CN113789068A - High-temperature ultrahigh-conductivity carbon black reaction furnace and method for producing ultrahigh-conductivity carbon black by using raffinate oil of high-temperature ultrahigh-conductivity carbon black reaction furnace - Google Patents
High-temperature ultrahigh-conductivity carbon black reaction furnace and method for producing ultrahigh-conductivity carbon black by using raffinate oil of high-temperature ultrahigh-conductivity carbon black reaction furnace Download PDFInfo
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Abstract
The invention provides a high-temperature ultrahigh-conductivity carbon black reaction furnace and a method for producing ultrahigh-conductivity carbon black by raffinate oil thereof, wherein the high-temperature ultrahigh-conductivity carbon black reaction furnace sequentially comprises a combustion section, a throat, a reaction section and a cooling section; one end of the combustion section is provided with an air inlet and a fuel gas inlet, the fuel gas inlet and the throat pipe are coaxially arranged, and the included angle alpha of the central axes of the air inlet and the fuel gas inlet is 45 degrees; the choke is provided with a raw oil inlet and a raw material gas inlet; a plasma heating device is arranged in the reaction section, a furnace body shell of the reaction furnace is made of nickel-based high-temperature alloy, and the lining is made of high-purity corundum bricks; the end of the cooling section is provided with a product outlet. The furnace body is made of nickel-based high-temperature alloy, and the plasma heating device is arranged at the reaction section, so that the temperature of the reaction section in the reaction furnace can be increased and kept at 2080 ℃ in 1980 so as to lead the quasi-graphite microcrystal structure of the particles to tend to be orderly arranged towards graphite crystals, and further improve the conductivity of the conductive carbon black.
Description
Technical Field
The invention belongs to the technical field of coal chemical production, and particularly relates to a high-temperature ultrahigh-conductivity carbon black reaction furnace and a method for producing ultrahigh-conductivity carbon black by using raffinate oil of the high-temperature ultrahigh-conductivity carbon black reaction furnace.
Background
The ultrahigh conductive carbon black is an indispensable additive in the lithium ion battery industry, and the additive is added into the positive electrode, the negative electrode and the conductive liquid of the lithium ion battery, so that the conductivity of the lithium ion battery can be greatly improved, and the performance of the lithium ion battery is improved. The ultrahigh conductive carbon black applied to the lithium ion battery at present is mainly prepared by cracking a complex mixture with high aromaticity such as coal tar or anthracene oil and the like serving as a raw material in a carbon black furnace at high temperature.
The furnace-method ultra-high conductive carbon black has small particle size and chain structure, and macroscopically shows high specific surface area and high dibutyl phthalate (DBP) absorption value, which is the main reason of high conductive performance of the carbon black. However, the raw materials of the common furnace carbon black are complex mixtures, so that the carbon black has more impurities and has larger influence on the performance of the lithium ion battery; meanwhile, the furnace temperature of the existing carbon black reaction furnace can not reach the crystallization temperature, so that the generated ultrahigh conductive carbon black has poor conductivity.
Disclosure of Invention
The first purpose of the invention is to provide a high-temperature and ultrahigh-conductivity carbon black reaction furnace, wherein a furnace body is made of high-nickel high-temperature alloy, and a plasma heating device is arranged in a reaction section to improve the temperature of the reaction section in the reaction furnace and keep the temperature at 1980-2080 ℃, so that the quasi-graphite microcrystal structure of particles tends to be orderly arranged towards graphite crystals, and the conductivity of the conductive carbon black is further improved; set up the cooling zone and adopt the mode of quench can fix the carbon black rapidly be the membrane structure, make its chain structure fixed rapidly simultaneously, keep shorter branched chain formula structure, keep suitable specific surface area and improve electric conductivity simultaneously, in addition the quench in-process, reaction temperature reduces makes graphite structure surface and oxygen's reaction reduce, and surface oxygen content is good, and then electric conductivity is good.
In order to achieve the purpose, the invention adopts the technical scheme that: a high-temperature ultrahigh-conductivity carbon black reaction furnace sequentially comprises a combustion section, a throat pipe, a reaction section and a cooling section; an air inlet and a fuel gas inlet are formed in one end, far away from the throat, of the combustion section, the fuel gas inlet and the throat are coaxially arranged, and an included angle alpha between the air inlet and the fuel gas inlet is 45 degrees; the choke is provided with a raw oil inlet and a raw material gas inlet; a plasma heating device is arranged in the reaction section, a furnace body shell of the reaction furnace is made of nickel-based high-temperature alloy, and an inner lining is made of high-purity corundum bricks; and a product outlet is arranged at the end part of the cooling section.
