JP4202807B2 - Method and apparatus for generating carbon particles - Google Patents

Description

[0001]
[Technical field to which the invention belongs]
The present invention mainly relates to a means for producing carbon particles for producing carbon used for making a carbon electrode plate as pure as possible and in the form of single crystal particles.
[0002]
[Prior art]
For example, as a means for obtaining carbon as a raw material for forming a carbon electrode plate, conventionally, soot produced by burning a hydrocarbon organic compound is collected and obtained.
[0003]
In addition, there is a means for generating crystals by using the material as a solution, heating the solution to a melting point or higher, and cooling the solution.
[0004]
[Problems to be solved by the invention]
The conventional means is to collect soot produced by burning hydrocarbon organic compounds, and the resulting carbon particles are rich in impurities, have a non-uniform crystal structure, and have a performance that is similar to that of the raw material carbon. There is a problem that it is not suitable as a material for forming a carbon electrode plate that depends on the crystal structure.
[0005]
In addition, in the means for forming a crystal by heating the material to a melting point or higher and slowly cooling it, if the solution before the crystal formation is rapidly lowered to a temperature below the melting point, Since segregation and extraneous flow boundaries occur, it is necessary to keep the solution at the melting point of the material or higher until the crystal is formed. However, there is a problem that high-quality single crystal particles cannot be mass-produced.
[0006]
An object of the present invention is to provide a new means capable of mass-producing pure and high-quality carbon particles that can be used as a material for a carbon electrode plate by solving the above-mentioned problems occurring in conventional means. .
[0007]
[Means for Solving the Problems]
The present invention has been completed based on knowledge obtained through various trials and errors in order to achieve the above-described object.
[0008]
In other words, in order to obtain carbon as a raw material for the carbon plate in the purest possible form, the hydrocarbon organic compound is not in solution but in solid form, such as argon gas. Organic hydrocarbons that are easy to vaporize if they are sent into a heating furnace maintained in an active gas atmosphere together with an inert gas of about 10 times the volume ratio, heated to high temperature by arc discharge, etc., and thermally decomposed. Hydrogen and impurities in the compound are gasified, taken into the inert gas, scattered and released, and only the high melting point carbon remains as tangible carbon particles, and this generation It has been found that high-purity carbon powder particles can be continuously produced by taking out the carbon particle particles from the induction tube.
[0009]
Also, the high purity carbon particles obtained by this are heated to a high temperature by heating during thermal decomposition in a heating furnace and are in a state of being pressurized to a high pressure by the temperature rising. From this, the pressure is pushed into the conduit by the induction coil, and the induction coil wound around the conduit guides the inside of the conduit, passes through the jacket through which the refrigerant circulates, cools rapidly, lowers the temperature and lowers the pressure. As a result, crystals are formed into micron-sized particulate crystals, and the rapidly cooled and depressurized carbon particles are surrounded by a jacket in which the refrigerant circulates at room temperature and normal pressure. It was found that it grew into a single crystal in millimeters by sending it to the cooling chamber held in the chamber and leaving it to stand.
[0010]
From this, in the present invention, the organic hydrocarbon compound described in claim 1 is solidified in an inert gas atmosphere in a heating furnace, and an arc is generated by an arc discharger and an electron is generated by an electron gun. more radiate the, warmed to a high temperature of several thousands degrees to 10,000 several thousand degrees allowed pyrolysis, impurities contained hydrogen and the hydrocarbon compounds incorporated into an inert gas by gasifying Thus, carbon having a high melting point is left in a tangible powder form, which is led out of the furnace by a conduit, rapidly cooled by a cooler using a refrigerant, and cooled and reduced in pressure to be crystallized into micron particles. And then cooling it by sending it to a cooling chamber kept at room temperature and normal pressure, allowing it to grow into a single crystal in millimeters, and taking it out of the cooling chamber. Raise Than is.
