CN215440292U - Preparation facilities of high porosity carbon black - Google Patents
Preparation facilities of high porosity carbon black Download PDFInfo
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- CN215440292U CN215440292U CN202121439154.2U CN202121439154U CN215440292U CN 215440292 U CN215440292 U CN 215440292U CN 202121439154 U CN202121439154 U CN 202121439154U CN 215440292 U CN215440292 U CN 215440292U
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Abstract
The utility model discloses a preparation device of high-porosity carbon black, which comprises a reaction device, an electric heating device, a transmission device, a riding wheel catch wheel device, a sealing device and an end cover, wherein the reaction device is arranged on the upper surface of the reaction device; the reaction device comprises a reaction kettle barrel; the reaction kettle barrel comprises a reaction kettle inner barrel and a reaction kettle outer barrel; a water jacket is arranged between the inner barrel body and the outer barrel body of the reaction kettle; a water inlet and a water outlet are formed in the outer barrel of the reaction kettle, and diversion trenches are respectively formed in the water outlet; a plurality of shoveling plates are arranged on the inner wall of the cylinder body in the reaction kettle; the electric heating device is a heating rod; the transmission includes a drive gear and a ring gear. The reaction kettle barrel in the process of the utility model is protected by the water jacket, so that higher reaction temperature can be reached, the requirement of high temperature on the material of the reaction kettle barrel is overcome, the temperature reaction condition of oxidant gas is met, the special reaction kettle barrel structure can ensure that gas molecules and carbon black are fully reacted, and the problem that the traditional carbon black reaction furnace cannot produce carbon black with high porosity is solved.
Description
Technical Field
The utility model relates to a preparation device of high-porosity carbon black, in particular to a preparation device for obtaining high-porosity carbon black by etching carbon black by using gas as an oxidant.
Background
Carbon black is a functional filler with a nano structure, and porous carbon black contributes to improving the conductivity of rubber or plastics due to the fact that the surface of carbon black is porous, the more particles of the same weight of carbon black are dispersed in the volume of a unit polymer, the larger the volume is, the distance between aggregates is reduced, and the conductive channel is increased, so that the conductivity is improved; the most common method for improving the porosity of carbon black is to prolong the residence time of the carbon black in a reaction furnace and prolong the time for etching the carbon surface by tail gas, but the method has the defects that the length of the reaction furnace is insufficient or the temperature is low, the reaction flow rate of the carbon black is unstable, and the technical conditions for producing the carbon black with higher porosity cannot be met. Another method is to add alkaline earth metal ions into the carbon black raw material to accelerate the carbon black etching by tail gas, but the method can leave impurities on the surface of the carbon black to influence the purity and the processing performance of the carbon black.
CN109096798A discloses a micro-oxidation activation method of waste tire pyrolytic carbon black, which is characterized in that the device used by the micro-oxidation activation method of waste tire pyrolytic carbon black comprises a waste tire pyrolytic furnace, a micro-oxidation activation furnace, a gas storage tank, a catalytic combustion furnace, a condensing device, a pyrolytic oil storage tank and a flue gas purification device; feeding pyrolysis oil condensed by a scrap tire pyrolysis furnace device after scrap tires are crushed and screened into a pyrolysis oil storage tank for storage, and feeding a pyrolyzed gaseous product into a catalytic combustion furnace through a gas storage tank; feeding pyrolytic carbon black formed in a waste tire pyrolysis furnace into a micro-oxidation activation furnace, carrying out surface micro-oxidation activation treatment on the pyrolytic carbon black at 500-800 ℃ under the condition of introducing trace air, wherein trace oxygen is in short contact with volatile matters, carbonaceous deposits and coking substances blocking pores on the surface of the pyrolytic carbon black to carry out oxidation reaction, so that the deposits are removed, internal polar functional groups are exposed, the blocked pore channels are opened, the modified carbon black after activation is discharged, volatile gas generated in the process is fed into a catalytic combustion furnace, the volatile gas and pyrolysis gaseous products generated in the pyrolysis process are fully combusted in the catalytic combustion furnace, a small amount of generated high-temperature flue gas and trace air are fed back to the micro-oxidation activation furnace for energy supply, and most of the high-temperature flue gas supplies energy to the waste tire pyrolysis furnace; and (4) sending the cooling flue gas subjected to heat exchange of the waste tire pyrolyzing furnace into a flue gas purifying device for treatment, and discharging after reaching the standard. The disadvantages of this process are 1. thermal carbon black is not protected by inert gas, but is heated to 500 to 800 ℃ in an air environment, in which case the carbon black is very easily decomposed; 2. when air is introduced to the pyrolysis carbon black for a short time, volatile components and other components on the surface of the carbon black cannot be fully pyrolyzed, and a part of the carbon black is decomposed.
