CN110590391B - Drainage plate of graphitization furnace and manufacturing method thereof - Google Patents
Drainage plate of graphitization furnace and manufacturing method thereof Download PDFInfo
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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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
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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
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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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
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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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
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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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
- C04B2235/658—Atmosphere during thermal treatment
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- 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
Abstract
The invention discloses a drainage plate of a graphitization furnace and a manufacturing method thereof, the drainage plate of the graphitization furnace is formed by compounding a PAN-based fiber carbon felt and modified metallurgical coke through a binder which is not easy to graphitize, firstly, the modified metallurgical coke and thermoplastic resin are mixed and heated to form hot slurry, then the PAN-based fiber carbon felt is soaked in the hot slurry, and then the drainage plate is manufactured through mould pressing and heat treatment. The drainage plate of the graphitization furnace manufactured by the invention has the advantages of high heating efficiency and long service life.
Description
Technical Field
The invention relates to a production device of an electrode material of a lithium ion battery, in particular to a drainage plate for a graphitization furnace and a manufacturing method thereof.
Background
With the increasing performance requirements of people on carbon products, more and more industries need to adopt carbon powder graphitization technology. The heating means of the carbon powder graphitization technology adopted at present is mainly to place carbon powder into a graphite crucible, and the graphite crucible is inhibited or directly heated as a heating body by a resistor material at the periphery of the graphite crucible. Therefore, this carbon powder graphitization technology relying on a graphite crucible has problems of high energy consumption, low productivity and high loss.
In order to solve the problems, patent No. CN201510562328.7 proposes a concept of enclosing graphite plates for a graphitization furnace into a box body, and then installing a strip-shaped heating core therein, wherein carbon powder can be directly put into the box body in the graphitization process, and heat is generated by the strip-shaped heating core. This patent mainly teaches the design and method of use of the graphitization furnace, and the heating core used has not been studied.
The invention provides a drainage plate suitable for a box-type graphitizing furnace, which is used as a heating body of the graphitizing furnace and has the characteristics of high heating efficiency and long service life.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a novel drainage plate for a graphitization furnace and a manufacturing method thereof.
The invention is realized by the following technical scheme:
the preparation method of the drainage plate of the graphitization furnace is characterized by comprising the following steps:
a1, mixing the modified metallurgical coke with thermoplastic resin, and heating to 200-500 ℃ under an inert atmosphere to obtain hot slurry;
a2, heating the mould, injecting hot slurry into the mould, adding the PAN-based fiber carbon felt, soaking the PAN-based fiber carbon felt in the hot slurry, isolating the mould, vacuumizing and standing;
a3, cooling the mold, then carrying out mold pressing on the material in the mold, further cooling to room temperature, and removing the mold to obtain a drainage plate precursor;
a4, heating the drainage plate precursor to 900-1300 ℃ in an inert atmosphere, and naturally cooling to obtain the drainage plate.
Preferably, the preparation method of the drainage plate of the graphitization furnace is characterized by comprising the following steps:
a1, mixing the modified metallurgical coke with a thermoplastic resin according to the weight ratio of 2: 1, and then heating to 200-500 ℃ in an inert atmosphere to obtain a hot slurry;
a2, heating a mould to 300 ℃, injecting 25% of hot slurry, then adding a PAN-based fiber carbon felt, soaking for 10min, injecting the remaining 75% of hot slurry into the mould for three times, wherein the injection amount of each time is 25% of the total amount of the hot slurry, the interval time of each time is 10min, and after the hot slurry is completely injected, isolating the mould and vacuumizing and standing for 2 h;
a3, naturally cooling the mold to 100 ℃, carrying out mold pressing on materials in the mold under 150Mpa, then further cooling to room temperature, and removing the mold to obtain a drainage plate precursor;
a4, heating the drainage plate precursor to 900-1300 ℃ at a heating rate of 0.5 ℃/min under an inert atmosphere, preserving heat for 50min, and naturally cooling to obtain the drainage plate.
Further, in the step A1, the mass ratio of the modified metallurgical coke to the thermoplastic resin is (1-3): 1;
further, in the step A1, the modified metallurgical coke is a product of commercial metallurgical coke after crushing and acid washing treatment, the ash content is less than or equal to 1 percent, and D5018 to 21 μm, D100Less than or equal to 90 mu m. The thermoplastic resin is one of polyethylene, polybutadiene and polystyrene.