[0011]
In addition to this, the heating furnace 1 in which the furnace body described in claim 2 is formed into a cylindrical shape with a refractory furnace material, and the lower end side is located at a substantially central portion of the internal space of the furnace body 10 of the heating furnace 1. The material supply cylinder 2 having an opening 20 and having an upper end located above the heating furnace 1 and an opening 31 on the upper end side face the opening 20 below the opening 20 at the lower end of the material supply cylinder 2, and the lower end side of the furnace body 10 is connected to a power source outside the furnace body 10, and is connected to a power source outside the furnace body 10, so that the opening 20 at the lower end of the material supply tube 2 and the upper end side of the discharge conduit 3 are connected. Electrodes 40... 41 of the arc generator 4 disposed around a portion facing the opening 31 of the metal, an electron gun 5 assembled to the furnace body 10 so as to inject electrons into the heating furnace 1, and the heating furnace 1. Inert gas provided along the material supply cylinder 2 so as to feed the inert gas together with the material It is intended to raise the generator of carbon powder particles consisting of a pipe 6.
[0012]
Furthermore, as an apparatus for carrying out the means for generating the carbon particle, the heating furnace 1 in which the furnace body is formed into a cylindrical shape with a refractory furnace material, and the furnace body 10 of which the lower end side is the heating furnace 1 are described. The material supply cylinder 2 whose upper end side is located above the heating furnace 1 and the upper end side opening 31 are located below the lower end opening 20 of the material supply cylinder 2. Opposite to the opening 20, the lower end side is connected to a carbon particle discharge conduit 3 led out of the furnace body 10 and a power source outside the furnace body 10, so that the lower end of the material supply tube 2 is heated in the heating furnace 1. The electrodes 40... 41 of the arc generator 4 disposed around the facing portion between the opening 20 and the opening 31 on the upper end side of the discharge conduit 3, and the furnace body 10 are assembled so as to inject electrons into the heating furnace 1. The inert gun is sent along with the material to the electron gun 5 to be attached and the heating furnace 1 The inert gas pipe 6 provided along the material supply tube 2 and the downstream side of the conduit 3 are passed through a jacket 80 through which a refrigerant circulates, and the carbon particles flowing in the conduit 3 are rapidly cooled. The cooler 8 is connected to the outlet 3a on the downstream side of the conduit 3 coming out of the jacket 80 of the cooler 8, and is surrounded by a jacket 90 through which a refrigerant for cooling the carbon particles flowing out from the outlet 3a circulates. An apparatus for generating carbon powder composed of the cooling chamber 9 is proposed.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
Next, embodiments of the means of the present invention will be described in detail with reference to the drawings.
FIG. 1 shows an organic hydrocarbon compound as a raw material, which is thermally decomposed at a high temperature to separate carbon and hydrogen in the hydrocarbon compound, thereby gasifying hydrogen that is easily vaporized and a small amount of impurities contained therein. The heating furnace for producing | generating the carbon with high melting | fusing point which is hard to convert into powder form is shown.
[0014]
The heating furnace 1 has a furnace body 10 made of a refractory material such as a refractory brick and formed into a cylindrical shape.
[0015]
The furnace body 10 only needs to form a heating chamber whose internal space can withstand high temperatures, and the shape of the furnace body 10 may be arbitrarily designed. In the illustrated embodiment, the furnace body 10 In order to reduce the amount of heat supplied to the interior space, the inner wall surface of the furnace body 10 has an inverted mortar shape in which the inner diameter of the upper opening 11 is smaller than the diameter of the bottom furnace floor 12. It is formed in a cylindrical shape with a cone shape.
[0016]
2 is a material supply cylinder for introducing and supplying an organic hydrocarbon compound into the internal space of the furnace body 10 of the heating furnace 1, which is formed in a cylindrical cylinder, and the lower end side of the material supply cylinder is A portion that is inserted through the opening 11 at the top of the body 10 and whose opening 20 on the lower end side occupies a substantially axial center portion of the internal space of the furnace body 10 in a plan view, and is located approximately in the middle in the vertical direction in a side view Is placed in a state of being opened downward, and is supported in this state by an appropriate support 21, and the hydrocarbon compound of the material is made into a liquid or solid state from the opening 22 on the upper end side thereof. To supply.
