KR20190032336A - Mixing chamber apparatus for fabrication of polymer composite material - Google Patents

Abstract

The present invention relates to an agitating apparatus for manufacturing a polymer composite material by agitating a raw material of a polymer material. More particularly, the present invention relates to an agitating apparatus for manufacturing a polytetrafluoroethylene-carbon nanotube composite material. In the present invention, an agitating chamber and a mixing screw provided in the agitating chamber are simultaneously rotated in opposite directions to perform agitation, and a sliding contact plate made of PTFE is formed on a lid fixed with respect to the rotating agitating chamber to realize a rotating sealing. The present invention provides an agitating apparatus for manufacturing a composite material by combining carbon nanotubes with PTFE which is difficult to bind with other materials by temperature and pressure control and rotation control.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polymer composite material,

The present invention relates to a polymer composite material such as a polytetrafluoroethylene-carbon nanotube composite material having an electroconductive function capable of replacing a metal by incorporating a carbon-based material into a polytetrafluoroethylene (PTFE) resin having excellent chemical resistance. To an agitating device for producing the agitator.

There are a large number of industries that deal with hazardous chemicals in the industrial field. Hazardous compounds are strong acids, strong alkalis, toxic substances such as hydrochloric acid, nitric acid, and sulfuric acid, and there are chemical manufacturing plant PCBs and plating plants that make semiconductor harmful compounds.

However, in recent years, there has been an increase in the leakage of harmful compounds, resulting in an increase in property losses due to environmental accidents, secondary accidents caused by the fires, and accidents. Analysis of this accident shows that the carelessness of the workers is the biggest and the following is the lack of facility management. The key to such facility management is the need for a highly sensitive sensor with excellent chemical resistance to detect fluid leaks.

For example, in the semiconductor industry, a device for detecting a solution leakage in a process of washing with an acidic solution, that is, a high sensitivity sensor, is required, and excellent electrical conductivity is required for fast signal transmission. Metals, which are excellent electrical conductors, are unusable because of their very low chemical resistance to acidic materials.

In this way, there is no material for the sensor that can not use the metal because of the corrosion of the material of the sensor, and particles must not be generated in the high clean management area such as the semiconductor.

Therefore, a new material suitable for the sensor needs to be solved. The new material should not generate particles, and must have a chemical resistance that is not corroded, and can withstand high temperatures, especially metals that function as high- New materials are needed.

Conventionally, as a material which can replace metals, composite materials in which a conductive filler for electric conductivity is mixed with a polymer resin have been developed and used in various fields. A fine metallic powder such as known carbon black, graphite, silver, copper, nickel, aluminum and the like can be uniformly dispersed as a conductive filler in the production of a polymer resin There is a method of dispersion.

However, in order for these conductive fillers to impart conductivity to the polymer, it is necessary to form a pathway in which the fillers have continuity between the particles in the polymer resin. That is, the metal particles or the carbon black particles are in close contact with each other in the material, so that the conductive particles can jumping electrons to each other

For example, when carbon black is blended with a urethane resin to impart electrical conductivity, about 15 to 30% by weight of carbon black is used relative to the weight of the resin. However, in order to obtain better conductivity, the carbon black is used in an amount of 40% It is required to be used.

However, the introduction of such a large amount of carbon black makes it difficult for the particles to be uniformly dispersed, reduces the melt viscoelasticity of the resin, and causes the filler particles to aggregate with each other, resulting in an extremely increased viscosity. As a result, the self-characteristics of the polymer resin is remarkably lowered, and problems such as contamination due to abrasion and short-circuiting of electric conductivity occur. On the other hand, in the case of using a metal powder, the metal powder has a specific surface area smaller than that of carbon black and must be compounded by an amount of 2 to 3 times or more to cause conductivity. In this case, the dispersibility becomes poor and the specific gravity becomes heavy.

Specific examples that disclose a method for imparting conductivity to a polymer resin or an elastomer include those disclosed in Japanese Patent Laid-Open Nos. 9-000816, 2000-077891, 6,768,524, 6,784,363, and 4,548,862 have.

Examples of conductive composite materials using polymer resins and carbon nanotubes are disclosed in Korean Patent Laid-Open Publication No. 10-2012-0077647, " Method for producing a composite material of polymer / carbon nanotubes ", Korean Patent Laid-Open Publication No. 10-2011-0078154 &Quot; Carbon nanotube-polymer nanocomposite material using fluidized bed multiwall carbon nanotubes, and a manufacturing method thereof ".

However, the above-described prior art techniques require a high enough chemical resistance, such as a sensor material for detecting leakage of harmful chemical substances, as well as a sufficient electrical conductivity enough to replace a metal, It was not suitable as a material for a high-sensitivity sensor for solution leakage in the process.

Therefore, it is required to develop new materials that can be used in specific places and environments where it is required to prevent contamination such as chemical resistance, chemical resistance, chemical resistance, low electric resistance, and clean process.

As a result, PTFE (Polytetrafluoroethylene) resin, which is known to have the best chemical resistance in polymeric materials with excellent chemical resistance, is selected and a multi-walled carbon nanotube, which is the most advanced nanomaterial known to have the highest electrical conductivity among the fillers Nanotube (MWCNT) is selected and MWCNT is synthesized as an electroconductive filler in PTFE with chemical resistance.

However, since PTFE is not well bonded to other materials due to its nature, it is difficult to develop PTFE as a composite material. In particular, a product combining CNTs is not known at present.

Therefore, there is a need to develop a separate stirrer capable of manufacturing a composite material by bonding CNT to PTFE.

Korean Patent Laid-Open No. 10-2012-0077647 " Method for producing polymer / carbon nanotube composite material " Korean Patent Laid-Open Publication No. 10-2011-0078154 "Carbon nanotube-polymer nanocomposite material applying fluidized-bed multiwall carbon nanotube and method for manufacturing the same"

SUMMARY OF THE INVENTION An object of the present invention is to provide a stirring device for producing a polymer composite material such as a polytetrafluoroethylene-carbon nanotube composite material having electrical conductivity in order to solve the above problems.

SUMMARY OF THE INVENTION [0008]

A stirring device for producing a PTFE-CNT composite material having an electric conductivity function by charging PTFE, CNT, and a metal coupling agent,

A stirring chamber installed to be rotatable for stirring the raw material;

A lid rotatably coupled with the upper surface of the stirring chamber to seal the upper surface of the stirring chamber;

A lid raising / lowering device for raising / lowering the lid to open / close the upper portion of the stirring chamber;

A mixing screw inserted into the stirring chamber 10 through the lid;

A stirring chamber rotating device for rotating the stirring chamber;

A mixing screw rotating device for rotating the mixing screw by rotating a rotating shaft passing through the lid;

A temperature regulating device provided on the lower surface of the lid for controlling the temperature in the agitator chamber;

A pressure regulator for detecting a pressure inside the stirring chamber through the lid and provided with a pressure variation, and regulating the pressure;

A control device for controlling the stirring chamber rotating device, the mixing screw rotating device, the pressure regulating device and the temperature regulating device by inputting and manipulating the setting of the driver;

The present invention provides a stirring device for producing a polymer composite material containing a polymer.

In addition, in the lid raising and lowering apparatus of the stirring apparatus for producing the polymer composite material of the present invention,

A ball screw coupling part formed on the lid and coupled to the lower end of the ball screw so as not to be detached from the lid and movable up and down at a predetermined interval;

A fixing piece fixed to a ball screw having a predetermined height from an upper surface of the lid;

And elastic means inserted between the fixing piece and the lid to elastically support the lid on the upper surface of the stirring chamber.

