GB2616699A - High-efficiency and energy-saving preparation method of artificial graphite powder based on rotary kiln - Google Patents
High-efficiency and energy-saving preparation method of artificial graphite powder based on rotary kiln Download PDFInfo
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- GB2616699A GB2616699A GB2217638.2A GB202217638A GB2616699A GB 2616699 A GB2616699 A GB 2616699A GB 202217638 A GB202217638 A GB 202217638A GB 2616699 A GB2616699 A GB 2616699A
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- United Kingdom
- Prior art keywords
- graphite powder
- artificial graphite
- ceramic pot
- energy
- rotary kiln
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910021383 artificial graphite Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 28
- 239000010426 asphalt Substances 0.000 claims abstract description 22
- 239000002775 capsule Substances 0.000 claims abstract description 19
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000013268 sustained release Methods 0.000 claims abstract description 5
- 239000012730 sustained-release form Substances 0.000 claims abstract description 5
- 238000011049 filling Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims abstract 2
- 239000002918 waste heat Substances 0.000 claims abstract 2
- 239000002002 slurry Substances 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 7
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 238000005087 graphitization Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000009818 secondary granulation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present disclosure belongs to the technical field of preparation of new energy materials and relates to a high-efficiency and energy-saving preparation method of an artificial graphite powder based on a rotary kiln. The preparation method of an artificial graphite powder includes the following steps: providing asphalt and a graphene capsule with a ratio of 10:1 to 8:1 as raw materials, wherein the graphene capsule conducts sustained release of the asphalt; filling the raw materials into a high-temperature resistant ceramic pot to fill 80% to 90% of a volume of the ceramic pot; placing the ceramic pot in gaps of a rotary kiln with a temperature of 600°C to 1000°C; covering the ceramic pot to control an internal calcination gas atmosphere; conducting calcination for 12 hours; removing the ceramic pot and naturally cooling to a room temperature to obtain the artificial graphite powder. The high temperature waste heat of the rotary kiln may be used in the calcination.
Description
HIGH-EFFICIENCY AND ENERGY-SAVING PREPARATION METHOD OF
ARTIFICIAL GRAPHITE POWDER BASED ON ROTARY KILN
TECHNICAL FIELD
[0001] The present disclosure belongs to the technical field of preparation of new energy materials, and in particular, relates to a high-efficiency and energy-saving preparation method of a novel artificial graphite powder material.
BACKGROUND
[0002] Graphite powder is widely used in catalyst carriers, conductive plastics, conductive coatings, advanced lubricants, lithium-ion batteries, fuel cells and other industries. Graphite powder is also a precursor for preparing high-purity ultrafine graphite powder and high-purity submicron graphite powder. Artificial graphite powder is mostly prepared from petroleum coke and needle coke through powder making, secondary granulation, asphalt coating, carbonization, graphitization and other processes. The long production processes, high manufacturing cost, and high energy consumption limit the development and application of artificial graphite powder to a certain extent. Research and development of artificial graphite powder with desirable quality and high cost performance is an important way to promote its subsequent development and utilization. The artificial graphite powder, compared with natural graphite powder, has a manufacturing cost that mainly depends on the type of raw material and the high-temperature graphitization. The selection and ratio of raw materials and the technology of graphitization become a core technology to control the cost of artificial graphite powder. Therefore, rational selection of raw materials and research on the ratio, as well as using the heat lost in gaps of the rotary kiln as a heat source, can make the production process more reasonable, thereby greatly reducing production cost, increasing production efficiency, and improving working conditions to achieve efficient and safe production. For example, Chinese patent 201921074542.8 provided a combined device for preparing a high-purity artificial graphite powder. In the combined device, a milling machine for clearing and milling adherents on the surface of an artificial graphite electrode and a machine tool for finishing the artificial graphite electrode are matched together with a graphite powder collection system. However, the combined device has no reduction in production cost, limiting the subsequent functional application of artificial graphite powder.
