CN109020546A - Utilize the method for discarded carbon raw preparation high strength carbon cellulosic material - Google Patents
Utilize the method for discarded carbon raw preparation high strength carbon cellulosic material Download PDFInfo
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- CN109020546A CN109020546A CN201811084134.0A CN201811084134A CN109020546A CN 109020546 A CN109020546 A CN 109020546A CN 201811084134 A CN201811084134 A CN 201811084134A CN 109020546 A CN109020546 A CN 109020546A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The present invention relates to carbon materials preparation fields, a kind of more particularly to method using discarded carbon raw preparation high strength carbon cellulosic material, include the following steps, the fine powder assembled on scraping pitch coke milling deduster, collect lithium cell cathode material micro mist, choose carbon fiber, fine powder successively successively is added into kneading pot, micro mist and carbon fiber, start kneading pot kneading, shut down kneading pot, into kneading pot, watering is wet to material in kneading pot, it opens kneading pot kneading and heats, binder is added into kneading pot, heating, kneading, obtain thickener, by thickener by 4 rollings, obtain roller sheet, it is D50 5-8um that roller sheet, which is milled to partial size, obtain two wheat-middlings, two wheat-middlings are passed through into 150-180Mpa isostatic pressing, obtain green compact, heating curve is set, green compact are roasted, then graphite is carried out Change, obtain finished product high strength carbon cellulosic material, can effectively utilize resource, carbon product performance obtained high.
Description
Technical field
The present invention relates to carbon materials preparation fields more particularly to a kind of utilize to discard the high-intensitive carbon of carbon raw preparation
The method of material.
Background technique
It is milled in pitch coke process, flour mill is connected with deduster, carries out during milling
Dedusting, the fine powder being enriched on deduster need timing to clear up, this material shows most company and all disposes at a low price, and existing market is big
General price causes to waste at 1500 yuan/ton or so.
Lithium cell cathode material requirement is very stringent, and negative electrode material generally uses petroleum coke, needle coke, mesocarbon micro-
Ball, these belong to low ash low-sulfur material, and require graphitization also very high.Negative electrode material is by milling, cladding, graphite
The processes such as change, screening.It is divided into three kinds of granularities in screening process: as certain producer needs to be greater than partial size of 200 mesh less than 300 mesh.Stone
Inkization negative electrode material is greater than 200 target materials in screening process can also be milled uses again, less than 200 mesh greater than 300 purposes
Material, is exactly the product of lithium cell cathode material, belongs to micro mist less than 200 target materials, because granularity is too thin, cannot make lithium
Cell negative electrode material, micro mist would generally be sold to the producer for making carburant at a low price, 1800 yuan/ton of current market price or so, cause wave
Take.
Summary of the invention
It is an object of the invention to overcome deficiency in the prior art, resource can effectively be utilized, be made by providing one kind
Carbon product performance it is high utilization discard carbon raw preparation high strength carbon cellulosic material method.
The present invention is achieved by the following technical solutions: a kind of to prepare high strength carbon cellulosic material using discarded carbon raw
Method, which comprises the following steps:
Step 1 scrapes the fine powder assembled on pitch coke milling deduster, collects lithium cell cathode material micro mist, chooses carbon fiber
Dimension；
Fine powder, micro mist and carbon fiber that step 1 obtains successively successively are added into kneading pot, starts kneading pot kneading for step 2
8-10min shuts down kneading pot, and into kneading pot, watering is wet to material in kneading pot, opens kneading pot kneading 80-100min simultaneously
It is heated to 130-140 DEG C；
Step 3, into step 2 heat after kneading pot in binder is added, be warming up to 160-170 DEG C, kneading 40-45min,
Obtain thickener；
Step 4 obtains roller sheet by thickener by 4 rollings；
Step 5, it is D50 5-8um that roller sheet, which is milled to partial size, obtains two wheat-middlings；
Two wheat-middlings are passed through 150-180Mpa isostatic pressing, obtain green compact by step 6；
Heating curve is arranged in step 7, and the heating upper limit is 900 DEG C, roasts to green compact, is then graphitized, is obtained into
Product high strength carbon cellulosic material,
Fine powder, micro mist, the weight ratio between three kinds of materials of binder are 68:15:17, please illustrate carbon fiber and fine powder, micro mist, viscous
Knot three kinds of materials of agent the ratio between total weight be.