SUMMERY OF THE UTILITY MODEL
The utility model discloses a preparation device of high-porosity carbon black, which comprises a reaction device, an electric heating device, a transmission device, a riding wheel catch wheel device, a sealing device and an end cover, wherein the reaction device is arranged on the upper surface of the reaction device; the reaction device comprises a reaction kettle barrel; the reaction kettle barrel comprises a reaction kettle inner barrel and a reaction kettle outer barrel; a water jacket is arranged between the inner barrel body and the outer barrel body of the reaction kettle; a water inlet and a water outlet are formed in the outer barrel of the reaction kettle, and diversion trenches are respectively formed in the water outlet; a plurality of shoveling plates are arranged on the inner wall of the cylinder body in the reaction kettle; the electric heating device is a heating rod; the transmission device comprises a driving gear and a gear ring; the gear ring is positioned on the wall of the outer cylinder of the reaction kettle; the bottom of the front end and the bottom of the rear end of the outer cylinder of the reaction kettle are respectively provided with a riding wheel retaining wheel device; the outer cylinder body of the reaction kettle is provided with a rolling ring; the sealing device comprises a compression spring and a sealing ring; the end cover and the reaction kettle are fastened through a positioning bolt; the inner side of the end cover is made of high-temperature-resistant heat-insulating castable; end cover sliding supports are arranged on two sides of the outer wall of the end cover; and the outer wall of the end cover is provided with an air inlet, an air outlet and a vacuum pipeline port.
The water jacket is used for cooling the circular flow of water and cooling the inner cylinder of the reaction kettle; the guide groove guides and directionally discharges the cooling water.
The outer barrel of reation kettle is equipped with 1 water inlet and 2 delivery ports.
And the water outlet is respectively provided with 1 diversion trench.
6 to 18 shovelling plates are arranged on the inner wall of the cylinder body in the reaction kettle; the height of the shoveling plates accounts for 1/20-1/10 of the inner diameter of the reaction kettle barrel; the shoveling plates are uniformly distributed on the inner wall of the reaction kettle barrel in parallel; the shoveling plate can ensure that the carbon black is fully and uniformly heated in the reaction process, and the reaction efficiency is improved.
The electric heating device comprises 1 to 6 heating rods; the heating rod is a groove-shaped heating rod; the heating rods are high-temperature-resistant and corrosion-resistant silicon-carbon rods or silicon-molybdenum rods, the heating temperature can reach 1500 ℃, and the heating length and the number of the heating rods can be adjusted according to the size of a cylinder body in the reaction kettle and the required temperature.
The gear ring is positioned on the wall of the outer cylinder of the reaction kettle and drives the whole reaction kettle cylinder to rotate through meshing with the driving gear.
The riding wheel supports the whole device through a rolling ring which is arranged on the outer barrel of the reaction kettle and is supported, the rotation of the reaction kettle in the operation process is ensured, and the blocking wheel prevents the reaction kettle from sliding in the operation process.
The sealing device comprises a compression spring and a sealing ring, when the sealing device is extruded by external force, the sealing ring has certain flexibility due to the expansion of the compression spring, the abrasion of the sealing ring can be reduced, the end cover and the reaction kettle are fastened through a positioning bolt, the sealing mechanism is firmer, the bolt is loosened during feeding, the end cover is opened, and materials are placed in the reaction kettle.
The inner side of the end cover device is made of high-temperature-resistant heat-insulating pouring materials, so that the overtemperature of the end cover is prevented.
And end cover sliding supports are arranged on two sides of the outer wall of the end cover, so that the end cover can horizontally slide along the guide rail at the bottom to open or close the end cover.
The outer wall of the end cover is provided with a pressure gauge and a temperature control system, the pressure gauge is used for monitoring the pressure inside the reaction kettle in real time, and the temperature and the heating time in the kettle can be controlled through the temperature control system.
The vacuum pipeline port is connected with a vacuum pump, and air in the kettle is pumped out before gas is introduced, so that the reaction kettle is in a micro negative pressure state. The micro negative pressure is-0.03 MPa to-0.12 MPa.
