CN115709982B - Preparation method and device of carbon powder for hard carbon negative electrode material - Google Patents
Preparation method and device of carbon powder for hard carbon negative electrode material Download PDFInfo
- Publication number
- CN115709982B CN115709982B CN202211538694.5A CN202211538694A CN115709982B CN 115709982 B CN115709982 B CN 115709982B CN 202211538694 A CN202211538694 A CN 202211538694A CN 115709982 B CN115709982 B CN 115709982B
- Authority
- CN
- China
- Prior art keywords
- chamber
- carbon powder
- carbon
- gas
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 177
- 229910021385 hard carbon Inorganic materials 0.000 title claims abstract description 43
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 94
- 239000007789 gas Substances 0.000 claims abstract description 89
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 57
- 239000003345 natural gas Substances 0.000 claims abstract description 47
- 238000001816 cooling Methods 0.000 claims abstract description 44
- 230000008021 deposition Effects 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000000428 dust Substances 0.000 claims description 45
- 238000007664 blowing Methods 0.000 claims description 15
- 230000007246 mechanism Effects 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 6
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 16
- 230000001276 controlling effect Effects 0.000 description 10
- 238000009826 distribution Methods 0.000 description 9
- 239000003575 carbonaceous material Substances 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010924 continuous production Methods 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 239000010406 cathode material Substances 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 239000007770 graphite material Substances 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 229910021383 artificial graphite Inorganic materials 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 239000002194 amorphous carbon material Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- -1 i.e. Substances 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 235000019241 carbon black Nutrition 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 208000028659 discharge Diseases 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 229910021469 graphitizable carbon Inorganic materials 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 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
- 239000011331 needle coke Substances 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- 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
Abstract
The application relates to a preparation method and a device of carbon powder for a hard carbon negative electrode material, wherein the preparation method comprises the following steps: s1: vacuumizing the reaction chamber to absolute pressure below 500 Pa; s2: rapidly heating the reaction chamber to 1000-1150 ℃ and controlling absolute pressure below 1000 Pa; s3: maintaining the temperature of the reaction chamber at 1000-1150 ℃, introducing natural gas, and controlling the absolute pressure at 2000-10000Pa to obtain carbon-containing powder mixed gas; s4: cooling the mixed gas containing carbon powder; s5: filtering the cooled carbon-containing powder mixed gas to perform solid-gas separation, and purifying the collected solid to obtain carbon powder for the hard carbon negative electrode material. The preparation device comprises a carbon powder deposition chamber, a gas cooling chamber, a carbon powder collecting chamber and a gas collecting chamber which are communicated through pipelines in sequence. The application has the advantages of reducing cost and reducing environmental pollution.
Description
Technical Field
The application relates to the technical field of carbon powder preparation, in particular to a preparation method and device of carbon powder for a hard carbon negative electrode material.
Background
Lithium ion batteries are generally batteries using lithium alloy metal oxides as positive electrode materials, graphite as negative electrode materials, and nonaqueous electrolytes. At present, the cathode material of the commercial lithium ion battery is mainly made of carbon materials, and has high specific capacity, low electrode potential, good cycle performance and stable physicochemical properties. Carbon materials can be classified into graphite materials and amorphous carbon materials according to the degree of crystallization. The graphite material is characterized by good conductivity, high crystallinity, stable layered structure, suitability for intercalation-deintercalation of lithium and the like, and becomes an ideal lithium battery cathode material, and the artificial graphite and the natural graphite are two main graphite materials, wherein the artificial graphite is a graphite material prepared by calcining graphitizable carbon (petroleum coke, needle coke, asphalt and the like) at a certain temperature, crushing, forming, grading and graphitizing at a high temperature, and the high crystallinity is formed by graphitizing at a high temperature. Through continuous modification research, the artificial graphite is close to or even surpasses natural graphite in capacity, first cycle efficiency, cycle life and the like, and at present, the negative electrode material of the lithium battery is mainly made of graphite materials, but high-temperature graphitization also brings high-cost defects, serious environmental pollution and the like, the preparation process is mature, but the performance of the artificial graphite is limited by the structure, the development space is small, and the requirements of increasingly promoted downstream markets are difficult to meet.