Further, the partial size of fine powder is D10 0.98um, D50 5.52um, D90 15.68um in step 1, and fine powder contains
Ash content is not higher than 0.30wt% not higher than 0.35wt%, sulfur-bearing, and the partial size of micro mist is D10 0.98um, D50 5.52um, D90
15.68um, micro mist are not higher than 0.22 wt % not higher than 0.1 wt %, sulfur-bearing containing ash content, and carbon fiber phosphorus content is higher than 95wt%.
Further, the binder is that high temperature restructures pitch.
Further, the thickness of 4 rollings is followed successively by 3-3.2mm, 1.8-2mm, 1mm, 0.8mm in step 4, wherein rolling
The temperature of roller processed is 120-130 DEG C.
Further, the roasting in step 7 the following steps are included:
Green compact are spaced apart in steel box body by A, and the spacing between two neighboring green compact is 2-6mm；
Steel box body is placed in roaster by B, and setting heating curve is roasted.
Further, heating curve includes with the next stage:
Temperature is uniformly heating to 300 DEG C by room temperature by the first stage；
Temperature is uniformly heating to 650 DEG C by 300 DEG C by second stage；
Temperature is uniformly heating to 900 DEG C by 650 DEG C by the phase III.
The beneficial effects of the present invention are: pitch coke fine powder, negative electrode material micro mist market are easy buying and cheap, use
When production, the minimum raw material of partial size can be directly obtained, effectively reduces production cost, improves production efficiency, pitch coke
Fine powder, negative electrode material micro mist all belong to low ash low-sulfur, and raw material index is stablized.More importantly the partial size of two kinds of materials extremely connects
Closely, and the exclusive advantage for doing hyperfine structure product has been reached, pitch coke is not easy to be graphitized, with the negative electrode material of high graphitization degree
To make up the defect, high yield rate.
Specific embodiment
Pitch coke fine powder is the pitch coke of milling table mountain east carbon limited liability company production in following embodiment
The fine powder collected in the process, fine powder laboratory indexes, ash content 0.33wt%, 0.35 wt % of fugitive constituent, 0.30 wt % of sulphur, partial size
For D10 0.98um, D50 5.52um, D90 15.68um；Lithium cell cathode material micro mist selects the prosperous power material of China of Xinxiang City
Co., Ltd produces the micro mist that negative electrode material is rejected, micro mist laboratory indexes, 0.1 wt % of ash content, 0.18 wt % of fugitive constituent, sulphur
0.22 wt %, 80 Ω m of powder resistivity, partial size are D10 0.98um, D50 5.52um, D90 15.68um；Carbon fiber is carbon containing
Amount is higher than 95wt%；High temperature modified pitch is selected in agent, specially selects the high temperature modified drip of Nanjing Mei Shan chemical general factory Co., Ltd
Blueness, this high temperature modified asphalt coking value is 58-60%, softening is 110 DEG C, content of ashes 0.2wt%；4 times rolling thickness according to
Secondary is 3-3.2mm, 1.8-2mm, 1mm, 0.8mm, and wherein the temperature of Rolling roller is 120-130 DEG C, can increase the intensity of tablet,
Density is improved, the stomata in thickener is thoroughly discharged, roasts the following steps are included: A, green compact are spaced apart in steel box body
Interior, the spacing between two neighboring green compact is 2-6mm, B, and steel box body is placed in roaster, and setting heating curve carries out
Roasting；Heating curve includes with the next stage: the first stage, by 120min, temperature is uniformly heating to 300 DEG C by room temperature, energy
Enough to soften green compact, temperature is uniformly heating to 650 DEG C by 300 DEG C, can made in green compact by second stage using 150min
Volatile component volatilization, temperature is uniformly heating to 900 DEG C by 650 DEG C, passes through roasting by the phase III using 120min
Product yield rate be can be improved to 92%, the total duration of heating curve is 620h, fine powder, micro mist, between three kinds of materials of binder
Weight ratio is 68:15:17, fine powder, micro mist, the total weight of three kinds of materials of binder and carbon fiber weight ratio be 100:3.
In following embodiment, in step 2, the mode of watering is to be sprinkled water by shower into kneading pot, and watering amount is
0.8-1kg causes in kneading pot without obvious suspended particulate.