SUMMARY
[0003] Aiming at the defects in the background, the present disclosure proposes a high-efficiency and energy-saving preparation method of an artificial graphite powder based on a rotary kiln. The preparation method uses a graphene capsule and asphalt as raw materials, adjusts a ratio of the raw materials, utilizes heat energy lost in gaps of a rotary kiln, and introduces the graphene capsule to conduct sustained release of the asphalt, so as to prepare an artificial graphite powder with multi-level interfaces. The preparation method has a high efficiency, a low cost, energy-saving properties, and environmental friendliness.
[0004] In order to achieve the above objective, the present disclosure adopts the following technical solutions.
[0005] The present disclosure provides a high-efficiency and energy-saving preparation method for an artificial graphite powder based on a rotary kiln, including the following steps: [0006] step 1: preparing a slurry using asphalt and a graphene capsule with a suitable ratio of 10:1 to 8:1 as raw materials, where the graphene capsule conducts sustained release of the asphalt to achieve a certain degree of graphitization and functionalizati on; filling the slurry into a high-temperature-resistant ceramic pot with a sealing cover of 80% to 90% of a volume of the ceramic pot, to control high-temperature calcination under anoxic conditions; and [0007] step 2: placing the ceramic pot containing the slurry of the graphene capsule and the asphalt in gaps at different temperatures of 600°C to 1,000°C of a rotary kiln, covering the sealing cover of the ceramic pot to control an internal calcination gas atmosphere; conducting calcination for 12 h, removing the ceramic pot, and naturally cooling to a room temperature to obtain an artificial graphite powder sample.
[0008] Further, in step 1, the ceramic pot has an inner diameter of 20 cm and a wall thickness of 1.2 cm.
[0009] Further, in step 2, the graphene capsule and the asphalt are thoroughly mixed by mechanical stirring for 3 h. [0010] Compared with the prior art, the present disclosure has the following beneficial effects. 100111 In the present disclosure, the residual temperature in the gaps of the rotary kiln is creatively used as a heat source, and the low-cost asphalt is used as a raw material, thereby effectively reducing the cost of the artificial graphite powder, and fully realizing energy-saving and environment-friendly artificial synthesis of the graphite powder, which has a strong commercial application value. The artificial graphite powder material has a certain degree of graphitization, with a particle size concentrated at 5 um to 10 jn, and an internal pore size of 5 nm to 8 nm, averagely about 6.53 nm. Therefore, the present disclosure provides a high-efficiency, energy-saving, and low-cost method for artificially synthesizing graphite powder, which is of great significance for promoting the functional application of artificial graphite powder, showing desirable commercial values and development prospects.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 shows a photo of a ceramic pot for firing a graphite powder in step 2 of Example 3, [0013] FIG. 2 shows a scanning electron microscopy (SEM) image of the graphite powder obtained in step 2 of Example 3; [0014] FIG. 3 shows a particle size distribution diagram of the graphite powder obtained in step 2 of Example 3; [0015] FIG. 4 shows an X-ray diffraction (XRD) pattern of the graphite powder obtained in step 2 of Example 3; [0016] FIG. 5 shows an X-ray photoelectron spectroscopy ()CPS) pattern of the graphite powder obtained in step 2 of Example 3; [0017] FIG. 6 shows a Raman spectrum of the graphite powder obtained in step 2 of Example 3; and [0018] FIG. 7 shows an adsorption-desorption curve of the graphite powder obtained in step 2 of Example 3.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0019] The technical solutions of the present disclosure will be further described below through specific examples.
[0020] Example 1
[0021] A high-efficiency and energy-saving preparation method of an artificial graphite powder included the following steps: [0022] Step 1: asphalt and a graphene capsule were used as raw materials, where the graphene capsule was used for sustained release of the asphalt; the asphalt and the graphene capsule were prepared at a ratio of 10:1 to obtain a slurry, which was mixed homogeneously by mechanical stirring; the slurry was put into a high-temperature-resistant ceramic pot with a cover, where the slurry accounted for 80% to 90% of a volume of the ceramic pot. As shown in FIG. 1, the prepared slurry was put into the ceramic pot, and covered for simple sealing.