Furthermore, six cooling manifolds are arranged in the cooling section in parallel and are uniformly distributed; and the outer wall of each cooling manifold is provided with a quenching boiler heat exchanger, and each quenching boiler heat exchanger is connected with a quenching boiler.
Further, the air inlet is provided with a plurality of, and is a plurality of air inlet evenly sets up along the axis circumference of gas inlet.
Further, the end part of the air inlet is an inclined plane, the end b of the inclined plane is far away from the fuel gas inlet, and the end a of the inclined plane is close to the fuel gas inlet.
Furthermore, two raw oil inlets are arranged, one raw material gas inlet is arranged, and the raw oil inlets and the raw material gas inlets are uniformly distributed along the throat; the end part of the raw oil inlet is an inclined plane, and the inclined plane is arranged towards the combustion section.
Furthermore, a necking section is arranged on the throat pipe and is arranged between the raw oil inlet and the reaction section.
The second purpose of the invention is to provide a method for producing the ultrahigh conductive carbon black by using the raffinate oil as a carbon source, wherein the raffinate oil is a byproduct of natural gas exploitation, is low in price, mainly comprises C6-C8 alkane, and has few impurities, so that the purity of the product is improved; acetylene is used as a heating agent and an additive, and a plasma heating device is added in a reaction section, so that the furnace temperature is increased, and the graphitization degree of the product is improved; acetylene is added in the reaction section, so that the reaction rate is improved, the three-dimensional chain structure of the product is enhanced, common vacuoles in a furnace-method graphite structure are filled, and the conductivity is improved.
The technical scheme adopted by the invention is as follows: a method for producing ultrahigh conductive carbon black by raffinate oil comprises the following steps:
1) preparing raw oil by raffinate oil processing: pumping the raffinate oil into an air flotation separation device through an oil pump, adding a water absorbent, wherein the water absorbent is solid potassium carbonate, standing after air flotation stirring, and then extracting supernatant liquid to obtain raw oil through a filter press;
by the treatment, high-purity raw oil with the water content of less than or equal to 0.05 percent and the solid content of less than or equal to 0.001 percent can be obtained and poured into an oil storage tank for storage; the step is used for removing impurities from the raffinate oil to obtain high-purity raw oil;
2) the mixed gas is combusted in the combustion section: injecting mixed fuel gas into a combustion section from a fuel gas inlet of the high-temperature ultrahigh conductive carbon black reaction furnace through an air pump at the flow rate of 300-; the mixed fuel gas is obtained by mixing acetylene and methane in any volume ratio through a gas mixing valve; the volume ratio of the air introduced into the combustion section to the mixed gas is (10-12): 1.
in the step, mixed gas and air are introduced to be used for combustion in the combustion section, so that the furnace temperature is kept at a higher temperature, high-pressure gas is conveniently formed, raw oil is conveniently atomized when the throat is introduced, and the raw oil and acetylene gas are uniformly mixed.
3) Mixing and atomizing raw oil and acetylene gas: heating the raw oil obtained in the step 1) to 260-300 ℃ through a preheater, spraying acetylene gas into the throat from a raw oil inlet of the high-temperature ultrahigh conductive carbon black reaction furnace at a flow rate of 900-1800kg/h and a pressure of 1.2-1.5MPa, spraying the acetylene gas into the throat from a raw material gas inlet of the high-temperature ultrahigh conductive carbon black reaction furnace at a flow rate of 20-40kg/h and a pressure of 1.2-1.5MPa, and allowing the raw oil and the acetylene gas to enter a reaction section after being fully and uniformly mixed at the throat;
in the step, the raw oil and the acetylene gas are atomized under the impact of the high-temperature gas of the combustion section, so that the raw oil and the acetylene are fully mixed, the raw oil is atomized by the high-pressure high-temperature gas, and the raw oil passes through the necking section, so that the inner diameter is reduced, and the turbulent flow is improved, so that the raw oil and the acetylene gas are uniformly mixed.
4) Cracking raffinate oil to generate ultrahigh conductive carbon black: the plasma heating device is operated to keep the furnace temperature of the reaction section at 1980-2080 ℃; the raw oil is decomposed in the reaction section to generate carbon black;
in the step, the plasma heating device heats the reaction section, so that the furnace temperature of the reaction section is kept within the range of 1980-2080 ℃, the crystallization degree of graphite is further improved, the specific surface area of the graphite structure is easily overlarge due to overhigh temperature of the reaction furnace, acetylene is introduced into the reaction section and enters the vacuoles in the graphite structure, the vacuoles are filled after pyrolysis, the vacuole rate is reduced, and the problem that the specific surface area is overlarge due to the fact that the vacuoles are easily generated due to high-temperature crystallization is solved. Wherein, the cracking formula of the raw oil is as follows: c(6-8)H(12-16)+O2→C+H2O。
5) Quenching and cooling the carbon black: the carbon black enters the cooling section from the reaction section and is rapidly cooled to 260-280 ℃ at the speed of 600-1200 ℃/s to obtain the ultrahigh conductive carbon black with a short branched chain structure and a stable structure, and then the ultrahigh conductive carbon black is discharged from a product outlet and is continuously cooled to 50-60 ℃ for collection.