[0017]
At this time, the upper opening 11 of the furnace body 10 into which the lower end side of the material supply cylinder 2 is inserted is opened as a gap communicating with the outside between the lower end side outer peripheral surface of the material supply cylinder 2 and From there, when supplying the vaporized gas of hydrogen and impurities in the hydrocarbon compound and the material generated during the thermal decomposition of the material of the hydrocarbon compound supplied into the furnace body 10 via the material supply cylinder 2 The inert gas fed into the interior space of the furnace body 10 together with the material passes through a gap formed between the outer peripheral surface on the lower end side of the material supply cylinder 2 and the opening edge 11 of the upper opening 11 of the furnace body 10. The gas is discharged outside the furnace body 10.
[0018]
3 is a conduit for receiving carbon particles generated by thermal decomposition of the hydrocarbon compound material supplied to the internal space of the furnace body 10 by the material supply cylinder 2 and leading it to the outside of the furnace body 10. The inside of the furnace body 10 is formed in the funnel portion 30 so that the opening 31 whose diameter is enlarged is close to the opening 20 on the lower side close to the opening 20 on the lower end side of the material supply cylinder 2. A main body portion 32 that occupies the axial center portion of the space and is connected to the funnel-shaped upper end portion is formed to have a larger diameter than the material supply cylinder 2 and extends downward in the axial center portion of the internal space of the furnace body 10. The lower end side is formed in a small-diameter portion 33 that penetrates the furnace floor 12 downward, bends laterally, and extends to the outside of the furnace body 10.
[0019]
4 is an arc generator that generates high heat in the furnace body 10 for pyrolyzing the hydrocarbon compound material supplied into the furnace body 10 via the material supply cylinder 2 described above. Surrounding the periphery of the portion facing the opening 20 of the lower opening of the material supply cylinder 2 serving as the mouth and the opening 31 serving as the upper opening of the conduit 3, and the outer periphery of the material supply cylinder 2 and the outer periphery of the conduit 3 in the vicinity thereof. In the part, it arrange | positions so that it may be parallel in multiple stages up and down.
[0020]
As shown in FIG. 2, each arc generator 4 has a pair of opposing anodes 40 and cathodes 41 arranged in an annular shape surrounding the outer periphery of the material supply cylinder 2 and the outer periphery of the conduit 3 in plan view. Each of the anode 40 and the cathode 41 is connected to a plus-side wiring 42 and a minus-side wiring 43 arranged inside the furnace body 10, respectively. By connecting to a power source and supplying a high-voltage current, arc discharge is performed between the anode 40 and the cathode 41, thereby generating high-temperature heat in the internal space of the furnace body 10. .
[0021]
At this time, the high voltage current supplied to the arc generator 4 may be a voltage of about 5000 to 6000 V, and thereby, the axial center portion of the internal space of the furnace body 10 surrounded by the anode 40 and the cathode 41 of the arc generator 4. The temperature of is sometimes raised to a high temperature close to 20,000 degrees C. The temperature for heating the internal space of the furnace body 10 is desirable to some extent at a high temperature, but a temperature of about several thousand degrees C to 6,000 degrees C is sufficient.
[0022]
Reference numeral 5 denotes an electron gun for injecting electrons into the internal space of the furnace body 10 in order to make heating at a high temperature inside the furnace body 10 more effective. 10 is installed so as to be driven out toward the axial center of the internal space.
[0023]
6 is a pipe for supplying an inert gas such as argon gas into the furnace body 10 together with the material when the material hydrocarbon compound is charged and supplied into the furnace body 10 by the material supply cylinder 2. It is arranged along the inner wall surface of the supply cylinder 2, the downstream end thereof opens near the opening 20 on the lower end side of the material supply cylinder 2, and the upstream side is filled with an inert gas. The cylinder 60 is connected via a valve 61.
