CN111217368A - Production process and device of hard carbon negative electrode material - Google Patents
Production process and device of hard carbon negative electrode material Download PDFInfo
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- CN111217368A CN111217368A CN202010095406.8A CN202010095406A CN111217368A CN 111217368 A CN111217368 A CN 111217368A CN 202010095406 A CN202010095406 A CN 202010095406A CN 111217368 A CN111217368 A CN 111217368A
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/318—Preparation characterised by the starting materials
- C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G7/00—Distillation of hydrocarbon oils
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The device comprises an asphalt melting tank, a resin melting tank, a mixing tank, a coking tower, a distillation tower, a crusher, a screening machine, a roller kiln and a high-temperature carbonization furnace, wherein the asphalt melting tank and the resin melting tank are connected with the mixing tank, the mixing tank is connected with the coking tower, a light phase extraction outlet of the coking tower is connected with the distillation tower, a coke outlet of the coking tower feeds materials to the crusher, the crusher feeds materials to the screening machine, the screening machine feeds materials to the roller kiln, and the roller kiln feeds materials to the high-temperature carbonization furnace. The invention melts the asphalt raw material, then mixes the asphalt raw material with resin uniformly for coking, carries out activation treatment after coke discharging, and then carries out carbonization, thus obtaining the hard carbon cathode material with excellent electrochemical performance and stable material structure. The hard carbon cathode material prepared by the invention has the advantages of high battery safety performance, good rate capability, high capacity, excellent cycle performance and outstanding anti-attenuation capability, and the process method is simple, feasible and continuous, and is an excellent raw material for rate type and capacity type battery equipment.
Description
Technical Field
The invention belongs to the field of negative electrode materials, and particularly relates to a production process and a device of a hard carbon negative electrode material.
Background
With the increasing exhaustion of fossil fuels and the gradual deterioration of the environment, environmental protection measures and new energy development plans are drawn out from governments of various countries, and environment-friendly renewable energy sources are urgently needed to replace the traditional fossil energy sources which are used on a large scale at present. Therefore, the development of new energy becomes an important strategic industry of all countries to preempt the development of advanced points in the future. The lithium ion secondary battery is used as a green new energy battery, the development of the lithium ion secondary battery is from the 80 th of 20 th century, the lithium ion secondary battery is rapidly developed since the commercialization of the Japan Sony company in 1992, the lithium ion secondary battery is an internationally recognized ideal chemical energy source at present, has the advantages of high voltage, high energy density, long cycle life, small self-discharge rate, no memory effect, green environmental protection and the like, is widely applied to the fields of consumer electronics, electric tools, medical electronics and the like, is widely applied to the fields of pure electric vehicles, hybrid electric vehicles, electric bicycles, rail transit, aerospace, ships and naval vessels, industrial energy conservation, green buildings, space technology and the like, is a new generation of sustainable green energy, and particularly is a new energy automobile, and the market demand of a cathode material serving as the core of a power battery is increased day by day.
The hard carbon cathode material is used as a new cathode material and has higher Li due to the stereo cross-linked structure+The lithium ion battery cathode material has the characteristics of diffusion coefficient, wider lithium intercalation potential range, suitability for large-current charge and discharge, high rate performance, high specific capacity, low cost and the like, and is also considered to be the most potential lithium ion battery cathode material in the future. However, the hard carbon negative electrode materials in the current market are pyrolytic carbons with a structure close to amorphous carbon, and generally>The graphite is difficult to graphitize by treatment at 20000 ℃, the graphite is generally prepared by heat treatment of organic matters (such as phenolic resin, epoxy resin, organic compound pyrolytic carbon, polyglycitol PEA and the like), and the graphite has the problems of low cycle retention rate, serious lithium precipitation in cycle composition and the like, and is expensive and low in market utilization rate.
