CN111217368B - Production process and device of hard carbon anode material - Google Patents

Production process and device of hard carbon anode material Download PDF

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Publication number
CN111217368B
CN111217368B CN202010095406.8A CN202010095406A CN111217368B CN 111217368 B CN111217368 B CN 111217368B CN 202010095406 A CN202010095406 A CN 202010095406A CN 111217368 B CN111217368 B CN 111217368B
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coking
asphalt
melting tank
tower
tank
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CN111217368A (en
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陈雪
和凤祥
武全宇
吕晗
张勇
刘书林
屈滨
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Sinosteel Anshan Research Institute of Thermo Energy Co Ltd
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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
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/336—Preparation characterised by gaseous activating agents
    • 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
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • 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
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Electrochemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)

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 is used for feeding the crusher, the crusher is used for feeding the screening machine, the screening machine is used for feeding the roller kiln, and the roller kiln is used for feeding the high-temperature carbonization furnace. According to the invention, asphalt raw materials are melted and then are uniformly mixed with resin for coking, after the coking is carried out, and then the hard carbon anode material with excellent electrochemical performance and stable material structure is obtained. The hard carbon cathode material prepared by the invention has the advantages of high safety performance, good multiplying power performance, high capacity, excellent cycle performance and outstanding anti-attenuation capability, and the process method is simple and feasible and continuous in production, and is an excellent raw material for multiplying power type and capacity type battery equipment.

