KR20000025050A - Method for manufacturing soluble polypyrrole using mixed dopants - Google Patents

Method for manufacturing soluble polypyrrole using mixed dopants Download PDF

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KR20000025050A
KR20000025050A KR1019980041959A KR19980041959A KR20000025050A KR 20000025050 A KR20000025050 A KR 20000025050A KR 1019980041959 A KR1019980041959 A KR 1019980041959A KR 19980041959 A KR19980041959 A KR 19980041959A KR 20000025050 A KR20000025050 A KR 20000025050A
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South Korea
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mol
dbsa
dopants
mixed
dopant
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KR1019980041959A
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Korean (ko)
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KR100304054B1 (en
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장관식
민혜경
오응주
독고정
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권호택
대우전자부품 주식회사
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/022—Electrolytes; Absorbents
    • H01G9/025—Solid electrolytes
    • H01G9/032—Inorganic semiconducting electrolytes, e.g. MnO2

Abstract

PURPOSE: A method is provided to enhance solubility with respect to organic solvents by mixing polarized dopants having a large particle size and a long chain. CONSTITUTION: Mixed dopants having 0.1 mol of polarized dopants (alkoxy, carboxyl,sulfonyl, hydroxyl) of a large particle size and 0.1 mol of DBSA of a long chain (CnH2n+1C6H5SO3H, n=8 - 12) is reacted with o.4 mol of pyrrole to manufacture soluble polypyrrole. 80 ml of distilled water is well stirred with 0.4 mol of pyrrole and 0.05 mol of DBSA and then separately 20ml of distilled water including 0.05 mol of DBSA and 0.1 mol of polarized dopants(alkoxy, carbonyl, sulfonyl, hydroxyl, and so on) is mixed with 0.08 mol of (NH4)2S2O8.

Description

혼합 도판트를 사용한 가용성 폴리피롤의 제조방법Method for preparing soluble polypyrrole using mixed dopant

본 발명은 알루미늄 콘덴서나 탄탈콘덴서와 같은 콘덴서 제조시 전도체로 사용되는 혼합 도판트를 사용한 가용성 폴리피롤의 제조방법에 관한 것이다.The present invention relates to a method for producing soluble polypyrrole using a mixed dopant used as a conductor in the manufacture of a capacitor such as an aluminum capacitor or tantalum capacitor.

폴리피롤은 정전기방지, 전자기파차폐, 축전지, photoelectrochemical 전지, ePolypyrrole is antistatic, electromagnetic shielding, storage battery, photoelectrochemical battery, e

-lectrochromic display, 부식방지, resistive heating, cableshielding, micro- wave absorbor, 온도센서, 충격센서, 화학적 센서 등에 이용되고, 특히 높은 전기전도도와 열적안정성, 저렴한 단가, 고주파 영역에서의 이상적인 저임피던스 가능, 우수한 노이즈(noise) 흡수성, 넓은 온도, 주파수영역에서의 안정한 정전 용량 때문에 고체 전해 콘덴서의 전해질층으로 사용된다.-Used in electrochromic display, corrosion protection, resistive heating, cableshielding, micro wave absorbor, temperature sensor, shock sensor, chemical sensor, etc., especially high electrical conductivity and thermal stability, low cost, low impedance, ideal for high frequency range, excellent noise It is used as an electrolyte layer in solid electrolytic capacitors because of its absorbency, wide temperature, and stable capacitance in the frequency domain.

기존의 폴리피롤의 제조방법은 500ml 증류수속에 0.30mol 피롤과 0.15mol DBSA를 혼합하고 섞는다. 별도로 0.06mol (NH4)2S2O8를 100ml 증류수에 혼합하여 섞는다. 0℃에서 24시간 반응시키고 메탄올, 아세톤, 증류수로 세척후 여과한다. 여과된 분말을 30℃에서 12시간 진공오븐에서 건조하여 폴리피롤 분말을 제조한다.The existing method for producing polypyrrole is mixed with 0.30mol pyrrole and 0.15mol DBSA in 500ml distilled water. Separately, 0.06mol (NH 4 ) 2 S 2 O 8 is mixed with 100ml distilled water. The reaction was carried out at 0 ° C. for 24 hours, washed with methanol, acetone, and distilled water, followed by filtration. The filtered powder is dried in a vacuum oven at 30 ° C. for 12 hours to prepare polypyrrole powder.