The specific implementation process is as follows: putting a certain amount of carbon black into a cylinder in a reaction kettle, closing an end cover, fastening the end cover by using a positioning bolt, opening a vacuum pump, pumping air in the cylinder in the reaction kettle out through a vacuum pipeline port to enable the air to be under-0.03 MPa to-0.12 MPa, opening an air inlet to introduce inert gas, opening an air outlet when the pressure in the cylinder in the reaction kettle reaches about 0MPa, and adjusting the flow rate of the air inlet to enable the pressure in the cylinder in the reaction kettle to be kept stable. Opening a heating device to set the temperature and the heating rate of the reaction kettle, opening a water inlet and a water outlet to cool and protect a barrel in the reaction kettle, starting a transmission device and a riding wheel catch wheel device in the heating process to ensure that the carbon black is fully and uniformly heated, closing the inert gas at the air inlet when the required high temperature is reached under the protection of the inert gas, starting an oxidant gas, adjusting the air inlet flow rate to ensure that the gas is closed after the reaction is carried out for 0.5 to 15 hours under the high-temperature environment, then cooling the barrel of the reaction kettle by adopting cooling water under the protection of the inert gas, completing the 'in-situ' etching of the carbon black, and preparing the carbon black with high porosity.
The porosity referred to herein means the porosity of the carbon black, which is one of the surface characteristics of the carbon black. The degree of micropores on the surface of the carbon black particles was characterized. Is the ratio of the total specific surface area to the external specific surface area of the carbon black. If the ratio of the total specific surface area to the external specific surface area of the carbon black particles is equal to 1, the carbon black has no porosity, if this ratio is clearly higher than 1, which indicates that these carbon blacks have a high porosity. The larger the ratio, the rougher and porous the surface of the carbon black, and the higher the porosity. The present invention uses the ratio of BET to STSA, BET/STSA, to characterize porosity. The present invention determines BET and STSA according to the national standard GB/T10722-2014. The high-porosity carbon black obtained by the utility model has the porosity of 1.2-3; preferably 1.4 to 2.9; more preferably 1.6-2.8; most preferably 1.8-2.6.
As used herein, carbon black used to prepare high porosity carbon black refers to carbon black obtained by any method, including but not limited to contact, furnace and fumed carbon blacks.
The carbon black obtained by the process of the utility model has a density of from 1S/cm to 12S/cm; preferably 2S/cm to 10S/cm; more preferably 3S/cm to 8S/cm; most preferably 4S/cm to 7S/cm.
The inert gas used in the present invention may preferably be one or more of nitrogen, helium and argon. The inert gas is introduced into the reaction kettle in order to remove air in the reaction kettle, and the carbon black is heated to the specified reaction temperature under the inert gas environment.
The oxidant referred to in the present invention may be a gas, and may be a gas containing one or more of oxygen, ozone, water vapor, nitric oxide, nitrogen dioxide, sulfur trioxide, and carbon dioxide. Preferably one or more of water vapor, nitric oxide, nitrogen dioxide and carbon dioxide gas, more preferably water vapor or carbon dioxide gas, and most preferably carbon dioxide gas. The gas flow rate is 2L/min-20L/min; preferably 3L/min-15L/min; more preferably 8L/min-12L/min; the reaction time is 0.5h-15 h; preferably 1h-10 h; more preferably from 2h to 8 h. At this gas flow rate, the reaction time is controlled so that the surface of the carbon black in the system is "etched" to some extent, thereby obtaining carbon black with a specified porosity.
The term "etching" as used herein refers to an oxidation reaction between the oxidizing agent and the surface of the carbon black, wherein the faster the flow rate of the oxidizing agent gas, the longer the reaction time, and the deeper the oxidation reaction between the oxidizing agent and the surface of the carbon black, the higher the porosity of the obtained carbon black.
The in-situ etching of the carbon black refers to the following steps: the molecules of the oxidant react with the active sites on the surface of the carbon black in a high-temperature environment, the exposed carbon atoms are continuously attacked after the carbon atoms on the surface are removed, and the carbon black with certain porosity can be obtained by controlling the reaction time and the flow rate of the oxidant in the reaction kettle.
Technical effects
1. The reaction kettle barrel in the process of the utility model is protected by the water jacket, so that higher reaction temperature can be reached, the requirement of high temperature on the material of the reaction kettle barrel is overcome, the temperature reaction condition of oxidant gas is met, the special reaction kettle barrel structure can ensure that gas molecules and carbon black fully react, the gas utilization rate is improved, carbon black particles with high specific surface area and uniform porosity can be prepared, and the problem that the traditional carbon black reaction furnace cannot produce carbon black with high porosity is solved. The preparation method of the high-porosity carbon black disclosed by the utility model can carry out etching reaction on the carbon black by using gas as an oxidant, has the advantages of simple production process, environmental protection, stable reaction conditions and high gas utilization rate, and can obtain carbon black particles with low impurity content, large specific surface area and high porosity.
