossil energy has a great research value.
However, unlike petroleum coke, pitch, etc., carbonized products of lignocellulosic raw materials are non-graphitizable amorphous carbons, and efficient graphitization conversion is difficult to occur even when heated to 3000 ℃, so the present invention addresses this problem by using Ni as a catalyst to achieve graphitization of lignocellulosic raw materials at relatively low temperatures (e.g., 1400 ℃). After graphitization treatment, Ni is converted into a simple substance form and exists in the product without being washed by concentrated acid, the preparation process is green and environment-friendly, and the prepared graphitized sample has good conductivity which can exceed 100S/cm under 20MPa, and has good application prospect and development potential in the fields of conductivity and electromagnetic shielding.
Disclosure of Invention
The invention aims to provide a preparation method of a wood fiber-based high-conductivity carbon material with high efficiency and low energy consumption.
The technical scheme of the invention is as follows: a preparation method of a wood fiber-based high-conductivity carbon material comprises the following steps:
firstly, carbonizing wood fiber raw materials and loading a metal catalyst: placing wood fiber raw material in a closed crucible, high-temperature carbonizing treatment, and soaking the product in a solution containing a certain amount of Ni2+The water solution is kept overnight, and then the carbon loaded with Ni is obtained by drying for standby;
secondly, putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace for reaction for a certain time, converting Ni into simple substance Ni due to the reduction action of the carbon, further performing catalytic graphitization reaction, and cooling to obtain a final product.
The first step carbonization temperature is 400-600 ℃.
The metal Ni loading amount of the Ni-loaded carbon in the first step is 2-5 mmol/g.
The graphitization reaction temperature is 1200-1600 ℃.
The graphitization reaction time is 2-5 h.
The high-conductivity carbon material obtained by the preparation method of the wood fiber-based high-conductivity carbon material adopts Ni as a catalyst, so that the conductivity of a product obtained by effectively graphitizing and converting wood fiber raw materials at a relatively low temperature is over 100S/cm under 20 MPa.
Has the advantages that:
1. the Ni catalysis method can effectively graphitize the wood fiber raw material which is difficult to graphitize at a relatively low temperature, which is significantly lower than 2800 ℃ required by the traditional graphitization. The obtained product can achieve complete graphitization conversion, the crystallinity is close to natural graphite, and the conductivity of the product can exceed 100S/cm under 20 MPa.
2. After the graphitization reaction, the metal as the catalyst exists in a simple substance form, which is beneficial to improving the electromagnetic shielding efficiency of the product, and simultaneously, the step of concentrated acid washing is avoided, so that the preparation process is green and environment-friendly.
Drawings
FIG. 1 is an XRD spectrum of cellulose and lignin after graphitization treatment.
Fig. 2 is a TEM photograph of cellulose and lignin after graphitization treatment.
FIG. 3 is a graph of the conductivity of the product at different pressures.
Detailed Description
A preparation method of a wood fiber-based high-conductivity carbon material comprises the following specific steps:
(1) fully drying raw materials of cellulose and lignin at 140 ℃, placing the dried raw materials in a closed crucible, and carbonizing the raw materials at 400 ℃ for 1 h. Immersing the carbonized product in a solution containing a certain amount of Ni2+After overnight, dried at 140 ℃ until ready for use.
(2) Putting the Ni-loaded carbon into a high-temperature resistant closed crucible, putting the crucible into a high-temperature furnace for reaction for a certain time, and cooling to obtain a final product.
Aiming at the problem that the wood fiber raw material is difficult to graphitize by the conventional method, the product with higher graphitization degree is successfully prepared by adopting the Ni catalytic method, has a graphite structure with more than 40 layers, and has the temperature greatly lower than 2800 ℃ required by the conventional graphitization. The conductivity of the obtained product can exceed 100S/cm under 20MPa, and the product has a good application prospect.
Example 1:
placing the cellulose in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1200 ℃ to react for 3h to obtain a final product. The product was calculated to have a degree of graphitization of 43.6% and an electrical conductivity of 57S/cm at 20 MPa.
Example 2:
placing the cellulose in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 3h to obtain a final product. The product was calculated to have a degree of graphitization of 62.7% and an electrical conductivity of 89S/cm at 20 MPa.
Example 3:
placing the cellulose in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, heating to 1600 ℃, and reacting for 3 hours to obtain a final product. The product was calculated to have a degree of graphitization of 69.2% and an electrical conductivity of 104S/cm at 20 MPa.
Example 4:
placing the cellulose in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 4 mmol. Will be provided withPutting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 3h to obtain a final product. The product was calculated to have a degree of graphitization of 57.1% and an electrical conductivity of 68S/cm at 20 MPa.
Example 5:
placing the cellulose in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 10 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 3h to obtain a final product. The product was calculated to have a degree of graphitization of 68.4% and an electrical conductivity of 76S/cm at 20 MPa.
Example 6:
placing the cellulose in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 2h to obtain a final product. The product was calculated to have a degree of graphitization of 61.3% and an electrical conductivity of 59S/cm at 20 MPa.
Example 7:
placing the cellulose in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 5 hours to obtain a final product. The product was calculated to have a degree of graphitization of 70.5% and an electrical conductivity of 84S/cm at 20 MPa.
