CN117819518A - High-compaction porous carbon material and preparation method thereof - Google Patents
High-compaction porous carbon material and preparation method thereof Download PDFInfo
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- CN117819518A CN117819518A CN202311725405.7A CN202311725405A CN117819518A CN 117819518 A CN117819518 A CN 117819518A CN 202311725405 A CN202311725405 A CN 202311725405A CN 117819518 A CN117819518 A CN 117819518A
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 52
- 238000005056 compaction Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 21
- 239000007833 carbon precursor Substances 0.000 claims abstract description 15
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 14
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000007921 spray Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 17
- 238000001694 spray drying Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000011268 mixed slurry Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 3
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920005546 furfural resin Polymers 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 18
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 abstract description 14
- 238000005469 granulation Methods 0.000 abstract description 9
- 230000003179 granulation Effects 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 7
- 238000001994 activation Methods 0.000 abstract description 6
- 230000004913 activation Effects 0.000 abstract description 6
- 238000007711 solidification Methods 0.000 abstract description 6
- 230000008023 solidification Effects 0.000 abstract description 6
- 239000005543 nano-size silicon particle Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000003763 carbonization Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 abstract description 4
- 239000010406 cathode material Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000004927 fusion Effects 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 11
- 238000005406 washing Methods 0.000 description 9
- 239000003513 alkali Substances 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- 239000007773 negative electrode material Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000005539 carbonized material Substances 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 238000005096 rolling process Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a high-compaction porous carbon material, which is characterized in that an organic carbon source and a carbon nano tube are subjected to spray granulation, so that the preparation of a high-compaction porous carbon precursor by multi-process fusion of dispersion, granulation, pre-solidification and the like is realized, the process flow is greatly simplified, and the preparation stability of the material is improved; in the process of primary calcination, three processes of solidification, carbonization and activation are integrated into one-step process by adopting three-section temperature intervals, so that the process flow of preparing porous carbon by a conventional alkaline method is simplified; the introduction of the high-strength carbon nano tube can enhance the compressive strength of the particles, improve the conductivity of the material and be beneficial to improving the rate capability of the cathode material. The high-compaction porous carbon material has an obvious spherical structure, and the surface is smooth and compact, so that the limited-area deposition of nano silicon in the subsequent preparation of silicon carbon is facilitated.
Description
Technical Field
The invention belongs to the technical field of porous carbon materials, relates to a high-pressure solid porous carbon material, and further relates to a preparation method of the high-pressure solid porous carbon material.
Background
The porous carbon material has very important application in the fields of adsorption, hydrogen storage, super capacitors and lithium battery cathodes. Along with the increasing requirements of super-capacitors and lithium batteries on energy density, in particular to the process of preparing pole pieces, the requirements on compaction density are increased. However, the porous carbon materials prepared by the conventional method have irregular particle morphology, a fragile carbon skeleton and poor compaction resistance.
At present, research on improving compaction density of porous carbon materials is mainly carried out by selecting different carbon sources, such as coke, biomass, resin and the like, as raw materials, adopting a chemical alkali activation method or a physical method (steam and carbon dioxide activation) for pore-forming, and regulating and controlling carbonization temperature to obtain porous carbon. However, the porous carbon material prepared in this way still has difficulty in meeting the technical requirements of the anode material on the porous carbon, and the preparation process flow is complex. Particularly, the porous carbon taking the novel silicon carbon negative electrode as a technical carrier directly determines the compaction density of the silicon carbon negative electrode material by the skeleton strength of the porous carbon, thereby influencing the improvement of the energy density and the cycle performance of the battery.
Disclosure of Invention
The invention aims to provide a preparation method of a high-compaction porous carbon material, which solves the problem of poor compaction density in the prior art.
The technical scheme adopted by the invention is that the preparation method of the high-compaction porous carbon material comprises the following steps:
step 1, respectively dissolving and dispersing resin, carbon nano tubes and KOH in ethanol, and mixing to obtain mixed slurry;
step 2, spray drying the mixed slurry to obtain a porous carbon precursor;
step 3, calcining the porous carbon precursor to obtain black powder;
step 4, cleaning and drying the black powder to obtain porous carbon;
and 5, purifying the porous carbon at high temperature to obtain the high-compaction porous carbon material.
