KR101286751B1 - Method and apparatus for continuous manufacturing carbon fiber or carbon nanotube fused carbon fiber using injection means - Google Patents

Abstract

PURPOSE: A carbon fiber manufacturing apparatus is provided to generate carbon fiber having various characteristics such as flame retarded fiber, carbon fiber or graphite fiber by controlling the inflowing of gas and heater in one reaction unit. CONSTITUTION: A carbon fiber manufacturing apparatus which fused with continuous carbon fiber or carbon nanotube using the spray comprises a reaction unit (100) which undiluted solution reacts, an undiluted solution supply unit (200') which supplies the undiluted solution to the reaction unit and a gas supply unit (300) which supplies gas to the reaction unit. The reaction comprises a reactor having reaction space inside; a heater which installed at the external periphery of the reactor to control the temperature of the reaction space; an undiluted solution injection nozzle (131) and an air supply nozzle (133) which respectively installed at the inner side of the top end portion of the reactor; a gas supply nozzle (132) which installed at the inner side of the lower end portion of the reactor; and a product emission unit (140) which installed at the lower end portion of the reactor. The undiluted supply unit comprises a liquid resin formation unit (210) which forms liquid resin by stirring the injected resin material and the solution which dissolves the resin material; and a transfer pump (240) which supplies the liquid resin formed in the liquid resin formation unit to the material spray nozzle.

Description

Method and apparatus for continuous manufacturing carbon fiber or carbon nanotube fused carbon fiber using injection means}

The present invention relates to an apparatus and method for producing carbon fibers fused with carbon fibers or carbon nanotubes, and more specifically, to a pretreatment section, a carbide section, and graphite by spraying a resin catalyst mixture solution in which a liquid resin or a liquid resin and a catalyst dispersion are mixed. The present invention relates to a continuous carbon fiber or a carbon nanotube fused carbon fiber manufacturing apparatus and method by spraying the oxidized section continuously through the carbon fiber or carbon nanotube fused carbon fiber.

Carbon fiber (CF) refers to a fibrous carbon material having a fine graphite crystal structure made through a special heat treatment process after fiberizing polyacrylonitrile (Polyacrylonitril, PAN) resin, coal / petroleum pitch, and the like.

These carbon fibers are used in various fields because they have excellent heat resistance, impact resistance, chemical resistance, antimicrobial properties, etc., and are lighter than aluminum but have stronger elasticity and strength than iron.

The present invention is devised to efficiently produce carbon fibers fused with carbon fibers or carbon nanotubes used in various fields as described above, the resin catalyst mixture liquid mixed liquid resin or liquid resin and catalyst dispersion by section By spraying in one reactor that can produce a different atmosphere, by allowing the injected liquid resin or resin catalyst mixture to fall through the pre-treatment section, the carbonization section and the graphitization section continuously, by controlling the temperature by section in one reactor To provide a continuous carbon fiber or carbon nanotube fused carbon fiber manufacturing apparatus and method using a spray to enable the production of carbon fibers fused with carbon nanotubes or carbon nanotubes of various forms through gas supply control The purpose is.

Continuous carbon fiber or carbon nanotubes fusion apparatus using a spray according to the present invention for achieving the above object is a reaction unit to react the stock solution, the stock solution supply unit for supplying the stock solution to the reaction unit; A gas supply unit for supplying gas to the reaction unit, wherein the reaction unit comprises: a reactor having a reaction space therein; A heater installed around the outside of the reactor to control a temperature of the reaction space; Stock solution injection nozzles and air supply nozzles respectively installed on the inner top of the reactor; A gas supply nozzle installed at an inner lower end of the reactor; And a product discharge part installed at the bottom of the reactor, wherein the stock solution supply unit comprises: a liquid resin forming unit which forms a liquid resin by stirring the added water support material and the solution dissolving the water support material; And a transfer pump for supplying the liquid resin formed in the liquid resin forming unit to the stock solution spray nozzle side, wherein the atmosphere is introduced into the reaction space inside the reactor through the air supply nozzle. In the state where the gas is introduced through the gas supply nozzle to the stop and the lower end, when the liquid resin formed in the liquid resin forming unit by the operation of the transfer pump is injected through the raw liquid injection nozzle, the injected liquid resin is Carbon fibers are produced by pretreatment, carbonization and graphitization while sequentially falling from the top to the bottom of the reaction space inside the reactor.

