KR100367637B1 - Process for producing a polyaniline and an apparatus for the same in large quantities - Google Patents

Abstract

Disclosed are a manufacturing apparatus and a method for producing an optimal conductive polymer for the ideal mass production in the production of polyaniline, a conductive polymer. According to the present invention, 30 L of 1 M hydrochloric acid (HCl) solution is placed in a 60 L main reactor, and the aniline monomer is added thereto at a concentration of 0.22 Mol, and then dissolved while keeping the temperature of the main reactor cooled to 0 DEG C. Into a secondary reactor connected to the main reactor through a first pipeline and maintained at a temperature of 0 ° C., 20 L of a 1 M concentration of HCl solution was added to a concentration of 0.05 Mol (Ammonium peroxydisulfate, [(NH ₄ ) ₂ S ₂ O ₈ ]) is added to dissolve, and the first solution dissolved in the auxiliary reactor is introduced into the main reactor through the first pipeline and the internal temperature of the main reactor is maintained at 0 ° C. React for 90 minutes, introduce the reaction product of the main reactor through a second and third pipeline into the filter connected to the main reactor and then filter To obtain a cake-like form over the polyaniline precipitates. The polyaniline thus prepared is applicable to electrolyte materials for electrolytic capacitors and electromagnetic wave shielding materials, electrode materials for secondary batteries, conductive paint materials, resistance paste materials, antistatic materials, and the like.

Description

Process for producing a polyaniline and an apparatus for the same in large quantities}

The present invention relates to a conductive polymer production apparatus for the ideal mass production in the production of polyaniline (Polyaniline).

Conductive polymers are used as electrolyte materials for electrolytic capacitors, electromagnetic wave shielding materials, secondary battery electrode materials, conductive paint materials, resistive paste materials, and antistatic materials. In addition, it has excellent mechanical strength and electromagnetic properties. Therefore, researches for synthesizing conductive polymers having such characteristics and applying them to industry have been actively conducted, and may soon be spotlighted as cutting-edge new materials.

This trend has led to the need for a production apparatus and an optimum conductive polymer manufacturing process design for the ideal mass production in the production of polyaniline.

The present invention has been made to solve the above problems, the first object of the present invention is an electrolytic capacitor electrolyte material and electromagnetic wave shielding material, secondary battery electrode material, conductive paint material, resistance paste material, The present invention provides a method for producing polyaniline that can be applied as an antistatic material.

It is a second object of the present invention to provide a production apparatus for producing a conductive polymer having such characteristics.

1 is a view schematically showing the overall configuration of a conductive polymer manufacturing apparatus according to the present invention, and

FIG. 2 is an enlarged view of the filtration device shown in FIG. 1.

<Explanation of symbols for the main parts of the drawings>

10: conductive polymer manufacturing apparatus 13: floor frame

20: main reactor 21,31: motor

22,32: cover 24,34: control box

25,35: sight glass 30: auxiliary reactor

41,42,43: pipeline 51,52: fixed-supply pump

60: cooler 70: filtration device

76 funnel 78 filter

In order to achieve the first object described above, the present invention,

30 L of 1 M hydrochloric acid (HCl) solution was placed in a 60 L main reactor, and the aniline monomer was added thereto at a concentration of 0.22 Mol, and then dissolved while maintaining the temperature of the main reactor cooled to 0 ° C., separately from the first pipeline. Into the secondary reactor is connected to the main reactor through the cooling and maintained at a temperature of 0 ℃ 20L of 1M HCl solution was added to the concentration of 0.05Mol ammonium peroxydisulfate ([NH ₄ ) ₂ S ₂ O ₈ ]) is added to dissolve, the first solution dissolved in the auxiliary reactor is introduced into the main reactor for 10-20 minutes through the first pipeline, maintaining the internal temperature of the main reactor at 0 ℃, React for 90 minutes with stirring by a stirrer and react the reaction of the main reactor into a filtration device connected to the main reactor via second and third pipelines. After introducing water and filtered to provide a mass production method of producing a polyaniline, characterized in that to obtain a cake-like form of the polyaniline precipitates.