Currently, amorphous carbon materials, i.e., carbon materials without fixed crystalline shapes, mainly comprise soft carbon and hard carbon, and hard carbon negative electrode materials currently mainly comprise resin carbons (such as phenolic resins, epoxy resins, and the like), organic polymer pyrolytic carbons (such as PFA, PVC, PVDF, and the like), carbon blacks, biomass carbons, and the like. Compared with graphite negative electrode materials, the hard carbon negative electrode material has the advantages of high reversible specific capacity, excellent multiplying power characteristics, good low-temperature performance, high charge and discharge speed, high safety, long service life and obvious performance advantage. In order to improve the product performance, carbon powder is one of the main materials for producing hard carbon at present, and when a hard carbon negative electrode material is used as a negative electrode material of a lithium battery, the cost is high and the pollution is large when the carbon powder for producing the hard carbon negative electrode material is produced at present, so how to reduce the production cost and the environmental pollution is one of the important research directions of the industry.
Disclosure of Invention
In order to reduce cost and reduce environmental pollution, the application provides a preparation method and a device of carbon powder for a hard carbon negative electrode material.
In a first aspect, the present application provides a method for preparing carbon powder for a hard carbon negative electrode material, which adopts the following technical scheme: the preparation method of the carbon powder for the hard carbon negative electrode material comprises the following steps:
s1: vacuumizing the reaction chamber to absolute pressure below 500 Pa;
s2: rapidly heating the reaction chamber to 1000-1150 ℃ and controlling absolute pressure below 1000 Pa;
s3: maintaining the temperature of the reaction chamber at 1000-1150 ℃, introducing natural gas, and controlling the absolute pressure at 2000-10000Pa to obtain carbon-containing powder mixed gas;
s4: cooling the mixed gas containing carbon powder;
s5: filtering the cooled carbon-containing powder mixed gas to perform solid-gas separation, wherein the collected solid is carbon powder for the obtained hard carbon negative electrode material.
By adopting the technical scheme, the hard carbon has higher specific capacity as the negative electrode material of the lithium ion battery, the carbon powder is prepared by adopting natural gas to react under certain temperature and pressure environment, in the process of preparing the carbon powder into the hard carbon material, the hard carbon is carbon which is difficult to graphitize, namely carbon which is difficult to obtain good crystallinity at high temperature is carbonized, the obtained carbon powder is amorphous carbon, and the carbon powder has a large number of defects, and the defects can help to contain lithium ions, and for the specific structures, the hard carbon material prepared by the carbon powder has larger specific surface area, is rich in mesopores and micropores, or has relatively rough surface, can be subjected to desorption of lithium ions in the charging and discharging process, and can also form lithium molecules and lithium ion clusters in the pores; moreover, as the carbonization of the obtained hard carbon material is incomplete, the material also has H, N, O atom residues, and doped atoms can be bonded with Li to generate additional capacity; because the size, distribution and morphology of the carbon powder particles influence a plurality of performance indexes of the negative electrode material, the distribution of the particle size of the carbon powder is a very critical step for preparing the qualified negative electrode material. The smaller the particles are, the better the multiplying power performance and the cycle life are, but the worse the first efficiency and the compaction density are, and vice versa, the better the particle size distribution of the carbon powder obtained by the method can effectively improve the performance of the cathode material; and the reasonable particle size distribution (mixing large particles and small particles) can improve the specific capacity of the cathode; and because the raw materials adopt natural gas, the content of the impurities in the obtained carbon powder is low, and the carbon powder for the hard carbon material is prepared by adopting the natural gas as a carbon source, the cost is low, and the pollution to the environment is less.
Optionally, S4, cooling the carbon powder-containing mixed gas by heat exchange, and controlling the temperature at 150-350 ℃ after cooling.
Through adopting above-mentioned technical scheme, in the in-process that obtains the carbon dust through the natural gas reaction under specific condition, through controlling carbon dust mixed gas cooling temperature in above-mentioned temperature range for the carbon dust that generates has better stability, guarantees to produce the particle diameter scope of carbon dust, is convenient for collect the carbon dust.