[0024]
7 is a room constructed so as to surround the heating furnace 1 when it is installed, and is configured in a building shape with a partition wall 70 that maintains airtightness. Is projected above the ceiling wall 71 of the chamber 7 so that the material supply operation is performed on the upper surface side of the ceiling wall 71 of the chamber 7 and the pipe 6 for supplying the inert gas is provided. The cylinder 60 and the valve 61 to be connected are also provided on the upper surface side of the ceiling wall 71.
[0025]
Further, in this chamber 7, hydrogen and impurities vaporized gas generated by the thermal field of the hydrocarbon compound in the furnace body 10 and an inert gas supplied into the furnace body 10 are opened at the top of the furnace body 10. A suction port 72 is provided for drawing out the gas discharged from the port 11 into the chamber 7 to the outside, and a suction pump or a wind exhauster 73 is connected to this through a valve 74.
[0026]
Carbon particle generation performed using the carbon particle generation apparatus A configured as described above is performed by selecting as pure a hydrocarbon compound as a material as possible, for example, pine or the like, and powdering it as a solid. Or dissolved in a solvent or supplied as a molten state by heating.
[0027]
At this time, an inert gas having a volume ratio of about 10 times the material to be supplied is fed into the furnace body 10.
[0028]
The hydrocarbon compound supplied thereby is thermally decomposed in the core portion maintained at a high temperature by an arc discharge by the arc generator 4 and an electron injection from the electron gun 5 in an atmosphere filled with an inert gas. The gas of hydrogen molecules and the gas of impurities that are easily vaporized thereby are taken into the inert gas and scattered and discharged from the furnace body 10 together with the inert gas, and only the carbon molecules having the melting point are Solid carbon particles remain and fall into the funnel portion 30 which is the upper opening of the conduit 3, and are pushed into the conduit 3 by the pressure generated by the high temperature rise during the thermal decomposition. It is led to the downstream side protruding outside the furnace body 10 and is taken out therefrom.
[0029]
The carbon particles are guided to the outside of the furnace body 10 by winding a magnetic field line induction coil a around the outer periphery of the heat insulating material 34 surrounding the small diameter portion 33 on the downstream side bent to the side of the conduit 3. The carbon particles in the conduit 3 may be guided to flow downstream by the magnetic force generated by energizing the coil, and this is effective for taking out the generated carbon particles out of the furnace body 10. It is.
[0030]
The carbon particles thus taken out from the hydrocarbon compound used as a raw material are hydrogenated and impurities gasified and removed by being taken into the inert gas, leaving only carbon molecules as solid particles. Thus, since the carbon particles are produced, it is almost pure carbon and has extremely high purity.
[0031]
Next, FIG. 3 shows that the heating furnace 1 described above is combined with the cooler 8 and the cooling chamber 9 so that the generated carbon powder grows into a single crystal, and the crystal structure becomes uniform. The carbon particle production | generation apparatus which enabled it to take out as a uniform carbon particle is shown.
[0032]
In the figure, 1 is the heating furnace described above, and 8 is a carbon powder produced by high-temperature heat treatment in the heating furnace 1 to take out the carbon particles heated to high heat and cool it rapidly. A cooler 9 is a cool chamber in which the carbon powder cooled by the cooler 8 and cooled down is further cooled at normal temperature and normal pressure.
[0033]
The heating furnace 1 is the heating furnace described with reference to FIGS. 1 and 2 and is configured in the same manner, but the small-diameter portion 33 that bends to the side on the lower end side of the conduit 3 incorporated in the heating furnace 1 slightly toward the downstream side. As the upward gradient, the downstream side is made to enter the bottom of the jacket 80 for circulating the refrigerant in the cooler 8 disposed adjacent to the heating furnace 1.