[0023] Step 2: the ceramic pot containing the slurry of the graphene capsule and the asphalt was placed in a gap at 600°C of a rotary kiln, the sealing cover of the ceramic pot was covered to control an internal calcination gas atmosphere to carbonize the asphalt. After 12 h of calcination, the ceramic pot was removed and naturally cooled to room temperature to obtain an artificial graphite powder sample.
[0024] Example 2
[0025] In this example, step 1 was the same as that of Example 1, the difference was that: in step 2, the ceramic pot containing the slurry of the graphene capsule and the asphalt was placed in a gap at 800°C of a rotary kiln, the sealing cover of the ceramic pot was covered to control an internal calcination gas atmosphere. After 12 h of calcination, the ceramic pot was removed and naturally cooled to room temperature to obtain an artificial graphite powder sample.
[0026] Example 3
[0027] FIG. 2 and FIG. 3 showed an SEM image and a particle size distribution diagram of the artificial graphite powder obtained in Example 3. It was seen from the SEM image that the precursor carbon source after calcination presented a granular and porous surface. It was seen from the particle size distribution diagram that the artificial graphite powder had a particle diameter distribution concentrated at 5!km to 15 Inn, and larger particles could reach about 30 RM.
[0028] FIG. 4 showed an XRD pattern of the artificial graphite powder sample obtained in Example 3, and the artificial graphite powder had diffraction peaks existing at 20=25.6°, 43.2°. The diffraction peak at 20=43.2° corresponded to a (100) plane of the graphite powder material, and there was a relatively broad (002) plane diffraction peak at 20=25.6°. This was due to the random stacking of graphite powder, and the more irregular stacking meant a less obvious diffraction peak. The diffraction peaks shown in the figure were relatively obvious, indicating that the stacking of artificial graphite powder was relatively regular.
[0029] FIG. 5 showed an XPS total spectrogram of the artificial graphite powder sample obtained in Example 3. It was seen from the XPS total spectrogram that a small amount of 0 and N elements were distributed in the artificial graphite powder, which should be due to incomplete carbonization during the calcination; meanwhile, the peak of the C element was higher than that of 0 and N elements, indicating that the main material was still graphite powder.
[0030] FIG. 6 showed a Raman spectrum of the artificial graphite powder sample obtained in Example 3. It was seen from the Raman spectrum that the G peak of graphite powder (representing an E25 vibrating membrane of graphite) was much higher than the D peak (representing a peak of disordered carbon). This showed that there were a large number of graphite crystal structures in the graphite powder, and the D peak and the G peak had a peak intensity ratio 16/10 of 0.89, further indicating that the material had a certain degree of graphitization. This could demonstrate the successful manufacture of graphite powder.
[0031] FIG. 7 showed an adsorption-desorption curve of the artificial graphite powder sample obtained in Example 3. The figure showed that a stagnation loop phenomenon occurred when there was a high relative pressure. This was because the capillary condensation made the adsorption steeper at the position of relatively high pressure (P/P0=0.9-1), and desorption was slower than the adsorption. This proved that the graphite powder material had a relatively narrow pore size distribution. Combined with a BET test report, the graphite powder material had an internal pore size distribution of 5 tun to 8 nm, with an average pore size of 6.53 nm, indicating that the graphite powder material had a mesoporous structure. In addition, according to a BET specific surface area calculation, the graphite powder particles had a specific surface area of 3.43 m2/g.