In addition,

And a plurality of impellers are installed on the rotary screw.

Wherein the rotating screw comprises:

The upper and lower impellers are provided on the rotary screw, and the upper impeller and the lower impeller,

And the impeller may have different shapes, or may be installed at different angles in the same shape, or may be any one of impellers having different sizes, or a combination thereof.

Further, the stirring apparatus for producing the polymer composite material according to the present invention

An upper rim of the stirring chamber and a lower rim of the lid corresponding thereto,

A stirring chamber sliding contact plate in which the stirring chamber rotatably and mutually slidingly contacts with the stopped lid, and a lid sliding contact plate.

Further, the sliding contact plate of the stirring chamber,

A step portion is formed at the outer end of the upper surface and the inner side is opened,

And the outer peripheral surface of the sliding contact plate of the lid is seated on the step portion so as to be caught by the engaging jaw.

The sliding contact plate of the stirring chamber is formed with a seating groove formed as a groove on an upper surface thereof, and a sliding contact plate of the lid is installed such that a part of the sliding contact plate is inserted into the seating groove.

Further, the lid is further formed with a protrusion protruding in a predetermined length having a diameter corresponding to the inner circumferential surface of the stirrer chamber, on the inside of which the sliding contact plate of the lid is formed.

Further, in the above temperature control device,

A thermoelectric element provided on a lower surface of the lid,

And the temperature control device controls the driving current direction and the driving time for driving the thermoelectric element based on the measured temperature from the temperature sensing means for measuring the temperature inside the stirrer chamber to perform heating or cooling control.

The stirring device may further include a stirring chamber tilting device capable of tilting the stirring chamber so that the lid is opened and the stirring chamber is tilted so that the internal stirring material can be poured into another container.

Further, in the stirring chamber of the stirring apparatus according to the present invention,

Can be made of a single cylinder. In this case, the temperature is controlled by the ambient temperature at which the stirring device is installed without any separate temperature control for the stirring chamber itself.

In another embodiment of the stirring chamber,

In order to control the temperature effectively, it is made up of a double tube in which the inner passage outer body is integrally formed, a temperature controlling medium is injected between the inner and outer tubes, and the temperature of the temperature controlling medium is controlled during the stirring chamber stopping, . In this case, the structure is configured to rotate the entire agitation chamber made of the inner passageway.

In addition, another embodiment of the stirring chamber may include:

Wherein the stirring chamber is formed of a separating type in which the inner passage and the outer cylinder are separated from each other, and the inner cylinder is rotated, and a temperature control medium is injected between the inner and outer passages, And a control device is installed.

In addition, in the structure for rotating only the inner cylinder, it is also possible to further include a heating means for directly heating the temperature control medium between the inner and outer passages, and a cooling means for cooling.

The heating and cooling means may be configured to use a thermoelectric element using a Peltier effect and automatically control the on / off and current direction by automatically detecting the temperature of the temperature control medium and following the set temperature.

Further, in the present invention,

And controls the mixing screw rotating device and the stirring chamber rotating device to rotate in directions opposite to each other.

The mixing screw rotating device is rotated at 5,000 to 15,000 RPM, and the stirring chamber rotating device is rotated at 10 to 100 RPM.

Also, the apparatus for controlling the temperature of the stirring chamber controls the initial temperature to be 10 to 30 ° C. and the temperature to be controlled within a temperature range of 10 to 100 ° C. after the start of stirring.

In addition, the pressure control device of the stirring chamber controls the initial pressure to 1 to 10 N / cm 2, and controls the pressure to be in the range of 10 to 20 N / cm 2 after the start of stirring.

The pressure adjusting device of the stirring chamber is characterized in that the pressure in the stirring chamber is controlled to be within a set pressure range by injecting or exhausting air or gas.

In addition, the PTFE is loaded with a raw material having a size of 10 to 50 nm, a solvent is added to the organic solvent, and the size of the PTFE is adjusted to 0.5 탆 or less by a stirring process to prevent re-agglomeration of the PTFE.

Also, the multi-walled carbon nanotubes are dispersed in 5 to 15 nm.

As the GRAFT catalyst, a metal coupling agent is used.

On the other hand, as a material of a sensor for detecting the leakage of harmful compounds having strong alkaline toxicity in places such as semiconductor processing, chemical manufacturing process, PCB manufacturing process and plating process, polytetrafluoroethylene-carbon Nanotube composite materials can be used.

The present invention relates to a stirring device for producing a PTFE + CNT composite material having an electroconductive function, which comprises a rotating screw installed so as to be able to rotate at a high speed inside a stirring chamber, and a stirrer chamber itself, There is an effect that can be performed.

It is another object of the present invention to provide a structure for sealing the upper inlet of a stirring chamber, which is a rotating body, with a lid of a fixed chain, thereby realizing a stirring process for rotating the inner rotating screw in the opposite direction while rotating the chamber, It is possible to provide a structure in which pressure leakage is not generated.

Further, in order to adjust the internal temperature of the stirring chamber, which is a rotating body, it is possible to provide a thermoelectric element on the bottom surface of the lid so as to be heated and cooled, thereby easily adjusting the temperature in the rotating body.

In addition, according to another embodiment of the present invention, the stirring device is formed as an integral unit of the through-pass pipe, a heat exchange medium is injected therebetween, and the temperature inside the stirrer chamber is adjusted by adjusting the temperature of the heat exchange medium. This makes it possible to uniformly control the temperature inside the stirrer chamber, thereby obtaining a uniform stirring effect of the stirring material.

According to another embodiment of the present invention, there is provided a stirrer chamber in which a stirrer chamber is constituted by an inner passage outer cylinder, a structure in which only inner cylinder is rotated, a temperature control medium is injected between the inner passage and the outer cylinder, Or the temperature can be controlled by cooling. This is effective for processes requiring precise temperature control since the temperature can be precisely controlled even during the manufacturing process of rotating the stirrer chamber.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a classification comparison chart of electrical resistance of a composition to which electrical conductivity is imparted to a polymer resin. FIG.
2 is a manufacturing process diagram for explaining an embodiment of the present invention.
3 is a graph of change in electrical resistance according to the amount of carbon nanotubes according to the present invention.
Fig. 4 is a comparative photograph of measurement of gloss and contamination of a surface according to the present invention. Fig.
FIG. 5 is an explanatory view illustrating measurement of electric volume resistance of a PTFE + MWCNT composite material according to the present invention. FIG.
6 is a schematic diagram of a polymer resin composite stirring apparatus according to the present invention.
7 is a block diagram of a polymer resin composite stirring apparatus according to the present invention.
8 (A) and 8 (B) are diagrams showing the configuration of the lid resilient supporting means of the stirring apparatus according to the present invention.
9 and 10 illustrate exemplary sliding contact plates in accordance with an embodiment of the present invention.
11 is a conceptual diagram illustrating another embodiment of the stirring chamber according to the present invention.
12 is a conceptual diagram illustrating another embodiment of the stirring chamber according to the present invention.

Hereinafter, the production of a composite material of PTFE + CNT and the electric resistance value of the PTFE + CNT will be described in detail with reference to the accompanying drawings, which show a superconducting polymer resin as a resistance value capable of replacing metals. . The application and modification contents not described here are sufficiently technically inferior to those skilled in the art, so that the description thereof will be omitted.