Here, the heater may be adjusted to at least one different area according to the height of the reactor to control the temperature.

In addition, the stock solution injection nozzle may be composed of a rotary atomizer.

In addition, the stock solution supply unit, a catalyst forming unit for forming a catalyst dispersion by stirring the added catalyst and the solution for dispersing the catalyst; And a mixing unit for mixing the liquid resin and the catalyst dispersion from the liquid resin forming unit and the catalyst forming unit, respectively, to stir the liquid resin and the catalyst dispersion to form a resin catalyst mixture. The resin catalyst mixture formed in the mixing unit is supplied to the stock injection nozzle side, and the gas supply unit supplies the gas for carbon nanotube growth through the gas supply nozzle to the stop and the lower end of the reaction space, thereby allowing the reactor. In the state that the atmosphere is introduced through the air supply nozzle to the top of the reaction space therein, and the gas for carbon nanotube growth is introduced through the gas supply nozzle to the stop and the bottom of the reaction space, When the resin catalyst mixture liquid formed in the mixing portion by the operation is injected through the stock solution injection nozzle, the powder The resin catalyst whereby the mixture while sequentially falls from the top to the bottom of the reaction space inside the reactor, pre-treatment, carbonization and graphitization has the carbon nanotubes fused carbon fibers can be produced.

On the other hand, the continuous carbon fiber or carbon nanotube fusion method using a spray according to the present invention for achieving the above object, the step of forming a liquid resin by stirring a solution for dissolving the water support material and the water support material ; Spraying the liquid resin into a reactor, the temperature of which is controlled by a heater and filled with a gas for reaction; Pretreatment at the top of the reactor while the liquid resin injected into the reactor falls; Carbonizing at the reactor stop while dropping the pretreated liquid resin at the top of the reactor; Graphitizing at the bottom of the reactor while the carbonized liquid resin is dropped at the reactor stop; And recovering the carbonized fibers that have undergone the pretreatment, carbonization, and graphitization.

Here, the temperature inside the reactor is divided into at least one different area according to the height is adjusted, and the pretreatment step, the carbonization step and the graphitization step may be made at least one step selectively.

On the other hand, the continuous carbon fiber or carbon nanotubes fusion method using the spray according to the present invention for achieving the above object, by forming a liquid resin by stirring a solution for dissolving the water support material and the water support material step; Stirring the catalyst and the solution dispersing the catalyst to form a catalyst dispersion; Mixing the liquid resin and the catalyst dispersion to form a resin catalyst mixture; Spraying the resin catalyst mixture into a reactor, the temperature of which is controlled by a heater and filled with a gas for the reaction; Pretreatment at the top of the reactor while the resin catalyst mixture sprayed on the reactor falls; Carbonizing at the reactor stop while dropping the pretreated resin catalyst mixture at the top of the reactor; Graphitizing at the bottom of the reactor while the carbonized resin catalyst mixture is dropped at the reactor stop; And recovering carbon fibers fused with carbon nanotubes which have been subjected to the pretreatment, carbonization, and graphitization.

According to the carbon fiber manufacturing apparatus and method in which the continuous carbon fiber or carbon nanotubes are fused using the spray according to the present invention, the following effects are obtained.

First, by controlling a heater and a gas inlet in one reaction unit, it is possible to produce carbon fibers having various characteristics such as flame retardant fibers, carbon fibers or graphite fibers.

In addition, since each reaction is not performed separately in each reactor, but is continuously performed in one reactor, the yield may be increased.

In addition to the pure carbon fiber, by mixing and spraying the liquid resin and the catalyst dispersion liquid can be produced carbon fibers with carbon nanotubes grown.

In addition, the carbon fiber produced by controlling the pressure and the injection amount of the injection liquid injection nozzle, or by adjusting the ratio of the solution for dissolving the water support material and the water support material injected into the liquid resin forming portion to control the concentration of the liquid resin You can also adjust the shape and size.

In addition, the shape of the carbon fiber may be adjusted to a spherical shape or a filament shape by controlling the raw liquid injection nozzle.

1 is a view for explaining a continuous carbon fiber manufacturing apparatus using a spray according to an embodiment of the present invention.
2 is a view for explaining a continuous carbon fiber manufacturing method using the injection according to an embodiment of the present invention.
3 is a view for explaining a carbon fiber manufacturing apparatus fused with continuous carbon nanotubes using the injection according to an embodiment of the present invention.
4 is a view for explaining a method of manufacturing a carbon fiber fused with continuous carbon nanotubes using the injection according to an embodiment of the present invention.

