CN114381145A - Preparation method of low-viscosity acetylene carbon black - Google Patents
Preparation method of low-viscosity acetylene carbon black Download PDFInfo
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- CN114381145A CN114381145A CN202111531407.3A CN202111531407A CN114381145A CN 114381145 A CN114381145 A CN 114381145A CN 202111531407 A CN202111531407 A CN 202111531407A CN 114381145 A CN114381145 A CN 114381145A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/54—Acetylene black; thermal black ; Preparation thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/8663—Selection of inactive substances as ingredients for catalytic active masses, e.g. binders, fillers
- H01M4/8673—Electrically conductive fillers
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention belongs to the technical field of conductive carbon black materials, and particularly discloses a preparation method of low-viscosity acetylene carbon black. According to the method provided by the invention, on the basis of keeping the primary structure of the aggregate, the regrowth of the primary particles of the acetylene black can be better promoted, and simultaneously, the formation of a new acetylene black crystal nucleus is inhibited, the nanometer action energy among the acetylene black aggregates is reduced, and the secondary structure size generated by the physical agglomeration of the acetylene black particles is reduced, so that the preparation of the low-viscosity high-conductivity acetylene black can be realized on the premise of not reducing the conductivity of the acetylene black, and the performance requirement of the lithium battery on the conductive acetylene black in the assembly and processing process can be met.
Description
Technical Field
The invention belongs to the technical field of conductive carbon black materials, and particularly relates to a preparation method of low-viscosity acetylene carbon black.
Background
The thermal decomposition method of carbon black refers to a method of generating carbon black by intermittently (i.e. two stages of combustion heat storage and thermal decomposition) or continuously (single thermal decomposition) thermally cracking natural gas or acetylene gas in a preheated reaction furnace under the condition of isolating air. Carbon black produced by intermittent (i.e. two stages of combustion heat accumulation and thermal decomposition) cracking natural gas as a raw material under the condition of air isolation is called pyrolytic carbon black. The acetylene black is produced by continuous (single thermal decomposition) exothermic cracking of acetylene gas as a raw material in the absence of air.
In the production process of carbon black, the carbon black primary particles produced by cracking are always in a high temperature condition, and collide with each other and are fused to each other to form a chain-like aggregate occupying a three-dimensional space, which is called a primary structure of carbon black. The primary structures are further agglomerated into agglomerates due to physical effects such as nano-interaction energy or van der waals force, and the like, and are called secondary structures. The primary structure is inherent in the carbon black, and the secondary structure size is related to factors such as the specific surface area of the carbon black, the primary particle size and the like.
Acetylene black is used as a common conductive agent for the positive electrode and the negative electrode of the lithium ion battery, and an excellent conductive network can be constructed in the pole piece. The current preparation process of the positive electrode and the negative electrode of the lithium ion battery is generally as follows: the electrode active material, the conductive carbon black and the binder are dispersed in a solvent according to a certain proportion (for example, the positive electrode solvent is N-methyl pyrrolidone, the negative electrode solvent is water, and the solvents are polar solvents) to form slurry, and the slurry is coated on a metal foil and dried to obtain the electrode active material. However, since the conductive carbon black generally has a high specific surface area, secondary agglomeration is likely to occur between aggregates, which results in excessively high viscosity of a dispersion system and difficulty in processing, and simultaneously, the conductive performance of the product is not easily achieved.
In the prior art, the technology of regulating and controlling low-viscosity acetylene black by a cracking method is less, and Chinese patent CN 107820504A discloses that the material has low viscosity and low resistivity in a dispersion as shown by a relatively high compression OAN/OAN ratio. Such materials can be advantageously used in various applications, for example in the manufacture of lithium ion batteries or as conductive additives in polymer composites. But does not relate to how to realize the preparation of acetylene black with high conductivity and low viscosity through a cracking reaction process in industrial production.
Thus, there is a strong need for acetylene black with low viscosity as a conductive additive without losing high conductive properties to meet the needs of product processing.
Disclosure of Invention
In order to overcome the defects that acetylene black produced by the prior art has high viscosity and causes large processing difficulty in a polar dispersion system, the invention provides a preparation method of low-viscosity acetylene black.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of low-viscosity acetylene carbon black comprises the following steps: acetylene gas is added in batches, the acetylene gas is introduced into an air inlet at the top end of the cracking furnace for the first time, and then an air inlet is additionally arranged in the middle of a reaction zone of the acetylene carbon black cracking furnace to supplement the added acetylene gas.
Preferably, the position of the additional air inlet is 3/10-7/10 of the position of the reaction zone of the cracking furnace.
Preferably, the temperature of the cracking furnace is 1400-2000 ℃.
Preferably, the flow rate of the acetylene gas charged for the first time is 80-220 kg/h.