Optionally, the natural gas introduced in S3 is a cyclone gas.
Through adopting above-mentioned technical scheme, through the natural gas that will let in the reaction chamber be the whirl gas, not only can improve the utilization ratio of natural gas, and then can effectively improve the productivity ratio of carbon dust to can also effectively reduce the temperature gradient in the reaction chamber, improve product structure controllability and prevent the coking of reaction chamber inner wall face.
Optionally, the flow rate of the natural gas introduced in the S3 is controlled to be 1-3Nm 3 /h。
By adopting the technical scheme, in the process of preparing the carbon powder, in order to improve the production efficiency, when the flow control of the natural gas is controlled within the range, the utilization rate of the natural gas can be further effectively improved and the production efficiency is improved while the production efficiency is ensured.
In a second aspect, the present application provides a device for preparing carbon powder for a hard carbon negative electrode material, which adopts the following technical scheme: the utility model provides a preparation facilities of carbon dust for hard carbon negative pole material, includes the carbon dust deposition chamber, gas cooling room, carbon dust collection room and the gas collection room that loop through the pipeline intercommunication, the carbon dust deposition chamber is used for carrying out the heating reaction to the natural gas, the gas cooling room is used for cooling the carbon dust mixed gas of the indoor production of carbon dust deposition, the intercommunication has the vacuum pump package on the carbon dust collection room, the carbon dust collection room includes main chamber, auxiliary chamber and sack formula filter core, the auxiliary chamber is located the main chamber bottom is used for collecting the carbon dust, the sack formula filter core is located the main chamber top, the main chamber top is equipped with the gas vent with the gas collection room intercommunication, gas vent and gas collection room intercommunication.
Through adopting above-mentioned technical scheme, in the carbon dust production process, through letting in the carbon dust deposition room with natural gas, heat in the carbon dust deposition room and make the natural gas reaction obtain carbon dust mixed gas, then in the rethread pipeline carries carbon dust mixed gas to the cooling of gas cooling room back entering main room, under the effect of pocket type filter core, carbon dust is filtered in main room, gas gets into the gas collection room through the gas vent and carries out the collection processing, the carbon dust collection that is filtered gets into the auxiliary room and carries out the collection processing, continuous production, the energy saving.
Optionally, the carbon powder collecting chamber further comprises a back blowing mechanism, and the back blowing mechanism is arranged at the top of the main chamber and is used for blowing air into the cloth bag filter element.
Through adopting above-mentioned technical scheme, through setting up blowback mechanism, in the carbon dust production process, along with the deposit of carbon dust on the pocket type filter core is more and more, can cause the shutoff to pocket type filter core surface's hole, blowback nitrogen gas in to the pocket type filter core through blowback mechanism for the carbon dust of adhesion on the pocket type filter core is shaken off, and then effectively improves the collection efficiency to the carbon dust.
Optionally, a discharge valve is arranged at the bottom of the auxiliary chamber, and control valves are arranged at the communication positions of the auxiliary chamber and the main chamber.
Through adopting above-mentioned technical scheme, when carrying out the transportation of unloading to the carbon dust, at first closing the control valve between main room and the auxiliary chamber, then opening the discharge valve for the carbon dust in the auxiliary chamber shifts to in the hopper through collecting the transportation, and rethread closes the discharge valve after collecting, opens the control valve and continues to collect.
Optionally, an air charging pipe is arranged on the auxiliary chamber, the air charging pipe is communicated with an air source pipeline of the back blowing mechanism, and an adjusting valve is arranged on the air charging pipe.