The present invention provides a stirring device for producing a polytetrafluoroethylene-carbon nanotube composite material having an electrically conductive function by bonding carbon nanotubes for imparting electrical conductivity to polytetrafluoroethylene (PTFE).

The polytetrafluoroethylene (PTFE) is a material excellent in chemical resistance, non-tackiness, antifouling property, heat resistance and friction characteristics, and carbon nanotubes are used to impart electric conductivity which is insufficient in PTFE, so that the whole composite material has electric conductivity do.

Accordingly, the present invention can provide a composite material having excellent electrical conductivity such as a metal while maintaining the basic properties of polytetrafluoroethylene.

The present invention was developed based on polytetrafluoroethylene (PTFE) (CF ₂ CF ₂ ), which is superior in chemical stability among polymer materials.

Polytetrafluoroethylene (PTFE) is excellent in various properties such as chemical resistance, electrical characteristic, non-tackiness, antifouling property, heat resistance and friction characteristics. PTFE materials are commonly used in various applications such as sealing of rotors, friction and gaskets, o-rings, chemical transfer pipes, heat-resistant anti-fouling films, It is widely used in industry.

Since PTFE (Polytetra fluoroethylene) does not accept other external substances, the chemical and antifouling properties are the best among the existing polymer materials. However, due to such excellent properties, it is very difficult to impart electrical conductivity to PTFE (Polytetra fluoroethylene) polymer resin with a special function.

On the other hand, to replace the metal, the electrical resistance should show a minimum resistance (<1.0E + 00Ω.cm Volume Resistivity).

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a classification comparison chart of electrical resistance of a composition to which electrical conductivity is imparted to a polymer resin. Fig.

A general polymer resin is an insulator having a volume resistivity (hereinafter, referred to as "electric resistance") (<1.00E + 13Ω.cm to 1.00E + 14Ω.cm ↑), and a conductive filler is injected into the polymer resin, (Dissipative) of electrical resistance (l.00E + 04Ω.cm to 1.00E + 06Ω.cm), electrical resistance of the resistor (1.00E + 07Ω.cm to 1.00E + 12Ω.cm) (1.00E + 01Ω.cm to 1.00E + 3Ω.cm), and conventional compositions containing a conductive filler added to the polymer resin are applicable. The electric resistance of general PTFE resin shows (1.0E + 15Ω.cm).

The electrical resistance required to replace the metal is less than 1.00E + 00 ?. OMEGA. Cm. However, it has not been possible to achieve a low electrical resistance (volume resistivity of 1.0E + 00 ?. to 1.0E-02? The PTFE + MWCNT composite material ('patented composition') realized electrical resistance of (1.00E-01Ω.cm to 1.00E-02Ω.cm volume resistivity).

(1.0E + 00.OMEGA.cm to 1.0E-02. ohm): 1.0 is an integer, indicating that + is not a positive number, and 00 to a negative power of 10 and a minus 2 power of -0210.

In order to impart electric conductivity to a polymer material of PTFE (Polytetrafluoroethylene) by applying a method for imparting electrical conductivity to a general polymer resin, one or more of carbon-based carbon black, carbon nanotubes, graphene, But it is very difficult to synthesize, and there is no domestic material producer.

In terms of competition, there is no composite material that synthesizes PTFE and CNT globally, so it can not be directly compared, but the company that is the most advanced in this field can be regarded as Saint Gobain of France. St. Govain uses carbon black as a conductive material, which is problematic for use in high-clean areas due to particles. The specification of conductive PTFE product of Goba is very different from -2 ohm which can be used as a substitute metal as 3 ohms in electric resistance. Another company is Dyneon Corp, which has a durability and application limitations because the material is in the form of ink using Carbon Black (INK).

In addition, graphene, carbon black, graphite, carbon fibers and the like are inferior to carbon nanotubes in terms of electrical conductivity. In order to jumping electrons to each other, conductive particles must be added in a large amount, , Abrasion, and contamination. In the electrically conductive region, a mixture of carbon nanotubes and one or more materials has a good effect, but a contamination due to a short circuit occurs when mixed.

Further, the above-mentioned PTFE product of Goba can not have electrical conductivity enough to replace the metal (< 1.0E + 03 ?. cm. Volume resistivity) and is difficult to use in places such as a sensor field requiring sensitivity. There are many limitations in the field of use.

Accordingly, the present invention solves the problem of contamination by abrasion or the like, and it is solved by solely injecting the carbon nanotubes as a conductive filler, and the problem of the electric conductivity is solved by using a carbon nanotube and PTFE in a graft method To combine with PTFE on a matrix to maximize the electrical conductivity of carbon nanotubes and solve the problem of short circuit contamination. Here, the carbon nanotubes may be single wall carbon nanotubes or multi wall carbon nanotubes, but multiwall carbon nanotubes are used in the aspect ratio.

In the present invention, PTFE, MWCNT, and an organic solvent are placed in a stirring chamber and stirred. Then, a metal coupling agent is added thereto and stirred, and then the organic solvent is removed using a centrifuge to prepare a composition. A multi-walled carbon nanotube (PTFE) is added to the polymer substance PTFE (Polytetra fluoroethylene) so as to have electrical conductivity such as resistance (<1.0E + 00Ω.cm to 1.0E-2Ω.cm volume resistivity) It is possible to provide a PTFE + MWCNT composite material having an electric conductivity function that maintains the properties such as chemical resistance, abrasion resistance, high heat resistance, and high gloss of PTFE while maintaining sufficient electrical conductivity to replace the metal.

[Example 1]

2 is a manufacturing process diagram for explaining an embodiment of the present invention.

The order of PTFE + MWCNT composites composition was 100 weight%

1. Preparation step (S10) of automatically cooling and heating the stirring chamber temperature by 30 to 60 degrees.

2. Add 10 wt% to 30 wt% of a PTFE powder (10um to 250um) resin into a stirring chamber, add 1 wt% to 10 wt% of MWCNT carbon nanotubes to a stirring chamber, add organic solvent VOC (Volatile Organic Compounds) 59.9 wt.% To 88.1 wt.%.

3. A primary agitation step (S30) in which the agitator mixing screw is driven to change the RPM of 5,000 to 15,000 while adjusting the agitator pressure (10 to 20 N / cm2) .

4. When the viscosity of the inside of the stirring chamber is 3,000 CPS to 5,000 CPS, a metal coupling agent is injected at a rate of 0.1% by weight to 0.9% by weight of the metal coupling agent (S40).

5. Second stirring step (S50) in which the reaction is stopped by stirring the reaction for 30 minutes to 60 minutes after the metal coupling agent is added.

6. Transferring from the stirring chamber to the centrifugal separator to remove the organic solvent in the liquid phase (S60).

7. A low-temperature drying step (S70) in which the remaining gas (< 50 PPM) of the composite material composition in which the liquid organic solvent is removed is managed.

8. The composite material completed in the low-temperature drying step (S70) may be pulverized into a suitable size for commercialization and then commercialized as a powder, or may be formed into a sheet or a bar using powders.

In the manufacturing method according to the present invention,

In preparation step S10, PTFE powder, MWCNT powder, organic solvent and metal coupling agent are prepared as raw materials. Here, the MWCNT may use single-walled carbon nanotubes, and preferably multi-walled carbon nanotubes. In addition, carbon nanotubes use a dispersed MWCNT as a material having its own aggregation phenomenon. That is, a van der Waals force is weakened to prepare a dispersed MWCNT in which the aggregation due to the ambient temperature is removed. The stirring chamber is adjusted to a suitable temperature. In the experiment of the present invention, the temperature is adjusted to 30 to 60 ° C.