DETAILED DESCRIPTION Hereinafter, exemplary embodiments of the present invention will be described with reference to the accompanying drawings, but some components irrelevant to the gist of the present invention will be omitted or compressed, but the omitted elements are not necessarily required in the present invention. The invention can be used in combination by those skilled in the art.

1 is a view for explaining a continuous carbon fiber manufacturing apparatus (hereinafter referred to as "carbon fiber manufacturing apparatus") using the injection according to an embodiment of the present invention. As shown in FIG. 1, the carbon fiber manufacturing apparatus according to the embodiment of the present invention includes a reaction unit 100, a stock solution supply unit 200, and a gas supply unit 300.

The reaction unit 100 includes a reactor 110, a heater 121, 122, 123, a raw liquid spray nozzle 131, an air supply nozzle 133, a gas supply nozzle 132, a gas discharge port 134, and a product discharge unit 140. It consists of.

The reactor 110 is provided with reaction spaces 111, 112, and 113 in a vertically extending cylindrical shape. A first heater 121, a second heater 122, and a third heater 123 are sequentially installed at the top, middle, and bottom of the outer periphery of the reactor 110. Therefore, the temperature of the reaction spaces 111, 112, and 113 inside the reactor 110 may be controlled by the operation of the heaters 121, 122, and 123.

The stock solution injection nozzle 131 and the air supply nozzle 133 are respectively installed at the upper end of the reactor 110. The stock solution injection nozzle 131 is connected to the stock solution supply unit 200 and sprays the liquid resin supplied from the stock solution supply unit 200 to the reaction spaces 111, 112, and 113 inside the reactor 110. Here, when the high viscosity liquid resin is injected through the raw liquid injection nozzle 131, the liquid resin tends to be stretched, so that carbon fibers having a long and thick shape (see the bottom left enlarged view of FIG. 1) may be manufactured. Here, it is also possible to use a rotary atomizer (not shown) as a method for injecting a liquid resin rather than a spray nozzle method. In the case of using an atomizer, the liquid resin is supplied by rotating and dispersing the liquid resin, so that the product is closer to a longer shape than a spherical shape.

In addition, the air supply nozzle 133 is connected to the outside of the reactor 110 to introduce the outside air into the reaction space (111, 112, 113). In this case, a pump (not shown) for introducing an external atmosphere through the air supply nozzle 133 may be provided.

The gas supply nozzle 132 installed at the bottom of the reactor 110 is connected to the gas supply unit 300 so that the gas necessary for the reaction can be supplied into the reactor 110. That is, the gas supply unit 300 is composed of a gas tank 310 and the gas supply control unit 320, the gas required by the control of the gas supply control unit 320 is discharged from the gas tank 310, the gas supply nozzle 132 It may be introduced into the reactor 110 through.

Here, the air supply nozzle 133 is installed at the top of the reactor 110 to supply air to the upper region of the reactor 110, the gas discharge port 134 is installed on the reactor 110, the reactor 110 The gas and the atmosphere supplied therein may rise upward in the reactor 110 to exit through the gas discharge port 134. Therefore, even if the atmosphere is introduced into the upper region of the reaction space inside the reactor 110, the atmosphere does not go down from the upper portion of the reaction space inside the reactor 110, it stays only in the upper region by the rising gas reactor 110 It is discharged to the upper gas discharge port 134. Therefore, even if all reaction spaces inside the reactor 110 are connected, the area where the air stays can be distinguished from the area where other gases stay.

At the lower end of the reactor 110, a product discharge part 140 through which product such as carbon fiber manufactured in the reaction spaces 111, 112, and 113 is discharged is installed.

The stock solution supply unit 200 includes a liquid resin forming unit 210 and a transfer pump 240.

When the liquid resin forming unit 210 has a space formed therein and a solution for dissolving the water support material and the water support material is added to the internal space, the injected water support material and the solution are uniformly agitated and the water support material is dissolved in the liquid resin solution. Is made.