Through adopting above-mentioned technical scheme, in the carbon dust production process, because keep certain pressure in the system, at the in-process of collecting the carbon dust, when the carbon dust is collected after a period of time, when need transporting the unloading to the carbon dust, at first close the control valve between main room and the auxiliary chamber, charge nitrogen gas to the auxiliary chamber through the gas tube for reach the ordinary pressure state in the auxiliary chamber, open the discharge valve again and advance to unload, make the in-process of unloading safer, and avoid producing a large amount of raise dust and influence operational environment when collecting.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the preparation method of the carbon powder is characterized in that the carbon powder is prepared by adopting natural gas to react under a certain temperature and pressure environment, so that the obtained carbon powder is amorphous carbon when the carbon powder is used for preparing the hard carbon negative electrode material, and the carbon powder has a large number of defects, which can help to contain lithium ions and generate extra capacity, and the carbon powder for preparing the hard carbon material by adopting the natural gas as a carbon source has lower cost and less pollution to the environment;
2. the natural gas introduced in the carbon powder production process is controlled to be cyclone gas, and the flow is controlled to be 1-3Nm 3 And/h, the utilization rate of the natural gas can be further effectively improved, and the production efficiency is improved;
3. through setting up preparation facilities and passing through carbon dust deposition chamber, gas cooling room, carbon dust collection room and the gas collection room of pipeline intercommunication in proper order, heat in the carbon dust deposition chamber and make natural gas reaction obtain carbon dust mixed gas, then carry carbon dust mixed gas to the gas cooling room through the pipeline and get into the main room after cooling down and collect, can carry out continuous production, effective energy saving.
Drawings
Fig. 1 is a schematic perspective view of a device for preparing carbon powder for a hard carbon negative electrode material according to an embodiment of the present application.
Fig. 2 is a schematic plan view of a device for preparing carbon powder for a hard carbon negative electrode material according to an embodiment of the present application.
FIG. 3 shows a distribution diagram of particle diameters of carbon powder obtained in the example of the present application, wherein a is the particle diameter in Table 2, and b is the content in Table 2.
Reference numerals: 1. a carbon powder deposition chamber; 11. a heat preservation layer; 12. a furnace body; 13. a furnace cover; 14. an electric heater; 2. a gas cooling chamber; 21. a water-cooled heat exchanger; 22. a housing; 3. a carbon powder collection chamber; 31. a main chamber; 32. a sub-chamber; 33. a cloth bag type filter element; 34. an exhaust port; 35. a back-blowing mechanism; 36. a discharge valve; 37. a control valve; 38. an inflation tube; 39. a regulating valve; 4. a gas collection chamber; 5. a vacuum pump set.
Detailed Description
The present application is described in further detail below in conjunction with figures 1-3.
Example 1
The embodiment of the application discloses a preparation method of carbon powder for a hard carbon negative electrode material. Referring to fig. 1 and 2, the method comprises the following steps: s1: opening a valve, starting a vacuum pump set 5 to start vacuumizing, and vacuumizing a carbon powder preparation device to an absolute pressure of 400Pa; s2: starting an electric heater 14 of the carbon powder deposition chamber 1, quickly heating to 1000 ℃, and controlling the absolute pressure to be 800Pa;
s3: the temperature of the carbon powder deposition chamber 1 is kept at 1000 ℃, the valve of the air supply pipeline is opened to introduce natural gas, the natural gas is changed into rotational flow gas under the action of the rotational flow gas port in the carbon powder deposition chamber 1, and the flow rate of the natural gas is controlled at 1Nm 3 And/h, controlling the absolute pressure in the carbon powder deposition chamber 1 at 2000Pa to obtain carbon powder-containing mixed gas;
s4: cooling the mixed gas containing carbon powder through a water-cooling heat exchanger 21 of a gas cooling chamber 2, and cooling the mixed gas containing carbon powder through heat exchange, wherein the temperature is controlled at 150 ℃ after cooling;
s5: filtering the cooled carbon-containing powder mixed gas to perform solid-gas separation, and purifying the collected solid by a purifying furnace to obtain carbon powder for the hard carbon cathode material.
The productivity calculation result shows that the productivity of the carbon powder of this example is 30% after 24 hours of continuous production.