In addition, the present invention, in order to achieve the second object described above,

It is located a certain height upward from the bottom frame by a pair of first vertical frame extending vertically upward from the bottom frame, the built-in stirrer driven by the first motor disposed on the upper side, An auxiliary reactor sealed by a first cover, having a first cooling jacket disposed at a radial outer side, and a first control box disposed at one side thereof;

A pair of second vertical frames extending vertically upwardly from the bottom frame, spaced upwards from the bottom frame by a predetermined height, disposed at a lower position than the auxiliary reactor, and rotated by a second motor disposed above A main reactor having a built-in stirrer, the upper part of which is closed by a second cover, a second cooling jacket disposed at a radial outer side, and a second control box disposed at one side;

A first pipeline extending between said secondary reactor and said main reactor to direct mixed dissolved solution within said secondary reactor into said main reactor;

A filtration device connected to the main reactor via a second pipeline and a third pipeline, for filtering the mixed dissolved solution in the main reactor with a funnel arranged vertically in turn;

A second fixed feed pump disposed between the second pipeline and the third pipeline to regulate the amount of solution transferred from the main reactor to the filtration apparatus through the second pipeline and the third pipeline; ; And

It is disposed on the bottom frame, and provides a conductive polymer manufacturing apparatus comprising a cooling device connected to the cooling jacket through a refrigerant flow line to maintain a constant temperature condition of the main reactor and the auxiliary reactor. do.

Preferably, the first metered feed pump is disposed in the middle of the first pipeline.

According to the present invention by operating the mass production apparatus of the structure described above as an electrolytic capacitor electrolyte material and electromagnetic wave shielding material, secondary battery electrode material, conductive paint material, resistance paste material, antistatic material, etc. The polyanyl phosphorus which can be applied is mass-produced.

Hereinafter, a conductive polymer manufacturing apparatus and a manufacturing process according to the present invention will be described in detail.

1 is a view schematically showing the overall configuration of a conductive polymer manufacturing apparatus according to the present invention, Figure 2 is an enlarged view of the filtration device shown in FIG.

1 and 2, the conductive polymer manufacturing apparatus 10 according to the present invention includes a main reactor 20 and an auxiliary reactor 30. The main reactor 20 and the auxiliary reactor 30 are separated from the bottom by a pair of second vertical frames 12 and first vertical frames 11 extending vertically upwardly from the bottom frame 13 in which the flatness is maintained. It is located at a certain height upwards. At this time, the auxiliary reactor 30 is disposed at a position higher than the main reactor 20.

The auxiliary reactor 30 has a built-in stirrer (not shown) that is rotationally driven by the first motor 31 disposed above the auxiliary reactor 30. The impeller of the stirrer is made of an acid resistant material, and the rotation speed is controlled by an inverter. The upper part of the cylindrical auxiliary reactor 30 is closed by the first cover 32. The first cover 32 prevents the reaction solution from contacting the external air during the synthesis reaction in the auxiliary reactor 30. A first cooling jacket 33 is disposed on the radially outer side of the auxiliary reactor 30, and a first viewing window 35 is formed on the front surface of the auxiliary reactor 30. The first viewing window 35 is made of a transparent material so that the reaction phenomenon and the change occurring in the auxiliary reactor 30 can be visually observed from the outside. One side of the auxiliary reactor 30 is disposed a first control box 34 for controlling the operation of the auxiliary reactor (30).

The main reactor 20 is constructed similarly to the auxiliary reactor 30. The main reactor 20 contains a stirrer (not shown) which is rotationally driven by the first motor 21 disposed above the main reactor 20. The impeller of the stirrer is made of acid resistant material, and the rotation speed is controlled by the inverter. The upper part of the cylindrical main reactor 20 is closed by the second lid 22. The second cover 22 prevents the reaction solution from contacting external air during the synthesis reaction in the main reactor 20. A second cooling jacket 23 is disposed on the radially outer side of the main reactor 20, and a second viewing window 25 is formed on the front surface of the main reactor 20. The second viewing window 25 is made of a transparent material so that the reaction phenomenon and the change occurring in the main reactor 20 can be visually observed from the outside. One side of the main reactor 20 is disposed a second control box 24 for controlling the operation of the main reactor 20.