[0034]
In the cooler 8, as shown in FIG. 4, a jacket 80 for circulating the refrigerant is formed in a cylindrical shape in plan view by concentric inner and outer partition walls 81 and 82, and the inside of the cylindrical jacket 80 is The extension 35 on the downstream side of the conduit 3 is formed in a serpentine shape and is inserted so that the end of the extension 35 protrudes from the outer peripheral surface on the upper end side of the jacket 80. .
[0035]
And on the outer periphery of the cooler 8, the above-mentioned magnetic field line induction coil a is formed in a spiral shape on the bottom surface side and the upper surface side, respectively, and the magnetic field line induction coil a is disposed on the outer periphery of the trunk peripheral wall. It is arranged so as to be wound in a coil shape, and the carbon particles are induced to flow through the extension 35 of the conduit 3 wound in a serpentine shape by the magnetic lines of force generated by energizing the coil. It is.
[0036]
The cooling of the carbon particles by the cooler is performed in a state where the carbon particles are heated to several thousand degrees C to 5,000 degrees C and flow downstream from the heating furnace 1 to the side of the conduit 3. However, when the refrigerant flows through the extension 35 of the serpentine tube 3 disposed in the jacket 80 through which the refrigerant circulates and exits from the downstream end of the extension 35, the temperature is about 5 hundred degrees C. Cool down to descend.
[0037]
By the rapid cooling by the cooler 8, the carbon powder particles become carbon particles in units of microns as the carbon crystallizes.
[0038]
Then, the carbon powder particles that have passed through the cooler 8 are discharged into a cooling chamber 9 disposed adjacent to the cooler 8, and are left to cool down.
[0039]
The cooling chamber 9 surrounds the outer periphery of the chamber 91 formed of a pure carbon plate with a jacket 90 made of inner and outer partition walls for circulating the refrigerant, and the magnetic field line induction coil a insulated in the jacket 90 is cooled by the cooling described above. Similar to the jacket 80 of the vessel 8, the bottom surface and the top surface are formed in a spiral shape and disposed around the outer periphery of the body portion in a coiled manner and approach the lower end of the body portion. The downstream end of the extension portion 35 of the serpentine tubular conduit 3 in the jacket 80 of the cooler 8 is connected to the portion and opened, and the ceiling portion is put into the chamber 91 and is taken out of the carbon particles. In this configuration, 92 is opened.
[0040]
The cooling chamber 9 is maintained at a normal temperature by cooling with a refrigerant / brine circulated in the jacket 90 and at a normal pressure by an outlet 92 opened to the outside. It is made to do.
[0041]
The carbon particles in which carbon crystals are generated by being rapidly cooled through the cooler 8 are fed to the cooling chamber 9 maintained at room temperature and normal pressure and allowed to cool for several hours. As a result, carbon crystals grow into single crystals and become carbon particles in millimeters. At this time, the growth of the single crystal further proceeds when the cool powder chamber 9 is surrounded by the magnetic field line induction coil a and the carbon powder particles flow under the influence of the magnetic field lines. In FIG. 3, b indicates a building that surrounds the cooling chamber 8, and c indicates a building that surrounds the cooling chamber 9.
[0042]
【The invention's effect】
As described above, according to the means of the present invention, carbon powder particles used as a material for forming the carbon electrode plate can be continuously generated as high-purity carbon.
[0043]
In addition, the high-purity carbon powder particles can be obtained as single-crystal particles having a uniform crystal structure.
[Brief description of the drawings]
FIG. 1 is a longitudinal front view of a heating furnace used for implementing the means of the present invention.
FIG. 2 is a cross-sectional plan view of the above.
FIG. 3 is a longitudinal front view of the whole carbon powder generating apparatus used in the means of the present invention.
FIG. 4 is a plan view of a portion of the apparatus.