In the step, the graphite structure of the carbon black can be rapidly fixed by adopting a rapid cooling mode, meanwhile, the chain structure of the carbon black is rapidly fixed, a short branched chain structure is kept, the conductivity is improved, and meanwhile, a good specific surface area is kept.
The ultrahigh conductive carbon black prepared by the method for producing the ultrahigh conductive carbon black by the raffinate oil has the particle size of 70-90nm and the BET surface area of 50-90m2/g,DBP oil absorption value is 4.6ml/g-4.8ml/g, pH is 7.9-8.2, and resistivity is 0.83-0.85 omega.m.
Many furnace-process carbon blacks use petroleum refining tailings such as tar, so that the finally prepared carbon black has too high content of metal, particularly iron, and the performance of the lithium ion battery is affected; the invention adopts raffinate oil as a carbon source to carry out cracking reaction to prepare the ultrahigh conductive carbon black, the metal content in the ultrahigh conductive carbon black is extremely little and almost nonexistent, so that the ultrahigh conductive performance can be kept well. When in use, the performance of the lithium ion battery is not affected.
The invention has the advantages and positive effects that:
1. according to the high-temperature ultrahigh-conductivity carbon black reaction furnace, the furnace body is made of high-nickel high-temperature alloy, and the plasma heating device is arranged in the reaction section, so that the temperature of the reaction section in the reaction furnace can be increased and kept at 2080 ℃ in 1980), and therefore the quasi-graphite microcrystal structures of the particles tend to be orderly arranged towards graphite crystals, and the conductivity of the conductive carbon black is improved; the cooling section is arranged, the carbon black can be rapidly fixed by adopting a quenching mode, the chain structure of the cooling section is rapidly fixed, the short branched chain structure is kept, the appropriate specific surface area is kept, the conductivity is improved, in addition, the reaction temperature is reduced in the quenching process, so that the reaction between the surface of the cooling section and oxygen is reduced, the oxygen content of the surface is good, and the conductivity is good.
2. The method for producing the ultrahigh conductive carbon black by using the raffinate oil uses the raffinate oil as a carbon source, the raffinate oil is a byproduct of natural gas exploitation, is low in price and mainly comprises C6-C8 alkane, and impurities are few, so that the purity of the product is improved; acetylene is used as a heating agent and an additive, and a plasma heating device is added in a reaction section, so that the furnace temperature is increased, and the graphitization degree of the product is improved; acetylene is added in the reaction section, so that the reaction rate is improved, the three-dimensional chain structure of the product is enhanced, common vacuoles in a furnace-method graphite structure are filled, and the conductivity is improved.
3. The ultrahigh conductive carbon black prepared by the method for producing the ultrahigh conductive carbon black by using the raffinate oil has a high branched chain structure, strong conductive performance and low cost.
Drawings
FIG. 1 is a schematic structural view of a high-temperature ultra-high conductivity carbon black reactor according to the present invention;
FIG. 2 is a schematic view of the structure of the combustion section of a high temperature ultra-high conductivity carbon black reactor of the present invention;
FIG. 3 is a cross-sectional view A-A of FIG. 2;
FIG. 4 is a schematic structural view of a throat in a high temperature ultra-high conductivity carbon black reaction furnace according to the present invention;
FIG. 5 is an electron microscope image of the ultra-high conductive carbon black prepared by the present invention;
FIG. 6 is an electron microscope image of a common commercial ultra-high conductive carbon black;
in the figure:
1-air inlet, 101-b end, 102-a end;
2-a gas inlet;
3-raw oil inlet;
4-plasma heating means;
5-a cooling manifold;
6-quenching boiler heat exchanger;
7-a combustion section;
8-throat pipe, 81-necking section;
9-a reaction section;
10-a cooling section;
11-product outlet.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings.