In the raw material input step S20, PTFE powder, MWCNT powder, and organic solvent are introduced. The organic solvent is solvent, and PTFE is put into a size of 10-50 nm. When the organic solvent containing solvent is added and stirred, the PTFE's van der Waals force is weakened Thereby preventing re-aggregation. The CNTs are loaded with 5 to 15 nm of dispersed multiwall carbon nanotubes (MWCNT).

In the primary stirring step (S30), the rotating screw inserted in the stirring chamber and the stirring chamber itself are rotated and stirred. At this time, the temperature and pressure inside the stirring chamber should be appropriately adjusted. The temperature starts stirring at about 10 ° C or higher as set in the preparation step, and the pressure starts stirring at a pressure of about 1 atm, that is, 10 N / cm 2. That is, in the initial start step, stirring can be started at normal room temperature and atmospheric pressure without separately adjusting pressure and temperature. However, during the stirring, the temperature rise and the pressure increase, so it is necessary to adjust to keep the temperature and pressure range obtained experimentally. Preferably, the temperature is increased to 10 to 30 DEG C at the start of stirring, but not more than 100 DEG C in the stirring step, stirring is started at a pressure of 10 N / cm2 at the start step, / Cm &lt; 2 &gt;.

In the stirring method, the rotating screw in the stirring chamber is rotated while varying the speed in the range of 5,000 to 15,000 RPM, and the stirring chamber is rotated while varying the speed in the range of 10 to 200 RPM. At this time, the rotating screw in the stirrer and the stirring chamber are rotated in opposite directions to perform double reverse rotation, so that the rotational pressure to be received by the materials to be agitated is doubled, so that stirring is further performed. The internal pressure and the temperature are raised by high-speed rotation stirring. The pressure is limited to about 10 N / cm 2 to 20 N / cm 2, and the temperature should not exceed 100 ° C. Temperature and pressure can be adjusted by controlling temperature control device and pressure control device in the stirring chamber and by controlling the rotating speed of stirring.

In the step of injecting the metal coupling agent (S40), when the viscosity of the stirring material is a predetermined viscosity, the metal coupling agent is charged with the capacity according to the predetermined recipe. It is difficult to measure the viscosity of the substance to be stirred in the stirring chamber. Therefore, the primary stirring time is determined experimentally to determine the viscosity of the raw material to be 3,000 CPS to 5,000 CPS in accordance with the total amount of raw material input, and the primary stirring time is determined. Accordingly, when the primary stirring time corresponding to the total amount of the starting material is elapsed, the viscosity of the stirring internal material is expected to be in the range of 3,000 to 5,000 CPS, and when the primary stirring time has elapsed, the metal coupling agent is introduced .

The metal coupling agent is a metal oxide based (C 60 H 123 O 15 P 3 Ti) nanocoupling agent which is added at a weight of 100% by weight to increase the affinity and reactivity between the PTFE and one or more materials and the interface 0.3% by weight to 0.6% by weight.

The second agitation step (S50) is a step of injecting a metal coupling agent and performing reaction stirring, and the temperature, pressure, and time are experimentally determined and a secondary stirring step is performed according to the determined recipe. When the secondary agitation is carried out, the solid absorbs the gas and the liquid to form an 80 wt% paste-state intermediate product.

In the organic solvent removing step (S60), the paste-like intermediate product produced by the stirring step is transferred to a centrifuge to separate liquid and gas.

In the low-temperature drying step (S70), the organic solvent in the liquid state is removed from the intermediate product, and the intermediate product in the paste state is dried at low temperature together with the dehumidification. If desired, the desired composition can be obtained by making it bake by low temperature drying.

Thereafter, the thus obtained composition is made into a product according to the intended use. Powdered powder obtained by crushing the baked composition into a pulverized composition or a sheet or rod obtained by crushing the powder into a sheet or rod is extruded or otherwise produced into a desired shape.

The present invention provides a PTFE + CNT composite material having an electrically conductive function manufactured by the above-described production method.

The optimal ratio, optimal pressure, and optimal temperature conditions for PTFE + CNT agitation,

(C60H123O15P3Ti) Nano Coupling Agent Weight was added in an amount of 0.3% by weight to 0.6% by weight in 100% by weight of the weight of the PTFE and one or more materials to improve the affinity and reactivity between the interface and the interface. The chamber temperature was maintained at 60 to 70 ° C in the second stirring step, the graft method was performed under the conditions of a pressure of 10 to 20 N / cm 2, a mixing screw rotating speed of 5,000 to 10,000 RPM and a time of 30 to 60 minutes. , And the mechanical properties and electrical properties of PTFE were compared with each other [Table 1]. At this time, the best results were obtained in terms of mechanical properties, electrical properties and appearance.

The composite material obtained by synthesizing CNT with PFFE can be described as the following structural formula.

[constitutional formula]

(n is an integer)

The left side of the above [Structural Formula] is a basic structural formula of PTFE, and the right side is a structural formula for a composite material of the present invention having CNT bonded to PTFE. That is, in the unit structure of PTFE, one "F" is replaced with "CNT". The present invention is not a simple mixing of powders but a graft polymerization method.

Heat is applied to the bond between the PTFE molecules to increase the potential between the molecules. The optimum temperature is the ideal temperature of PTFE melting point (about 325 ℃), but unfortunately PTFE is hardened by heat and grafting process with carbon nanotubes is impossible.

Therefore, the high heat should be done in the final product molding operation. In this developed product, a pressure chamber is used to widen the distance between the molecules by using the minimum heat. The pressure is increased from 10 N / Lt; 2 &gt; Through the above-described experiment, it was confirmed that the composition of the present invention has better physical properties than those of conventional products.

In addition, the carbon nanotubes used in the present invention were prepared by dispersing MWCNTs having improved bundles, and the Aspect Ratio had an aspect ratio (diameter) of 5 nm or less and a length of 50 nm or less Respectively. In this study, the aspect ratio of the composition was the most excellent.

3 is a graph of electrical resistance change according to the amount of carbon nanotubes according to the present invention.

In order to obtain a low resistance value, the weight% of the carbon nanotubes in the composition weight 100% by weight is 3 to 4% by weight, the volume resistivity is 1.0E + The weight of 1.0E-02? Cm is preferably 4 to 6%, and in order to obtain a further lower resistance value, 7 to 10% by weight is added, but the electrical resistivity volume resistivity 1.0E-02? . The target value of the experiment was expected to decrease in proportion to increasing the CNT input amount, but it can be seen that there is a convergence section in which there is substantially no change in resistance.

3, when the CNT is not added to the PTFE, the electric resistance is 1.0E + 14 ?. cm, the electric resistance is 1.0E-01? 占 시 m when the CNT is 5wt%, the electric resistance is 6wt% The electric resistance of 1.0E-02 ?. cm was obtained and the electrical resistance at 1.0 wt% of CNT was 1.0E-02 ?. cm.

In this experiment, the carbon nanotubes showed a maximum range of 1.0E-02? 占 함 m of the composition weight 100% by weight of the sugar content of 6 wt% to 7 wt%, and the convergence interval in which the electrical resistance did not change was confirmed even when the addition amount was increased.