Further, in the step A2, the mold is heated to 260-350 ℃, 25% of the total amount of the hot slurry is injected into the mold, then the PAN-based fiber carbon felt is added, the PAN-based fiber carbon felt is soaked in the hot slurry for 5-30 min, then the remaining 75% of the hot slurry is injected into the mold for three times, the injection amount is 25% of the total amount of the hot slurry each time, the interval time is 5-15 min each time, and after the hot slurry is completely injected, the mold is isolated and vacuumized and kept stand for 1-3 h.
Further, in the step A2, the PAN-based fiber carbon felt is commercially available, and the areal density is 500-1000 g/m2The electrical resistivity is 4-9 omega.mm, the thermal conductivity is 0.06W/(m.K), and the ash content is less than or equal to 0.3%.
Further, in the step a2, the mass ratio of the PAN-based fiber carbon felt to the total amount of the hot slurry is 1: (2-6).
Further, in the step A3, cooling the mold to 80-150 ℃, carrying out mold pressing on materials in the mold under 100-200 Mpa, then further cooling to room temperature, and removing the mold to obtain the drainage plate precursor.
Further, in the step A4, heating the drainage plate precursor to 900-1300 ℃ at a heating rate of 0.3-0.8 ℃/min under an inert atmosphere, preserving the temperature for 30-70 min, and naturally cooling to obtain the drainage plate.
Further, the inert atmosphere is argon, nitrogen or gas which does not react with the drainage plate precursor at high temperature.
The utility model provides a graphitizing furnace drainage plate which characterized in that: the drainage plate of the graphitization furnace is formed by compounding a PAN-based fiber carbon felt and modified metallurgical coke.
The utility model provides a graphitizing furnace drainage plate which characterized in that: the graphitizing furnace drainage plate is prepared according to the manufacturing method.
Compared with the prior art, the invention has the following beneficial effects:
the invention firstly provides a drainage plate which is prepared by using PAN-based fiber carbon felt as a framework, compounding the carbon felt and modified metallurgical coke together through a binder which is not easy to graphitize, and finally performing mould pressing and heat treatment.
The PAN-based fiber carbon felt has strong flexibility and high temperature resistance, so that the drainage plate can be ensured to have long service life; generally speaking, the service life of the carbonaceous drainage plate is less than or equal to 5 times, the service life of the graphite drainage plate is 8-10 times, the service life of the drainage plate manufactured by the method is 15-20 times, and the drainage plate can work for 300-400 days at high temperature according to the time of 20 days for each use.
Modified metallurgical coke, the PAN-based fiber carbon felt and the used adhesive in the drainage plate are not easy to graphitize, so that the resistance of the drainage plate is not obviously reduced at high temperature, and the heating effect of the drainage plate is ensured. Generally speaking, the electrothermal efficiency of the graphite drainage plate is 20-30%, while the electrothermal efficiency of the carbonaceous drainage plate can reach 40%, and the electrothermal efficiency of the drainage plate related by the invention is 45-55%.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
2000g of modified metallurgical coke and 1000g of polyethylene are mixed uniformly and heated to 220 ℃ to prepare hot slurry. The modified metallurgical coke is a product obtained by crushing and pickling commercial metallurgical coke, the ash content is less than or equal to 1 percent, and D5018 to 21 μm, D100Less than or equal to 90 mu m. Preferably, the upgraded metallurgical coke ash used is 0.21%, D50=19.6μm，D100=70.3μm。
At 300mm by 500mm die750g of hot slurry was injected into the mold, followed by 1000g of PAN based fiber carbon felt. The PAN-based fiber carbon felt is commercially available and has the surface density of 500-1000 g/m2The electrical resistivity is 4-9 omega.mm, the thermal conductivity is 0.06W/(m.K), and the ash content is less than or equal to 0.3%. And (3) soaking the PAN-based fiber carbon felt in the hot slurry for 10min, injecting the rest hot slurry into the mold for three times, wherein the injection amount is 750g each time, the interval time is 10min, and after the hot slurry is completely injected, isolating the mold and vacuumizing and standing for 2 h.
And naturally cooling the mold to 100 ℃, carrying out mold pressing on the materials in the mold under 150Mpa, further cooling to room temperature, and removing the mold to obtain the drainage plate precursor.