Example 1:
referring to fig. 1 to 4, the present embodiment provides a high-temperature ultrahigh-conductivity carbon black reacting furnace, which sequentially comprises a combustion section 7, a throat 8, a reaction section 9 and a cooling section 10; an air inlet 1 and a fuel gas inlet 2 are arranged at one end of the combustion section 7, which is far away from the throat 8, the fuel gas inlet 2 and the throat 8 are coaxially arranged, and the included angle alpha of the central axes of the air inlet 1 and the fuel gas inlet 2 is 45 degrees; the throat 8 is provided with a raw oil inlet 3 and a raw material gas inlet; a plasma heating device 4 is arranged in the reaction section 9, the furnace body shell of the reaction furnace is made of nickel-based high-temperature alloy, and the lining is made of high-purity corundum bricks; in the present embodiment, the nickel-base superalloy is of the type GH3028, and the end of the cooling section 10 is provided with a product outlet 11. The combustion section 7 is used for combusting acetylene and methane, the throat 8 is used for mixing and atomizing raw oil and acetylene, the reaction section 9 is used for cracking the raw oil to produce carbon black, and the cooling section 10 is used for rapidly cooling the carbon black so as to fix the crystallization structure of the carbon black. The plasma heating device 4 is arranged in the reaction section 9 to heat the reaction section, so that the furnace temperature of the reaction section is kept at 2080 ℃ in 1980 and 2080 ℃, and further the graphite crystallization degree is improved.
In the present embodiment, six cooling manifolds 5 are arranged in parallel in the cooling section 10, and the six cooling manifolds 5 are uniformly distributed; a quenching boiler heat exchanger 6 is arranged on the outer wall of each cooling manifold 5, and each quenching boiler heat exchanger 6 is connected with a quenching boiler.
In the present embodiment, the air inlet 1 is provided in plurality, and the plurality of air inlets 1 are uniformly arranged along the circumference of the axis of the gas inlet 2. In this embodiment, the number of the air inlets 1 is specifically 4.
In this embodiment, the end of the air inlet 1 is a bevel, the b-end 101 of the bevel being located away from the gas inlet 2, and the a-end 102 of the bevel being located adjacent to the gas inlet 2. This design is convenient for carry out intensive mixing with gas mixture and air, especially still sets up at 45, is convenient for mix the back and burns.
In this embodiment, two raw oil inlets 3 are provided, one raw material gas inlet is provided, and the raw oil inlets and the raw material gas inlets are uniformly distributed along the throat 8; the end of the raw oil inlet 3 is an inclined plane which is arranged towards the combustion section 7.
In this embodiment, the throat 8 is provided with a neck section 81, and the neck section 81 is provided between the feedstock inlet 3 and the reaction section 9. The inner diameter of the neck section 81 is small, so that the turbulent speed of gas flow can be accelerated, and acetylene and raw oil are fully mixed and atomized.
According to the high-temperature ultrahigh-conductivity carbon black reaction furnace, the furnace body is made of high-nickel high-temperature alloy, and the plasma heating device is arranged in the reaction section, so that the temperature of the reaction section in the reaction furnace can be increased and kept at 2080 ℃ in 1980), and therefore the quasi-graphite microcrystal structures of the particles tend to be orderly arranged towards graphite crystals, and the conductivity of the conductive carbon black is improved; set up the graphite structure that the cooling zone adopted the mode of quench can fix carbon black rapidly, make its chain structure fixed rapidly simultaneously, keep shorter branched chain formula structure, keep suitable specific surface area and improve electric conductivity simultaneously, in addition the quench in-process, reaction temperature reduces and makes the reaction of graphite structure surface and oxygen reduce, and surface oxygen content is good, and then electric conductivity is good.
Example 2:
a method for producing ultrahigh conductive carbon black by raffinate oil comprises the following steps:
1) preparing raw oil by raffinate oil processing: pumping the raffinate oil into an air flotation separation device through an oil pump, adding a water absorbent, wherein the water absorbent is solid potassium carbonate, carrying out air flotation stirring for 2 hours, standing and storing for 6 hours, extracting supernatant, removing residual impurities through a filter press, and thus obtaining high-purity raw oil with the water content of 0.05% and the solid content of 0.001%, and filling the high-purity raw oil into an oil storage tank for storage;
2) the mixed gas is combusted in the combustion section 7: injecting mixed fuel gas into a combustion section 7 from a fuel gas inlet 2 through an air pump at the flow rate of 300kg/h and the pressure of 120KPa, preheating air to 900 ℃, injecting the air into the combustion section from an air inlet 1 through the air pump at the pressure of 120KPa, combusting in the combustion section and keeping the furnace temperature at 1560 ℃; wherein, the mixed fuel gas is acetylene and methane, and the ratio of 3.2: the volume ratio of 1 is obtained through a gas mixing valve; the volume ratio of the air introduced into the combustion section 7 to the mixed gas is 10: 1;
3) mixing and atomizing raw oil and acetylene gas: heating the raw oil obtained in the step 1) to 260 ℃ through a preheater, spraying the raw oil into a throat pipe 8 from a raw oil inlet 3 at a flow rate of 900kg/h and a pressure of 1.2MPa, spraying acetylene gas into the throat pipe 8 from a raw material gas inlet at a flow rate of 20kg/h and a pressure of 1.2MPa, atomizing the raw oil and the acetylene gas under the impact of high-temperature gas of a combustion section, and simultaneously fully and uniformly mixing the raw oil and the acetylene gas at a necking section 81 to enter a reaction section 9;
4) cracking raffinate oil to generate carbon black: the plasma heating device 4 is operated to keep the furnace temperature of the reaction section 9 at 1980 ℃; the raw oil is decomposed in the reaction section 9 to generate carbon black;
5) quenching and cooling the carbon black: the carbon black enters the cooling section 10 from the reaction section 9 and is rapidly cooled to 280 ℃ at the speed of 600 ℃/s to form the ultrahigh conductive carbon black with stable structure, and then the ultrahigh conductive carbon black is discharged from the product outlet 11 and is continuously cooled to 60 ℃ for collection.