Description

Production process and device of hard carbon anode material
Technical Field
The invention belongs to the field of negative electrode materials, and particularly relates to a production process and a production device of a hard carbon negative electrode material.
Background
With the increasing exhaustion of fossil fuels and gradual deterioration of the environment, various governments have come out of environmental protection measures and new energy development planning, and there is an urgent need for environmentally friendly renewable energy sources to replace the conventional fossil energy sources currently being used on a large scale. Therefore, the development of new energy source is an important strategic industry for preempting the future development high point in various countries. The lithium ion secondary battery is taken as a green new energy battery, the development is from the 80 th century, the lithium ion secondary battery is rapidly developed from the commercialization of Sony corporation in Japan in 1992, is an ideal chemical energy source internationally recognized 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, has been widely applied in the fields of consumer electronics, electric tools, medical electronics and the like, has been widely applied in the fields of pure electric vehicles, hybrid electric vehicles, electric bicycles, rail transit, aerospace, ships and warships, industrial energy conservation, green architecture, space technology and the like, has become a new generation of sustainable development green energy source, and particularly has been the market demand of a new energy automobile as a cathode material of a core of a power battery.
The hard carbon anode material is used as an emerging anode material, and has higher Li due to a three-dimensional crosslinking structure + The diffusion coefficient and the wider lithium intercalation potential interval are suitable for high-current charge and discharge, and the characteristics of high rate performance, high specific capacity, low cost and the like are also considered as the lithium ion battery cathode material with the most potential in the future. However, the hard carbon negative electrode materials in the current negative electrode material market are all pyrolytic carbon with a near amorphous carbon structure, and are generally>Graphitization is difficult even when the catalyst is treated at 20000 ℃, and the catalyst is generally prepared by heat treatment of organic matters (such as phenolic resin, epoxy resin, pyrolytic carbon of organic compounds, and polyglycitol PEA), and has the problems of low cycle retention rate, serious lithium precipitation in cycle composition, high price and low market utilization rate.
Disclosure of Invention
The invention provides a process and a device for producing a hard carbon negative electrode material, wherein different asphalt raw materials are subjected to coarse breaking or direct melting and then are mixed with resin in a mixing tank to be coked in a coking tower, crushed and screened after coke is discharged, and then enter a roller kiln for activation treatment, and finally enter a high-temperature carbonization furnace for carbonization, so that the hard carbon negative electrode material with excellent electrochemical performance and stable material structure is obtained. The hard carbon cathode material prepared by the invention has the advantages of high safety performance, good multiplying power performance, high capacity, excellent cycle performance and outstanding anti-attenuation capability, and the process method is simple and feasible and continuous in production, and is an excellent raw material for multiplying power type and capacity type battery equipment.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the production process of hard carbon negative electrode material includes the steps of smelting asphalt material, mixing with resin, coking in a coking tower, crushing, sieving, activating in a roller kiln, and carbonizing in a high temperature carbonizing furnace to obtain hard carbon negative electrode material; the specific process steps comprise:
1) Pretreatment of raw materials: asphalt is pumped into an asphalt melting tank for melting; resin is injected into a resin melting tank for melting;
2) Mixing: the materials in the resin melting tank and the asphalt melting tank are pumped into a mixing tank, heated and stirred uniformly;
3) Coking: the materials in the mixing tank are put into a coking tower for coking;
4) Distillation tower: the distillate oil obtained by pressurized coking of the coking tower enters the bottom of a distillation tower, and light phase oil and heavy phase oil are obtained through distillation;
5) Crushing and screening: after the coking tower is coked, raw coke enters a pulverizer for pulverization, and a sieving machine is used for sieving and grading;
6) Activating: the graded coke powder enters a roller kiln for activation treatment;
7) Carbonizing: and (5) feeding the powder processed 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 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 size D50 of the crushing and sieving particle in the step 5) is 10-25 mu m.
The activator in the step 6) is water or carbon dioxide, the dosage of the activator 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 heating rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
The utility model provides a device that hard carbon negative pole material's production technology used, includes pitch melting tank, resin melting tank, blending tank, coking tower, distillation column, breaker, screening machine, roller kiln, high temperature carbonization stove, the blending tank is connected to pitch melting tank and resin melting tank, the blending tank is connected the coking tower, the distillation column is connected to the light phase of coking tower adopts the mouth, the coke outlet 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 the roller kiln pay-off, and the roller kiln is to the high temperature carbonization stove 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 combines the excellent cycle performance of the soft carbon negative electrode material with the higher rate performance of the hard carbon negative electrode material through a unique production process, charges and discharges under the condition of high power density, has stable material structure and outstanding attenuation resistance, and can be widely applied to the field of various large battery materials;
2) The negative electrode material prepared by the invention has excellent electrochemical performance, and can be widely applied to quick-charging battery equipment, lithium ion battery equipment 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 productivity is ensured, and the economic benefit is considerable;
4) The distillation tower adopted by the invention recovers distilled distillate oil, distilled light phase oil is sold, and heavy phase oil can be recovered to be used as a special asphalt raw material.
5) The activation process adopted by the activation process is easy to realize, and the activated raw materials have 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-a soft asphalt raw material; 2-a hard asphalt raw material; 3-resin raw material; 4-asphalt pulverizer; 5-bucket elevator; 6, a storage bin; 7-a screw feeder; 8-an asphalt melting tank; 9-a resin melting tank; 10-a mixing tank; 11-1# coking tower; a 12-2# coking tower; 13-a crusher; 14-sieving machine; 15-roller kiln; 16-a high-temperature carbonization furnace; 17-a finished product bin; 18-distillation column.
Detailed Description
Embodiments of the invention are further described below in conjunction with specific examples:
as shown in figure 1, in the production process of the hard carbon cathode material, different asphalt raw materials are mixed with resin in a mixing tank 10 after coarse breaking or direct melting, and then the mixture is coked in a coking tower, crushed and screened into a roller kiln 15 after coke discharging, activated, and then carbonized in a high-temperature carbonization furnace 16 to obtain the hard carbon cathode material, wherein the specific capacity of the hard carbon cathode material is greater than 380mAh/g, and the first efficiency is greater than 80%, and the specific process comprises the following steps:
1) Pretreatment of raw materials: the soft asphalt is pumped out from a raw material tank through a pump and directly enters 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 a screw feeder 7 drives the hard asphalt into an asphalt melting tank 8 for melting; pumping resin into a resin melting tank 9 for melting; asphalt powder with coarse breaking granularity of less than 1cm is used for hard asphalt;
2) Mixing: resin melting tank 9 and asphalt melting tank 8 are mixed according to the mass ratio: asphalt=1:8-9 is pumped into a mixing tank 10, heated and stirred uniformly;
3) Coking: pumping the materials in the mixing tank 10 into a coking tower through a pump for coking;
4) Distillation tower: the distillate oil from the coking tower pressurization coking enters the bottom of a distillation tower 18, and light phase oil and heavy phase oil are obtained through distillation; the light phase oil is sold; and the heavy phase oil part is driven into a raw material tank area to be used as a special asphalt raw material.
5) Crushing and screening: after the coking tower is coked, raw coke enters a pulverizer for pulverization, and a sieving machine is used for sieving and grading;
6) Activating: the classified coke powder enters a roller kiln 15 for activation treatment;
7) Carbonizing: the powder processed by the roller kiln 15 enters a high-temperature carbonization furnace 16 for carbonization;
8) And (3) a finished product: and (5) enabling the carbonized material to enter a finished product bin through a belt corridor 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 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 size D50 of the crushing and sieving particle in the step 5) is 10-25 mu m.
The activator in the step 6) is water or carbon dioxide, the dosage of the activator 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 heating rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
The utility model provides a device that hard carbon negative pole material's production technology used, includes pitch melting tank 8, resin melting tank 9, compounding jar 10, coking tower, distillation column 18, breaker 13, screening machine 14, roller kiln 15, high temperature retort 16, pitch melting tank 8 and resin melting tank 9 connect compounding jar 10, the coking tower is connected to compounding jar 10, the light phase of coking tower is adopted the export and is connected distillation column 18, the export of coking tower is to breaker 13 pay-off, and breaker 13 is to screening machine 14 pay-off, and screening machine 14 is to roller kiln 15 pay-off, and roller kiln 15 is to high temperature retort 16 pay-off.
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 for melting, and the hard asphalt raw material 2 is lifted into a storage bin 5 through a hopper after being coarsely broken 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 a heater and a stirrer.
The number of the coking towers is two, namely a No. 1 coking tower 11 and a No. 2 coking tower 12; coking and coke discharging are used alternately, so that continuous production is realized.
Examples:
by adopting the production process of the hard carbon anode material, 5 batches of main indexes are recorded in table 1;
table 1 raw materials and main index for each batch
Batch of Raw asphalt Softening point (. Degree. C.) QI(wt％) Ash (wt%)
1 Coal series soft asphalt 31 2.50 0.08
2 Coal-based 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 pitch: petroleum asphalt=1:1 mix 36 1.68 0.10
The process parameters of the coking tower in the examples are shown in Table 2:
TABLE 2 Main parameters of delayed coking Process
The activation process parameters for each batch in the examples are shown in Table 3:
TABLE 3 activation process parameters
The carbonization process parameters of each batch in the examples are shown in Table 4:
TABLE 4 carbonization process parameters
The index of the anode material of each batch in the examples is shown in Table 5
TABLE 5 Main index of negative electrode materials
Batch of D50(μm) d 002 (nm) Specific charge capacity (mAh/g) First time 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 implemented on the premise of the technical solution of the present invention, but are merely embodiments of the stand of the present invention, not limited to other forms of the present invention, and any simple modification, equivalent transformation and variation made by those skilled in the art without departing from the technical solution of the present invention according to the technical spirit and concept of the present invention still fall within the protection scope of the present invention.

