CN115849363A - Method for processing cathode material by using inner-string graphitization furnace - Google Patents
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- 238000005087 graphitization Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000012545 processing Methods 0.000 title claims abstract description 9
- 239000010406 cathode material Substances 0.000 title claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- 239000010426 asphalt Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000004898 kneading Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 8
- 239000010935 stainless steel Substances 0.000 claims abstract description 8
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 230000005540 biological transmission Effects 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 5
- 239000002006 petroleum coke Substances 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 4
- 239000007931 coated granule Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000011331 needle coke Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000000571 coke Substances 0.000 claims 1
- 238000007873 sieving Methods 0.000 claims 1
- 239000007773 negative electrode material Substances 0.000 abstract description 9
- 230000014759 maintenance of location Effects 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000002010 green coke Substances 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910021382 natural graphite Inorganic materials 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 229910021383 artificial graphite Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000006253 pitch coke Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Abstract
The invention relates to a method for processing a negative electrode material by using an internal-string graphitization furnace, which comprises the following steps: adding the ground raw materials and modified asphalt accounting for 10-40% of the weight of the raw materials into a kneading pot, and carrying out isostatic pressing on the kneaded powder by adopting a double-layer kneading pot to obtain a blank; sawing two end faces of the blank along the long axis direction, putting the rectangular blank into a stainless steel crucible, and putting the stainless steel crucible into a roasting furnace for graphitization; and after graphitization, cooling the negative electrode block for post treatment. The preparation method has the advantages of simple and easy process, wide raw material source and low cost. The discharge capacity, the first efficiency and the cycle life of the graphite cathode prepared by the method are all improved.
Description
Technical Field
The invention relates to the field of batteries, in particular to a method for processing a cathode material by using an inner series graphitization furnace.
Background
The graphite material is one of the main choices of the global hot lithium battery cathode materials at the present stage, wherein the artificial graphite cathode material is unique in the cathode raw material due to the advantages of stable performance, good electrical conductivity, rich raw materials and the like. For the artificial graphite cathode product, graphitization is a key technical link in the industrial production process. In recent years, the process for producing and manufacturing the artificial graphite cathode material in China is gradually developed and advanced, but the graphitization process of the raw material is still a difficulty for most production enterprises. Different processes cause high cost of graphitization, difficult technology and complicated equipment. According to the heating mode, the graphitizing equipment is divided into direct heating and indirect heating, the internal series type graphitizing furnace is a direct heating furnace, and the material to be subjected to heat treatment is taken as a heating body. The internal-series graphitizing furnace is an internal-heating type serial graphitizing furnace invented by American Cassier sodium. The main difference between the internal series type graphitization process and the Acheson graphitization process is that the product is heated without the resistance material heating. The method is also a main characteristic of improvement of the inner-string type graphitization process compared with the Acheson graphitization process. Because the inner series type graphitization process does not contain the filler, the heat carrying-out can be reduced by 10 percent, and the power consumption is reduced by 20 to 35 percent. The internal-series graphitizing furnace has the characteristics of high thermal efficiency, short power transmission time and the like, and only needs 1-2 hours at a high-temperature stage. The resistance is uniform when the product is directly heated, the yield of the product is high, and the graphite electrode can be discharged after the yield is high for 10 days on average. Since the 80 th century, carbon factories in germany, the united states of america, japan, etc. have mostly adopted an internal series graphitization process to produce large-scale ultrahigh power graphite electrodes. The furnace types of the inner-string type graphitizing furnace can be divided into I-type U-type W-type and quincunx-type furnaces, wherein the number of the U-type furnaces is more, the U-type furnaces have single columns and multi-columns, and the U-type furnaces have two-fold, four-fold and even multi-fold. The powder is placed in a graphite crucible for graphitization in China, and a negative electrode material is not processed into a rectangular shape, is roasted and formed, is directly placed in a graphitization furnace, and is graphitized according to a graphite electrode process.
Chinese granted patent CN111354927B discloses a composite graphite negative electrode material, a lithium ion battery, and a preparation method and application thereof. The preparation method comprises the following steps: s1: preparing a kneaded material of calcined green coke powder, crystalline flake graphite powder, a graphitization catalyst and a graphitizable adhesive; wherein, the mass ratio of the calcined green coke powder to the crystalline flake graphite powder is 1.5-1, the dosage of the graphitization catalyst is 0.1-0.8% of the mass sum of the calcined green coke powder and the crystalline flake graphite powder, and the dosage of the graphitizable adhesive is 1-9% of the mass sum of the calcined green coke powder and the crystalline flake graphite powder; s2: carbonizing treatment; s3: and (4) carrying out catalytic graphitization high-temperature treatment. The lithium secondary battery prepared from the composite graphite cathode material has high charge-discharge capacity, high first-time efficiency and high capacity retention rate, the maximum charge-discharge capacity can reach 368.6mAh/g, and the maximum first-time discharge efficiency can reach 94.8%.