The invention is also characterized in that:
in the step 1, the mass ratio of the resin, the carbon nano tube and the KOH is 1:0.001 to 0.1:0.5 to 3.
The resin comprises phenolic resin, epoxy resin, furfural resin or urea-formaldehyde resin.
In the spray drying process in the step 2, the spray temperature is 150-200 ℃, and the frequency of the atomizer is 200-350 HZ.
In the step 2, the spray drying process adopts inert atmosphere protection, and the inert atmosphere is one of nitrogen and argon.
In the calcining process in the step 3, three-stage heating program is adopted, and the temperature is firstly kept at 0-200 ℃ for 1-4h; then continuously heating to 400-500 ℃ and preserving heat for 1-4h; finally, heating to 800-900 ℃, and preserving heat for 1-4h.
And in the step 3, inert atmosphere protection is adopted in the calcination process.
It is another object of the present invention to provide a highly compacted porous carbon material and use thereof as a carrier for the preparation of silicon carbon materials.
The invention adopts another technical scheme that the high-pressure solid porous carbon material is prepared by adopting the preparation method of the high-pressure solid porous carbon material.
The beneficial effects of the invention are as follows: the preparation method of the high-compaction porous carbon material of the invention carries out spray granulation on the organic carbon source and the carbon nano tube, thereby realizing multiple processes of dispersion, granulation, pre-solidification and the likeThe high-compaction porous carbon precursor is prepared by fusion, so that the process flow is greatly simplified, and the preparation stability of the material is improved; in the process of primary calcination, three processes of solidification, carbonization and activation are integrated into one-step process by adopting three-section temperature intervals, so that the process flow of preparing porous carbon by a conventional alkaline method is simplified; the introduction of the high-strength carbon nano tube can enhance the compressive strength of the particles, improve the conductivity of the material and be beneficial to improving the rate capability of the cathode material. The high-compaction porous carbon material has obvious spherical structure, smooth and compact surface and high pore volume (0.6-1.0 cm) 3 Per g) and a specific surface area of greater than 1500m 2 And/g), has a micropore structure, wherein the micropore (< 2 nm) accounts for more than 97%, has good compaction resistance and conductivity, and is very favorable for the limited-area deposition of nano silicon in the subsequent preparation of silicon carbon.
Drawings
FIG. 1 is a morphology diagram of a silicon-carbon negative electrode material obtained by a traditional method;
FIG. 2 is a roll graph of a silicon carbon negative electrode material compounded with graphite obtained by a conventional method;
FIG. 3 is a microscopic SEM image of a porous carbon material obtained by the method for preparing a highly compacted porous carbon material of the present invention;
FIG. 4 is a roll pattern of the silicon carbon negative electrode material prepared in example 1 after compounding with graphite in the preparation method of the highly compacted porous carbon material of the present invention;
fig. 5 is an electrochemical graph of the silicon carbon negative electrode material prepared in example 1 in the preparation method of the highly compacted porous carbon material of the present invention.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The preparation method of the high-compaction porous carbon material comprises the following steps:
step 1, according to the mass ratio of 1:0.001 to 0.1:0.5 to 3, respectively dissolving and dispersing the resin, the carbon nano tube and the KOH in ethanol, mixing the ethanol and the ethanol in a stirring kettle, and stirring the mixture to obtain mixed slurry; the resin comprises phenolic resin, epoxy resin, furfural resin or urea-formaldehyde resin;
step 2, spray drying the mixed slurry, wherein inert atmosphere protection is adopted in the process, the spraying temperature is 150-200 ℃, and the frequency of an atomizer is 200-350 HZ, so as to obtain a porous carbon precursor; the inert atmosphere is one of nitrogen and argon;
step 3, calcining the porous carbon precursor, wherein inert atmosphere protection is adopted in the process, a three-stage heating program is adopted, and the temperature is kept at 0-200 ℃ for 1-4h; then continuously heating to 400-500 ℃ and preserving heat for 1-4h; finally, heating to 800-900 ℃, and preserving heat for 1-4 hours to obtain black powder;
step 4, washing the black powder with deionized water to remove residual alkali, and drying to obtain black powder;
and 5, purifying the black powder at high temperature to obtain the high-compaction porous carbon material.