The embodiment of the application also discloses a preparation facilities for carbon dust for hard carbon negative pole material, refer to fig. 1 and 2, adopt foretell a preparation facilities for carbon dust for hard carbon negative pole material, preparation facilities is including the carbon dust deposition chamber 1 that loops through the pipeline intercommunication, gas cooling chamber 2, carbon dust collection chamber 3 and gas collection chamber 4, carbon dust deposition chamber 1 is used for carrying out the heating reaction to natural gas, carbon dust deposition chamber 1 includes furnace body 12, bell 13, heat preservation 11 and electric heater 14, heat preservation 11 is laid in the lateral wall of furnace body 12 and is close to one side outside the furnace body 12, the installation of motor heater is in one side that the furnace body 12 inner wall is close to the stove, bell 13 is installed at furnace body 12 top and is used for sealing furnace body 12. The furnace cover 13 is provided with a natural gas supply pipe, one end part of the natural gas supply pipe, which is positioned in the furnace body 12, is provided with a rotational flow air port, and when natural gas is conveyed into the furnace body 12 through the natural gas supply pipe, the natural gas flows in the furnace body 12 in a rotational flow way under the action of the rotational flow air port, so that the utilization rate of the natural gas is improved.
Referring to fig. 1 and 2, the gas cooling chamber 2 is configured to cool the carbon powder mixed gas produced in the carbon powder deposition chamber 1, and the gas cooling chamber includes a housing 22 and a water-cooling heat exchanger 21 installed in the housing 22, and after the carbon powder mixed gas reacted in the carbon powder deposition chamber 1 enters the gas cooling chamber 2, the carbon powder mixed gas is cooled by the water-cooling heat exchanger 21, so as to facilitate collection of the carbon powder.
Referring to fig. 1 and 2, the carbon powder collecting chamber 3 includes a main chamber 31, an auxiliary chamber 32 and a cloth bag filter element 33, the auxiliary chamber 32 is coaxially installed at the bottom of the main chamber 31 for collecting carbon powder, the main chamber 31 and the auxiliary chamber 32 are communicated through a vertical pipeline, the cloth bag filter element 33 is installed at the top of the main chamber 31, an exhaust port 34 communicated with the gas collecting chamber 4 is arranged at the top of the main chamber 31, the exhaust port 34 is communicated with the inside of the cloth bag filter element, and the other end of the exhaust port 34 is communicated with the gas collecting chamber 4. A discharge valve 36 is arranged at the bottom of the auxiliary chamber 32, a control valve 37 is arranged at the communication part of the auxiliary chamber 32 and the main chamber 31, and the discharge valve 36 and the control valve 37 are matched with each other to perform discharge treatment on the carbon powder collected in the auxiliary chamber 32.
Referring to fig. 1 and 2, the carbon powder collecting chamber 3 further includes a back-blowing mechanism 35, the back-blowing mechanism 35 is specifically a pulse-type air tube 38, the back-blowing mechanism 35 is communicated with a nitrogen air source pipeline, the back-blowing mechanism 35 is arranged at the top of the main chamber 31, and an air outlet hole of the back-blowing mechanism 35 extends into the cloth-bag filter core to blow air into the cloth-bag filter core. The auxiliary chamber 32 is provided with an inflation tube 38, the inflation tube 38 is communicated with a nitrogen gas source pipeline of the back blowing mechanism 35, and the inflation tube 38 is provided with a regulating valve 39. A vacuum pump set 5 is arranged on the carbon powder collecting chamber 3, and the vacuum pump set 5 is used for vacuumizing the whole device.
The implementation principle of the preparation device for the carbon powder for the hard carbon negative electrode material in the embodiment of the application is as follows: in the carbon powder production process, firstly, the device is vacuumized through a vacuum pump set 5, then natural gas is introduced into a carbon powder deposition chamber 1, the natural gas reacts under the action of an electric heater 14 to obtain carbon powder, the generated carbon powder and the carbon powder mixed gas formed by the participation gas enter a gas cooling chamber 2 to be cooled through a water-cooling heat exchanger 21, then enter a carbon powder collection chamber 3, the carbon powder is filtered under the action of a bag type filter element, and the carbon powder obtained by filtration is deposited in a secondary chamber 32 to be collected.