The preparation method of the embodiment is used for preparing the ultra-high conductive carbon black, and an electron microscope scanning image of the prepared ultra-high conductive carbon black is shown in fig. 5.
Example 3:
a method for producing ultrahigh conductive carbon black by raffinate oil comprises the following steps:
1) preparing raw oil by raffinate oil processing: pumping the raffinate oil into an air flotation separation device through an oil pump, adding a water absorbent, wherein the water absorbent is solid potassium carbonate, carrying out air flotation stirring for 2 hours, standing and storing for 10 hours, extracting supernatant, removing residual impurities through a filter press, and thus obtaining high-purity raw oil with the water content of 0.04% and the solid content of 0.001%, and filling the high-purity raw oil into an oil storage tank for storage;
2) the mixed gas is combusted in the combustion section 7: spraying mixed fuel gas into a combustion section 7 from a fuel gas inlet 2 through an air pump at the flow rate of 350kg/h and the pressure of 125KPa, preheating air to 935 ℃, spraying the air into the combustion section from an air inlet 1 through the air pump at the pressure of 125KPa, and combusting in the combustion section while keeping the furnace temperature at 1585 ℃; wherein, the mixed fuel gas is acetylene and methane, and the ratio of 4.2: the volume ratio of 1 is obtained through a gas mixing valve; the volume ratio of the air introduced into the combustion section 7 to the mixed gas is 11: 1;
3) mixing and atomizing raw oil and acetylene gas: heating the raw oil obtained in the step 1) to 280 ℃ through a preheater, spraying the raw oil into a throat pipe 8 from a raw oil inlet 3 at a flow rate of 1200kg/h and a pressure of 1.4MPa, spraying acetylene gas into the throat pipe 8 from a raw material gas inlet at a flow rate of 30kg/h and a pressure of 1.4MPa, atomizing the raw oil and the acetylene gas under the impact of high-temperature gas of a combustion section, and simultaneously fully and uniformly mixing the raw oil and the acetylene gas at a necking section 81 to enter a reaction section 9;
4) cracking raffinate oil to generate carbon black: the plasma heating device 4 is operated to keep the furnace temperature of the reaction section 9 at 2030 ℃; the raw oil is decomposed in the reaction section 9 to generate carbon black;
5) quenching and cooling the carbon black: the carbon black enters the cooling section 10 from the reaction section 9, the cutter is rapidly cooled at 270 ℃ at the speed of 900 ℃/s to form the ultrahigh conductive carbon black with a stable structure, and then the ultrahigh conductive carbon black is discharged from the product outlet 11 and is continuously cooled to 55 ℃ for collection.
Example 4:
a method for producing ultrahigh conductive carbon black by raffinate oil comprises the following steps:
1) preparing raw oil by raffinate oil processing: pumping the raffinate oil into an air flotation separation device through an oil pump, adding a water absorbent, wherein the water absorbent is solid potassium carbonate, carrying out air flotation stirring for 2 hours, standing and storing for 12 hours, extracting supernatant, removing residual impurities through a filter press, and thus obtaining high-purity raw oil with the water content of 0.05% and the solid content of 0.001%, and filling the high-purity raw oil into an oil storage tank for storage;
2) the mixed gas is combusted in the combustion section 7: injecting mixed fuel gas into a combustion section 7 from a fuel gas inlet 2 through an air pump at the flow rate of 400kg/h and the pressure of 130KPa, preheating air to 960 ℃, injecting the air into the combustion section from an air inlet 1 through the air pump at the pressure of 130KPa, and combusting in the combustion section and keeping the furnace temperature at 1610 ℃; wherein, the mixed fuel gas is acetylene and methane, and the ratio of 4.6: the volume ratio of 1 is obtained through a gas mixing valve; the volume ratio of the air introduced into the combustion section 7 to the mixed gas is 12: 1;
3) mixing and atomizing raw oil and acetylene gas: heating the raw oil obtained in the step 1) to 300 ℃ through a preheater, spraying the raw oil into a throat pipe 8 from a raw oil inlet 3 at a flow rate of 1800kg/h and a pressure of 1.5MPa, spraying acetylene gas into the throat pipe 8 from a raw material gas inlet at a flow rate of 40kg/h and a pressure of 1.5MPa, atomizing the raw oil and the acetylene gas under the impact of high-temperature gas of a combustion section, and simultaneously fully and uniformly mixing the raw oil and the acetylene gas at a necking section 81 to enter a reaction section 9;
4) cracking raffinate oil to generate carbon black: the plasma heating device 4 is operated to keep the furnace temperature of the reaction section 9 at 2080 ℃; the raw oil is decomposed in the reaction section 9 to generate carbon black;
5) quenching and cooling the carbon black: the carbon black enters the cooling section 10 from the reaction section 9 and is rapidly cooled to 280 ℃ at the speed of 1200 ℃/s to form the ultrahigh conductive carbon black with stable structure, and then the ultrahigh conductive carbon black is discharged from the product outlet 11 and is continuously cooled to 50 ℃ for collection.