(C 60 H 123 O 15 P 3 Ti) nanocoupling agent at a weight of 100% by weight and a weight of 0.3 wt% to 0.6 wt% in order to increase the affinity and reactivity between PTFE and one or more materials and the interface %, And the graft polymer was prepared by maintaining the chamber temperature at 60 ~ 70 ℃ and pressure 10 ~ 20N / ㎠, mixing screw 5,000 ~ 10,000 RPM and time 30 ~ 60 minutes. The polytetrafluoroethylene (PTFE) ) And mechanical properties and physical properties.

Comparison of mechanical properties and physical properties of conventional PTFE (polytetrafluoroethylene) and R & D PTFE
The tensile strength
kgf / cm2
ASTM D638
Flexural elasticity
kgf / cm2
ASTM D790
Impact strength
kqf / ㎠
ASTM D256
importance
ASTM D792
Exterior
resistance
Ω.cm
ASTM D257
Existing product

250 to 350
4,650
10-12
2.0 to 2.2
Great
1.0E + 02 ~ 03
The present invention product

400 to 500
5,800
11-13
2.0 to 2.2
Very good
1.0E-01 to -02

Here, the existing product is a conductive PTFE product of St. Gobain, France, and the existing product was compared with the present invention product produced by the present invention. Compared with the conventional carbon black added product, the product according to the present invention is improved almost in the field of measurement, and it can be seen that it has a low electric resistance which is possible to substitute metal.

In the present invention, a sheet having a composition of 0.3 mm in thickness was prepared, specimens were produced by a conventional method, and tensile strength, flexural elasticity, impact strength and specific gravity were measured and compared, and appearance was visually judged. And the result is measured through a measuring device. As a result of comparing the existing product with the present invention product, the tensile strength, flexural elasticity and impact strength were superior to those of the conventional products, the specific gravity was the same, and the appearance was excellent. Especially, And it is found that the resistance value for the purpose of replacing the metal is sufficiently realized.

FIG. 4 is a comparative photograph of measurement of gloss and contamination of the surface according to the present invention, and FIG. 5 is an explanatory diagram of electric volume resistance measurement of a PTFE + MWCNT composite material according to the present invention.

The composition of the present study and the existing products and research and development products were made into a film of 0.3 mm, and the state of the surface and the degree of contamination were measured and verified.

In the first photograph on the left side of Fig. 4 (a), 1. General conductive PTFE samples of conductive PTFE containing carbon black of the existing foreign company were sampled, which resulted in sludge generation due to abrasion and electrical conductivity short-circuit . 2. The CNT 5% + PTFE in the middle photograph (B) is for a composite material synthesized by adding 5 wt% CNT to PTFE, and the surface state is poor due to the appearance of white spots and pinholes on the surface state . 3.CNT5% + PTFE + CA in the right picture (c) shows the result of synthesizing 5 wt% of carbon nanotubes and coupling agent into PTFE, showing excellent results in surface roughness and dispersed contamination state . That is, when 5 wt% of CNT was added to PTFE, a metal coupling agent (C.A.) was added and stirred to obtain the best result.

Comparative evaluation of composition (?: Very good,?: Good,?: Fair, X: poor)
▶ Existing conductivity
PTFE
▶ Carbon nanotubes 5%
▶ PTFE
▶ Carbon nanotubes 5%
▶ PTFE
▶ Coupling Agent
▶ Carbon nanotubes 8%
▶ PTFE
▶ Coupling Agent
Composition
Exterior illumination
○
X
◎
△
Composition
Internal cross-section
○
X
◎
△
Composition
Illumination and staining
X
△
◎
△

Here, conventional conductive PFTE samples a conductive PTFE to which Goba's carbon block is added. The appearance of the sample sheet was visually inspected for the appearance of each sample sheet, and the cross section of the inner surface was observed. The illuminance and the degree of contamination were the illuminance reflectance, and the degree of contamination was the degree of contamination Respectively. In addition, although it is not shown in the table, whether the electrical conductivity is uniform or not is measured by measuring the electrical conductivity at each position of the entire area of the sheet using a measuring contact as shown in Fig.

The electric volume resistance of the PTFE + CNT composite material according to the present invention was measured by preparing a sheet having a thickness of 0.3 mm as shown in Fig. 5 (a), preparing a specimen having a width of 1 inch, i.e., 15 cm x 10 cm x 0.3 mm , And foreign substances on the surface are removed. The volume resistance in the 1 inch / sq interval was measured according to the ASTM D257 measurement method using a low resistance meter (HIOKI M-3548) as in the second photograph of (B). The resistance of the measurement band was 1.0E + 14? The above conditions were maintained. The specimen prepared by the present invention, that is, the composite material prepared by stirring 5 wt% of CNT and coupling agent into PTFE was measured by the above measurement method, and as a result, the result of 1.0E-02? .

As described above, PTFE (Polytetrafluoroethylene) resin, which is known to have the highest chemical resistance among the polymer materials, was selected as described above. The electrical resistance of general PTFE resin shows the volume resistivity (1.0E + 15Ω.cm). The volume resistivity of 1.0E + 00Ω.cm to 1.0E-02Ω.cm, which is a low electric resistance range, has not been possible. However, the composition of the present invention has a volume resistance of 1.0E + 00Ω.cm to 1.0E-02Ω.cm )).

PTFE (Polytetrafluoroethylene) has already been widely used in the chemical industry. However, the electrical resistance of conventional conductive PTFE material (1.0E + 01Ω.cm to 1.0E + 03Ω.cm volume resistivity) It is developed by incorporating metal, which causes problems of wear and contamination.

Therefore, its use is extremely limited in certain places and environments where it is required to prevent contamination such as chemical resistance, chemical resistance, low electric resistance and clean process.

The present invention solves the above problems and maintains the PTFE (Polytetrafluoroethylene) own properties and realizes superior electrical resistance (1.0E + 00Ω.cm to 1.0E-02Ω.cm) than conventional products. It has proven to be very effective in pollution.

This result does not solve the problem of resistance and contamination simply because the content of the conductive material is increased. In order to overcome this problem, the present R & D composition has resulted in various experiments as shown in FIG. 3, FIG. 4 and [Table 1] and [Table 2].

We have succeeded in development of products with 10 times to 100,000 times better electrical resistance than existing conductive PTFE (Polytetrafluoroethylene) products and no pollution caused by carbon. This is the high price of conductive PTFE products that depend on national economic development and importation, , Has solved the A / S problem and can be widely used in various industrial fields such as semiconductor, chemical, medical, electromagnetic (EMC) design and so on.

As described in the present invention, the superconducting PTFE + CNT nanocomposite resin has been found to be superior to the conventional products, and it can be applied to various fields such as electric, electronic, communication, automobile, medical, Of the product.

As described above, in order to implement the PTFE + CNT composite material having the electric conductivity function of the present invention, an appropriate stirring device is required.

FIG. 6 is a schematic view of a polymer resin composite stirring apparatus according to the present invention, and FIG. 7 is a block diagram of a polymer resin composite stirring apparatus according to the present invention.