Claims (7)
- WHAT IS CLAIMED IS: 1. A high-efficiency and energy-saving preparation method of an artificial graphite powder based on a rotary kiln, comprising the following steps: step 1: preparing a slurry using asphalt and a graphene capsule with a suitable ratio of 10:1 to 8:1 as raw materials, wherein the graphene capsule conducts sustained release of the asphalt; filling the slurry into a high-temperature-resistant ceramic pot with a sealing cover of 80% to 90% of a volume of the ceramic pot, to control high-temperature calcination under anoxic conditions; and step 2: placing the ceramic pot containing the slurry of the graphene capsule and the asphalt in gaps at different temperatures of 600°C to 1,000°C of a rotary kiln, covering the sealing cover of the ceramic pot to control an internal calcination gas atmosphere; conducting calcination for 12 h, removing the ceramic pot, and naturally cooling to a room temperature to obtain an artificial graphite powder sample.
- 2. The high-efficiency and energy-saving preparation method of an artificial graphite powder according to claim 1, wherein in step 1, a calcined material is a mixture of the asphalt and the graphene capsule.
- 3. The high-efficiency and energy-saving preparation method of an artificial graphite powder according to claim 1, wherein in step 1, the asphalt and the graphene capsule have a ratio of 10:1 to 8:1
- 4. The high-efficiency and energy-saving preparation method of an artificial graphite powder according to claim 1, wherein in step 1, the asphalt and the graphene capsule have a filling ratio of 80% to 90% in the ceramic pot.
- 5. The high-efficiency and energy-saving preparation method of an artificial graphite powder according to claim 1, wherein in step 2, the calcination of the artificial graphite powder is conducted by the high-temperature waste heat of the rotary kiln.
- 6. The high-efficiency and energy-saving preparation method of an artificial graphite powder according to claim 1, wherein in step 2, the rotary kiln has a temperature of 600°C to 1,000°C.
- 7. The high-efficiency and energy-saving preparation method of an artificial graphite powder according to claim 1, wherein in step 2, the calcination of the ceramic pot in the rotary kiln is conducted for 12 h.
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CN202210267046.4A CN114590806A (en) | 2022-03-17 | 2022-03-17 | Efficient and energy-saving preparation method based on artificial graphite powder of rotary kiln |
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CN114590806A (en) * | 2022-03-17 | 2022-06-07 | 电子科技大学长三角研究院(湖州) | Efficient and energy-saving preparation method based on artificial graphite powder of rotary kiln |
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CN112421029A (en) * | 2020-11-19 | 2021-02-26 | 萝北瑞喆烯碳新材料有限公司 | Graphite negative electrode material capable of being charged and discharged rapidly and preparation method thereof |
CN112768689A (en) * | 2021-01-12 | 2021-05-07 | 湖南金阳烯碳新材料有限公司 | Graphene modified graphite negative electrode material and preparation method thereof |
CN113023725A (en) * | 2020-11-26 | 2021-06-25 | 宁波杉杉新材料科技有限公司 | Coated modified artificial graphite negative electrode material, preparation method thereof and lithium ion battery |
CN114590806A (en) * | 2022-03-17 | 2022-06-07 | 电子科技大学长三角研究院(湖州) | Efficient and energy-saving preparation method based on artificial graphite powder of rotary kiln |
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- 2022-03-17 CN CN202210267046.4A patent/CN114590806A/en active Pending
- 2022-11-25 GB GB2217638.2A patent/GB2616699A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112421029A (en) * | 2020-11-19 | 2021-02-26 | 萝北瑞喆烯碳新材料有限公司 | Graphite negative electrode material capable of being charged and discharged rapidly and preparation method thereof |
CN113023725A (en) * | 2020-11-26 | 2021-06-25 | 宁波杉杉新材料科技有限公司 | Coated modified artificial graphite negative electrode material, preparation method thereof and lithium ion battery |
CN112768689A (en) * | 2021-01-12 | 2021-05-07 | 湖南金阳烯碳新材料有限公司 | Graphene modified graphite negative electrode material and preparation method thereof |
CN114590806A (en) * | 2022-03-17 | 2022-06-07 | 电子科技大学长三角研究院(湖州) | Efficient and energy-saving preparation method based on artificial graphite powder of rotary kiln |
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GB202217638D0 (en) | 2023-01-11 |
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