Comparative example 1:
the preparation method of the comparative example is the same as that of example 2, except that acetylene gas is not introduced into the throat 8 and only raw oil is introduced during the preparation process.
Comparative example 2:
the conductive carbon black sold in the market is Tianjin Xinglogtai ultra-high conductive carbon black # 5. The scanning electron microscope image of the commercially available highly conductive carbon black is shown in FIG. 6.
Experimental example 1:
the conductive carbon blacks prepared in examples 2 to 4 and comparative example 1 and the commercially available conductive carbon black selected in comparative example 2 were respectively subjected to performance tests, and the test results are shown in table 1:
wherein, the BET surface area is detected according to GB/T10722-2014;
the DBP oil absorption value is detected according to GB/T3780.2-2017;
the detection of the PH value is based on GB/T3780.7-2016;
the detection of the resistivity is based on GB/T245255-2018.
TABLE 1 results of testing the properties of conductive carbon blacks
Item | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
Particle size (nm) | 90 | 72 | 70 | 89 | 165 |
BET surface area ( |
76 | 89 | 50 | 205 | 216 |
DBP oil absorption number (ml/g) | 4.65 | 4.69 | 4.72 | 4.95 | 4.82 |
PH | 7.9 | 8.0 | 8.2 | 8.2 | 8.1 |
Resistivity (omega. m) | 0.85 | 0.84 | 0.85 | 1.45 | 1.12 |
From the experimental data of table 1, it can be seen that:
the ultrahigh conductive carbon black produced by using the ultrahigh conductive carbon black reaction furnace and the method for producing the ultrahigh conductive carbon black by using the raffinate oil has the advantages of low resistivity, good conductive performance, more branched chains, uniform particle size, moderate BET surface area and good product performance.
Compare fig. 5 and fig. 6:
as can be seen from FIG. 5, the highly conductive carbon black prepared by the present invention has uniform particle size, diameter of about 100 nm, and is branched, which is mainly because the temperature is rapidly reduced to 260-280 ℃ within 1.5s-3s in the cooling section, the temperature reduction speed is fast, and the particles are cooled without agglomeration after crystallization to form a branched chain, so the conductivity is good.
As can be seen from FIG. 6, the commercially available carbon black has the advantages of obvious disordered agglomeration, inconsistent particle size, diameter distribution between 200 and 100 nanometers, and obviously poorer electrical conductivity compared with the carbon black prepared by the invention.
Experimental example 2:
the experimental example is used for examining the influence of adding raw oil at different flow rates on the product performance, wherein the preparation method and parameters in the experimental example are the same as those in example 2, and only the addition flow rate of the raw oil is changed; the test results are shown in table 2:
TABLE 2 flow rate test results of raw oil
Item | Raw oil flow rate (kg/h) | Particle size (nm) | BET surface area ( |
DBP oil absorption number (ml/g) | PH | Resistivity (omega. m) |
Example 2 | 900 | 90 | 76 | 4.65 | 7.9 | 0.85 |
Example 5 | 800 | 250 | 350 | 5.69 | 8.0 | 2.56 |
Example 6 | 1200 | 82 | 80 | 4.75 | 7.8 | 0.84 |
Example 7 | 1500 | 80 | 62 | 4.69 | 7.9 | 0.82 |
Example 8 | 1800 | 90 | 53 | 4.72 | 8.0 | 0.84 |
Example 9 | 1900 | 150 | 30 | 5.65 | 7.9 | 1.95 |
Example 10 | 2000 | 142 | 28 | 5.48 | 7.8 | 2.63 |
From the experimental data of table 2, it can be seen that:
when the flow rate of the raw oil is 900-1800kg/h, the generated ultrahigh conductive carbon black can be ensured to have good performance, low resistivity and good conductivity.