In addition, chinese granted patent CN103855395B discloses a preparation method of a natural graphite negative electrode material of a lithium ion battery and the prepared natural graphite negative electrode material of the lithium ion battery, which comprises the following steps: (1) under the temperature condition of 500-600 ℃, the spherical natural graphite is pretreated at high temperature for 4-6 hours; (2) uniformly mixing the spherical natural graphite, the graphitization catalyst and the petroleum asphalt in the step (1) to obtain a mixture; (3) carbonizing the mixture in the step (2), cooling, and then carrying out catalytic graphitization high-temperature treatment; (4) and (4) grading, namely. The preparation method of the graphite cathode material is simple and feasible, and is suitable for industrial production. The graphite cathode material has the advantages of large discharge capacity (the highest discharge capacity can reach 366.3 mAh/g), good cycle performance, excellent comprehensive performance of the button cell prepared from the graphite cathode material, and the highest first charge-discharge efficiency can reach 93.5%.
However, how to further improve the discharge capacity and the first charge-discharge efficiency of the graphite negative electrode still remains a technical problem to be solved by those skilled in the art.
Disclosure of Invention
Based on the above background, the technical problem to be solved by the present invention is to provide a method for processing a negative electrode material by using an internal graphitizing furnace. In order to realize the purpose of the invention, the following technical scheme is adopted:
the invention relates to a method for processing a cathode material by using an internal-series graphitization furnace, which is characterized by comprising the following steps:
(1) Pulverizing petroleum coke, needle coke or pitch coke or their mixture to powder with D50 of 2-45 micrometer (preferably 5-10 micrometer); grinding the modified asphalt by using an airflow pulverizer until the D50 is less than or equal to 10 mu m;
(2) Adding the ground raw materials and modified asphalt accounting for 10-40% of the weight of the raw materials into a kneading pot, heating the raw materials and the modified asphalt while stirring to 20-50 ℃ above the softening point of the modified asphalt, coating and granulating the modified asphalt, putting the coated granules into a second-layer kneading pot, adding 1-5% of catalyst and high-temperature asphalt with the softening point of 100-200 ℃, stirring again, cooling while stirring, and cooling the materials to room temperature;
(3) Scattering the kneaded powder material through a 50-100 micron sieve, filling the sieved powder material into a soft mold made of polyurethane or PE and PP materials, and vacuumizing, wherein the specification of the mold is a cuboid of 200-600mm multiplied by 1000-1500 mm; isostatic pressing is adopted, the pressing pressure is 40-200MPa (preferably 50-90 MPa), and the holding time is 2-5 minutes, so that a blank is obtained;
(4) Sawing two end surfaces of the blank along the long axis direction, putting the rectangular blank into a stainless steel crucible, putting the stainless steel crucible into a roasting furnace, and heating the blank to 1000-1400 ℃ in a closed manner;
(5) Placing the sintered blank into an inner-string graphitization furnace, placing the sintered blank between conductive electrodes of the graphitization furnace in a tandem manner along a conductive section, ensuring the end face of a negative block to be tightly connected, filling heat preservation materials around the sintered blank after the sintered blank is tightly pressed by a hydraulic device, and delivering power after charging, wherein the current density is 2.5-3.5A/cm 2 Keeping the highest power for 5-9 hours, and stopping power transmission and cooling after the power transmission time is 24-30 hours;
(6) After graphitization, the negative block can be taken out of the furnace after being cooled for 8-10 days, surface cleaning, crushing, scattering and deironing are carried out, and the particle size is controlled to be less than or equal to 50 micro-materials in the range during screening.
In a preferred embodiment of the present invention, the catalyst is one or more of nano white carbon ink, iron oxide, silicon carbide and silicon dioxide.
In a preferred embodiment of the invention, the catalyst is one or a combination of two of nano-silica and nano-iron oxide; particularly preferably, the catalyst is a combination of nano silicon dioxide and nano ferric oxide, and the weight ratio of the nano silicon dioxide to the nano ferric oxide is 1:1.5-2.5, the discharge capacity, the first efficiency and the capacity retention rate can be simultaneously further improved by adopting the preferable catalyst.
The average particle size of the nano-silica is not particularly limited, but the average particle size of the nano-silica is preferably 3 to 20nm, and particularly preferably 4 to 6nm, from the viewpoint of improving the discharge capacity.