More preferably, the flow rate of the acetylene gas for the second charging is 30-200 kg/h.
Most preferably, the flow rate of the acetylene gas charged for the second time is 50-70 kg/h.
The method provided by the invention can promote the continuous growth of carbon black primary particles and control the size of a carbon black secondary structure, optimizes an acetylene cracking gas inlet scheme by combining proper gas inlet positions and proper flow rate control, adds an air inlet in the middle of a reaction area of an acetylene carbon black cracking furnace to supplement acetylene gas, promotes the continuous growth of the carbon black particles in the furnace, and regulates (reduces) the carbon black secondary structure by increasing the particle size of the carbon black primary particles, reducing the nano-interaction energy and van der Waals force agglomeration among the carbon black particles.
The viscosity of carbon black in a dispersion is mainly influenced by the secondary structure of carbon black. The secondary structure mainly refers to the degree of aggregation between carbon black aggregates due to van der waals force. The high secondary structure has more structural gaps and strong liquid absorption capacity, so that the free solvent in a dispersion system is reduced, the apparent solid content is increased, the viscosity of the system is increased, and the dispersion difficulty is increased. Therefore, low viscosity carbon blacks must have a low secondary structure.
The scheme of the invention achieves the purpose mainly because:
acetylene carbon black is generated by first charging acetylene for cracking, crystal seeds are provided for second charging acetylene for cracking, and a chemical reaction can be carried out by preferentially selecting a reaction path with small activation energy, so that the advantageous reaction is the continuous growth of original carbon black particles, the particle size of the carbon black primary particles is increased, the proper secondary gas charging flow rate can simultaneously assist in reducing the nano-interaction energy and van der Waals force agglomeration among the carbon black particles, and the two comprehensively reduce the secondary structure size of the carbon black.
More specifically, acetylene gas, when cracked, undergoes two stages of nucleation (formation of new carbon black particles) and growth, with competition between carbon black particle nucleation and particle growth. Carbon black particle nucleation requires a greater activation energy than does the continued growth of the carbon black particles. Therefore, when the middle part of the reaction zone of the acetylene carbon black cracking furnace is additionally provided with the air inlet for supplementing acetylene gas for the second time, the carbon precursor formed by the second cracking preferentially takes the carbon black particles generated by the first charging of acetylene for cracking as seed crystals and is carried out in the direction of continuous growth, so that the particle size of the carbon black particles is effectively increased. The reaction can be stably carried out at a proper flow rate, and finally, the size effect can be reduced based on the nanometer effect among large particles, so that the secondary agglomeration of carbon black particles is effectively inhibited, and the secondary structure of carbon black is reduced; when the conductive additive is used as a conductive additive component, the viscosity of the system can be effectively reduced, and the processability is improved.
The acetylene black cracking furnace is simply improved by adding the gas inlet, and the gas inlet is additionally arranged in the middle of the reaction zone of the acetylene black cracking furnace. Acetylene gas is added in batches for carrying out cracking reaction, firstly, the acetylene gas is introduced into an acetylene carbon black cracking furnace from a raw gas inlet at the top end, after the acetylene gas is cracked and nucleated to generate initial carbon particles, the gas inlet is additionally arranged from the middle part of a reaction area for supplementing the acetylene gas, so that the acetylene carbon black can continue to grow on the basis of keeping the original primary structure, and the secondary structure of the acetylene carbon black can be effectively controlled based on the size effect of nano particles. The acetylene black with low agglomeration performance is further discharged from the furnace bottom after low-temperature hydrogen-rich backflow tail gas in a cooling zone of the cracking furnace is subjected to flame-stopping cooling and temperature reduction. And further decoking, pulse bag filter separation, screw compressor compression and packaging to finally obtain the acetylene black product with low viscosity.
According to the invention, through a viscosity test, in a carbon black material dispersion system formed by N-methyl-2-pyrrolidone (NMP), the dispersion formed by the conductive carbon black material provided by the invention has lower viscosity and better processing performance. The above also applies to dispersions of carbon black materials or conductive compositions in other liquid systems, such as water or water-based solvent mixtures.
The acetylene black product obtained by the invention can be used as a conductive agent in electrochemical cells such as lithium ion batteries or fuel cells, and can be prepared into conductive polymers, conductive coatings and the like.
The acetylene black product obtained by the invention is especially suitable for: to dispersions comprising a liquid such as N-methyl-2-pyrrolidone (NMP), water or a water-based solvent mixture, and a carbon black material or conductive composition as defined herein.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the method utilizes a cracking method, acetylene gas is added in batches in the acetylene cracking process, reaction conditions are controlled, and the preparation of the low-viscosity acetylene black can be realized on the premise of not reducing the conductive performance of the acetylene black, so that the performance requirements of lithium battery assembly processing on the conductive carbon black are met. The invention has simple, safe and environment-friendly production process, does not need to replace the existing cracking furnace equipment, and improves the product performance and the enterprise economic benefit.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The device used by the invention can refer to CN111269590A, the cracking furnace is the same, and CN111269590A is added with an alcohol and ester substance air inlet and is used as an acetylene gas air inlet.