And under the nitrogen atmosphere, heating the drainage plate precursor to 900 ℃ at the heating rate of 0.5 ℃/min, preserving the heat for 50min, and naturally cooling to obtain the No. 1 drainage plate.
Example 2
2353g of modified metallurgical coke and 1176g of polystyrene are uniformly mixed and heated to 400 ℃ to prepare hot slurry. The modified metallurgical coke is a product obtained by crushing and pickling commercial metallurgical coke, the ash content is 0.21 percent, and D is50=19.6μm，D100=70.3μm。
950g of the hot slurry was poured into a 300mm by 500mm mold, and 2000g of PAN-based fiber carbon felt was added thereto, the PAN-based fiber carbon felt having a surface density of 1000g/m2And a resistivity of 5. omega. mm. And soaking the PAN-based fiber carbon felt in the hot slurry for 10min, injecting the rest hot slurry into the mold for three times, wherein the injection amount is 950g each time, the interval time is 10min, and after the hot slurry is completely injected, isolating the mold and vacuumizing and standing for 2 h. And naturally cooling the mold to 100 ℃, carrying out mold pressing on the materials in the mold under 150Mpa, further cooling to room temperature, and removing the mold to obtain the drainage plate precursor.
And under the argon atmosphere, heating the drainage plate precursor to 1300 ℃ at the heating rate of 0.5 ℃/min, preserving the heat for 50min, and naturally cooling to obtain the 2# drainage plate.
Example 3
3000g of modified metallurgical coke and 1000g of polystyrene are mixed uniformly and heated to 500 ℃ to prepare the hot slurry. The modified metallurgical coke is commercially available metallurgyThe product of the coke after crushing and acid washing treatment has 0.21 percent of ash content and D50=19.6μm，D100=70.3μm。
Injecting 1000g of hot slurry into a mold with the thickness of 300mm x 500mm, and then adding 800g of PAN-based fiber carbon felt, wherein the surface density of the PAN-based fiber carbon felt is 1000g/m2And a resistivity of 5. omega. mm. And (3) soaking the PAN-based fiber carbon felt in the hot slurry for 30min, injecting the rest hot slurry into the mold for three times, wherein the injection amount is 1000g each time, the interval time is 15min, and after the hot slurry is completely injected, isolating the mold and vacuumizing and standing for 3 h. And cooling the mold to 80-150 ℃, carrying out mold pressing on the materials in the mold under 100-200 Mpa, further cooling to room temperature, and removing the mold to obtain the drainage plate precursor.
And heating the drainage plate precursor to 900-1300 ℃ at a heating rate of 0.3-0.8 ℃/min under an inert atmosphere, preserving the heat for 30-70 min, and cooling to obtain the 3# drainage plate.
Comparative example 1
Mixing natural graphite with a binder according to the weight ratio of 2: 1, placing the mixture into a 300 mm-500 mm mold, performing mold pressing on the material in the mold at 150Mpa, and performing heat treatment (the heat treatment system is the same as that of example 1) to obtain the graphite flow guide plate of the comparative example. Wherein the natural graphite has an ash content of 0.01% and D50=17.6μm，D100=50.1 μm. The adhesive is coal-series impregnated asphalt with a softening point of 120 ℃.
Comparative example 2
Mixing carbon powder and adhesive according to the ratio of 2: 1, and placing the mixture into a 300 mm-500 mm mold, and performing mold pressing on the material in the mold under 150MPa, and then performing heat treatment (the heat treatment system is the same as that of example 1) to obtain the carbon drainage plate of the comparative example. Wherein the carbon powder is calcined coke of petroleum coke, ash content is 0.01 percent, and D is50=19.5μm，D100=65.4 μm. The adhesive is coal-series impregnated asphalt with a softening point of 120 ℃.
The test is carried out on the No. 1 drainage plate, the No. 2 drainage plate, the No. 3 drainage plate, the graphite drainage plate and the carbonaceous drainage plate, and the performance data are shown in the following table:
Claims (9)
1. The preparation method of the drainage plate of the graphitization furnace is characterized by comprising the following steps:
a1, mixing the modified metallurgical coke with thermoplastic resin, and heating to 200-500 ℃ under an inert atmosphere to obtain hot slurry; wherein the modified metallurgical coke is a product obtained by crushing and acid-washing commercial metallurgical coke, the ash content is less than or equal to 1 percent, and D is5018 to 21 μm, D100≤90μm；
A2, heating the mould, injecting hot slurry into the mould, adding the PAN-based fiber carbon felt, soaking the PAN-based fiber carbon felt in the hot slurry, isolating the mould, vacuumizing and standing;
a3, cooling the mold, then carrying out mold pressing on the material in the mold, further cooling to room temperature, and removing the mold to obtain a drainage plate precursor;
a4, heating the drainage plate precursor to 900-1300 ℃ in an inert atmosphere, and naturally cooling to obtain the drainage plate.