A stirring device for producing a PTFE-CNT composite material having an electric conductivity function by charging PTFE, CNT, and a metal coupling agent,

A stirring chamber (10) rotatably installed for stirring the raw material;

A lid (20) rotatably coupled to the stirring chamber (10) to seal the upper surface of the stirring chamber (10);

 A mixing screw 40 inserted through the lid 20 and inserted into the stirring chamber 10;

A stirring chamber rotating device 80 for rotating the stirring chamber 10;

A lid raising / lowering device 30 for raising / lowering the lid 20 to open / close the upper portion of the stirring chamber 10;

A mixing screw rotating device (50) for rotating the mixing screw (40) by rotating a rotating shaft passing through the lid (20);

A sliding contact plate 11 (see FIG. 1) (see FIG. 1) in which the stirring chamber 10 is rotatably and reciprocally slidably contacted with the upper end of the stirring chamber 10 and the lid 20 installed at the edge of the lid 20 corresponding thereto 21);

A pressure regulating device (70) for detecting a pressure inside the stirring chamber (10) through a lid (20) and provided with a pressure side, and regulating the pressure;

A temperature regulating device 60 provided on the lower surface of the lid 20 for controlling the temperature in the agitator chamber 10;

The lid ascending / descending device 30, the stirring chamber rotating device 80, the mixing screw rotating device 40, the pressure regulating device 70 and the temperature regulating device 60, A control device (100) for controlling by operation;

And a control unit.

Here, reference numeral 1 denotes a raw material to be stirred, and reference numeral 2 denotes an agitator chamber rotating support.

The stirring apparatus according to the present invention having the above-

The stirring chamber 10, in which the raw material is charged and rotated and stirred, is rotatably installed. Since the stirring chamber 20 is in the form of a container with an open upper part, a lid 20 is required for rotating stirring. The lid 20 is lifted up and down by the lifting and lowering device 30 and is brought into close contact with the stirring chamber 10 in a rotatable manner so as to maintain the closed state or to rise upward to open the stirring chamber 10.

The lid ascending / descending device 30 may have an optional structure. When the lid ascending / descending device is not provided, the lid ascending / descending device 30 may be provided with a lid fixing device for fixing the lid coupled to the upper portion of the stirring chamber. It is also possible to disassemble the fixing device, manually open and close the lid, and fix the lid by fixing the fixing device. In the present invention, a lid is lifted and lowered by an electric motor to open and close the lid.

The stirring chamber 10 is provided therein with a rotation screw 40 and a stirring chamber rotating device 80 for rotating the stirring chamber 10 itself. And can be rotated at a lower speed than the rotating screw, and the rotation driving, the rotating speed, the rotating direction, and the like can be controlled by the stirring chamber rotating device (80).

The rotary screw 40 has an example in which the rotating shaft passes through the lid 20 and two impellers are installed on the rotary screw in the upper and lower parts of the chamber. The upper and lower impellers may have the same size or the same shape, but the installation angles of the upper and lower impellers may be different from each other, or may be different from each other.

The rotating screw 40 is driven to rotate by a rotating screw driving device 50 which is driven by a motor outside the lid 20. [ When the upper and lower impellers are arranged in different shapes, the upper raw material may be downwardly moved downward by the lower impeller, the lower raw material may be upwardly swapped by the upper side by the upper impeller, and the irregular stirring . The size, shape, and installation angle of the upper and lower impellers are configured to obtain the optimum efficiency in consideration of the stirring efficiency.

The lid ascending and descending apparatus 30 includes a rotation nut means for vertically moving the ball screw 31 up and down on an upper support 33. The lid 20 is fixed to an end of at least one ball screw 31, 32 and is configured to rotate the motor 34 by connecting the rotational force of the motor 34 to the rotating nut means 32 through the belt 35. [

Accordingly, when the rotation nut means 32 is rotated in one direction, the ball screw 31 is moved in one direction. When the rotation nut means 32 is rotated in the other direction, the ball screw 32 is moved in the other direction. And the lid 20 is lifted up and down by using this.

 It is possible to raise or lower the lid by selecting the forward / reverse rotation of the motor 34 and to open the upper inlet of the stirring chamber 10 by raising the lid 20, or by lowering the lid 20, To close the upper inlet of the chamber (10).

8 (A) and 8 (B) are structural diagrams of the lid resilient supporting means of the stirring apparatus according to the present invention.

The lower end of the ball screw 31 is coupled to the lid 20 with an upper and lower clearance space so that the ball screw 31 can move up and down within the ball screw engaging part 23 at predetermined intervals. A fixing piece 37 fixed to the ball screw 31 may be formed and an elastic means 36 may be provided between the fixing piece 37 and the lid. 8 (B), when the lid is brought into contact with the upper surface of the stirring chamber as shown in (B) of FIG. 8, the ball screw 37 is inserted into the ball screw engaging portion 23 The elastic means 36 is compressed by the distance moved in the lid 20, and the lid 20 is elastically urged toward the upper surface of the stirring chamber, so that the sealing effect can be enhanced.

On the other hand, when the lid 20 is coupled to the stirring chamber 10, the lid 20 is stopped and the stirring chamber 10 is rotated, 10).

Accordingly, in the present invention, a sliding contact plate 11 having a circular donut shape is provided on the upper surface of the stirring chamber 10, and a sliding contact plate 21 is provided on the lower outer peripheral surface of the lid 20 Install it.

A protruding portion 22 is formed on the lower end surface of the lid 20 to be inserted into the container of the stirring chamber 10.

When the lid 20 is coupled to the stirring chamber 10, the projection 22 is inserted into the stirring chamber 10 and the sliding contact plate 11 of the stirring chuck and the sliding contact plate 21 of the lid are engaged with each other. Are in the form of butting together. When the stirring chamber 10 is rotated in this state, the upper and lower sliding contact plates 21 and 11 are in close contact with each other to seal the pressure inside the stirring chamber 10. When the sliding contact plates 11 and 21 are used as a general material, sealing between the contact surface and the contact surface is not perfect, heat generation or abrasion problems occur, and leakage of the internal pressure of the stirring chamber 10 occurs, It becomes difficult to maintain.

Accordingly, in the present invention, a circular annular plate made of a PTFE material (i.e., Teflon) is used as the sliding contact plates 11 and 21. In the present invention, the PTFE material is also used as a sealing material of the rotating body. In the present invention, the PTFE material is installed as the sliding contact plates 11 and 21 between the lower stirring chamber 10 and the upper lid 20 of the fixed chain, It is possible to securely maintain the sealed state against the pressure inside the chamber 10. At this time, the lifting device (30) of the lid (20) is further provided with resilient supporting means for supporting the lower portion elastically, thereby preventing pressure leakage due to pressure rise or rotation.

9 and 10 are illustrations of a sliding contact plate according to an embodiment of the present invention.

As shown in FIG. 9, the sliding contact plate 11 of the stirring chamber is formed with a step portion 11b formed at an outer end of the upper surface thereof and an inner side opened. The outer peripheral surface of the sliding contact plate 21 of the lid 20 is seated on the step portion 11b so as to be caught by the engaging step 11a.

The stirring chamber 10 and the lid 20 are brought into contact with the outer side surface of the projecting portion 22 of the lid 20 and the inner side edge of the diagonal chamber 10 and the inner side surface of the sliding contact plate 11, The upper surface of the jaw portion 11a and the inner surface of the engaging step 11a are in contact with the lower surface and the outer surface of the sliding contact plate 21 formed on the lid 20. [ Therefore, the contact path bent at a right angle in two stages is generated to improve the sealing force.

10 is an illustration of a sliding plate showing another embodiment. 10, a seating groove 11c is formed on the upper surface of the sliding contact plate 11 formed in the stirring chamber 20, and the lower surface of the sliding contact plate 21 formed on the lid 20 A protruding portion corresponding to the seating groove 11c and a step portion 21a corresponding to an inner engaging jaw portion of the seating groove 11c are formed.

The projecting portion of the sliding contact plate 21 of the lid 20 is inserted and seated in the seating groove 11c formed in the sliding contact plate 11 of the stirring chamber 10, The jaw portions are inserted into the step portions 21a of the sliding contact plates of the lid and are butt-joined to each other.