Example 2
This example differs from example 1 in that the preparation method comprises the following steps:
s1: opening a valve, starting a vacuum pump set 5 to start vacuumizing, and vacuumizing the reaction chamber to an absolute pressure of 350Pa;
s2: starting an electric heater 14 of the carbon powder deposition chamber 1, quickly heating to 1150 ℃, and controlling the absolute pressure to be 850Pa;
s3: the temperature of the carbon powder deposition chamber 1 is maintained at 1150 ℃, the valve of the air supply pipeline is opened to introduce natural gas, the natural gas is changed into rotational flow gas under the action of the rotational flow gas port in the carbon powder deposition chamber 1, and the flow rate of the natural gas is controlled at 3Nm 3 And/h, controlling the absolute pressure in the carbon powder deposition chamber 1 at 10000Pa to obtain the carbon powder containingCarbon powder mixed gas;
s4: cooling the mixed gas containing carbon powder through a water-cooling heat exchanger 21 of a gas cooling chamber 2, and cooling the mixed gas containing carbon powder through heat exchange, wherein the temperature is controlled at 350 ℃ after cooling;
s5: filtering the cooled carbon-containing powder mixed gas to perform solid-gas separation, and purifying the collected solid by a purifying furnace to obtain carbon powder for the hard carbon cathode material.
The productivity calculation result shows that the productivity of the carbon powder of this example is 40% after 24 hours of continuous production.
Example 3
This example differs from example 1 in that the preparation method comprises the following steps:
s1: opening a valve, starting a vacuum pump set 5 to start vacuumizing, and vacuumizing the reaction chamber to the absolute pressure of 450Pa;
s2: starting an electric heater 14 of the carbon powder deposition chamber 1, quickly heating to 1110 ℃, and controlling the absolute pressure to be 900Pa;
s3: the temperature of the carbon powder deposition chamber 1 is kept at 1110 ℃, a valve of an air supply pipeline is opened to introduce natural gas, the natural gas is changed into rotational flow gas under the action of a rotational flow gas port in the carbon powder deposition chamber 1, and the flow rate of the natural gas is controlled at 2Nm 3 And/h, controlling the absolute pressure in the carbon powder deposition chamber 1 at 5000Pa to obtain carbon powder-containing mixed gas;
s4: cooling the mixed gas containing carbon powder through a water-cooling heat exchanger 21 of a gas cooling chamber 2, and cooling the mixed gas containing carbon powder through heat exchange, wherein the temperature is controlled at 250 ℃ after cooling;
s5: filtering the cooled carbon-containing powder mixed gas to perform solid-gas separation, and purifying the collected solid by a purifying furnace to obtain carbon powder for the hard carbon cathode material.
The productivity calculation result shows that the productivity of the carbon powder of this example is 50% after 24 hours of continuous production.
Comparative example 1
The difference between this example and example 1 is that the natural gas in this example was a direct current gas, and the productivity calculation result shows that the productivity of the carbon powder in this example was 21% after 24 hours of continuous production.
Comparative example 2
The difference between this example and example 1 is that the natural gas flow in this example is 0.5Nm 3 After 24 hours of continuous production, the yield calculation result of this example shows that the yield of the carbon powder of this example is 29%, but the carbon powder produced is 48% of the carbon powder produced in example 1.
By comparing examples 1-3 with comparative examples 1-2, the natural gas flow rate was controlled to 1-3Nm 3 In the time of/h, the utilization rate of the natural gas can be submitted, so that the yield is improved; the carbon powder yield of the example 1 is obviously higher than that of the comparative example 1, which indicates that the carbon powder yield can be effectively improved when natural gas is introduced in a cyclone mode; as is clear from comparison of example 1 and comparative example 2, the production efficiency of comparative example 1 is significantly lower than that of example 1, although the yields of example 1 and comparative example 2 are comparable.
Performance test
1. Particle size detection of carbon powder: 50g of each sample of examples 1-3 was removed, and the obtained carbon powder was tested according to GB/T19077-2016 particle size distribution laser diffraction method, the distribution diagram is shown in FIG. 3, the average value of the three data was taken, and the test data are shown in tables 1 and 2.