The liquid resin forming unit 210 is connected to the raw liquid injection nozzle 131 through a transfer pump 240. Therefore, when the transfer pump 240 is operated, the liquid resin made in the liquid resin forming unit 210 is transferred to the raw liquid injection nozzle 131 so that the liquid resin is reacted inside the reactor 110 through the raw liquid injection nozzle 131 ( 111,112,113).

Hereinafter, a carbon fiber manufacturing method using the carbon fiber manufacturing apparatus shown in FIG. 1 will be described with reference to FIG. 2.

First, when a solution for dissolving a water support fee and a water support fee is added to the liquid resin forming unit 210 of the stock solution supply unit 200, the injected support material and the solution are uniformly provided by an agitator installed in the liquid resin forming unit 210. Agitated to dissolve the water support in the solution to form a liquid resin (S205).

Then, the transfer pump 240 is operated so that the liquid resin made in the liquid resin forming unit 210 is injected into the reaction spaces 111, 112, and 113 inside the reactor 110 through the raw liquid spray nozzle 131 of the reaction unit 100. S210>. At this time, when the high-viscosity liquid resin is injected through the raw liquid injection nozzle 131, the liquid resin tends to hang and is sprayed in a long and thick form. In addition, the outside atmosphere is supplied to the upper portion of the reaction space inside the reactor 110 through the air supply nozzle 133, and the gas for the reaction is supplied through the gas supply nozzle 132 below.

The injected liquid resin is sequentially dropped from the top to the bottom of the reaction space (111, 112, 113). In this case, the reaction spaces 111, 112, and 113 may be divided into three sections according to sections in which temperature is controlled by the heaters 121, 122, and 123 from an upper end to a lower end. That is, the space at the top of which temperature is controlled by the first heater 121 is called the first reaction space 111, and the space where the temperature is controlled by the second heater 122 is the second reaction space 112. The space at the lower end of the temperature controlled by the third heater 123 is referred to as a third reaction space 113.

The first reaction space 111 is a pretreatment section, and the temperature of about 200 ° C. to 400 ° C. is maintained by the operation of the first heater 121. When the liquid resin is pretreated <S215> in the first reaction space 111, it becomes a fireproof fiber.

The second reaction space 112 is a carbonization section, and the temperature of about 400 ° C. to 2000 ° C. is maintained by the operation of the second heater 122. The liquid resin is pretreated in the first reaction space 111 and carbonized in the second reaction space 112 to become carbon fiber. The carbonized fibers thus produced may be recovered through the product discharge unit 140 without being reacted in the third reaction space 113 and used as carbonized fibers.

However, when the reaction is made in the third reaction space 113 becomes graphite fiber. That is, the third reaction space 113 is a graphitization section, and the temperature of about 2000 ° C. to 3200 ° C. is maintained by the operation of the third heater 123. The liquid resin is pretreated in the first reaction space 111, carbonized in the second reaction space 112, and graphitized <S225> in the third reaction space 113 to become graphite fibers.

Thus, the product of the flame-resistant fiber, carbon fiber or graphite fiber (collectively referred to as 'carbon fiber') produced while the liquid resin injected into the reactor 110 passes through a pretreatment section, a carbonization section or a graphitization section is a reactor ( 110 is recovered through the product discharge unit 140 at the bottom <S230>. Of course, even in the process of product recovery through the product discharge unit 140, the liquid resin is continuously injected in the reactor 110 and the process is continuously performed in each section.

Here, the time that the liquid resin injected into the reactor 110 passes through each section may be controlled, which may be controlled by adjusting the amount of gas introduced from the bottom, or the geometry of the reactor 110 (the length of each section). , Width, installation of a barrier, etc.), or by attaching a mechanical element such as a separate fan (not shown) under the reactor 110.

Meanwhile, when the liquid resin is reacted in each section, an atmosphere of air, nitrogen (N 2), or argon (ar) should be formed. The atmosphere (including oxygen) may be introduced through the air supply nozzle 133. Nitrogen (N2) or argon (Ar) may be supplied from the gas supply unit 300 through the gas supply nozzle 132 installed at the bottom of the reactor (110).

That is, the gas supply unit 300 is composed of a gas tank 310 and the gas supply control unit 320, the gas supply control unit 320 is to introduce the gas required from the gas tank 310 into the reactor 110. .

The atmosphere or the gas supplied into the reactor 110 may be discharged to the outside through the gas discharge port 134 installed on the top of the reactor 110.