The outer surface of the projecting portion 22 of the lid 20 is brought into contact with the upper end inner surface of the stirring chamber 10 and the inner surface of the stirring chamber sliding contact plate 11, Since the protruding portion of the sliding contact plate 21 of the lid 20 is inserted into the inside of the lid 20, a contact surface bent at a right angle at a plurality of steps is generated, so that the sealing effect can be further improved.

Therefore, the sliding contact plate 11 of the stirring chamber 10 and the sliding contact plate 21 of the lid 20 according to the present invention are structured as a first plane type and are sealed by surface contact. When the stirring chamber 10 is rotated in a state in which the lid 20 is pressed against the stirring chamber 10 in a press-contact manner, the inner pressure of the stirrer chamber 10 is supported by the lifting and lowering device 30 of the lid 20, And the contact surfaces of the sliding contact plates 11 and 21 are in contact with each other without gaps due to the nature of the Teflon.

Second, in the structure in which the stepped portion is formed on one of the upper and lower sliding contact plates and the other sliding contact plate is seated on the stepped portion, at least two right-angled bent contact surfaces are generated. The sealing effect can be further increased.

Thirdly, if a seating groove-shaped groove is formed in one of the upper and lower sliding contact plates and a stepped portion is formed on the inner side of the other sliding contact plate corresponding thereto, the longer the interval of the contact surface, The sealing effect can be further improved.

A rotating screw 40 is provided through the center of the lid 20, and a pressure regulating device 70 is installed. Although not shown in detail in FIG. 1, a temperature controller 60 is required in the stirring chamber 10. In the manufacturing method, the control temperature in the chamber is less than 10 to 100 DEG C, and the temperature is maintained at 60 to 70 DEG C in the secondary stirring. Therefore, the heating / cooling means can be provided on the lower surface of the lid to control the stirring chamber internal temperature. As the heating / cooling means, a thermoelectric element using the Peltier effect can be used.

For example, a thermoelectric element is provided as a heating / cooling means on the lower surface of the protruding portion 22, a heat radiating plate of the thermoelectric element is connected to the external body of the lid, and the heat is radiated through the body of the lid. The current direction of the thermoelectric element can be controlled so as to follow the set temperature to selectively operate in the heating or cooling mode.

The pressure regulating device 70 is provided so that the pressure measuring device and the pressure regulating side are exposed through the lid 20 and exposed to the inside of the chamber and the pressure regulating device and the pressure side regulating device are installed outside to pressurize or exhaust the pressure The pressure regulating valve is connected to the pressure regulating valve, and the pressure regulating valve is opened and exhausted to lower the pressure. This can control the pressure inside the stirring chamber by the pressure required in the stirring production process.

11 is a conceptual diagram illustrating another embodiment of the stirring chamber according to the present invention.

As shown therein, in another embodiment of the stirring chamber,

The stirring chamber 10 is formed of a double tube in which the inner tube 110 and the outer tube 120 are integrally formed and the temperature control medium 91 is injected between the inner tube 110 and the outer tube 120 And a temperature control device 90 is provided for controlling the temperature of the temperature control medium 91 when the stirring chamber 10 is stopped and adjusting the temperature of the temperature control medium 91 from the outside.

The temperature regulating device 90 may be provided with a thermoelectric module. In another embodiment, a heat exchange circulating device for circulating the temperature control medium 91 through heat exchange from the outside may be provided as the temperature control device 90. Since the stirring chamber 10 is a rotating body, it is possible to control the temperature by connecting the control power of the thermoelectric element from the outside only in a state where the rotation is stopped. In the heating medium circulation system, the injection and outlet are connected to the heat- The temperature of the medium can be adjusted.

The reason why the stirring chamber 10 can be stopped and the temperature can be controlled is that the temperature required in the production of the PTFE + CNT composite material is not required to be finely adjusted or the high or low temperature is required, There is a point at which the temperature and pressure can be adjusted before the initial operation and before the start of the secondary stirring.

That is, at the time of the secondary agitation, the agitation chamber is stopped, and then the metal coupling agent is put into the reactor and then the secondary agitation is performed. Therefore, there is a stopping point of the agitation chamber. At this time, after adjusting the pressure and temperature of the agitation chamber, Followed by secondary stirring.

12 is a conceptual diagram illustrating another embodiment of the stirring chamber according to the present invention.

Another embodiment of the stirring chamber, as shown in Figure 12,

The stirring chamber 10 is constructed such that the inner cylinder 110 and the outer cylinder 120 are separated from each other and only the inner cylinder 110 is rotated and a temperature control medium 91 is provided between the inner cylinder 110 and the outer cylinder 120, And a temperature regulating device 130 for regulating the temperature of the temperature regulating medium 91 at the outside of the outer cylinder 120 is installed.

In the structure in which only the inner cylinder 110 is rotated, heating means for directly heating the injected temperature control medium 91 between the inner cylinder 110 and the outer cylinder 120 and cooling means for cooling are installed as a temperature control device Alternatively, a temperature control device having a structure for circulating the heat control medium through heat exchange from the outside may be provided. Here, water can be used as the heat exchange medium.

The temperature control device provided with the heating and cooling means uses a thermoelectric element using a Peltier effect and automatically detects the temperature of the temperature control medium 91 and automatically controls the on / It is also possible to configure it to be controlled.

When the stirring chamber 10 is constructed so as to be separated from the inner cylinder 110 and the outer cylinder 120 and only the cylinder 110 can be rotated by the stirring chamber rotating device 80, the inner cylinder 110 and the outer cylinder 120 120 may be filled with a heat exchange medium, for example, water, and the temperature of the stirring chamber may be adjusted during the process of rotating the inner cylinder 110.

Here, since the rotating speed for rotating the inner cylinder of the stirrer chamber is relatively low, the rotational force applied to the temperature control medium (e.g., water) filled between the inner and outer cylinders is low, However, it is preferable that a structure in which a sliding contact plate is provided between the upper end faces of the inner barrel outer tube to seal the inner barrel while the rotation is supported.

Therefore, the stirring apparatus according to another embodiment of the present invention has an advantage that the temperature control can be precisely performed.

The control apparatus 100 according to the present invention includes a user operation panel, and is configured to set control information based on a user operation through a user operation panel, and to control each apparatus.

Stirring operation of the polymer resin For example, when the stirrer is driven to produce the PTFE + CNT composite material, the lid 20 is raised by operating the lid lifting device 30 first. The agitating chamber 10 is opened and the agitating raw material is introduced. As a stirring raw material, a predetermined amount of PTFE, CNT and an organic solvent are mixed with a predetermined recipe, and the lid 20 is closed. In order to close the lid 20, the control device 100 actuates the lid lifting device 30 to lower the lid 20. The lid 20 is brought into close contact with the upper surface of the stirring chamber 10 at an appropriate pressure and the lid is closed. At this time, to move to the proper position, the up / down length is set as the control value of the motor or the sensor is installed to determine the up / down position.

In a state in which the lid 20 is closed, the control device 100 controls the set pressure and the set temperature. After the initial start pressure and temperature are adjusted, the primary screw rotation is started by driving the rotary screw rotation device 50 and the stirring chamber rotation device 80.