When the flow rate of the raw oil is too high, the reaction is insufficient, the particle size is increased, branched chains are reduced, the specific surface area is reduced, and the conductivity is poor;
when the flow rate of the raw oil is too small, the specific surface area of the generated conductive carbon black is too large, a branched chain structure is difficult to form, the resistivity is increased, the conductivity is poor, and the cost is increased.
Experimental example 3:
the experimental example is used for examining the influence of adding acetylene gas at different flow rates on the product performance, wherein the preparation method and parameters in the experimental example are the same as those in example 2, and only the adding flow rate of the acetylene gas at the throat is changed; the test results are shown in table 3:
TABLE 3 experimental results of acetylene gas flow rate
Item | Acetylene gas flow rate (kg/h) | Particle size (nm) | BET surface area ( |
DBP oil absorption number (ml/g) | PH | Resistivity (omega. m) |
Example 2 | 20 | 90 | 76 | 4.65 | 7.9 | 0.85 |
Example 11 | 10 | 120 | 196 | 4.92 | 7.8 | 2.65 |
Example 12 | 15 | 112 | 126 | 4.86 | 7.9 | 1.92 |
Example 13 | 30 | 86 | 75 | 4.64 | 7.6 | 0.84 |
Example 14 | 40 | 84 | 72 | 4.72 | 7.8 | 0.85 |
Example 15 | 45 | 75 | 68 | 4.82 | 8.0 | 1.24 |
Example 16 | 50 | 62 | 156 | 4.95 | 7.9 | 2.62 |
From the experimental data in table 3, it can be seen that when the acetylene gas introduction rate affects the BET surface area of the ultra-high conductive carbon black, and when the acetylene introduction rate is too low, the BET surface area of the final product is too large, which does not meet the specification and cannot be used; when the introduction rate of the acetylene is 20-40kg/h, the BET surface area of the product can be well ensured to meet the national standard. In addition, when the flow rate of acetylene is too high, branched chains are reduced, single particles are increased, the particle size is reduced, the specific surface area is large, the resistivity is increased, and the conductivity is poor.
Experimental example 4:
the experimental example is used for examining the influence of different cooling modes on the product performance when the ultrahigh conductive carbon black is prepared, wherein the preparation method and parameters in the experimental example are the same as those in the example 2, and the difference is that only the cooling rate of the cooling section in the step 5) is changed (namely the cooling mode is changed by changing the cooling time through changing the cooling rate); the results of the experiment are shown in table 4:
TABLE 4 results of different cooling modes
Item | Cooling Rate (. degree. C/s) | Particle size (nm) | BET surface area ( |
DBP oil absorption number (ml/g) | PH | Resistivity (omega. m) |
Example 2 | 600 | 90 | 76 | 4.65 | 7.9 | 0.85 |
Example 17 | 100 | 139 | 40 | 4.40 | 7.9 | 3.69 |
Example 18 | 300 | 124 | 43 | 4.56 | 8.0 | 2.65 |
Example 19 | 500 | 106 | 49 | 4.55 | 7.9 | 1.34 |
Example 20 | 800 | 85 | 69 | 4.68 | 7.8 | 0.85 |
Example 21 | 1000 | 79 | 72 | 4.65 | 7.9 | 0.84 |
Example 22 | 1200 | 88 | 80 | 4.72 | 8.0 | 0.84 |
Example 23 | 1300 | 88 | 79 | 4.69 | 8.0 | 0.84 |
From the experimental data of table 4, it can be seen that:
when the cooling rate is kept at 600-.
When the cooling rate is greater than 1200 ℃/s, the performance of the prepared ultrahigh conductive carbon black and the performance of 600-1200 ℃/s are not obviously increased, so that the better performance of the product can be ensured when the cooling rate is greater than or equal to 600 ℃/s; however, since the faster the cooling rate, the more energy consumed and the higher the cost, the higher the requirement for the technology, the cooling rate of 600-.
When the cooling rate is less than 600 ℃/s, the cooling time is prolonged, so that the particle size is increased, the branched chains are reduced, the resistivity is increased, and the conductivity is poor.
While specific embodiments of the present invention have been described in detail, the description is merely illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. A high-temperature ultrahigh-conductivity carbon black reaction furnace is characterized in that: sequentially comprises a combustion section (7), a throat pipe (8), a reaction section (9) and a cooling section (10);
an air inlet (1) and a gas inlet (2) are formed in one end, far away from the throat pipe (8), of the combustion section (7), the gas inlet (2) and the throat pipe (8) are coaxially arranged, and an included angle alpha between central axes of the air inlet (1) and the gas inlet (2) is 45 degrees;
the throat (8) is provided with a raw oil inlet (3) and a raw material gas inlet;
a plasma heating device (4) is arranged in the reaction section (9), the furnace body shell of the reaction furnace is made of nickel-based high-temperature alloy, and the lining is made of high-purity corundum bricks;
the end of the cooling section (10) is provided with a product outlet (11).