Disclosure of Invention
The invention provides a production process and a device of a hard carbon cathode material, wherein different asphalt raw materials are coarsely crushed or directly melted and then are uniformly mixed with resin in a mixing tank to enter a coking tower for coking, the mixture is crushed and screened after being discharged from the coking tower and then enters a roller kiln for activation treatment, and then the mixture enters a high-temperature carbonization furnace for carbonization to obtain the hard carbon cathode material with excellent electrochemical performance and stable material structure. The hard carbon cathode material prepared by the invention has the advantages of high battery safety performance, good rate capability, high capacity, excellent cycle performance and outstanding anti-attenuation capability, and the process method is simple, feasible and continuous, and is an excellent raw material for rate type and capacity type battery equipment.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process of a hard carbon negative electrode material comprises the steps of melting an asphalt raw material, uniformly mixing the molten asphalt raw material with resin, coking the mixture in a coking tower, crushing and screening the coked mixture, introducing the coked mixture into a roller kiln, performing activation treatment, and carbonizing the activated mixture in a high-temperature carbonization furnace to obtain the hard carbon negative electrode material; the specific process steps comprise:
1) pretreatment of raw materials: pouring the asphalt into an asphalt melting tank for melting; pouring the resin into a resin melting tank for melting;
2) mixing materials: putting the materials in the resin melting tank and the asphalt melting tank into a material mixing tank, and heating and stirring uniformly;
3) coking: the materials in the mixing tank are thrown into a coking tower for coking;
4) a distillation column: the distillate oil which is obtained by pressurizing and coking the coking tower enters the bottom of the distillation tower and is distilled to obtain light-phase oil and heavy-phase oil;
5) crushing and screening: after coke is formed in the coking tower, the raw coke enters a crusher to be crushed, and a sieving machine is used for sieving and grading;
6) and (3) activation: the classified coke powder enters a roller kiln for activation treatment;
7) carbonizing: and (4) feeding the powder treated by the roller kiln into a high-temperature carbonization furnace for carbonization.
The melting temperature of the asphalt in the step 1) is 100-200 ℃, the heating rate is 1-15 ℃/min, and the constant temperature time is 0.5-5 h.
The melting temperature of the resin in the step 1) is 50-150 ℃, the heating rate is 1-15 ℃/min, and the constant temperature time is 0.5-5 h.
The temperature of the material mixing tank is 50-250 ℃, and the stirring speed is 20-50 r/min.
The pressure of the coking tower is 0.1-3 Mpa, the coking temperature is 480-600 ℃, the heating rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
The crushing and screening granularity D50 in the step 5) is 10-25 μm.
The activating agent in the step 6) is water or carbon dioxide, the dosage of the activating agent is 0.5-5 mL/min, the activation temperature is 500-1200 ℃, the activation time is 0.1-10 h, and the activation process needs inert gas protection.
The carbonization temperature in the step 7) is 1000-2000 ℃, the temperature rise rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
The utility model provides a device that hard charcoal cathode material's production technology used, includes that pitch melts jar, resin melting jar, compounding jar, coking tower, distillation column, breaker, screening machine, roller kilns, high temperature retort, pitch melts jar and resin melting jar connection compounding jar, the coking tower is connected to the compounding jar, the light looks of coking tower is adopted mouthful and is connected the distillation column, the play burnt mouth of coking tower is to the breaker pay-off, and the breaker is to the screening machine pay-off, and the screening machine is to roller kilns pay-off, and the roller kilns is to high temperature retort pay-off.
The number of the coking towers is two.
Compared with the prior art, the invention has the beneficial effects that:
1) the hard carbon negative electrode material prepared by the invention effectively considers the excellent cycle performance of the soft carbon negative electrode material and the higher rate performance of the hard carbon negative electrode material through a unique production process, is charged and discharged under the condition of high power density, has stable material structure and outstanding anti-attenuation capability, and can be widely applied to the field of various large battery materials;
2) the cathode material prepared by the invention has excellent electrochemical performance, and can be widely applied to quick-charging battery equipment and lithium ion and sodium ion battery equipment;
3) the coking tower adopted by the invention is a continuous production device, continuous production is realized, the maximization of the productivity is ensured, and the economic benefit is considerable;
4) the distillation tower adopted by the invention recovers the distillate oil, the light phase oil is distilled out for sale, and the heavy phase oil can be recovered and used as a special asphalt raw material.
5) The activation process adopted by the activation process is easy to realize, and the activation raw material has the characteristics of no secondary pollution, low cost and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
In the figure: 1-soft asphalt raw material; 2-hard asphalt raw material; 3-resin raw material; 4-asphalt pulverizer; 5-bucket elevator; 6-a storage bin; 7-a screw feeder; 8-asphalt melting tank; 9-a resin melting tank; 10-a mixing tank; 11-1# coker; 12-2# coker; 13-a crusher; 14-screening machine; 15-roller kiln; 16-high temperature carbonization furnace; 17-finished product warehouse; 18-distillation column.