In addition, rayon-based carbon fibers, PAN-based carbon fibers, or pitch-based carbon fibers may be produced by controlling the temperature of the heaters 121, 122, and 123 and controlling the gas inflow.

In order to produce rayon-based carbon fibers, the first reaction space 111, which is a pretreatment section, is maintained in an air atmosphere and the temperature is adjusted to about 260 ° C. In addition, the second reaction space 112, which is a carbonization section, is maintained in an argon (Ar) and nitrogen (N 2) atmosphere, and the temperature is adjusted to 400 ° C. to 2000 ° C. The third reaction space 113, which is a graphitization section, is maintained in an argon (Ar) and nitrogen (N 2) atmosphere, and the temperature is adjusted to 3000 ° C. to 3200 ° C. Here, the atmosphere of the first reaction space 111 is supplied through the air supply nozzle 133, and the argon (Ar) and nitrogen (N2) atmospheres of the second reaction space 112 and the third reaction space 113 are reactors. Each atmosphere may be maintained by being supplied through the gas supply nozzle 132 installed at the bottom of 110.

In order to produce PAN (Polyacrylonitrile) -based carbon fiber to maintain the first reaction space 111, which is a pretreatment section in the air (Air) atmosphere and the temperature is adjusted to 200 ℃ to 300 ℃. In addition, the second reaction space 112, which is a carbonization section, is maintained in an argon (Ar) and nitrogen (N2) atmosphere, and the temperature is adjusted to 1000 ° C to 1500 ° C. The third reaction space 113, which is a graphitization section, is maintained in an argon (Ar) and nitrogen (N 2) atmosphere, and the temperature is adjusted to 2000 ° C. to 3000 ° C.

In order to produce pitch-based carbon fibers, the first reaction space 111, which is a pretreatment section, is maintained in an atmosphere (including air and O 2) and the temperature is adjusted to 300 ° C. to 390 ° C. In addition, the second reaction space 112, which is a carbonization section, is maintained in an argon (Ar) and nitrogen (N 2) atmosphere, and the temperature is adjusted to 1500 ° C. to 1700 ° C. The third reaction space 113, which is a graphitization section, is maintained in an argon (Ar) and nitrogen (N 2) atmosphere, and the temperature is adjusted to 3000 ° C. to 3200 ° C.

That is, by controlling the inflow of the heaters 121, 122, 123 and gas in one reaction unit 100, the flame retardant fiber, carbon fiber or graphite fiber may be produced separately.

In addition, since each reaction is not performed separately in each reactor, but is continuously performed in one reactor 110, the yield may be increased.

In addition, by controlling the pressure and the injection amount injected from the raw liquid injection nozzle 131, or by adjusting the ratio of the solution for dissolving the water support material and the water support material injected into the liquid resin forming unit 210 by adjusting the concentration of the liquid resin By adjusting the size of the carbon fiber produced. Here, the stock solution injection nozzle 131 may be applied with various technologies such as an atomizer, a spray nozzle, and ultrasonic spraying.

Hereinafter, with reference to Figures 3 to 4 will be described with respect to the carbon fiber manufacturing apparatus and method fused with continuous carbon nanotubes using the injection according to an embodiment of the present invention.

Figure 3 is a view for explaining a carbon fiber manufacturing apparatus (hereinafter referred to as "carbon nanotube fused carbon fiber manufacturing apparatus) fused continuous carbon nanotubes using the injection according to an embodiment of the present invention. As shown in FIG. 3, the carbon nanotube fused carbon fiber manufacturing apparatus according to the embodiment of the present invention includes a reaction unit 100, a stock solution supply unit 200 ′, and a gas supply unit 300.

The reaction unit 100 includes a reactor 110, a heater 121, 122, 123, a raw liquid spray nozzle 131, an air supply nozzle 133, a gas supply nozzle 132, a gas discharge port 134, and a product discharge unit 140. The detailed description will be omitted since the description will be sufficiently inferred from the description of the reaction unit 100 shown in FIG. 1.

The stock solution supply unit 200 ′ is composed of a liquid resin forming unit 210, a catalyst forming unit 220, a mixing unit 230, and a transfer pump 240.

When the liquid resin forming unit 210 has a space formed therein and a solution for dissolving the water support material and the water support material is added to the internal space, the injected water support material and the solution are uniformly agitated and the water support material is dissolved in the liquid resin solution. Is made.

