KR100529553B1 - equipment and synthesis method of conducting polymer - Google Patents
equipment and synthesis method of conducting polymer Download PDFInfo
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- KR100529553B1 KR100529553B1 KR10-2003-0054938A KR20030054938A KR100529553B1 KR 100529553 B1 KR100529553 B1 KR 100529553B1 KR 20030054938 A KR20030054938 A KR 20030054938A KR 100529553 B1 KR100529553 B1 KR 100529553B1
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Abstract
본 발명은 전도성 고분자 합성방법 및 그 장치에 관한 것으로서 더욱 구체적으로는 다양한 특성을 갖는 전도성 고분자 피막을 제조할 수 있을 뿐만 아니라 공정의 제어가 용이하고 또 제조공정의 재현성이 있음은 물론 도펀트의 사용이 용이하여 특성이 서로 다른 여러가지의 전도성 고분자를 제조할 수 있도록 하며, 한편 미세 분무가 가능토록 하여 전도성 고분자의 피막층을 갖는 샘플의 대량생산이 용이하도록 한 중합법 및 그 장치를 얻을 수 있도록 한 것이다.The present invention relates to a method and a device for synthesizing a conductive polymer, and more particularly, to prepare a conductive polymer film having various characteristics, and to facilitate control of the process and to reproducibility of the manufacturing process. It is easy to produce a variety of conductive polymers having different characteristics, and to facilitate the micro-spray, it is possible to obtain a polymerization method and an apparatus for facilitating mass production of a sample having a conductive polymer coating layer.
즉, APS, 염화철등과 같은 산화제를 증류수에 녹여 만든 산화제 용액과 특성이 서로 다른 하나 이상의 전도성 고분자 모노머를 폴리비닐알코올과 함께 일정량의 증류수에 각기 녹여 만든 하나 이상의 고분자 모노머 용액을 각각의 챔버에 저수하고, 상기 산화제 용액과 모노머 용액이 저수된 챔버내에 공기를 주입함과 동시에 챔버 전체를 진동시켜 챔버내에서 산화제 용액 및 모노머 용액의 증기가 발생되도록 하며, 발생된 증기를 일정한 배출경로에 의거 중합챔버에 토출되도록 하여 중합반응과 동시에 하나 이상의 전도성 고분자가 합성될 수 있도록 하는 방법과 이를 실현시키기 위한 장치를 제공토록 한 것이다.That is, one or more polymer monomer solutions prepared by dissolving oxidizers such as APS and iron chloride in distilled water and one or more conductive polymer monomers having different characteristics with polyvinyl alcohol in a predetermined amount of distilled water are stored in each chamber. In addition, while injecting air into the chamber in which the oxidant solution and the monomer solution are stored, the entire chamber is vibrated to generate steam of the oxidant solution and the monomer solution in the chamber, and the generated vapor is converted into a polymerization chamber based on a constant discharge path. It is intended to provide a method and a device for realizing the same so that one or more conductive polymers can be synthesized at the same time as the polymerization reaction.
Description
본 발명은 전도성 고분자 합성방법 및 그 장치에 관한 것으로서, 이를 좀더 구체적으로 설명하자면 전도성이 높은 폴리아닐린(polyaniline), 폴리피롤 (polypyrrole), 폴리티오펜 (polyth ioplene)등과 같은 고분자의 합성을 신속, 용이하게 할 수 있는 방법 및 그 장치를 제공함에 그 목적이 있는 것이다.The present invention relates to a method and device for synthesizing a conductive polymer, which will be described in more detail. It is an object of the present invention to provide a method and an apparatus.