[Explanation of symbols]
A ... generator, a ... induction coil, b · c ... building, 1 ... heating furnace, 10 ... furnace body, 11 ... open port, 12 ... hearth, 2 ... material supply cylinder, 20 ... opening, 21 ... support, 22 ... Opening port, 3 ... Conduit, 3a ... Outlet, 30 ... Funnel part, 31 ... Opening, 32 ... Main part, 33 ... Small diameter part, 34 ... Thermal insulation, 35 ... Extension part, 4 ... Arc generator, 40 ... Anode 41 ... Cathode 42 ... 43 Wiring 5 ... Electron gun 6 ... Piping 60 ... Cylinder 61 ... Valve 7 ... Chamber 70 ... Bulkhead 71 ... Ceiling wall 72 ... Drawer 73 ... Exhaust Air blower, 74 ... valve, 8 ... cooler, 80 ... jacket, 81/82 ... partition wall, 9 ... cooling room, 90 ... jacket, 91 ... chamber, 92 ... take-out port.

Claims (3)

The organic hydrocarbon compound, in solid state, in an atmosphere of inert gas into the heating furnace, and more radiate the electron by the arc generation and the electron gun according to an arc discharger thousands times to 10,000 several thousand degrees of It is heated to a high temperature and pyrolyzed, and hydrogen in the hydrocarbon compound and impurities contained therein are gasified and incorporated into an inert gas, leaving high melting point carbon in a tangible powder form, It is led out of the heating furnace by a conduit, rapidly cooled by a cooler using a refrigerant, cooled and reduced in pressure to crystallize into micron-sized particles, and then sent to a cooling room kept at normal temperature and normal pressure. A method for producing carbon particles, wherein the method is allowed to cool at room temperature to grow into a single crystal in millimeters, and is taken out of the cooling chamber.   A heating furnace 1 in which a furnace body is formed into a cylindrical shape with a refractory furnace material, and a lower end side is located at a substantially central portion of the internal space of the furnace body 10 of the heating furnace 1 and an opening 20 is formed, and an upper end side is located above the heating furnace 1 The material supply tube 2 and the upper end side opening 31 face the opening 20 below the lower end opening 20 of the material supply tube 2 and the lower end side is led out of the furnace body 10. And connected to a power source external to the furnace body 10 and disposed in the heating furnace 1 around a portion facing the opening 20 at the lower end of the material supply tube 2 and the opening 31 at the upper end side of the discharge conduit 3. Electrodes 40... 41 of the arc generator 4, an electron gun 5 that is assembled to the furnace body 10 so as to drive electrons into the heating furnace 1, and a material supply cylinder that feeds an inert gas together with the material into the heating furnace 1. 2 is an apparatus for generating carbon powder particles.   A heating furnace 1 in which a furnace body is formed into a cylindrical shape with a refractory furnace material, and a lower end side is located at a substantially central portion of the internal space of the furnace body 10 of the heating furnace 1 and an opening 20 is formed, and an upper end side is located above the heating furnace 1 The material supply cylinder 2 and the opening 20 on the upper end side face the opening 20 below the opening 20 at the lower end of the material supply cylinder 2 and the carbon particle discharge conduit 3 whose lower end side is led out of the furnace body 10. And connected to a power source external to the furnace body 10 and disposed in the heating furnace 1 around a portion facing the opening 20 at the lower end of the material supply tube 2 and the opening 31 at the upper end side of the discharge conduit 3. Electrodes 40... 41 of the arc generator 4, an electron gun 5 that is assembled to the furnace body 10 so as to drive electrons into the heating furnace 1, and a material supply cylinder that feeds an inert gas together with the material into the heating furnace 1. 2 along the pipe 6 of the inert gas provided along the line 2 and the downstream side of the conduit 3 A cooler 8 that rapidly passes through the annular jacket 80 and cools the carbon particles flowing in the conduit 3, and an outlet 3 a downstream of the conduit 3 that exits the jacket 80 of the cooler 8. An apparatus for generating carbon particles comprising a cooling chamber 9 surrounded by a jacket 90 through which a refrigerant for cooling the carbon particles flowing out from the outlet 3a circulates.

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