The average particle size of the nano iron oxide is not particularly limited, but from the viewpoint of improving the capacity retention rate, the average particle size of the nano iron oxide is preferably 5 to 20nm, and particularly preferably 8 to 12nm.
Advantageous effects
The preparation method has the advantages of simple and easy process, wide raw material source and low cost. The discharge capacity, the first efficiency and the cycle life of the graphite cathode prepared by the method are all improved.
Detailed Description
In order to further understand the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Unless otherwise specified, the reagents used in the examples of the present invention are commercially available products, and all of them can be purchased from commercial sources.
Example 1:
a method for processing a lithium ion battery cathode material by using an internal-string graphitization processing furnace comprises the following specific steps:
(1) Crushing the petroleum coke raw material to be less than 5mm by using a hammer crusher;
(2) Grinding petroleum coke particles with the particle size of less than 5mm into powder with a jet mill until the D50 is 7 mu m;
(3) Grinding the modified asphalt at 250 ℃ by using an airflow pulverizer until the D50 is less than or equal to 10 mu m;
(4) Adding the ground petroleum coke powder with the particle size of 7 mu m into a kneading pot, and then adding the ground modified asphalt powder with the temperature of 250 ℃ for 5-coating granulation; heating while stirring by adopting a double-layer kneading pot, heating to 285 ℃, and keeping the temperature to continue stirring for 3 hours;
putting the coated granules into a second layer kneading pot, adding 3% of iron oxide catalyst and 5% of high-temperature asphalt powder with a softening point of 180 ℃, stirring and cooling to cool the materials to room temperature;
(5) Scattering the kneaded powder to pass through a 72-micron sieve, filling the powder passing through the 72-micron sieve into a soft mold made of polyurethane or PE and PP materials, and vacuumizing, wherein the specification of the mold is a cuboid of 400mm, 400mm and 1200 mm; 0 (6) isostatic pressing the vacuum-formed material, wherein the pressing pressure is 70MPa, and the pressure maintaining time is 3 minutes;
(7) Sawing two end surfaces of the pressed block material in the long axis direction to be flat, loading the rectangular blank material into a stainless steel crucible, loading the stainless steel crucible into a ring type roasting furnace, loading the embedded material into the ring type roasting furnace, heating to 1100 ℃, preserving heat for 24 hours, and cooling along with the furnace after the time comes;
(8) Placing the sintered blank into an inner string graphitization furnace, connecting the sintered blank in series along the front and back of a conductive section, placing the blank between conductive electrodes of the graphite furnace, ensuring tight connection of the end surfaces of a negative electrode block, filling and leveling the part with poor contact by using a graphite material 5, compacting the part with a hydraulic device after leveling, and then filling heat insulating materials with 0-2mm particles around the part;
(9) After charging, power transmission is carried out, the highest power which can be transmitted is transmitted, the highest power is reached, namely the highest power of 2.5 kilo volt-ampere, the highest power is maintained for 7 hours, and the finally reached current density is not less than 2.5A/cm 2 The total power transmission time is 26 hours, and the furnace is cooled after the power transmission is stopped;
(10) And after graphitization, the negative block can be taken out of the furnace after being cooled for 8-10 days, the surface is cleaned, crushing is carried out by a jaw 0 type crusher, scattering is carried out by a jet mill, screening is carried out after iron removal, and the particle size Dmax is controlled to be less than or equal to 50 μm when screening is carried out.
Example 2:
the catalyst was a silica powder having an average particle diameter of 5 nm and was added in an amount of 5% as in example 1.
Example 3: the same as example 1, except that the catalyst was silica powder having an average particle size of 5 nm and iron oxide powder having an average particle size of 10 nm, and the amounts of the catalyst added were 1% and 2%, respectively.
Comparative example 1:
the same as in example 1 except that the sintered compact was pulverized, and the sintered compact was placed between conductive electrodes of a graphite furnace in the form of powder.
The half cell test method comprises the following steps: the composite graphite negative electrode material, N-methyl pyrrolidone containing 6-7% of polyvinylidene fluoride and 2% of conductive carbon black are uniformly mixed according to the mass ratio of 91.6. The simulated cells were assembled in an argon-filled german braun glove box with electrolyte of 1mlipf6+ ec dmc =1 (volume ratio), metallic lithium sheet as counter electrode, electrochemical (discharge capacity and first efficiency) tests were performed on a us ArbinBT bt2000 type cell tester with a charge-discharge voltage range of 0.005 to 1.0V and a charge-discharge rate of 0.5C. Each group was repeated 3 times and the experimental results averaged.