Detailed Description
The following embodiments are further illustrated by reference to the following specific examples:
as shown in fig. 1, a production process of a hard carbon negative electrode material, different asphalt raw materials are mixed with resin uniformly in a mixing tank 10 for coking after being coarsely broken or directly melted, the mixture is crushed and screened after being discharged from the coking and then enters a roller kiln 15 for activation treatment, and then the mixture enters a high-temperature carbonization furnace 16 for carbonization to obtain the hard carbon negative electrode material, the specific capacity of the prepared hard carbon negative electrode material is more than 380mAh/g, the first efficiency is more than 80%, and the specific process steps comprise:
1) pretreatment of raw materials: pumping the soft asphalt from the raw material tank by a pump, and directly feeding the soft asphalt into an asphalt melting tank for melting; after being crushed by a coarse crusher, the hard asphalt enters a storage bin 6 through a bucket elevator 4, and the hard asphalt is thrown into an asphalt melting tank 8 by a screw feeder 7 to be melted; the resin is pumped into a resin melting tank 9 by a pump to be melted; asphalt powder with the coarse breaking particle size of less than 1 cm;
2) mixing materials: the resin melting tank 9 and the asphalt melting tank 8 are mixed according to the mass ratio of resin: adding asphalt 1: 8-9 into a material mixing tank 10, and heating and stirring uniformly;
3) coking: pumping the materials in the mixing tank 10 into a coking tower through a pump for coking;
4) a distillation column: the distillate oil which is obtained by pressurizing and coking the coking tower enters the bottom of a distillation tower 18, and light phase oil and heavy phase oil are obtained by distillation; selling light phase oil; and the heavy phase oil is partially injected into a raw material tank area to be used as a special asphalt raw material.
5) Crushing and screening: after coke is formed in the coking tower, the raw coke enters a crusher to be crushed, and a sieving machine is used for sieving and grading;
6) and (3) activation: the classified coke powder enters a roller kiln 15 for activation treatment;
7) carbonizing: the powder material treated by the roller kiln 15 enters a high-temperature carbonization furnace 16 for carbonization;
8) and (3) finished product: and (5) feeding the carbonized material into a finished product bin through a belt gallery, and packaging.
The melting temperature of the asphalt in the step 1) is 100-200 ℃, the heating rate is 1-15 ℃/min, and the constant temperature time is 0.5-5 h.
The melting temperature of the resin in the step 1) is 50-150 ℃, the heating rate is 1-15 ℃/min, and the constant temperature time is 0.5-5 h.
The temperature of the material mixing tank is 50-250 ℃, and the stirring speed is 20-50 r/min.
The pressure of the coking tower is 0.1-3 Mpa, the coking temperature is 480-600 ℃, the heating rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
The crushing and screening granularity D50 in the step 5) is 10-25 μm.
The activating agent in the step 6) is water or carbon dioxide, the dosage of the activating agent is 0.5-5 mL/min, the activation temperature is 500-1200 ℃, the activation time is 0.1-10 h, and the activation process needs inert gas protection.
The carbonization temperature in the step 7) is 1000-2000 ℃, the temperature rise rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
The utility model provides a device that hard charcoal cathode material's production technology used, includes that pitch melts jar 8, resin and melts jar 9, compounding jar 10, coking tower, distillation column 18, breaker 13, screening machine 14, roller kilns 15, high temperature retort 16, pitch melts jar 8 and resin and melts jar 9 connection compounding jar 10, the coking tower is connected to compounding jar 10, the distillation column 18 is connected to the light looks extraction mouth of coking tower, the play burnt mouth of coking tower is to 13 pay-offs of breaker, and breaker 13 is to 14 pay-offs of screening machine, and the screening machine 14 is to 15 pay-offs of roller kilns, and roller kilns 15 is to 16 pay-offs of high temperature retort.
The bucket elevator 4 is connected with a bin 6, and the bin 6 feeds hard asphalt raw materials to an asphalt melting tank 8 through a screw feeder 7. The soft asphalt raw material 1 directly enters an asphalt melting tank 8 to be melted, and the hard asphalt raw material 2 is coarsely broken, lifted into a bin 5 through a bucket and then enters the asphalt melting tank 8 through a screw feeder 7; the light phase extraction outlet of the coking tower is connected with the inlet of the distillation tower 18; the asphalt melting tank 8 and the resin melting tank 9 are provided with heaters and stirrers.
The number of the coking towers is two, namely a 1# coking tower 11 and a 2# coking tower 12; the coking and the coke discharging are alternately used, and continuous production is realized.