In following embodiment, in step 7, the roasting heat source temperature upper limit is 1150-1160 DEG C, and then makes green compact itself
Temperature can reach 900 DEG C, save its shrinkage, while can retain macromolecular ash content, graphitization temperature 2900-3000
℃。
Embodiment 1
A method of high strength carbon cellulosic material is prepared using discarded carbon raw, comprising the following steps:
Step 1 scrapes the fine powder assembled on pitch coke milling deduster, collects lithium cell cathode material micro mist, chooses carbon fiber
Dimension；
Fine powder, micro mist and carbon fiber that step 1 obtains successively successively are added into kneading pot, starts kneading pot kneading for step 2
8min shuts down kneading pot, and into kneading pot, watering is wet to material in kneading pot, opens kneading pot kneading 80min and is heated to
130 DEG C, wherein fine powder 68kg, micro mist 15kg, carbon fiber 3kg；
Step 3, into step 2 heat after kneading pot in be added binder 17kg, be warming up to 160 DEG C, kneading 40min is obtained
To thickener；
Step 4 obtains roller sheet by thickener by 4 rollings；
Step 5, it is D50 5um that roller sheet, which is milled to partial size, obtains two wheat-middlings；
Two wheat-middlings are passed through 160Mpa isostatic pressing, obtain green compact by step 6；
Heating curve is arranged in step 7, and the heating upper limit is 900 DEG C, roasts to green compact, is then graphitized, is obtained into
Product high strength carbon cellulosic material.
The finished product high strength carbon cellulosic material that the present embodiment obtains, testing result see attached list 1.
Embodiment 2
A method of high strength carbon cellulosic material is prepared using discarded carbon raw, comprising the following steps:
Step 1 scrapes the fine powder assembled on pitch coke milling deduster, collects lithium cell cathode material micro mist, chooses carbon fiber
Dimension；
Fine powder, micro mist and carbon fiber that step 1 obtains successively successively are added into kneading pot, starts kneading pot kneading for step 2
10min shuts down kneading pot, and into kneading pot, watering is wet to material in kneading pot, opens kneading pot kneading 100min and heats
To 125 DEG C, wherein fine powder 68kg, micro mist 15kg, carbon fiber 3kg；
Step 3, into step 2 heat after kneading pot in be added binder 17kg, be warming up to 170 DEG C, kneading 40min is obtained
To thickener；
Step 4 obtains roller sheet by thickener by 4 rollings；
Step 5, it is D50 8um that roller sheet, which is milled to partial size, obtains two wheat-middlings；
Two wheat-middlings are passed through 180Mpa isostatic pressing, obtain green compact by step 6；
Heating curve is arranged in step 7, and the heating upper limit is 900 DEG C, roasts to green compact, is then graphitized, is obtained into
Product high strength carbon cellulosic material.
The finished product high strength carbon cellulosic material that the present embodiment obtains, testing result see attached list 1.
Embodiment 3
A method of high strength carbon cellulosic material is prepared using discarded carbon raw, comprising the following steps:
Step 1 scrapes the fine powder assembled on pitch coke milling deduster, collects lithium cell cathode material micro mist, chooses carbon fiber
Dimension；
Fine powder, micro mist and carbon fiber that step 1 obtains successively successively are added into kneading pot, starts kneading pot kneading for step 2
10min shuts down kneading pot, and into kneading pot, watering is wet to material in kneading pot, opens kneading pot kneading 100min and heats
To 128 DEG C, wherein fine powder 68kg, micro mist 15kg, carbon fiber 3kg；
Step 3, into step 2 heat after kneading pot in be added binder 17kg, be warming up to 165 DEG C, kneading 40min is obtained
To thickener；
Step 4 obtains roller sheet by thickener by 4 rollings；
Step 5, it is D50 6um that roller sheet, which is milled to partial size, obtains two wheat-middlings；
Two wheat-middlings are passed through 150Mpa isostatic pressing, obtain green compact by step 6；
Heating curve is arranged in step 7, and the heating upper limit is 900 DEG C, roasts to green compact, is then graphitized, is obtained into
Product high strength carbon cellulosic material.
The finished product high strength carbon cellulosic material that the present embodiment obtains, testing result see attached list 1.