When the catalyst forming unit 220 has a space formed therein and a solution for dispersing the catalyst and the catalyst is introduced into the internal space, the catalyst and the solution are uniformly stirred to form a catalyst dispersion.

The mixing unit 230 is in communication with the liquid resin forming unit 210 and the catalyst forming unit 220, respectively, when the liquid resin and the catalyst dispersion made in the liquid resin forming unit 210 and the catalyst forming unit 220 is added The liquid resin and the catalyst dispersion are stirred to form a resin catalyst mixture.

The mixing unit 230 is connected to the raw liquid injection nozzle 131 through the transfer pump 240. Therefore, when the transfer pump 240 is operated, the resin catalyst mixture made by the mixing unit 230 is transferred to the raw liquid injection nozzle 131, and the resin catalyst mixture is reacted with the reaction space inside the reactor 110 through the raw liquid injection nozzle 131. 111,112,113).

Hereinafter, with reference to Figure 4 will be described a carbon nanotube fused carbon fiber manufacturing method using the carbon nanotube fused carbon fiber manufacturing apparatus shown in FIG.

First, when a solution for dissolving the water support fee and the water support fee is introduced from the liquid resin formation unit 210 of the stock solution supply unit 200 ′, the injected support material and the solution are uniformly formed by the agitator installed in the liquid resin formation unit 210. It is stirred so that the water support material is dissolved in the solution to form a liquid resin <S405>.

In addition, when a solution for dispersing the catalyst and the catalyst is introduced in the catalyst forming unit 220 of the stock solution supply unit 200 ', the injected catalyst and the solution are uniformly agitated by an agitator installed in the catalyst forming unit 220, thereby dispersing the catalyst dispersion. It is made <S410>.

Here, the catalyst for growing carbon nanotubes may be Fe, Co, Al, Mg, Ni and the like. In addition, the catalyst may be a metal catalyst with a support prepared by a supporting method, a probe method, a sol-gel method, a combustion method, or the like, or a catalyst without a support having a predetermined composition such as Fe, Co, or Ni.

The liquid resin made from the liquid resin forming unit 210 and the catalyst dispersion made from the catalyst forming unit 220 are combined and stirred in the mixing unit 230 to form a resin catalyst mixture <S415>.

Thereafter, the transfer pump 240 is operated so that the resin catalyst mixture made in the mixing unit 230 is injected into the reaction spaces 111, 112, and 113 inside the reactor 110 through the raw liquid injection nozzle 131 of the reaction unit 100. >. At this time, when the high-viscosity resin catalyst mixture is sprayed through the undiluted jet nozzle 131, it tends to sag, and thus is sprayed in a long and thick form. In addition, the outside atmosphere is supplied to the upper part of the reaction space inside the reactor 110 through the air supply nozzle 133, and a gas for growing carbon nanotubes is supplied through the gas supply nozzle 132 below. It is a state.

The gas for growing carbon nanotubes supplied to the reaction spaces 112 and 113 through the gas supply nozzle 132 may be hydrocarbon, hydrogen, nitrogen, argon, or the like. have. These gases are discharged into the reaction spaces 112 and 113 through the gas supply nozzles 132 through the gas supply nozzles 132 are discharged only the gas or a combination of gases required by the control of the gas supply control unit 320 in the state stored in the gas tank 310.

The injected resin catalyst mixture is sequentially dropped from the top to the bottom of the reaction space (111, 112, 113). In this case, the reaction spaces 111, 112, and 113 may be divided into three sections according to sections in which temperature is controlled by the heaters 121, 122, and 123 from an upper end to a lower end. That is, the space at the top of which temperature is controlled by the first heater 121 is called the first reaction space 111, and the space where the temperature is controlled by the second heater 122 is the second reaction space 112. The space at the lower end of which temperature is controlled by the third heater 123 may be referred to as a third reaction space 113.

The first reaction space 111 is a pretreatment section, and the temperature of about 200 ° C. to 400 ° C. is maintained by the operation of the first heater 121. When the resin catalyst mixture is pretreated <S425> in the first reaction space 111, it becomes a fireproof fiber.

The second reaction space 112 is a carbonization section, and the temperature of about 400 ° C. to 2000 ° C. is maintained by the operation of the second heater 122. The resin catalyst mixture is pretreated in the first reaction space 111 and carbonized in the second reaction space 112 to become carbon fibers. The carbonized fibers thus produced may be recovered through the product discharge unit 140 without being reacted in the third reaction space 113 and used as carbonized fibers.