Example (b):
by adopting the production process of the hard carbon negative electrode material, the main indexes of 5 batches are recorded in the table 1;
TABLE 1 batches of raw materials and their main indices
| Batches of | Raw material asphalt | Softening Point (. degree. C.) | QI(wt％) | Ash content (wt%) |
| 1 | Coal-series soft asphalt | 31 | 2.50 | 0.08 |
| 2 | Coal series hard asphalt | 98 | 5.64 | 0.24 |
| 3 | Petroleum asphalt | 42 | Trace amount of | 0.09 |
| 4 | Imported petroleum asphalt | 115 | 1.16 | 0.12 |
| 5 | Coal tar pitch: petroleum asphalt 1:1 blend | 36 | 1.68 | 0.10 |
The coking drum process parameters in the examples are shown in Table 2:
TABLE 2 delayed coking Process Main parameters
The activation process parameters for each batch in the examples are shown in table 3:
TABLE 3 activation Process parameters
The parameters of each batch of carbonization process in the examples are shown in Table 4:
TABLE 4 carbonization Process parameters
The indexes of the negative electrode materials of the respective batches in the examples are shown in Table 5
TABLE 5 Main indices of negative electrode materials
| Batches of | D50(μm) | d002(nm) | Specific charging capacity (mAh/g) | First efficiency (%) |
| 1 | 12.25 | 3.6950 | 391 | 93.12 |
| 2 | 22.13 | 3.7476 | 396 | 85.22 |
| 3 | 23.56 | 3.6514 | 383 | 92.15 |
| 4 | 17.42 | 3.6641 | 402 | 90.37 |
| 5 | 20.53 | 3.6889 | 415 | 90.76 |
The above embodiments are only examples of the foot stand of the present invention, and are not intended to limit the present invention in other forms, and any person skilled in the art may make any simple modification, equivalent change and modification without departing from the technical spirit and concept of the present invention, and still fall within the scope of the present invention.
Claims (10)
1. A production process of a hard carbon negative electrode material is characterized in that asphalt raw materials are melted and then uniformly mixed with resin to enter a coking tower for coking, the mixture is crushed and screened after being discharged from a coking tower to enter a roller kiln for activation treatment, and then the mixture enters a high-temperature carbonization furnace for carbonization to obtain the hard carbon negative electrode material; the specific process steps comprise:
1) pretreatment of raw materials: pouring the asphalt into an asphalt melting tank for melting; pouring the resin into a resin melting tank for melting;
2) mixing materials: putting the materials in the resin melting tank and the asphalt melting tank into a material mixing tank, and heating and stirring uniformly;
3) coking: the materials in the mixing tank are thrown into a coking tower for coking;
4) a distillation column: the distillate oil which is obtained by pressurizing and coking the coking tower enters the bottom of the distillation tower and is distilled to obtain light-phase oil and heavy-phase oil;
5) crushing and screening: after coke is formed in the coking tower, the raw coke enters a crusher to be crushed, and a sieving machine is used for sieving and grading;
6) and (3) activation: the classified coke powder enters a roller kiln for activation treatment;
7) carbonizing: and (4) feeding the powder treated by the roller kiln into a high-temperature carbonization furnace for carbonization.
2. The production process of the hard carbon negative electrode material according to claim 1, wherein the melting temperature of the pitch in the step 1) is 100-200 ℃, the heating rate is 1-15 ℃/min, and the constant temperature time is 0.5-5 h.
3. The production process of the hard carbon negative electrode material according to claim 1, wherein the melting temperature of the resin in the step 1) is 50-150 ℃, the heating rate is 1-15 ℃/min, and the constant temperature time is 0.5-5 h.
4. The production process of the hard carbon negative electrode material as claimed in claim 1, wherein the temperature of the material mixing tank is 50-250 ℃, and the stirring speed is 20-50 r/min.
5. The production process of the hard carbon negative electrode material according to claim 1, wherein the pressure of the coking tower is 0.1-3 Mpa, the coking temperature is 480-600 ℃, the temperature rise rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
6. The production process of the hard carbon negative electrode material as claimed in claim 1, wherein the crushing and screening particle size D50 in the step 5) is 10-25 μm.
7. The production process of the hard carbon anode material according to claim 1, wherein the activating agent in the step 6) is water or carbon dioxide, the dosage of the activating agent is 0.5-5 mL/min, the activation temperature is 500-1200 ℃, the activation time is 0.1-10 h, and the activation process needs inert gas protection.
8. The production process of the hard carbon negative electrode material according to claim 1, wherein the carbonization temperature in the step 7) is 1000-2000 ℃, the temperature rise rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
9. The device used in the production process of the hard carbon negative electrode material according to claim 1, which comprises an asphalt melting tank, a resin melting tank, a mixing tank, a coking tower, a distillation tower, a crusher, a screening machine, a roller kiln and a high-temperature carbonization furnace, wherein the asphalt melting tank and the resin melting tank are connected with the mixing tank, the mixing tank is connected with the coking tower, a light phase extraction outlet of the coking tower is connected with the distillation tower, a coke outlet of the coking tower feeds materials to the crusher, the crusher feeds materials to the screening machine, the screening machine feeds materials to the roller kiln, and the roller kiln feeds materials to the high-temperature carbonization furnace.
10. The device used in the production process of the hard carbon negative electrode material is characterized in that the number of the coking towers is two.
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2020
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| US20020075627A1 (en) * | 2000-06-27 | 2002-06-20 | Asahi Glass Company, Limited | Activated carbon material, process for producing the same and electric double layer capacitor employing the same |
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| Title |
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