일반적으로 전기 전도성 고분자라 함은 고분자에 전기 전도성을 부여한 것으로, 위 전도성 고분자는 표면장력 제어, 전자파 차폐, 연료전지, 가스센스, 폴리머전지, 반도체소자, 디스플레이소자, 인공망막등에 응용되고 있고, 특히 전기 전도성이 높은 폴리아닐린, 폴리피롤, 폴리티오펜등의 고분자는 대기중에 안정하여 전기화학적 중합이나 화학적 중합방법에 의해 쉽게 합성할 수 있다는 장점은 있으나, 전기화학적 중합방법에 의하여 만든 전도성 고분자는 균일한 전기 전도성 필름을 형성할 수는 있지만 분자간의 강한 인력 작용으로 인해 발생되는 불융 특성 때문에 실제로 많은 제약이 따르고, 또 화학적 중합에 의해서 만든 전도성 고분자 분말의 경우는 응용을 위해서 분말을 녹일 수 있는 용액을 만들어야 함은 물론 필요한 후 처리 공정이 있어야 하기 때문에 이 또한 응용에 많은 제약이 따른다.In general, electrically conductive polymers are those that impart electrical conductivity to polymers. The conductive polymers are applied to surface tension control, electromagnetic shielding, fuel cells, gas sense, polymer cells, semiconductor devices, display devices, artificial retinas, and the like. Polymers such as polyaniline, polypyrrole, and polythiophene, which have high electrical conductivity, are stable in the air and can be easily synthesized by electrochemical polymerization or chemical polymerization. However, conductive polymers made by electrochemical polymerization have a uniform electrical properties. Although conductive films can be formed, there are many limitations due to the incompatibility characteristics caused by the strong attraction between molecules, and in the case of conductive polymer powders made by chemical polymerization, a solution capable of melting the powder for application is required. Of course, there is a necessary post-processing process This also follows many restrictions on the application because.
한편 증기중합법은 제조 조건의 설정이 매우 까다롭기 때문에 제조의 재현성이 없으며 도펀트(dopant)의 사용도 용이하지 않는 단점이 있다.On the other hand, since the steam polymerization method is very difficult to set the manufacturing conditions, there is a disadvantage that the production is not reproducible and dopant (dopant) is not easy to use.
이러한 점을 해결하기 위하여 최근에는 전도성 고분자에 가공성을 부여하고자 하는 연구가 진행되고 있는데 그 중 하나가 화학중합에 의해서 수용성의 다성분계 복합 입자의 제조이다. 즉, 도데실벤젠술폰산 또는 파라톨루엔슬폰산과 같은 유기산을 도판트로 사용하여 암모늄퍼스술페이트를 산화제로 사용하고, ABS 에멀젠 라텍스 내에서 폴리아닐린 및 폴리피롤을 중합시키는 방법은 제시하고 있으나, 상기의 방법은 도펀트및 에멀젠 라텍스의 유화제의 이온 결합이 존재하여 모노머(단량체)가 중합될 때 수분에 대해서 불안정하여 바람직하지 않는 분말의 침전이 생성되는 문제점을 안고 있고, 이와 같은 침전된 분말은 투명한 필름을 얻기 어려울 뿐만 아니라 소자 코팅등에 응용되기 위해서는 파쇄 및 미세분산의 균일화 공정이 요구된다.In order to solve this problem, researches have recently been conducted to impart processability to conductive polymers, one of which is the preparation of water-soluble multicomponent composite particles by chemical polymerization. That is, a method of using ammonium persulfate as an oxidizing agent using an organic acid such as dodecylbenzenesulfonic acid or paratoluenesulfonic acid as a dopant, and polymerizing polyaniline and polypyrrole in ABS emulsion latex, but the above method The presence of an ionic bond of an emulsifier of a dopant and an emulsion latex is unstable to moisture when the monomer (monomer) is polymerized, which leads to undesirable precipitation of a powder, which results in a transparent film. Not only is it difficult, but also applied to the device coating, etc. requires the process of homogenization of crushing and fine dispersion.