A first pipeline 41 extends between the secondary reactor 30 and the main reactor 20. The first pipeline 41 is for guiding the mixed dissolved solution in the auxiliary reactor 30 into the main reactor 20. The connection portion and all joint portions of the first pipeline 41 are one-touch. It is made of one touch type, so it is easy to clean and maintain. In the middle of the first pipeline 41, a first metering pump 51 is disposed. The first drain valve 14 is disposed at the front position of the first metering pump 51 in the first pipeline 41.

The first metering feed pump 51 is for controlling the amount of solution transferred from the auxiliary reactor 30 to the main reactor 20 via the first pipeline 41. Alternatively, the end of the first pipeline 41 connected to the main reactor 20 may be connected to the auxiliary reactor 30 without the first metering pump 51 disposed in the first pipeline 41. It is also possible to give a step to be located at a position lower than the end of the one pipeline 41 to induce the solution in the auxiliary reactor 30 to fall freely by gravity into the main reactor 20.

The main reactor 20 is in fluid communication with the filtration device 70 via a second pipeline 42 and a third pipeline 43. The second pipe line 42 and the third pipe line 43 are for guiding the solution treated in the main reactor 20 toward the filtration device 70, and the connecting portions thereof and all the joint portions are provided in a one-touch manner. It is easy to clean and maintain. A second fixed quantity feed pump 52 is disposed between the second pipeline 42 and the third pipeline 43. Thus, the second pipeline 42 extends between the main reactor 20 and the second metering feed pump 52, and then a third pipe between the second metering feed pump 52 and the filtration device 70. Line 43 extends. At this time, the second drain valve 15 is disposed in the middle of the third pipeline 43. The second metering pump 52 is for controlling the amount of solution transferred from the main reactor 20 to the filtration device 70 through the second pipeline 42 and the third pipeline 43.

FIG. 2 is an enlarged view of the filtration device shown in FIG. 1.

As shown in FIG. 2, a vacuum supply line 71 extending from an external vacuum device (not shown) is connected to a lower side of the filtration device 70, and a vacuum exhaust is connected to an upper side of the filtration device 70. Line 72 is connected. In a position adjacent to the filtration device 70, a vacuum instrument panel 73 is provided in the vacuum supply line 71 and the vacuum exhaust line 72, respectively.

A door 74 that closes the chamber of the filtration device 70 is installed to be opened and closed at the front of the filtration device 70, and a cylindrical container 75 is placed at the bottom of the chamber of the filtration device 70. The funnel 76 is fixedly arranged by the hanger 77 on the upper side in the cylindrical container 75. At this time, most of the funnel 76 is exposed to the outside of the upper side of the filtering device 70, the circular filter 78 in the upper side of the exposed funnel 76 in the transverse direction of the inner space of the funnel 76 Placed across.

Referring back to FIG. 1, a cooler 60 is disposed on the bottom frame 13 to maintain a constant temperature condition of the main reactor 20 and the auxiliary reactor 30. The cooler 60 includes a compressor, a condenser, an evaporator, etc. as a general cooling device, and fluidly connects to the cooling jackets 23 and 33 of the main reactor 20 and the auxiliary reactor 30 through the refrigerant flow line 61. do.

The manufacturing process of mass-producing polyaniline using the conductive polymer manufacturing apparatus configured as described above will be described.

In the present invention, polyaniline, which is a conductive polymer, is obtained by polymerizing an aniline monomer with an oxidizing agent under an acid solution. Therefore, the prerequisites for the equipment materials constituting the above apparatus should be acid resistant and chemical resistant materials.

In order to prepare polyaniline, which is a conductive polymer, first, 30 L of a 1 M hydrochloric acid (HCl) solution is put into a 60 L main reactor 20, and 200 mL of aniline monomer is added thereto to a concentration of 0.22 Mol, and then into the main reactor 20. Dissolve using the built-in stirrer. At this time, the cooler 60 is operated to keep the temperature in the main reactor 20 cooled to 0 ° C.

Separately, 20 L of a 1 M HCl solution was added to the auxiliary reactor 30 and dissolved by adding 115 g of ammonium peroxydisulfate ([(NH ₄ ) ₂ S ₂ O ₈ ]) as an oxidizing agent to a concentration of 0.05 Mol. . At this time, the cooler 60 is operated to keep the temperature in the auxiliary reactor 30 cooled to 0 ° C.