The high-compaction porous carbon material is prepared by adopting the preparation method of the high-compaction porous carbon material.
Comparative example
Preparing a porous carbon material by a conventional alkaline method:
step 1, pre-carbonizing phenolic resin at a pre-carbonizing temperature of 500 ℃ to obtain a pre-carbonized material;
step 2, after crushing the pre-carbonized material, uniformly mixing the crushed pre-carbonized material with KOH according to a mass ratio of 1:2 to obtain a mixture;
step 3, placing the mixture into an activation furnace, and activating for 2 hours at 850 ℃;
step 4, placing the activated mixture material into a water washing kettle, repeatedly washing to be neutral, and drying;
and 5, further purifying the dried material at a high temperature of 800 ℃ to obtain the porous carbon material.
The silicon carbon material prepared by the porous carbon material obtained in the embodiment is shown in fig. 1, and can be seen to be an irregular porous carbon material with obvious irregular morphology. The schematic rolling diagram of the silicon carbon material and graphite after being compounded is shown in fig. 2, and it can be seen that the particle crushing condition is serious under the condition of the same compaction density.
Example 1
Step 1, according to the mass ratio of 1:0.01:1.5, respectively dissolving and dispersing phenolic resin, carbon nano tubes and KOH, then mixing the materials in a stirring kettle, and stirring the materials for 1h to obtain mixed slurry;
step 2, spray drying the mixed slurry in a spray drying granulation mode, wherein inert atmosphere protection is adopted in the process, the spraying temperature is 160 ℃, the frequency of an atomizer is 300HZ, and a porous carbon precursor is obtained;
step 3, calcining the porous carbon precursor, wherein inert atmosphere protection is adopted in the process, and the temperature is kept at 0-200 ℃ for 1h; heating to 400 ℃ and preserving heat for 1h; finally, heating to 800 ℃, and preserving heat for 2 hours to obtain black powder;
step 4, washing the black powder with deionized water, stirring for 10 hours, washing residual alkali in the black powder, and drying to obtain porous carbon, wherein the water-to-material ratio is 1:20;
and 5, purifying the porous carbon at a high temperature of 800 ℃ to obtain the high-compaction porous carbon material.
The spherical porous carbon material obtained in the embodiment has an obvious spherical structure, a compact surface and a microporous structure, as shown in fig. 3, which provides a good carbon skeleton matrix for subsequent silicon deposition and avoids local over-deposition of silicon. As shown in fig. 4, the pole piece rolling schematic diagram of the silicon-carbon composite material prepared by further depositing silicon by using the spherical porous carbon material obtained in the embodiment is compounded with graphite, and the pole piece rolling schematic diagram still has good particle shape under high compaction, and no obvious broken particles are found, so that the material has good compaction resistance. The charge-discharge curve of the obtained silicon-carbon material is shown in fig. 5, and the charge curve shows a good charge curve without obvious platforms, which indicates that the deposited nano-silicon has smaller size and no obvious nano-silicon enrichment. The capacity reaches 1930mAh/g, the initial effect is 93.5%, and the porous carbon material has good conductivity, so that the prepared silicon carbon material has higher initial effect.
Example 2
Step 1, according to the mass ratio of 1:0.01:2, respectively dissolving and dispersing phenolic resin, carbon nano tubes and KOH, then mixing the materials in a stirring kettle, and stirring the materials for 1h to obtain mixed slurry;
step 2, spray drying the mixed slurry in a spray drying granulation mode, wherein inert atmosphere protection is adopted in the process, the spraying temperature is 200 ℃, the frequency of an atomizer is 300HZ, and a porous carbon precursor is obtained;
step 3, calcining the porous carbon precursor, wherein inert atmosphere protection is adopted in the process, and the temperature is kept at 0-200 ℃ for 2 hours; heating to 400 ℃ and preserving heat for 2 hours; finally, heating to 800 ℃, and preserving heat for 2 hours to obtain black powder;
step 4, washing the black powder with deionized water, stirring for 10 hours, washing residual alkali in the black powder, and drying to obtain porous carbon, wherein the water-to-material ratio is 1:20;
and 5, purifying the porous carbon at a high temperature of 800 ℃ to obtain the high-compaction porous carbon material.