본 발명은 위와 같이 현재까지 제시되고 있는 전기 전도성 고분자 합성에 대한 문제점을 해결하기 위함에 그 기술적인 과제를 두고 발명된 것으로서, 특히 특성이 서로 다른 여러가지의 전도성 고분자를 신속하게 합성할 수 있도록 하는 방법과, 또 그 방법에 따른 장치에 의거하여 어떠한 제품(이하 "샘플"이라 함) 표면에 고분자 피막을 보다 얇게 형성할 수 있도록 함과 동시에 그 피막의 두께도 간편하게 조절할 수 있는 장치를 얻을 수 있도록 한 것이다. The present invention has been invented with the technical problem to solve the problems of the presently presented electrically conductive polymer synthesis, particularly a method for quickly synthesizing various conductive polymers having different characteristics. In addition, it is possible to form a thinner polymer film on the surface of a product (hereinafter referred to as "sample") based on the device according to the method, and to obtain a device that can easily adjust the thickness of the film. will be.
이를 보다 상세히 설명하면 다음과 같다. This will be described in more detail as follows.
APS(ammonium persulfate, Kanto Chemical Co. Inc), 염화철(FeCl4)등과 같은 산화제를 증류수에 녹여 만든 통상적인 산화제 용액과, 아닐린(aniline), 피롤 (pyrrole), 티오펜(thiophene)등과 같이 특성이 서로 다른 하나 이상의 전도성 고분자 모노머(단량체)를 폴리비닐알코올(PVA : polyvinyl alcohol. J.Baker. M.W. 77000 - 79000)과 함께 일정량(약50ml)의 증류수에 각기 녹여 만든 하나 이상의 통상적인 고분자 모노머 용액을 각각의 챔버에 저수하고, 상기 산화제 용액과 모노머 용액이 저수된 챔버내에 공기를 주입함과 동시에 챔버 전체를 진동시켜 챔버내에서 산화제 용액 및 모노머 용액의 증기가 발생되도록 하며, 발생된 증기를 일정한 배출경로에 의거 중합챔버에 토출되도록 하여 중합반응과 동시에 하나 이상의 전도성 고분자가 합성될 수 있도록 할 때 챔버의 진동은 초음파를 이용하고 공기주입은 펌프와 같은 유량 조절기를 사용하여 증기가 분무되도록 하며, 또 챔버에는 냉각장치를 부여하여서된 것이고,Typical oxidant solutions made by dissolving oxidizers such as APS (ammonium persulfate, Kanto Chemical Co. Inc), iron chloride (FeCl 4 ) in distilled water, and characteristics such as aniline, pyrrole, thiophene, etc. One or more conventional polymer monomer solutions prepared by dissolving one or more different conductive polymer monomers (monomers) in polyvinyl alcohol (PVA: polyvinyl alcohol.J. Baker. MW 77000-79000) in a predetermined amount (about 50 ml) of distilled water Water is stored in each chamber, the air is injected into the chamber in which the oxidant solution and the monomer solution are stored, and the entire chamber is vibrated to generate steam of the oxidant solution and the monomer solution in the chamber, and the generated steam is discharged uniformly. The vibration of the chamber uses ultrasonic waves when it is discharged to the polymerization chamber based on the path so that one or more conductive polymers can be synthesized simultaneously with the polymerization reaction. The air injection is made by spraying steam using a flow regulator such as a pump, and the cooling device is provided to the chamber,
또한 상기의 중합챔버 일측면에 샘플을 설치할 수 있도록 하되, 샘플 표면이 중합챔버 내에 위치되도록 하여서 된 것이다.In addition, the sample can be installed on one side of the polymerization chamber, but the sample surface is to be located in the polymerization chamber.
이와 같이 된 본 발명은 챔버는 산화제 용액 및 모노머 용액에 영향을 받지않는 재질을 사용하고, 챔버의 냉각장치는 초음파 진동으로 인하여 발생되는 열을 냉각하는 기능을 하며, 공기를 유입하는 유량조절기는 중합챔버 내로 분무되는 증기의 량 및 시간을 조절하는 작용을 하게된다.In the present invention as described above, the chamber is made of a material that is not affected by the oxidant solution and the monomer solution, and the cooling device of the chamber functions to cool the heat generated by the ultrasonic vibration, and the flow regulator for introducing the air is polymerized. Act to control the amount and time of vapor sprayed into the chamber.