However, when the reaction is made in the third reaction space 113 becomes graphite fiber. That is, the third reaction space 113 is a graphitization section, and the temperature of about 2000 ° C. to 3200 ° C. is maintained by the operation of the third heater 123. The resin catalyst mixture is pretreated in the first reaction space 111, carbonized in the second reaction space 112, and graphitized <S435> in the third reaction space 113 to become graphite fibers.

The product such as flame retardant fiber, carbon fiber or graphite fiber produced while the resin catalyst mixture sprayed on the reactor 110 is passed through a pretreatment section, a carbonization section or a graphitization section is a product discharge part 140 at the bottom of the reactor 110. It is recovered through <S440>. Of course, even in the process of recovering the product through the product discharge unit 140, the resin catalyst mixture is continuously injected in the reactor 110 and the process is continuously performed in each section.

Here, the time for which the resin catalyst mixture injected into the reactor 110 passes through each section may be controlled, which may be controlled by adjusting the amount of gas introduced from the bottom, or the geometry of the reactor 110 (the Length, width, installation of a barrier wall, or the like, or by attaching a mechanical element such as a separate fan (not shown) to the bottom of the reactor 110.

In this case, a catalyst for carbon nanotube growth is mixed in the resin catalyst mixture sprayed into the reactor 110, and the atmosphere of the reaction spaces 111, 112, and 113 is a gas for carbon nanotube growth (H2, N2, Ar, Hydrocarbon, etc.). Is a state in which a high temperature atmosphere is maintained by the heaters 121, 122, and 123, and thus, carbon nanotubes can grow around the carbon fiber with the manufacture of the carbon fiber. That is, referring to the expanded product in the lower left of Figure 3, it can be seen that the carbon nanotubes are grown around the carbon fiber.

Meanwhile, air or gas supplied into the reactor 110 may be discharged to the outside through the gas discharge port 134 installed on the reactor 110.

In addition, it is possible to produce rayon-based carbon fiber, PAN-based carbon fiber or pitch-based carbon fiber through the temperature control of the heaters (121, 122, 123) and the control of the gas inflow, which is described in detail above, so that redundant description will be omitted. do.

Meanwhile, although the carbon nanotubes fused with carbon nanotubes as shown in FIG. 4 may be manufactured through the apparatus shown in FIG. 3, the liquid crystals may be formed in the same manner as the apparatus shown in FIG. The resin may be reacted to produce pure carbon fibers in which no additional carbon nanotubes are grown.

As described in detail above, according to the present invention, flame retardant fibers, carbon fibers, or graphite fibers may be produced by controlling the heaters 121, 122, 123 and gas inflow in one reaction unit 100.

In addition, since each reaction is not performed separately in each reactor, but is continuously performed in one reactor 110, the yield may be increased.

In addition to the pure carbon fiber, by mixing and spraying the liquid resin and the catalyst dispersion liquid can be produced carbon fibers with carbon nanotubes grown.

The foregoing description of the preferred embodiments of the present invention has been presented for the purpose of illustration and it will be apparent to those skilled in the art that various modifications, additions and substitutions are possible within the spirit and scope of the invention, And additions should be considered as falling within the scope of the claims of the present invention.

100: reaction unit
110: reactor
111: first reaction space
112: second reaction space
113: third reaction space
121: first heater
122: second heater
123: third heater
131: liquid injection nozzle
132: gas supply nozzle
133: air supply nozzle
134: gas discharge port
140: product discharge unit
200,200 ': Stock solution supply unit
210: liquid resin forming part
220: catalyst forming unit
230: mixing unit
240: transfer pump
300: gas supply unit
310: gas tank
320: gas supply control unit

Claims (7)