Example 8:
putting the lignin in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. To be loaded with NiPlacing the carbon in a high-temperature-resistant closed crucible, placing the crucible in a high-temperature furnace, and heating to 1200 ℃ to react for 3h to obtain a final product. The product was calculated to have a graphitization degree of 39.7% and an electrical conductivity of 44S/cm at 20 MPa.
Example 9:
putting the lignin in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 3h to obtain a final product. The product was calculated to have a graphitization degree of 54.2% and an electrical conductivity of 62S/cm at 20 MPa.
Example 10:
putting the lignin in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, heating to 1600 ℃, and reacting for 3 hours to obtain a final product. The product was calculated to have a degree of graphitization of 61.5% and an electrical conductivity of 84S/cm at 20 MPa.
Example 11:
putting the lignin in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 4 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 3h to obtain a final product. The product was calculated to have a degree of graphitization of 56.8% and an electrical conductivity of 54S/cm at 20 MPa.
Example 12:
putting the lignin in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 10 mmol. Placing Ni-loaded carbon inAnd (3) placing the crucible in a high-temperature-resistant closed crucible into a high-temperature furnace, and heating the crucible to 1400 ℃ for reaction for 3h to obtain a final product. The product was calculated to have a graphitization degree of 57.7% and an electrical conductivity of 59S/cm at 20 MPa.
Example 13:
putting the lignin in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 2h to obtain a final product. The product was calculated to have a degree of graphitization of 56.4% and an electrical conductivity of 51S/cm at 20 MPa.
Example 14:
putting the lignin in a closed crucible, and carbonizing at 400 ℃ for 1 h. Weighing 2g of carbonized product, and soaking the carbonized product in a solution containing a certain amount of Ni2+After overnight drying at 140 c until ready for use, the Ni loading in the charcoal sample was 6 mmol. Putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace, and heating to 1400 ℃ for reaction for 5 hours to obtain a final product. The product was calculated to have a degree of graphitization of 59.6% and an electrical conductivity of 60S/cm at 20 MPa.
Claims (6)
1. The preparation method of the wood fiber-based high-conductivity carbon material is characterized by comprising the following steps of:
firstly, carbonizing wood fiber raw materials and loading a metal catalyst: placing wood fiber raw material in a closed crucible, high-temperature carbonizing treatment, and soaking the product in a solution containing a certain amount of Ni2+The water solution is kept overnight, and then the carbon loaded with Ni is obtained by drying for standby;
secondly, putting the Ni-loaded carbon into a high-temperature-resistant closed crucible, putting the crucible into a high-temperature furnace for reaction for a certain time, converting Ni into simple substance Ni due to the reduction action of the carbon, further performing catalytic graphitization reaction, and cooling to obtain a final product.
2. The method for preparing the wood fiber-based high-conductivity carbon material according to claim 1, wherein the first carbonization temperature is 400-600 ℃.
3. The preparation method of the wood fiber-based high-conductivity carbon material as claimed in claim 1, wherein the metal Ni loading of the Ni-loaded carbon in the first step is 2-5 mmol/g.
4. The method for preparing the wood fiber-based high-conductivity carbon material according to claim 1, wherein the graphitization reaction temperature is 1200-1600 ℃.
5. The method for preparing the wood fiber-based high-conductivity carbon material according to claim 1, wherein the graphitization reaction time is 2-5 h.
6. The high-conductivity carbon material obtained by the preparation method of the wood fiber-based high-conductivity carbon material as claimed in any one of claims 1 to 5, wherein Ni is used as a catalyst, and the conductivity of a product obtained by performing effective graphitization conversion on a wood fiber raw material at a relatively low temperature is over 100S/cm under 20 MPa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3309326A (en) * | 1963-02-22 | 1967-03-14 | United Coke & Chemicals Compan | Production of electrically conducting carbon |
| US20040232392A1 (en) * | 2001-07-09 | 2004-11-25 | Tsutomu Masuko | Graphite fine powder, and production method and use thereof |
| CN105682442A (en) * | 2016-04-06 | 2016-06-15 | 常州市奥普泰科光电有限公司 | Preparation method for light-weight graphite fiber foam nickel electromagnetic shielding material |
| CN106744915A (en) * | 2016-12-16 | 2017-05-31 | 中国林业科学研究院林产化学工业研究所 | A kind of cellulose base graphitized material and preparation method thereof |
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- 2021-01-08 CN CN202110023095.9A patent/CN112624104A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3309326A (en) * | 1963-02-22 | 1967-03-14 | United Coke & Chemicals Compan | Production of electrically conducting carbon |
| US20040232392A1 (en) * | 2001-07-09 | 2004-11-25 | Tsutomu Masuko | Graphite fine powder, and production method and use thereof |
| CN105682442A (en) * | 2016-04-06 | 2016-06-15 | 常州市奥普泰科光电有限公司 | Preparation method for light-weight graphite fiber foam nickel electromagnetic shielding material |
| CN106744915A (en) * | 2016-12-16 | 2017-05-31 | 中国林业科学研究院林产化学工业研究所 | A kind of cellulose base graphitized material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 唐锠世, 冶金工业出版社 * |
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