2. The preparation method of the drainage plate of the graphitization furnace as claimed in claim 1, characterized by comprising the following steps:
a1, mixing the modified metallurgical coke with a thermoplastic resin according to the weight ratio of 2: 1, and then heating to 200-500 ℃ in an inert atmosphere to obtain a hot slurry;
a2, heating a mould to 300 ℃, injecting 25% of hot slurry, then adding a PAN-based fiber carbon felt, soaking for 10min, injecting the remaining 75% of hot slurry into the mould for three times, wherein the injection amount of each time is 25% of the total amount of the hot slurry, the interval time of each time is 10min, and after the hot slurry is completely injected, isolating the mould and vacuumizing and standing for 2 h;
a3, naturally cooling the mold to 100 ℃, carrying out mold pressing on materials in the mold under 150Mpa, then further cooling to room temperature, and removing the mold to obtain a drainage plate precursor;
a4, heating the drainage plate precursor to 900-1300 ℃ at a heating rate of 0.3-0.8 ℃/min under an inert atmosphere, preserving heat for 30-70 min, and naturally cooling to obtain the drainage plate.
3. The preparation method of the drainage plate of the graphitization furnace as claimed in claim 1, which is characterized in that: in the step A1, the mass ratio of the modified metallurgical coke to the thermoplastic resin is (1-3): 1.
4. the preparation method of the drainage plate of the graphitization furnace as claimed in claim 1, which is characterized in that: in step a1, the thermoplastic resin is one of polyethylene, polybutadiene, and polystyrene.
5. The preparation method of the drainage plate of the graphitization furnace as claimed in claim 1, which is characterized in that: in the step A2, the mould is heated to 260-350 ℃, 25% of the total amount of the hot slurry is injected into the mould, then the PAN-based fiber carbon felt is added, the PAN-based fiber carbon felt is soaked in the hot slurry, after the soaking time is 5-30 min, the remaining 75% of the hot slurry is injected into the mould for three times, the injection amount is 25% of the total amount of the hot slurry each time, the interval time is 5-15 min each time, and after the hot slurry is completely injected, the mould is isolated and vacuumized and kept stand for 1-3 h.
6. The preparation method of the drainage plate of the graphitization furnace as claimed in claim 1, which is characterized in that: in the step A2, the PAN-based fiber carbon felt is commercially available and has an areal density of 500-1000 g/m2The resistivity is 4-9 omega.mm, and the heat conductivity is 0.06W-(m.K), ash content is less than or equal to 0.3 percent.
7. The preparation method of the drainage plate of the graphitization furnace as claimed in claim 1, which is characterized in that: in the step A2, the mass ratio of the PAN-based fiber carbon felt to the total amount of the hot slurry is 1: (2-6).
8. The preparation method of the drainage plate of the graphitization furnace as claimed in claim 1, which is characterized in that: and step A3, cooling the mold to 80-150 ℃, carrying out mold pressing on the materials in the mold under 100-200 Mpa, further cooling to room temperature, and removing the mold to obtain the drainage plate precursor.
9. The utility model provides a graphitizing furnace drainage plate which characterized in that: the drainage plate of the graphitization furnace is formed by compounding a PAN-based fiber carbon felt and modified metallurgical coke; the drainage plate of the graphitization furnace is manufactured according to the preparation method of any one of claims 1-8.
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| DE102010001787A1 (en) * | 2010-02-10 | 2011-08-11 | Sgl Carbon Se, 65203 | A method of making a molded article from a carbon material using recycled carbon fibers |
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| JPH03138886A (en) * | 1989-10-24 | 1991-06-13 | Hanawa Netsuden Kinzoku Kk | Manufacture of carbon fiber/carbon composite heating element |
| CN1678546A (en) * | 2002-08-27 | 2005-10-05 | 尤卡碳工业有限公司 | Process of making carbon electrodes |
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