Subordinate list 1
Since in the present invention, fine powder and micro mist are the small powders of granularity, and are the raw materials by coking, carbon material is being prepared
During material, the process of multiple coking is eliminated, can will be reduced to the production cycle 4 months, and can be good at waste material
Recycling, fine powder structure distribution epigranular integrally see that particle mutually binds securely in particle, along with incorporation carbon fiber and cathode
Micro mist, the defect for overcoming different materials realize complementation, produce ultra-fine high intensity using the carbon dust of low value to reach
Product, filled up the blank of domestic carbon industry, high strength carbon cellulosic material real density obtained is small, compression strength and anti-folding are strong
Degree is high, hardness is big, is suitable for electric spark industry and high-precision end field.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (6)
1. a kind of method using discarded carbon raw preparation high strength carbon cellulosic material, which comprises the following steps:
Step 1 scrapes the fine powder assembled on pitch coke milling deduster, collects lithium cell cathode material micro mist, chooses carbon fiber
Dimension；
Fine powder, micro mist and carbon fiber that step 1 obtains successively successively are added into kneading pot, starts kneading pot kneading for step 2
8-10min shuts down kneading pot, and into kneading pot, watering is wet to material in kneading pot, opens kneading pot kneading 80-100min simultaneously
It is heated to 130-140 DEG C；
Step 3, into step 2 heat after kneading pot in binder is added, be warming up to 160-170 DEG C, kneading 40-45min,
Obtain thickener；
Step 4 obtains roller sheet by thickener by 4 rollings；
Step 5, it is D50 5-8um that roller sheet, which is milled to partial size, obtains two wheat-middlings；
Two wheat-middlings are passed through 150-180Mpa isostatic pressing, obtain green compact by step 6；
Heating curve is arranged in step 7, and the heating upper limit is 900 DEG C, roasts to green compact, is then graphitized, is obtained into
Product high strength carbon cellulosic material,
Fine powder, micro mist, the weight ratio between three kinds of materials of binder be 68:15:17, three kinds of fine powder, micro mist, binder materials
The weight ratio of total weight and carbon fiber is 100:3.
2. the method according to claim 1 using discarded carbon raw preparation high strength carbon cellulosic material, which is characterized in that
The partial size of fine powder is D10 0.98um, D50 5.52um, D90 15.68um in step 1, and fine powder is not higher than containing ash content
0.35wt%, sulfur-bearing are not higher than 0.30wt%, and the partial size of micro mist is D10 0.98um, D50 5.52um, D90 15.68um, micro mist
It is not higher than 0.22 wt % not higher than 0.1 wt %, sulfur-bearing containing ash content, carbon fiber phosphorus content is higher than 95wt%.
3. the method according to claim 1 using discarded carbon raw preparation high strength carbon cellulosic material, which is characterized in that
The binder is that high temperature restructures pitch.
4. the method according to claim 1 using discarded carbon raw preparation high strength carbon cellulosic material, which is characterized in that
The thickness of 4 rollings is followed successively by 3-3.2mm, 1.8-2mm, 1mm, 0.8mm in step 4, and wherein the temperature of Rolling roller is 120-
130℃。
5. the method according to claim 1 using discarded carbon raw preparation high strength carbon cellulosic material, which is characterized in that
Roasting in step 7 the following steps are included:
Green compact are spaced apart in steel box body by A, and the spacing between two neighboring green compact is 2-6mm；
Steel box body is placed in roaster by B, and setting heating curve is roasted.
6. the method according to claim 5 using discarded carbon raw preparation high strength carbon cellulosic material, which is characterized in that
Heating curve includes with the next stage:
Temperature is uniformly heating to 300 DEG C by room temperature by the first stage；
Temperature is uniformly heating to 650 DEG C by 300 DEG C by second stage；
Temperature is uniformly heating to 900 DEG C by 650 DEG C by the phase III.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110642248A (en) * | 2019-11-19 | 2020-01-03 | 平顶山市天宝特种材料有限公司 | Production method of fine-structure high-purity graphite with changed molecular arrangement combination |
| CN113880070A (en) * | 2021-11-05 | 2022-01-04 | 平顶山东方碳素股份有限公司 | Production method and production equipment for preparing high-strength carbon material |
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| CN105668553A (en) * | 2015-12-31 | 2016-06-15 | 平顶山东方碳素股份有限公司 | Process of preparing high-strength carbon material from waste materials |
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| CN110642248A (en) * | 2019-11-19 | 2020-01-03 | 平顶山市天宝特种材料有限公司 | Production method of fine-structure high-purity graphite with changed molecular arrangement combination |
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Application publication date: 20181218 |