Example 3
Step 1, according to the mass ratio of 1:0.1:3, respectively dissolving and dispersing phenolic resin, carbon nano tubes and KOH, then mixing the materials in a stirring kettle, and stirring the materials for 1h to obtain mixed slurry;
step 2, spray drying the mixed slurry in a spray drying granulation mode, wherein inert atmosphere protection is adopted in the process, the spraying temperature is 200 ℃, the frequency of an atomizer is 300HZ, and a porous carbon precursor is obtained;
step 3, calcining the porous carbon precursor, wherein inert atmosphere protection is adopted in the process, and the temperature is kept at 0-200 ℃ for 4 hours; heating to 400 ℃ and preserving heat for 4 hours; finally, heating to 800 ℃, and preserving heat for 4 hours to obtain black powder;
step 4, washing the black powder with deionized water, stirring for 10 hours, washing residual alkali in the black powder, and drying to obtain porous carbon, wherein the water-to-material ratio is 1:20;
and 5, purifying the porous carbon at a high temperature of 800 ℃ to obtain the high-compaction porous carbon material.
The properties of the highly compacted porous carbon materials obtained in comparative examples and examples 1 to 3 are compared with the following table:
from the above table, the high-compaction porous carbon material obtained by the preparation method provided by the invention has good compaction resistance and good conductivity.
By adopting the mode, the preparation method of the high-compaction porous carbon material disclosed by the invention has the advantages that the organic carbon source and the carbon nano tube are subjected to spray granulation, so that the preparation of the high-compaction porous carbon precursor by multi-process fusion such as dispersion, granulation, pre-solidification and the like is realized, the process flow is greatly simplified, and the preparation stability of the material is improved; in the process of primary calcination, three processes of solidification, carbonization and activation are integrated into one-step process by adopting three-section temperature intervals, so that the process flow of preparing porous carbon by a conventional alkaline method is simplified; the introduction of the high-strength carbon nano tube can enhance the compressive strength of the particles, improve the conductivity of the material and be beneficial to improving the rate capability of the cathode material. The high-compaction porous carbon material has obvious spherical structure, smooth and compact surface, high pore volume (0.6-1.0 cm < 3 >/g) and large specific surface (more than 1500m < 2 >/g), has a microporous structure, has a micropore (less than 2 nm) occupying ratio of more than 97%, has good compaction resistance and conductivity, and is very favorable for the limited-area deposition of nano silicon in the subsequent preparation of silicon carbon.
Claims (8)
1. The preparation method of the high-compaction porous carbon material is characterized by comprising the following steps of:
step 1, respectively dissolving and dispersing resin, carbon nano tubes and KOH in ethanol, and mixing to obtain mixed slurry;
step 2, spray drying the mixed slurry to obtain a porous carbon precursor;
step 3, calcining the porous carbon precursor to obtain black powder;
step 4, cleaning and drying the black powder to obtain porous carbon;
and 5, purifying the porous carbon at high temperature to obtain the high-compaction porous carbon material.
2. The method for preparing a highly compacted porous carbon material according to claim 1, wherein the mass ratio of the resin, the carbon nanotubes and the KOH in the step 1 is 1:0.001 to 0.1:0.5 to 3.
3. The method of preparing a highly compacted porous carbon material according to claim 1, wherein the resin comprises a phenolic resin, an epoxy resin, a furfural resin or a urea-formaldehyde resin.
4. The method of claim 1, wherein the spray temperature is 150 to 200 ℃ and the atomizer frequency is 200 to 350HZ during the spray drying in step 2.
5. The method of claim 1, wherein the spray drying in step 2 is performed in an inert atmosphere, wherein the inert atmosphere is one of nitrogen and argon.
6. The method for preparing a highly compacted porous carbon material according to claim 1, wherein in the calcination process in step 3, a three-stage temperature raising procedure is adopted, and the temperature is kept at 0-200 ℃ for 1-4 hours; then continuously heating to 400-500 ℃ and preserving heat for 1-4h; finally, heating to 800-900 ℃, and preserving heat for 1-4h.
7. The method of claim 1, wherein the calcination in step 3 is performed in an inert atmosphere.
8. A highly compacted porous carbon material, characterized in that it is prepared by the method of any one of claims 1 to 7.
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