TABLE 1
| Particle size μm | Interval content% | Cumulative content% |
| 0.100-5.000 | 44.07 | 44.07 |
| 5.000-10.00 | 19.03 | 63.10 |
| 10.00-20.00 | 18.19 | 81.29 |
| 20.00-30.00 | 8.13 | 89.42 |
| 30.00-40.00 | 3.96 | 93.38 |
| 40.00-50.00 | 2.40 | 95.78 |
| 50.00-60.00 | 1.61 | 97.39 |
| 60.00-70.00 | 1.10 | 98.49 |
| 70.00-80.00 | 0.67 | 99.16 |
| 80.00-90.00 | 0.42 | 99.58 |
| 90.00-100.00 | 0.23 | 99.81 |
| 100.00-200.00 | 0.19 | 100 |
TABLE 2
Referring to table 1, the hard carbon powder material obtained in the present application has a preferable particle size distribution, a particle size distribution of about 10 μm, and a small particle size, and does not require crushing treatment.
The foregoing are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.
Claims (6)
1. A preparation method of carbon powder for a hard carbon negative electrode material is characterized by comprising the following steps of: the method comprises the following steps:
s1: vacuumizing the reaction chamber to absolute pressure below 500 Pa;
s2: rapidly heating the reaction chamber to 1000-1150 ℃ and controlling absolute pressure below 1000 Pa;
s3: maintaining the temperature of the reaction chamber at 1000-1150 ℃, introducing natural gas, and controlling the absolute pressure at 2000-10000Pa to obtain carbon-containing powder mixed gas; the natural gas is cyclone gas, and the flow rate of the natural gas is controlled to be 1-3Nm 3 /h；
S4: cooling the mixed gas containing carbon powder;
s5: filtering the cooled carbon-containing powder mixed gas to perform solid-gas separation, wherein the collected solid is carbon powder for the obtained hard carbon negative electrode material.
2. The method for preparing carbon powder for hard carbon negative electrode material according to claim 1, wherein the method comprises the following steps: s4, carrying out heat exchange and cooling on the carbon powder-containing mixed gas, and controlling the temperature at 150-350 ℃ after cooling.
3. The preparation facilities of carbon dust for hard carbon negative pole material, its characterized in that: adopt the preparation method of hard carbon powder of any one of claims 1-2, preparation facilities includes carbon powder deposition chamber (1), gas cooling chamber (2), carbon powder collection chamber (3) and gas collection chamber (4) that loop through the pipeline intercommunication in proper order, carbon powder deposition chamber (1) is used for carrying out the heating reaction to the natural gas, gas cooling chamber (2) are used for carrying out the cooling to the carbon powder mixed gas of production in carbon powder deposition chamber (1), the intercommunication has vacuum pump group (5) on carbon powder collection chamber (3), carbon powder collection chamber (3) include main chamber (31), auxiliary chamber (32) and sack formula filter core (33), auxiliary chamber (32) are located main chamber (31) bottom is used for collecting the carbon powder, sack formula filter core (33) are located main chamber (31) internal top, main chamber (31) top is equipped with gas vent (34) with gas collection chamber (4) intercommunication, gas vent (34) and gas collection chamber (4) intercommunication.
4. A device for preparing carbon powder for a hard carbon negative electrode material according to claim 3, wherein: the carbon powder collecting chamber (3) further comprises a back blowing mechanism (35), and the back blowing mechanism (35) is arranged at the top of the main chamber (31) and is used for blowing air into the cloth bag type filter element (33).
5. The device for preparing carbon powder for a hard carbon negative electrode material according to claim 4, wherein: the bottom of the auxiliary chamber (32) is provided with a discharge valve (36), and the communicating parts of the auxiliary chamber (32) and the main chamber (31) are provided with control valves (37).