다음으로 중합챔버 일측에 샘플을 설치하게 되면 분무되면서 중합반응과 합성이 동시에 이루어지는 전도성 고분자 막이 형성되게 되는데, 이 때 챔버 진동의 세기(15KHz ~ 70KHz)를 조절함으로써 고분자 막의 두께 및 입자 크기를 제어할 수 있으며, 또 중합반응의 온도(-15 - 20℃)를 조절하여 전도성 고분자의 중합속도를 조절할 수 있으며, 이는 중합률 및 고분자 입자 형상의 향상시킬 수 있게되며, 그리고 중합반응시 중합 분위기는 진공(vacuum), 에어, 비활성 가스 분위기 하에서 실시하여 최적의 중합 분위기가 실현되도록 한다.Next, when the sample is installed on one side of the polymerization chamber, a conductive polymer membrane is formed by spraying simultaneously with the polymerization reaction and synthesis. At this time, the thickness and particle size of the polymer membrane can be controlled by controlling the intensity of the chamber vibration (15KHz ~ 70KHz). In addition, it is possible to control the polymerization rate of the conductive polymer by controlling the temperature of the polymerization reaction (-15-20 ℃), which can improve the polymerization rate and the shape of the polymer particles, and the polymerization atmosphere during the polymerization reaction is vacuum It is carried out in a vacuum (vacuum), air, inert gas atmosphere to achieve the optimum polymerization atmosphere.
한편 위와 같은 방법을 실현하기 위한 장치로는, 일정형태의 밀폐형 챔버(1)(2)(3) 수개를 나란히 배열하여 각각의 외면에 냉각관(41)을 권취한 후 서로 연결하는 것에 있어서, 각각의 챔버(1)(2)(3) 하단에 진동자(21)를 탈부착 가능케 장치하며, 챔버(1)(2)(3) 상면 양측에는 배출관(4)(5)(6) 및 공기유입관(7)(8)(9)을 각기 설치하여 각 배출관(4)(5)(6)은 챔버(3) 외측의 중합챔버(51) 내부까지 도입되는 분무관(511)에 연결하고 공기유입관(7)(8)(9)은 펌프와 같은 유량조절기(31)에 연결하여서 된 것이다. On the other hand, as a device for realizing the above method, in the arrangement of several closed chambers (1) (2) (3) of a certain form side by side and winding the cooling tubes 41 on each outer surface and then connecting them to each other, The vibrator 21 is detachably attached to the bottom of each chamber 1, 2, 3, and discharge pipes 4, 5, 6, and air inflows are provided on both sides of the chamber 1, 2, 3, respectively. Each of the discharge pipes 4, 5 and 6 is connected to a spray pipe 511 which is introduced to the inside of the polymerization chamber 51 outside the chamber 3 by installing pipes 7, 8 and 9 respectively. Inlet pipes (7) (8) (9) is to be connected to the flow regulator 31, such as a pump.
상기와 같이된 본 발명의 장치는 챔버(1)(2)(3) 하단에 설치되는 진동자(21)를 탈,부착가능케 하였으므로 고분자 막의 두께 및 입자 크기가 결정되는 진동의 세기 조절을 진동자(21)를 교체함으로써 달성할 수 있게되며, 또 챔버(1)(2)(3) 외면에 냉각관(41)이 권취되므로 냉각 효율이 증대되며 또 밀폐형 챔버(1)(2)(3) 내에 펌프와 같은 유량조절기(31)를 이용하여 공기를 주입하면 배출관(7)(8)(9)으로 배출되면서 분무관(511)으로 증기를 분무 시킬 수 있게된다.Since the apparatus of the present invention as described above allows the detachable and detachable vibrator 21 installed at the bottom of the chamber 1, 2, 3, the vibrator 21 controls the intensity of vibration in which the thickness and particle size of the polymer film are determined. ), And the cooling tube 41 is wound on the outer surface of the chambers 1, 2, 3 so that the cooling efficiency is increased and the pumps in the sealed chambers 1, 2, 3 Injecting air by using a flow regulator 31, such as to be discharged to the discharge pipe (7) (8) (9) it is possible to spray the steam to the spray pipe (511).