Next, the first metered feed pump 51 is operated while stirring the first solution containing the aniline monomer maintained at 0 ° C. in the main reactor 20 by using a stirrer to prepare the oxidant containing the oxidant in the auxiliary reactor 30. 2 solution is added via the first pipeline 41 into the main reactor 20 over 10-20 minutes.

At this time, in the main reactor 20, the reaction starts to occur simultaneously with the contact of the two solutions, and as the reaction proceeds, the mixed solution has a deep navy blue color and the surface of the mixed solution has a coppery luster. While maintaining the internal temperature of the main reactor 20 at 0 ° C., the reaction was continuously stirred to react for 90 minutes.

Next, the reactant reacted for 90 minutes is introduced into the filtration apparatus 70 through the second pipeline 42 and the third pipeline 43 using the second fixed quantity feed pump 52 made of acid resistant material. At this time, a vacuum is formed in the chamber of the filtering device 70 by the operation of an external vacuum supply source, and the reactant passes through the funnel 76 of the filtering device 70 by the vacuum pressure. Collected into). As a result, a synthesized conductive polymer precipitate is obtained.

As described above, according to the present invention, polyaniline, which is a conductive polymer applicable to an electrolytic capacitor electrolyte material and an electromagnetic wave shielding material, a secondary battery electrode material, a conductive paint material, a resist paste material, an antistatic material, or the like Mass production is possible.

Although the above has been described with reference to a preferred embodiment of the present invention, those skilled in the art will be able to variously modify and change the present invention without departing from the spirit and scope of the invention as set forth in the claims below. It will be appreciated.

Claims (5)

delete A first motor 31 positioned upwardly from the bottom frame 13 by a predetermined height by a pair of first vertical frames 11 extending upwardly from the bottom frame 13 and arranged above Built-in stirrer is driven by the rotation, the upper part is sealed by the first cover 32, the first cooling jacket 33 is disposed on the radially outer side, the first control box 34 is disposed on one side Reactor 30; Positioned upwardly from the bottom frame 13 by a pair of second vertical frames 12 extending vertically upwardly from the bottom frame 13 and positioned at a lower position than the auxiliary reactor 30. A built-in stirrer that is rotationally driven by a second motor 21 disposed at an upper side thereof, an upper portion thereof is sealed by a second cover 22, and a second cooling jacket 23 is disposed at a radially outer side thereof, and one side thereof. The main reactor 20, the second control box 24 is disposed; A first pipeline (41) extending between the secondary reactor (30) and the main reactor (20) to guide the mixed dissolved solution in the secondary reactor (30) into the main reactor (20); Filtration device for filtering the mixed dissolved solution in the main reactor 20 in a funnel arranged vertically connected to the main reactor 20 via a second pipeline 42 and a third pipeline 43. 70; The second pipeline 42 to regulate the amount of solution transferred from the main reactor 20 to the filtration device 70 through the second pipeline 42 and the third pipeline 43. A second fixed feed pump (52) disposed between and the third pipeline (43); And The cooling jackets 23 and 33 are disposed on the bottom frame 13 through the refrigerant flow line 61 to maintain the temperature conditions of the main reactor 20 and the auxiliary reactor 30 at a constant level. Conductive polymer production apparatus comprising a cooling device 60 connected to. 3. The conductive polymer manufacturing apparatus according to claim 2, wherein a first quantitative supply pump (51) is disposed in the middle of the first pipeline (41). The method of claim 2, wherein the auxiliary reactor 30 and the main reactor 20, the conductive polymer manufacturing apparatus, characterized in that the first viewing window 35 and the second viewing window 25 made of a transparent material are formed respectively, respectively. . 3. The vacuum supply line 71 of claim 2, wherein a vacuum supply line 71 extending from an external vacuum device is connected to a lower side of the filtering device 70, and a vacuum exhaust line 72 is connected to an upper side of the filtering device 70. The cylindrical container 75 is placed in the bottom of the chamber in the filtering device 70, and the funnel 76 is fixedly disposed by the hanger 77 on the upper side of the cylindrical container 75, and the filtering device ( The upper side of the funnel (76) exposed to the outside of the upper side of the 70) circular filter 78 is characterized in that the conductive polymer manufacturing apparatus, characterized in that disposed across the inner space of the funnel (76) in the transverse direction.