2. The high-temperature ultra-high conductivity carbon black reaction furnace according to claim 1, wherein: a plurality of cooling manifolds (5) are uniformly arranged in the cooling section (10); each cooling manifold (5) is connected with a quenching boiler heat exchanger (6), and each quenching boiler heat exchanger (6) is connected with a quenching boiler.
3. The high-temperature ultra-high conductivity carbon black reaction furnace according to claim 1, wherein: the gas burner is characterized in that the air inlets (1) are arranged in a plurality of numbers, and the air inlets (1) are uniformly arranged along the circumference of the axis of the gas inlet (2).
4. The high-temperature ultra-high conductivity carbon black reaction furnace of claim 3, wherein: the end part of the air inlet (1) is an inclined plane, the end b (101) of the inclined plane is far away from the gas inlet (2), and the end a (102) of the inclined plane is close to the gas inlet (2).
5. The high-temperature ultra-high conductivity carbon black reaction furnace according to claim 1, wherein: the device is characterized in that two raw oil inlets (3) are arranged, one raw material gas inlet is arranged, and the raw oil inlets (3) and the raw material gas inlets are uniformly distributed along the throat (8); the end part of the raw oil inlet (3) is an inclined plane, and the inclined plane is arranged towards the combustion section (7).
6. The high-temperature ultra-high conductivity carbon black reaction furnace of claim 5, wherein: the throat pipe (8) is provided with a necking section (81), and the necking section (81) is arranged between the raw oil inlet (3) and the reaction section (9).
7. A method for producing ultrahigh conductive carbon black by raffinate oil is characterized by comprising the following steps: the ultrahigh conductive carbon black is prepared by using the raffinate oil as a carbon source and acetylene as an additive and using the high-temperature ultrahigh conductive carbon black reaction furnace as claimed in any one of claims 1 to 6.
8. The method for producing ultra-high conductive carbon black from raffinate oil as claimed in claim 7, wherein: the method comprises the following steps:
1) preparing raw oil by raffinate oil processing: pumping the raffinate oil into an air flotation separation device through an oil pump, adding a water absorbent which is solid potassium carbonate, standing after air flotation stirring, and then extracting supernatant liquid to obtain raw oil through a filter press;
2) the mixed gas is combusted in the combustion section (7): injecting mixed fuel gas into a combustion section (7) from a fuel gas inlet (2) of the high-temperature ultrahigh conductive carbon black reaction furnace according to any one of claims 1 to 6 at a flow rate of 300-;
3) mixing and atomizing raw oil and acetylene gas: heating the raw oil obtained in the step 1) to 260-300 ℃ through a preheater, spraying the raw oil from a raw oil inlet (3) of the high-temperature ultrahigh conductive carbon black reaction furnace according to any one of claims 1-6 into a throat (8) at a flow rate of 900-1800kg/h, spraying acetylene gas into the throat (8) from a raw material gas inlet of the high-temperature ultrahigh conductive carbon black reaction furnace according to any one of claims 1-6 at a flow rate of 20-40kg/h, and allowing the raw oil and the acetylene gas to enter a reaction section (9) after being fully and uniformly mixed at the throat (8);
4) cracking raffinate oil to generate carbon black: the plasma heating device (4) is operated so that the furnace temperature of the reaction section (9) is kept in the range of 1980-2080 ℃; the raw oil is fully decomposed in the reaction section (9) to generate carbon black;
5) quenching and cooling the carbon black: the carbon black enters the cooling section (10) from the reaction section (9) and is rapidly cooled to 260-280 ℃ at the speed of 600-1200 ℃/s to form the ultrahigh conductive carbon black with stable structure, and then the ultrahigh conductive carbon black is discharged from the product outlet (11).
9. The method for producing ultra-high conductive carbon black from raffinate oil as claimed in claim 8, wherein: in the step (2), the mixed fuel gas is obtained by mixing acetylene and methane through a gas mixing valve; the volume ratio of the air introduced into the combustion section (7) to the mixed gas is (10-12): 1.
10. an ultra-high conductive carbon black produced by the method for producing an ultra-high conductive carbon black according to the raffinate oil of claim 8 or 9, wherein: the BET surface area of the ultrahigh conductive carbon black is 50-90m2(ii) a resistivity of 0.83 to 0.85. omega. m.
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