DBSA(dodecyl benzene sulfonic acid)를 도판트를 사용하여 m-cresol, chloro- form, THF, DMF의 일부 유기용매에 용해가 가능한 폴리피롤을 제조하였다.Dodecyl benzene sulfonic acid (DBSA) was used to prepare polypyrrole that can be dissolved in some organic solvents of m-cresol, chloro-form, THF, and DMF.

이러한 긴 사슬의 DBSA만을 도판트로 사용하였기 때문에 도판트와 용매에 대한 상호작용을 고려하지 않은 결과가 되어m-cresol, o-chlorophenol, chloroform, dichloromethane, THF, DMSO, NMP, DMF, trifluoroethanol, trifluoroacetic acid, benzyl alchol 와 같은 일반적인 유기용매에 대한 용해도가 매우 낮고 가공성이 떨어지는 단점이 있었다.Since only the long chain DBSA was used as the dopant, the interaction between the dopant and the solvent was not considered, resulting in m- cresol, o-chlorophenol, chloroform, dichloromethane, THF, DMSO, NMP, DMF, trifluoroethanol, and trifluoroacetic acid. However, the solubility in general organic solvents such as benzyl alchol was very low and the processability was poor.

본 발명은 전술한 바와 같은 문제점을 해결하기 위하여 안출한 것으로서, 일반적인 유기용매에 대해 높은 용해성을 가지는 폴리피롤을 제조하기 위한 것이다.The present invention has been made to solve the problems described above, and is for producing a polypyrrole having high solubility in a general organic solvent.

긴 사슬(CnH2n+1C6H5SO3H, n=8∼12)의 DBSA 0.1mol와 큰 입자크기의 극성을 갖는 도판트(alkoxy, carboxyl, sulfonyl, hydroxyl) 0.1mol 과의 혼합도판트를 피롤 0.4mol과 반응시켜 가용성 폴리피롤을 제조하는 것을 특징으로 하는 혼합 도판트를 사용한 가용성 폴리피롤의 제조방법을 제공한다.Between 0.1 mol of DBSA of long chain (C n H 2n + 1 C 6 H 5 SO 3 H, n = 8-12) and 0.1 mol of dopant (alkoxy, carboxyl, sulfonyl, hydroxyl) of large particle size It provides a method for producing soluble polypyrrole using a mixed dopant, characterized in that the mixed dopant is reacted with 0.4 mol of pyrrole to produce soluble polypyrrole.

긴 사슬(CnH2n+1C6H5SO3H, n=8∼12)의 DBSA 0.1mol와 큰 입자크기의 극성을 갖는 도판트(alkoxy, carboxyl, sulfonyl, hydroxyl 등) 0.1mol 와의 혼합도판트를 피롤 0.4mol과 반응시켜 가용성 폴리피롤을 제조한다.DBSA 0.1 mol of long chain (C n H 2n + 1 C 6 H 5 SO 3 H, n = 8-12) and 0.1 mol of dopant (alkoxy, carboxyl, sulfonyl, hydroxyl, etc.) with large particle size polarity Soluble polypyrrole is prepared by reacting a mixed dopant with 0.4 mol of pyrrole.

상기의 방법에 의한 일실시예를 설명하면 다음과 같다.An embodiment according to the above method will be described.