Acetylene gas is introduced into the acetylene carbon black cracking furnace from a raw gas inlet at the top end, and the acetylene gas is cracked at the upper end of a reaction zone of the cracking furnace to generate initial carbon particles; and an air inlet is additionally arranged in the middle of the reaction zone, acetylene gas is charged again, so that carbon black particles continue to grow, the acetylene carbon black particles further grow at the lower part of the reaction zone of the acetylene carbon black cracking furnace, and acetylene carbon black aggregates are discharged from the bottom of the furnace after being cooled and cooled by the low-temperature hydrogen-rich backflow tail gas flame-stopping in the cooling zone of the acetylene carbon black cracking furnace. Further decoking, pulse bag filter separation, screw compressor compression and packaging to obtain the final product.
Example 1
A preparation method of low-viscosity acetylene carbon black comprises the following steps:
firstly, acetylene gas is introduced into an air inlet at the top end of a cracking furnace, the flow rate of the introduced acetylene gas is 120kg/h, the reaction temperature in the cracking furnace is controlled to be 1800 ℃, and continuous reaction is carried out.
Then, an air inlet is additionally arranged in the middle of a reaction zone of the acetylene black cracking furnace to supplement and add acetylene gas, the flow rate of the charged acetylene gas is 60kg/h, and the reaction temperature in the cracking furnace is controlled to be 1800 ℃. The carbon black particles continue to grow, and the generated acetylene carbon black particles further grow at the lower part of the reaction zone of the cracking furnace; after the low-temperature hydrogen-rich backflow tail gas in the cooling zone of the acetylene black cracking furnace is subjected to flame-stopping cooling and temperature reduction, the tail gas is discharged from the furnace bottom. Further decoking, pulse bag filter separation, screw compressor compression and packaging to obtain the final product.
Example 2
A preparation method of low-viscosity acetylene carbon black comprises the following steps:
firstly, acetylene gas is introduced into an air inlet at the top end of a cracking furnace, the flow rate of the charged acetylene gas is 100kg/h, the reaction temperature in the cracking furnace is controlled to be 1600 ℃, and continuous reaction is carried out.
Then, an air inlet is additionally arranged in the middle of a reaction zone of the acetylene carbon black cracking furnace to supplement and add acetylene gas, the flow rate of the charged acetylene gas is 60kg/h, and the reaction temperature in the cracking furnace is controlled to be 1600 ℃. The carbon black particles continue to grow, and the generated acetylene carbon black particles further grow at the lower part of the reaction zone of the cracking furnace; after the low-temperature hydrogen-rich backflow tail gas in the cooling zone of the acetylene black cracking furnace is subjected to flame-stopping cooling and temperature reduction, the tail gas is discharged from the furnace bottom. Further decoking, pulse bag filter separation, screw compressor compression and packaging to obtain the final product.
Comparative example 1
A preparation method of low-viscosity acetylene carbon black comprises the steps of introducing acetylene gas into an air inlet at the top end of a cracking furnace without batch charging, wherein the flow rate of the acetylene gas is 160 kg/h. The reaction temperature in the cracking furnace was controlled to 1800 ℃. After the reaction is collided at the middle part, the carbon black particles continue to grow, and the generated acetylene carbon black particles further grow at the lower part of the reaction zone of the cracking furnace; after the low-temperature hydrogen-rich backflow tail gas in the cooling zone of the acetylene black cracking furnace is subjected to flame-stopping cooling and temperature reduction, the tail gas is discharged from the furnace bottom. Further decoking, pulse bag filter separation, screw compressor compression and packaging to obtain the final product.
Comparative example 2
A preparation method of low-viscosity acetylene carbon black comprises the following steps:
firstly, acetylene gas is introduced into an air inlet at the top end of a cracking furnace, the flow rate of the charged acetylene gas is 80kg/h, the reaction temperature in the cracking furnace is controlled to be 1600 ℃, and continuous reaction is carried out.
Then, an air inlet is additionally arranged in the middle of a reaction zone of the acetylene carbon black cracking furnace to supplement and add acetylene gas, the flow rate of the charged acetylene gas is 100kg/h, and the reaction temperature in the cracking furnace is controlled to be 1600 ℃. The carbon black particles continue to grow, and the generated acetylene carbon black particles further grow at the lower part of the reaction zone of the cracking furnace; after the low-temperature hydrogen-rich backflow tail gas in the cooling zone of the acetylene black cracking furnace is subjected to flame-stopping cooling and temperature reduction, the tail gas is discharged from the furnace bottom. Further decoking, pulse bag filter separation, screw compressor compression and packaging to obtain the final product.