2. According to the utility model, the carbon black is etched by adopting an oxidant, and the surface structure of the carbon black is changed under a high-temperature condition by utilizing a specific gas-phase reaction kettle cylinder, so that the porosity of the surface of the carbon black is increased, the carbon black is crushed into aggregates with smaller particle size, the roughness of the surface of the carbon black and the average contact area among particles are obviously improved, and meanwhile, functional groups on the surface of the carbon black are reduced, so that the conductivity of the carbon black is obviously improved.
Drawings
FIG. 1 is a schematic view of the structure of a production apparatus of the present invention.
Fig. 2 is a partial schematic view of the end cap.
1. A reaction kettle inner cylinder body; 2. an outer cylinder of the reaction kettle; 3. an electric heating device; 4. an end cap; 4.1 end cover sliding support; 5. a transmission device; 6. a riding wheel catch wheel device; 6.1 riding wheels; 6.2 catch wheels; 7. rolling a ring; 8. a ring gear; 9. a water inlet; 10. a water outlet; 10.1 diversion trenches; 11. a sealing device; 12. shoveling plates; 13. an air inlet; 14. an air outlet; 15. a temperature control system; 16. a pressure gauge; 17. a vacuum line port.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Example 1
Referring to the attached drawing 1, the highly porous carbon black reaction kettle provided by the utility model is realized by adopting the following technical scheme: a reaction device comprises a reaction kettle inner cylinder body 1, a reaction kettle outer cylinder body 2, an electric heating device 3, an end cover 4, a transmission device 5, a riding wheel catch wheel device 6, a sealing device 11 and a temperature control system 15. A water jacket is arranged between the inner barrel body 1 of the reaction kettle and the outer barrel body 2 of the reaction kettle and is used for cooling the inner barrel body through circulating flow of cooling water. The outer barrel body 2 of the reaction kettle is respectively provided with a water inlet 9 and a water outlet 10, the water outlet 10 is provided with a diversion trench 10.1, and the diversion trench can conduct and discharge circulating water in a directional manner. The inner wall of the barrel 1 in the reaction kettle is provided with the shoveling plates 12, and the height of the shoveling plates accounts for 1/20-1/10 of the inner diameter of the barrel of the reaction kettle, so that carbon black can be fully and uniformly heated in the reaction process, and the reaction efficiency is improved. The electric heating device 3 is a groove-shaped heating rod, the material of the heating rod is a high-temperature-resistant and corrosion-resistant silicon-carbon rod or silicon-molybdenum rod, the heating temperature can reach 1500 ℃, and the heating length and the number of the heating rods can be adjusted according to the size of the inner cylinder of the reaction kettle and the required temperature. The transmission device 5 comprises a driving gear 5.1 and a gear ring 8, wherein the gear ring 8 is positioned on the wall of the outer cylinder of the reaction kettle, and drives the whole reaction kettle cylinder to rotate through meshing with the driving gear 5.1. The bottom of the front end and the rear end of the outer barrel body 2 of the reaction kettle are respectively provided with a riding wheel retaining wheel device 6, the riding wheels 6.1 support the whole equipment through rolling rings arranged on the outer barrel body of the reaction kettle, the rotation of the reaction kettle in the operation process is ensured, and the retaining wheels 6.2 prevent the reaction kettle from sliding in the operation process. Sealing device 11 includes compression spring and sealing ring, and when receiving external force extrusion, compression spring makes the sealing ring have certain elasticity, can alleviate the wearing and tearing of sealing ring, and end cover 4 and reation kettle barrel pass through positioning bolt fastening, make sealing mechanism more firm, loosen the bolt when throwing the material, open the end cover, place the material in among the reation kettle. The inner side of the end cover device 4 is made of high-temperature-resistant heat-insulating pouring materials, so that the overtemperature of the end cover is prevented. And end cover sliding supports 4.1 are arranged on two sides of the outer wall of the end cover 4, so that the end cover can horizontally slide along the guide rail at the bottom to open or close the end cover. As shown in fig. 2, the outer wall of the end cover 4 is provided with a pressure gauge 16 and a time-temperature control system 15, the pressure gauge 16 monitors the pressure inside the reaction kettle in real time, and the time-temperature control system 15 can control the temperature and heating time inside the kettle. The outer wall of end cover 4 is equipped with air inlet 13, gas outlet 14 and vacuum pipeline mouth 17, the air inlet can lead to more than 1 kind of inert gas through the trachea adapter, vacuum pipeline mouth 17 connects the vacuum pump, is used for evacuating the air in the cauldron before letting in gas to its reation kettle is in little negative pressure state.