6. The device for preparing carbon powder for a hard carbon negative electrode material according to claim 5, wherein: the auxiliary chamber (32) is provided with an air charging pipe (38), the air charging pipe (38) is communicated with an air source pipeline of the back blowing mechanism (35), and the air charging pipe (38) is provided with an adjusting valve (39).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211538694.5A CN115709982B (en) | 2022-12-02 | 2022-12-02 | Preparation method and device of carbon powder for hard carbon negative electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211538694.5A CN115709982B (en) | 2022-12-02 | 2022-12-02 | Preparation method and device of carbon powder for hard carbon negative electrode material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115709982A CN115709982A (en) | 2023-02-24 |
| CN115709982B true CN115709982B (en) | 2023-06-27 |
Family
ID=85235456
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211538694.5A Active CN115709982B (en) | 2022-12-02 | 2022-12-02 | Preparation method and device of carbon powder for hard carbon negative electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115709982B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO176522C (en) * | 1992-04-07 | 1995-04-19 | Kvaerner Eng | Process for the production of carbon with defined physical properties and apparatus for carrying out the process |
| CN101081991A (en) * | 2005-07-22 | 2007-12-05 | 许锦明 | Artificial petroleum and coal |
| CN102226091A (en) * | 2011-05-18 | 2011-10-26 | 浙江工业大学 | Apparatus for producing synthetic gas by pyrolysis gasification of biomass |
| CN113774365A (en) * | 2021-08-09 | 2021-12-10 | 山西中电科新能源技术有限公司 | Self-heating carbon-carbon vapor deposition furnace |
-
2022
- 2022-12-02 CN CN202211538694.5A patent/CN115709982B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN115709982A (en) | 2023-02-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108946704A (en) | A kind of serialization prepares the method and device of high-purity carbon nanotube | |
| CN112133915A (en) | Preparation method of silicon-carbon composite material | |
| KR20120120034A (en) | SiOx-based complex powder, preparation method thereof and the use of the same | |
| CN112875680B (en) | Preparation method of flaky Fe-based alloy catalytic growth carbon nanotube array | |
| WO2023115762A1 (en) | Method for preparing nano silicon powder by means of pyrolysis of silane with inductive plasma | |
| CN111463022A (en) | Preparation method of cobalt molybdenum oxide/nickel cobalt phosphide composite material | |
| WO2020134242A1 (en) | Negative electrode material for lithium ion battery, negative electrode for lithium ion battery, lithium ion battery, battery pack and battery powered vehicle | |
| CN111747416B (en) | Production of SiOxApparatus and method of | |
| CN114388770B (en) | High-capacity high-first-efficiency silicon oxide anode material and preparation method thereof | |
| CN114249326B (en) | Method for preparing sub-nano silicon-carbon composite material by liquid phase method | |
| CN115709982B (en) | Preparation method and device of carbon powder for hard carbon negative electrode material | |
| CN106207251B (en) | Carbon coating method of hydrothermal lithium iron phosphate | |
| CN105977483A (en) | Carbon-based nanocomposite material for electrode | |
| CN213824705U (en) | Reactor and system for preparing silicon-carbon composite material | |
| CN112028067A (en) | Silicon-carbon negative electrode material and preparation method thereof | |
| CN112993225B (en) | Antimony-based composite electrode material and preparation method and application thereof | |
| CN115172723A (en) | Preparation process of silicon-carbon composite material for lithium ion battery | |
| CN111348685B (en) | Graphene-based composite material and preparation method and application thereof | |
| CN108598377A (en) | The preparation method of sulphur-silicon carbide doped carbon nano-tube material | |
| CN114639805A (en) | Preparation method and application of porous-structure nickel phosphide @ carbon negative electrode material | |
| CN110537272B (en) | Silicon powder especially suitable for anode of lithium ion battery and its production method and use | |
| CN107863528B (en) | LiFePO4Modification method for O site modification of anode material | |
| CN112479177A (en) | Preparation method of ordered mesoporous silicon-carbon composite material | |
| CN111533108A (en) | Method for preparing lithium cobalt phosphate by using waste lithium cobalt oxide | |
| KR100269514B1 (en) | Carbonaceous anode material for lithium secondary battery and manufacturing method and apparatus thereof (Carboneous material for anodes of rechargeable lithium-ion battery and its synthesis method and apparatus) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 710608 Factory Building 2, No. 2299 Qinwang Second Road, Weibei New City, Xi'an Economic and Technological Development Zone, Shaanxi Province Patentee after: Shaanxi Meilan New Materials Co.,Ltd. Patentee after: Xi'an Meilan New Material Co.,Ltd. Address before: No. 56, Qinwang Second Road, Lintong District, Xi'an, Shaanxi 710600 Patentee before: SHAANXI MEILANDO CARBON CO.,LTD. Patentee before: Xi'an Meilan New Material Co.,Ltd. |