증류수 80ml속에 0.4mol의 피롤과 0.05mol의 DBSA를 넣어 잘 섞은 후 별도로 20ml 증류수에 0.05mol의 DBSA 와 0.1mol의 극성을 갖는 도판트(alkoxy, carbonyl, sulfonyl, hydroxyl 등)를 산화제인 (NH4)2S2O80.08mol과 혼합하여 섞는다. 0℃에서 20시간 반응시키고 증류수 또는 0.1 M의 극성을 갖는 도판트(alkoxyl, carbonyl, sulfonyl, hydroxyl 등) 수용액로 세척하여 여과한다. 여기서 얻어진 분말을 24시간 진공 건조 라인에서 건조시켜 폴리피롤 분말을 얻는다.After mixing 0.4 mol of pyrrole and 0.05 mol of DBSA in 80 ml of distilled water and mixing well, dopant (alkoxy, carbonyl, sulfonyl, hydroxyl, etc.) having 0.05 mol of DBSA and 0.1 mol of polarity was added to 20 ml of distilled water (NH 4 ) Mix with 2 S 2 O 8 0.08mol. The reaction was carried out at 0 ° C. for 20 hours and washed with distilled water or an aqueous dopant (alkoxyl, carbonyl, sulfonyl, hydroxyl, etc.) having a polarity of 0.1 M. The powder obtained here is dried in a vacuum drying line for 24 hours to obtain polypyrrole powder.

DBSA 만을 도판트로 사용하였을 경우에는 DBSA의 낮은 극성으로 인하여 대부분의 극성 용매에 대해 친화성을 보이지 않아 용해도가 떨어지는 단점을 가지고 있다. 그러나 극성을 갖는 도판트(alkoxyl, carbonyl, sulfonyl, hydroxyl 등)을 첨가하면 대부분의 극성 용매에 대해 친화성이 증가하여 일반적인 유기용매에 대한 용해성이 증가된다.When only DBSA is used as a dopant, due to the low polarity of DBSA, there is a disadvantage in that the solubility is lowered because affinity for most polar solvents is not shown. However, addition of polar dopants (alkoxyl, carbonyl, sulfonyl, hydroxyl, etc.) increases the affinity for most polar solvents, increasing the solubility in common organic solvents.

전술한 바와 같은 본 발명의 효과는 긴 사슬과 큰 입자크기의 극성 도판트를 혼합하여 사용하면 일반적인 유기용매(m-cresol, chloroform, dichloroform, NMP, DMSO, THF, DMF, benzylalcohol, trifluoroethanol 등)에 대해 용해성을 향상시킬 수 있다.As described above, the effects of the present invention can be achieved by mixing a long chain and a large particle size polar dopant in a general organic solvent (m-cresol, chloroform, dichloroform, NMP, DMSO, THF, DMF, benzylalcohol, trifluoroethanol, etc.). Solubility can be improved.

Claims (1)

긴 사슬(CnH2n+1C6H5SO3H, n=8∼12)의 DBSA 0.1mol와 큰 입자크기의 극성을 갖는 도판트(alkoxy, carboxyl, sulfonyl, hydroxyl) 0.1mol 과의 혼합도판트를 피롤 0.4mol과 반응시켜 가용성 폴리피롤을 제조하는 것을 특징으로 하는 혼합 도판트를 사용한 가용성 폴리피롤의 제조방법.Between 0.1 mol of DBSA of long chain (C n H 2n + 1 C 6 H 5 SO 3 H, n = 8-12) and 0.1 mol of dopant (alkoxy, carboxyl, sulfonyl, hydroxyl) of large particle size A method for producing soluble polypyrrole using a mixed dopant, wherein the mixed dopant is reacted with 0.4 mol of pyrrole to produce soluble polypyrrole.
KR1019980041959A 1998-10-08 1998-10-08 Making method of solubility polypyrrole to make of use mixed dofant KR100304054B1 (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020088976A (en) * 2001-05-22 2002-11-29 파츠닉(주) Making method of solubility polypyrrole having a high electric conductivity

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KR20030000642A (en) * 2001-06-26 2003-01-06 파츠닉(주) Electrolyte layer forming method tantalum capacitor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020088976A (en) * 2001-05-22 2002-11-29 파츠닉(주) Making method of solubility polypyrrole having a high electric conductivity

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