Taking carbon black gas phase etching reaction as an example, in the using process, opening the end cover 4, putting a certain amount of carbon black into the inner cylinder body 1 of the reaction kettle, closing the end cover 4 and fastening by using a positioning bolt, opening the vacuum pump to pump out air in the inner cylinder body 1 through the vacuum pipeline port 17 to enable the inner cylinder body to be in a micro negative pressure state, opening the air inlet 13 to introduce inert gas, opening the air outlet 14 when the pressure in the inner cylinder body of the reaction kettle reaches about 0MPa, and adjusting the air inlet flow rate to enable the pressure in the inner cylinder body of the reaction kettle to be kept stable. Opening the heating device 3 to set the temperature and the heating rate of the reaction kettle, opening the water inlet 9 and the water outlet 10 to protect the inner barrel from temperature reduction, starting the transmission device 5 and the riding wheel catch wheel device 6 in the heating process to ensure that the carbon black is fully and uniformly heated, closing the inert gas at the air inlet 13 when reaching the required high temperature under the protection of the inert gas, starting another oxidant gas, adjusting the air inlet flow rate to ensure that the inert gas is closed after reacting for 0.5-15h under the high-temperature environment, then adopting cooling water to cool the barrel under the protection of the inert gas, completing the 'in-situ' etching of the carbon black, and preparing the carbon black with high porosity.
Claims (8)
1. A preparation device of high-porosity carbon black comprises a reaction device, an electric heating device, a transmission device, a riding wheel catch wheel device, a sealing device and an end cover, and is characterized in that the reaction device comprises a reaction kettle barrel; the reaction kettle barrel comprises a reaction kettle inner barrel and a reaction kettle outer barrel; a water jacket is arranged between the inner barrel body and the outer barrel body of the reaction kettle; a water inlet and a water outlet are formed in the outer barrel of the reaction kettle, and diversion trenches are respectively formed in the water outlet; a plurality of shoveling plates are arranged on the inner wall of the cylinder body in the reaction kettle; the electric heating device is a heating rod; the transmission device comprises a driving gear and a gear ring; the gear ring is positioned on the wall of the outer cylinder of the reaction kettle; the bottom of the front end and the bottom of the rear end of the outer cylinder of the reaction kettle are respectively provided with a riding wheel retaining wheel device; the outer cylinder body of the reaction kettle is provided with a rolling ring; the sealing device comprises a compression spring and a sealing ring; the end cover and the reaction kettle are fastened through a positioning bolt; the inner side of the end cover is made of high-temperature-resistant heat-insulating castable; end cover sliding supports are arranged on two sides of the outer wall of the end cover; and the outer wall of the end cover is provided with an air inlet, an air outlet and a vacuum pipeline port.
2. The preparation device of claim 1, wherein the outer cylinder of the reaction kettle is provided with 1 water inlet and 2 water outlets.
3. The manufacturing apparatus as set forth in claim 1, wherein the water outlets are respectively provided with 1 flow guide groove.
4. The preparation device of claim 1, wherein 6 to 18 shovelling plates are arranged on the inner wall of the inner cylinder of the reaction kettle.
5. The preparation device of claim 4, wherein the shoveling plates are uniformly distributed on the inner wall of the reaction kettle cylinder in parallel.
6. The preparation device of claim 5, wherein the height of the shoveling plates accounts for 1/20-1/10 of the inner diameter of the reaction kettle barrel.
7. The manufacturing apparatus of claim 1, wherein the electrical heating means is 1 to 6 heating rods.
8. The manufacturing apparatus according to claim 7, wherein the heating rod is a groove-shaped heating rod; the heating rod is a silicon-carbon rod or a silicon-molybdenum rod.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113402905A (en) * | 2021-06-28 | 2021-09-17 | 青岛黑猫新材料研究院有限公司 | High-porosity carbon black, preparation method and preparation device thereof |
| CN115537044A (en) * | 2022-09-19 | 2022-12-30 | 青岛黑猫新材料研究院有限公司 | Modified pyrolysis carbon black and preparation method and application thereof |
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2021
- 2021-06-28 CN CN202121439154.2U patent/CN215440292U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113402905A (en) * | 2021-06-28 | 2021-09-17 | 青岛黑猫新材料研究院有限公司 | High-porosity carbon black, preparation method and preparation device thereof |
| CN115537044A (en) * | 2022-09-19 | 2022-12-30 | 青岛黑猫新材料研究院有限公司 | Modified pyrolysis carbon black and preparation method and application thereof |
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