또한 상기의 중합챔버(51) 일측면에는 냉각기능(냉각팬,라디에타(radiator)등)을 가진 샘플설치부(512)를 형성하되, 샘플(61) 표면이 중합챔버(51)내에 위치되도록 하고, 샘플(81)과 라디에타(611) 사이에 열전대(613)를 설치한 다음 상기 열전대(613)를 이용하여 샘플(81)의 온도를 조절하여 중합반응 속도를 제어하도록 하여서된 것이다. In addition, the sample installation portion 512 having a cooling function (cooling fan, radiator, etc.) is formed on one side of the polymerization chamber 51, so that the surface of the sample 61 is located in the polymerization chamber 51. The thermocouple 613 is installed between the sample 81 and the radiator 611, and then the temperature of the sample 81 is adjusted using the thermocouple 613 to control the polymerization reaction rate.
따라서 본 발명은 상기한 바와 같이 챔버 내에 산화제 용액과 고분자 모노머 용액의 중합반응을 초음파 진동을 이용함으로써 중합반응 시간이 짧고, 또 합성고분자 막을 보다 얇고 다양하게 형성할 수 있는 장점이 있으므로 증기 중합법과 화학 중합법을 장점을 결합시킨 초음파 중합법이라 할 수 있으며, 이러한 중합법은 다양한 특성을 갖는 전도성 고분자 피막을 제조할 수 있을 뿐만 아니라 공정의 제어가 용이하고 또 제조공정의 재현성이 있음은 물론 도펀트의 사용이 용이하여 특성이 서로 다른 여러가지의 전도성 고분자를 제조할 수 있는 이점이 있으며, 한편 미세 분무가 가능하여 전도성 고분자의 피막층을 갖는 샘플의 대량생산이 용이하고, 특히 초음파 중합법으로 제조된 가스센스 경우에는 감도가 우수하여 휘발성 유기화합물 측정용 센서로 사용이 가능하게 된다.Therefore, the present invention has the advantage that the polymerization time of the oxidizing agent solution and the polymer monomer solution in the chamber as described above by using ultrasonic vibration, the polymerization reaction time is short, and the synthetic polymer film can be formed thinner and more diversely. The polymerization method can be called an ultrasonic polymerization method that combines advantages, and this polymerization method can not only produce a conductive polymer film having various characteristics, but also can easily control the process and reproducibility of the manufacturing process. It is easy to use and has the advantage of manufacturing various conductive polymers having different characteristics, and it is possible to finely spray, so that mass production of samples having a conductive polymer coating layer is easy, and especially gas sense manufactured by ultrasonic polymerization In this case, it has a high sensitivity so This use is made possible by.
도 1은 본 발명의 전체적인 구성을 나타낸 예시도이다.1 is an exemplary view showing the overall configuration of the present invention.
*도면의 중요부분에 대한 부호의 설명* Explanation of symbols on important parts of drawing
1,2,3 : 챔버 4,5,6,: 배출관1,2,3: Chambers 4,5,6,: discharge pipe
7,8,9 : 공기유입관 21 : 진동자 7,8,9: air inlet pipe 21: vibrator
31 : 유량조절기 41 : 냉각관31: flow regulator 41: cooling tube
411 : 냉각조 51 : 중합챔버411 cooling tank 51 polymerization chamber
511 : 분무관 512 : 샘플설치부511: spray tube 512: sample installation
61 : 샘플 611 : 라디에타61: Sample 611: Radiata
612 : 냉각팬 613 : 열전대612 cooling fan 613 thermocouple
71 : 진동부여수단 72 : 트랜스71: vibration imparting means 72: trans
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