In this case, the control device 100 controls the mixing screw rotating device 50 and the stirring chamber rotating device 80 to rotate in opposite directions. By rotating in opposite directions, the rotational force of the internal raw material is doubled, so it is equivalent to applying an ultra-high rotational torque, and the potential of PTFE is increased based on temperature, pressure and rotational speed, Quot; CNT " becomes an excited state that can be alternatively combined.

The mixed screw rotating device 40 is rotated at 5,000 to 15,000 RPM while the stirring chamber rotating device 80 is rotated at 10 to 100 RPM. That is, the stirring chamber 10 is controlled at a low speed for the sake of safety and the inner rotating screw 40 is controlled at a high speed. At this time, each rotation speed is controlled by changing it. The change is controlled by varying the speed by a preset stirring pattern, for a predetermined time acceleration, a constant time deceleration, a constant time constant speed, and the like.

In addition, the temperature controller 60 of the stirring chamber controls the initial temperature to be 10 to 30 ° C., and the temperature is controlled to be 10 to 100 ° C. after the start of the stirring.

In addition, the pressure control device of the stirring chamber controls the initial pressure to 1 to 10 N / cm 2, and controls the pressure to be in the range of 10 to 20 N / cm 2 after the start of stirring.

 This may be done by starting the stirring at a normal room temperature and heating or cooling the temperature in a special case. After the primary stirring is completed and the metal coupling agent (CA) is added, the temperature and pressure are adjusted again, After adjusting the temperature and pressure, start secondary agitation.

The stirring apparatus further includes a stirring chamber tilting device, which is not shown in the drawing, but which can tilt the stirring chamber so that the lid is opened and the stirring chamber 10 is tilted so as to pour the internal stirring material into another container. That is, the stirring chamber 10 is inclined so that the internal intermediate product can be transferred to another container and boiled. When the second stirring step is completed, the paste and the gas liquid are mixed and transferred to a centrifuge, and the organic solvent in the liquid phase is removed by a centrifugal separator to obtain a paste-like resultant , Which is then dried to obtain the final product. Therefore, the stirring apparatus is configured so that the stirring chamber itself can be tilted so as to transfer the intermediate product obtained by mixing the liquid and the paste to the centrifuge.

As described above, the stirring apparatus according to the present invention is characterized in that the stirring screw is rotated in opposite directions to stir the raw material by rotating the rotating screw and the stirrer chamber so that they can rotate at a high speed in the stirring chamber . The second feature is that the upper inlet of the stirring chamber, which is a rotating body, is sealed by a fixed chain lid. This is because the sliding chamber is rotated while the lid is fixed and the sliding frictional contact plates using PTFE are provided so as to correspond to each other so that the rotation of the chamber in the raw material stirring process and the pressure in the chamber can be realized without pressure leakage. It is. The third feature is that the heating and cooling can be performed using the thermoelectric element to facilitate the temperature control of the stirring device.

In addition, according to another embodiment of the present invention, the stirring device is formed as an integral unit of the through-pass pipe, a heat exchange medium is injected therebetween, and the temperature inside the stirrer chamber is adjusted by adjusting the temperature of the heat exchange medium. This makes it possible to uniformly control the temperature inside the stirrer chamber, thereby obtaining a uniform stirring effect of the stirring material.

According to another embodiment of the present invention, there is provided a stirrer chamber in which a stirrer chamber is constituted by an inner passage outer cylinder, a structure in which only inner cylinder is rotated, a temperature control medium is injected between the inner passage and the outer cylinder, Or the temperature can be controlled by cooling. This is effective for processes requiring precise temperature control since the temperature can be precisely controlled even during the manufacturing process of rotating the stirrer chamber.

10: stirrer chamber 11, 21: sliding contact plate
20: lid 22: protrusion
30: lid lifting device 31: ball screw
32: rotation nut means 33: upper support
40: rotating screw 50: rotating screw rotating device
60, 90, 130: Temperature control device 70: Pressure control device
80: stirring chamber rotating device 91: heat exchange medium
100: control device 110: inner cylinder
120: outer tube

Claims (9)

A stirring device for producing a polymer composite material by stirring a raw material of a polymer material,
An agitating chamber in which an inner passage for introducing and stirring the agitating material and an outer container for separating the inner passage and the outer passage are spaced apart from each other;
A lid rotatably coupled with the upper surface of the stirring chamber to seal the upper surface of the stirring chamber;
A lid raising / lowering device for raising / lowering the lid to open / close the upper portion of the stirring chamber;
A mixing screw inserted into the stirring chamber through the lid;
A stirring chamber rotating device for rotating the stirring chamber;
A mixing screw rotating device for rotating the mixing screw by rotating a rotating shaft passing through the lid;
A pressure regulator for detecting a pressure inside the stirring chamber through the lid and provided with a pressure variation, and regulating the pressure;
A temperature regulating medium injected into a space between the inner passage and the outer chamber of the stirring chamber, and a temperature regulating device for regulating the temperature of the stirring chamber by regulating the temperature of the temperature regulating medium;
A control device for controlling the stirring chamber rotating device, the mixing screw rotating device, the pressure regulating device and the temperature regulating device by inputting and manipulating the setting of the driver; Lt; / RTI &gt;
A stirring chamber sliding contact plate provided at an upper edge of the stirring chamber and a lower edge of the lid corresponding thereto and having a stirring chamber rotatably mutually slidingly contacted with a stopped lid and a lid sliding contact plate,
The temperature regulating device includes:
Wherein the temperature control device is a temperature control device having a structure in which a temperature control medium is injected between the outer cylinder and the inner cylinder, and the temperature control medium is circulated through heat exchange from the outside.
The lid lifting / lowering device according to claim 1,
A ball screw coupling part formed on the lid and coupled to the lower end of the ball screw so as not to be detached from the lid and movable up and down at a predetermined interval;
A fixing piece fixed to a ball screw having a predetermined height from an upper surface of the lid;
And an elastic means inserted between the fixing piece and the lid to elastically support the lid on the upper surface of the stirring chamber.
[2] The apparatus of claim 1,
And a plurality of impellers are installed on the rotating screw.
[2] The apparatus of claim 1,
Two upper and lower impellers are installed on the rotary screw,
The upper and lower impellers,
Wherein the impeller has a different shape, has the same shape at different angles, or has an impeller of a different size or a composite structure thereof.
The method according to claim 1,
Wherein the sliding contact plate of the stirring chamber has a stepped portion formed with an engagement step at an outer end of the upper surface and an inner side opened,
And the outer peripheral surface of the sliding contact plate of the lid is seated on the step portion so as to be caught by the engaging jaw.
The stirring chamber according to claim 1, wherein a seating groove formed as a groove is formed on an upper surface of the sliding contact plate formed in the stirring chamber,
Wherein a protruding portion corresponding to the seating groove and a step portion corresponding to an inner engaging jaw portion of the seating groove are formed on the lower surface of the sliding contact plate formed on the lid.
The apparatus of claim 1,
Wherein a protruding portion protruding at a predetermined length having a diameter corresponding to an inner circumferential surface of the stirrer chamber is further formed on the inner side of the sliding contact plate of the lid.
The apparatus according to claim 1,
A thermoelectric module for heating or cooling the temperature control medium is installed between the outer cylinder and the inner cylinder, and a driving current direction and a driving time for driving the thermoelectric module are controlled to control heating or cooling And a temperature control device for controlling the temperature of the polymer composite material.
The stirring device for producing the polymer composite material according to claim 1,
Further comprising a stirring chamber tilting device capable of tilting the stirring chamber so that the lid is opened and the stirring chamber is tilted so that the inner stirring material can be poured into another container.

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