Claims (6)

1. A process for producing a hard carbon cathode material is characterized in that asphalt raw materials are melted and then are uniformly mixed with resin, the mixture is coked in a coking tower, crushed and screened into a roller kiln after being discharged, activated, and then the activated product is carbonized in a high-temperature carbonization furnace to obtain the hard carbon cathode material; the specific process steps comprise:
1) Pretreatment of raw materials: asphalt is pumped into an asphalt melting tank for melting; resin is injected into a resin melting tank for melting;
2) Mixing: the materials in the resin melting tank and the asphalt melting tank are pumped into a mixing tank, heated and stirred uniformly;
3) Coking: the materials in the mixing tank are put into a coking tower for coking;
4) Distillation tower: the distillate oil obtained by pressurized coking of the coking tower enters the bottom of a distillation tower, and light phase oil and heavy phase oil are obtained through distillation;
5) Crushing and screening: after the coking tower is coked, raw coke enters a pulverizer for pulverization, and a sieving machine is used for sieving and grading;
6) Activating: the graded coke powder enters a roller kiln for activation treatment;
the crushing and sieving granularity D50 in the step 5) is 10-25 mu m;
the activator is water or carbon dioxide, the dosage of the activator 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;
7) Carbonizing: feeding the powder processed by the roller kiln into a high-temperature carbonization furnace for carbonization;
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 carbonization temperature in the step 7) is 1000-2000 ℃, the heating rate is 1-30 ℃/min, and the constant temperature time is 1-8 h.
2. The process for producing a 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 process for producing a hard carbon negative electrode material according to claim 1, wherein the resin in the step 1) has a melting temperature of 50 to 150 ℃, a heating rate of 1 to 15 ℃/min, and a constant temperature time of 0.5 to 5 hours.
4. The process for producing the hard carbon anode material according to claim 1, wherein the temperature of the mixing tank is 50-250 ℃ and the stirring speed is 20-50 r/min.
5. The device for the production process of the hard carbon anode 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 port of the coking tower is connected with the distillation tower, a coke outlet of the coking tower feeds the crusher, the crusher feeds the screening machine, the screening machine feeds the roller kiln, and the roller kiln feeds the high-temperature carbonization furnace;
the bucket elevator is connected with a feed bin, and the feed bin feeds hard asphalt raw materials to the asphalt melting tank through a screw feeder; the soft asphalt raw material directly enters an asphalt melting tank for melting, and the hard asphalt raw material enters a storage bin through a bucket elevator after being coarsely broken and then enters the asphalt melting tank through a screw feeder; the asphalt melting tank and the resin melting tank are provided with a heater and a stirrer.
6. The apparatus for use in a process for producing a hard carbon negative electrode material according to claim 5, wherein the number of the coking towers is two.
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