The performance test method comprises the following steps:
firstly, viscosity testing:
5 wt% of each of the acetylene black products of examples 1 to 2 and comparative example 1 was dispersed in N-methyl-2-pyrrolidone to prepare a slurry, and the slurry was measured at 13 seconds using a rheometer-1The rheology of the dispersion was measured at shear rate and expressed in mpa.s, the test conditions were room temperature environment and the results are shown in table 1.
TABLE 1
| Sample (I) | Viscosity (mPa.s) |
| Example 1 | 1270 |
| Example 2 | 1189 |
| Comparative example 1 | 2870 |
| Comparative example 2 | 2200 |
The viscosity test directly illustrates the processability of acetylene black in liquid systems, and as can be seen from table 1, examples 1 and 2 show a greater degree of viscosity reduction than comparative examples 1 and 2, indicating that the magnitude of the flow rate and whether or not the batch feed has a greater effect on the viscosity properties of the product. Comparative example 1, which did not have a batch feed, produced acetylene black that had not undergone a significant improvement in viscosity during processing as a dispersion; in contrast, in comparative example 2, the flow rate of the second feeding is high, so that the generation of the primary structure and the secondary structure of the acetylene black is influenced, the secondary structure is increased, and the viscosity of the product is increased. In the carbon black material dispersion system formed by N-methyl-2-pyrrolidone (NMP), the viscosity of the material prepared in the example is lower, and the processing performance is better. The above also applies to dispersions of carbon black materials or conductive compositions in other liquid systems, such as water or water-based solvent mixtures.
Secondly, the resistivity of the sample is tested by using a resistivity test and is measured by referring to GB/T3781.9-2019, and the result is shown in Table 2.
TABLE 2 conductivity test results
| Examples | Conductivity (omega. m) |
| Example 1 | 1.3 |
| Example 2 | 1.2 |
| Comparative example 1 | 2.6 |
| Comparative example 2 | 2.3 |
Resistivity tests can show that the acetylene black prepared by the method has good conductivity, compared with products of comparative examples, the conductivity of the acetylene black is improved, and table 1 shows that the acetylene black can obtain better conductivity on the premise of not influencing the processing performance.
By combining the viscosity test results and the resistivity test results in tables 1 and 2, the method utilizes a cracking method, acetylene gas is added in batches in the acetylene cracking process, reaction conditions are controlled, the preparation of the conductive carbon black with low viscosity can be realized on the premise of not reducing the conductive performance of the acetylene carbon black, and the method is particularly suitable for a carbon black material dispersion system containing a mixture of N-methyl-2-pyrrolidone (NMP) and water or a water-based solvent, so as to meet the performance requirements of the conductive carbon black in the lithium battery assembly processing.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (9)
1. A preparation method of low-viscosity acetylene black is characterized in that acetylene gas is added in batches, the acetylene gas is introduced into an air inlet at the top end of a cracking furnace for the first time, and then an air inlet is additionally arranged in the middle of a reaction zone of an acetylene black cracking furnace for supplementing the acetylene gas.
2. The method for preparing low-viscosity acetylene black according to claim 1, wherein the flow rate of the acetylene gas to be charged for the first time is 80 to 220 kg/h.
3. The method for preparing low-viscosity acetylene black according to claim 1, wherein the flow rate of the acetylene gas to be charged for the second time is 30 to 200 kg/h.
4. The method for preparing low-viscosity acetylene black according to claim 3, wherein the flow rate of the acetylene gas to be charged for the second time is 50 to 70 kg/h.
5. The method for preparing low-viscosity acetylene black according to claim 1, wherein the temperature of the cracking furnace is 1400 to 2000 ℃.
6. The method for preparing acetylene black with low viscosity according to claim 1, wherein the position of the additional air inlet is 3/10 to 7/10 of the reaction zone of the cracking furnace.
7. Acetylene black produced by the process for producing low viscosity acetylene black of claim 1.
8. Use of the acetylene black of claim 7 as a conductive agent for electrochemical cells.
9. Use of the acetylene black of claim 7 in a carbon black material dispersion system comprised of N-methyl-2-pyrrolidone.
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| FR1462071A (en) * | 1964-12-30 | 1966-02-25 | Cabot Corp | Conductive carbon blacks and process for making them |
| US4013759A (en) * | 1973-05-15 | 1977-03-22 | Societe Anonyme: Produits Chimiques Ugine Kuhlmann | Acetylene-like black and process |
| US5264199A (en) * | 1989-03-04 | 1993-11-23 | Mitsubishi Kasei Corporation | Process for producing carbon black |
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