Reaction unit to which the stock solution is reacted, a stock solution supply unit for supplying the stock solution to the reaction unit and a gas supply unit for supplying gas to the reaction unit,
Wherein the reaction unit comprises:
A reactor having a reaction space therein;
A heater installed around the outside of the reactor to control a temperature of the reaction space;
Stock solution injection nozzles and air supply nozzles respectively installed on the inner top of the reactor;
A gas supply nozzle installed at an inner lower end of the reactor; And
Includes; product discharge unit is installed at the bottom of the reactor;
The stock solution supply unit,
A liquid resin forming unit which forms a liquid resin by stirring the added water support material and the solution for dissolving the water support material; And
And a transfer pump for supplying the liquid resin formed in the liquid resin forming unit to the stock solution injection nozzle side.
In the state where the air is introduced through the air supply nozzle to the top of the reaction space in the reactor, the gas is introduced through the gas supply nozzle to the stop and the bottom of the reaction space, by the operation of the transfer pump When the liquid resin formed in the liquid resin forming unit is sprayed through the stock solution injection nozzle, the injected liquid resin is sequentially dropped from the upper end of the reaction space inside the reactor to the lower end so that carbon fiber is produced by pretreatment, carbonization and graphitization. Continuous carbon fiber or carbon nanotube fused carbon fiber manufacturing apparatus using a spray.
The method of claim 1,
The heater is a continuous carbon fiber or carbon nanotube fused carbon fiber manufacturing apparatus using a spray, characterized in that the temperature can be controlled by dividing into at least one different area according to the reactor height.
The method of claim 1,
The stock solution injection nozzle is a continuous carbon fiber or carbon nanotube fused carbon fiber manufacturing apparatus using a spray atomizer, characterized in that composed of a rotary atomizer.
The method of claim 1,
The stock solution supply unit,
A catalyst forming unit for agitating the added catalyst and a solution for dispersing the catalyst to form a catalyst dispersion; And
When the liquid resin and the catalyst dispersion is introduced from the liquid resin forming unit and the catalyst forming unit, respectively, a mixing unit for forming a resin catalyst mixture by stirring the liquid resin and the catalyst dispersion;
The transfer pump supplies the resin catalyst mixture liquid formed in the mixing part to the stock solution injection nozzle side,
The gas supply unit, by supplying a gas for carbon nanotube growth through the gas supply nozzle to the stop and the bottom of the reaction space,
In the state that the atmosphere is introduced through the air supply nozzle to the top of the reaction space inside the reactor, the gas for carbon nanotube growth is introduced through the gas supply nozzle to the stop and the bottom of the reaction space, the transfer When the resin catalyst mixture formed in the mixing unit is injected through the stock solution injection nozzle by the operation of the pump, the injected resin catalyst mixture is sequentially dropped from the upper end of the reaction space inside the reactor to the lower end, pretreatment, carbonization and graphitization. By the continuous carbon fiber or carbon nanotube fused carbon fiber manufacturing apparatus using a spray so that the carbon nanotube fused carbon fiber is produced.
Stirring the solution for dissolving the water support material and the water support material to form a liquid resin;
Spraying the liquid resin into a reactor, the temperature of which is controlled by a heater and filled with a gas for reaction;
Pretreatment at the top of the reactor while the liquid resin injected into the reactor falls;
Carbonizing at the reactor stop while dropping the pretreated liquid resin at the top of the reactor;
Graphitizing at the bottom of the reactor while the carbonized liquid resin is dropped at the reactor stop; And
Recovering the carbon fiber after the pre-treatment, carbonization and graphitization process; Continuous carbon fiber or carbon nanotube fused carbon fiber manufacturing method using a spray comprising a.
The method of claim 5,
The inside of the reactor is controlled by dividing the temperature into at least one different area according to the height,
The pre-processing, carbonizing and graphitizing step is a continuous carbon fiber or carbon nanotube fused carbon fiber manufacturing method characterized in that at least one or more steps are selectively made.
Stirring the solution for dissolving the water support material and the water support material to form a liquid resin;
Stirring the catalyst and the solution dispersing the catalyst to form a catalyst dispersion;
Mixing the liquid resin and the catalyst dispersion to form a resin catalyst mixture;
Spraying the resin catalyst mixture into a reactor, the temperature of which is controlled by a heater and filled with a gas for the reaction;
Pretreatment at the top of the reactor while the resin catalyst mixture sprayed on the reactor falls;
Carbonizing at the reactor stop while dropping the pretreated resin catalyst mixture at the top of the reactor;
Graphitizing at the bottom of the reactor while the carbonized resin catalyst mixture is dropped at the reactor stop; And
Recovering the carbon fibers fused with the carbon nanotubes after the pretreatment, carbonization and graphitization process; continuous carbon fibers or carbon nanotubes fused carbon fiber manufacturing method using a spray comprising a.

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