The full cell testing method used by the invention comprises the following steps: the composite graphite negative electrode material, N-methyl pyrrolidone containing 6-7% of polyvinylidene fluoride and 2% of conductive carbon black are uniformly mixed according to the mass ratio of 91.6 6 + EC: DMC: EMC =1:1 (volume ratio) solution was used as an electrolyte to assemble a full cell, and the capacity retention rate after 1000 cycles of 1C charge-discharge cycle was tested. Each group was repeated 3 times and the experimental results averaged.
Table 1: performance parameters of graphite negative electrode materials of examples and comparative examples
| Group of | Discharge capacity (mAh/g) | First efficiency (%) | Capacity retention (%) |
| Example 1 | 369.6±1.8 | 94.9±1.2 | 85.3±1.4 |
| Example 2 | 375.4±1.6 | 95.6±1.4 | 88.6±1.1 |
| Example 3 | 378.2±1.3 | 96.7±1.3 | 90.5±1.2 |
| Comparative example 1 | 358.7±1.9 | 90.3±2.4 | 76.5±2.5 |
The experimental results show that the discharge capacities of the embodiments of the invention are all more than 360mAh/g, the first charge-discharge efficiency is more than 94%, and the capacity retention rate (1000 cycles of 1C charge-discharge cycle) is more than 85%. In particular, example 3, which is a preferred example of the present invention, has a discharge capacity of 378mAh/g or more, a first charge-discharge efficiency of 96% or more, and a capacity retention rate (1000 cycles of 1C charge-discharge cycle) of 90% or more.
The foregoing describes preferred embodiments of the present invention, but is not intended to limit the invention thereto. Those skilled in the art may make modifications and variations to the embodiments disclosed herein without departing from the scope and spirit of the invention.
Claims (9)
1. A method for processing a cathode material by using an inner series graphitization furnace is characterized by comprising the following steps:
(1) Grinding petroleum coke, needle coke or asphalt coke or their mixture to D50 of 2-45 micron; grinding the modified asphalt by using an airflow pulverizer until the D50 is less than or equal to 10 mu m;
(2) Adding ground raw materials and modified asphalt accounting for 10-40% of the weight of the raw materials into a kneading pot, heating the mixture to 20-50 ℃ above the softening point of the modified asphalt by adopting a double-layer kneading pot while stirring, coating and granulating the mixture by using the modified asphalt, putting the coated granules into a second-layer kneading pot, adding 1-5% of catalyst and high-temperature asphalt with the softening point of 100-200 ℃, stirring the mixture again, and cooling the mixture to room temperature while stirring;
(3) Scattering and sieving the kneaded powder, filling the sieved powder into a soft mold made of polyurethane or PE and PP materials, and vacuumizing the mold, wherein the specification of the mold is a cuboid of 200-600mm multiplied by 1000-1500 mm; isostatic pressing is adopted, the pressing pressure is 40-200MPa, and the holding time is 2-5 minutes, so that a blank is obtained;
(4) Sawing two end surfaces of the blank along the long axis direction, putting the rectangular blank into a stainless steel crucible, putting the stainless steel crucible into a roasting furnace, and heating the blank to 850-1400 ℃ in a closed manner;
(5) Placing the sintered blank into an inner-string graphitization furnace, placing the sintered blank between conductive electrodes of the graphitization furnace in a tandem manner along the front and back of a conductive section, ensuring the end face of a negative block to be tightly connected, filling heat preservation materials around the sintered blank after being tightly pressed by a hydraulic device, and filling the sintered blank into the graphite furnace after the charging is finishedFeeding with current density of 2.5-3.5A/cm 2 Keeping the highest power for 5-9 hours, and stopping power transmission and cooling after the power transmission time is 24-30 hours;
(6) After graphitization, the negative block can be taken out of the furnace after being cooled for 8-10 days, surface cleaning, crushing, scattering and deironing are carried out, and the particle size is controlled to be less than or equal to 50 micrometers in the screening process.
2. The preparation method according to claim 1, wherein the catalyst is one or more of nano white carbon ink, iron oxide, silicon carbide and silicon dioxide.
3. The preparation method according to claim 2, wherein the catalyst is one or a combination of two of nano-silica and nano-iron oxide.
4. The method of claim 3, wherein the catalyst is a combination of nano-silica and nano-iron oxide.
5. The preparation method of claim 4, wherein the weight ratio of the nano silicon dioxide to the nano iron oxide is 1:1.5-2.5.
6. The method according to claim 5, wherein the nanosilica has an average particle size of 3-20nm.
7. The method according to claim 5, wherein the nanosilica has an average particle size of 4-6nm.
8. The method according to claim 5, wherein the nano iron oxide has an average particle size of 5 to 20nm.
9. The method according to claim 5, wherein the nano iron oxide has an average particle size of 8 to 12nm.
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