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전해법에 의한 Adiponitrile 의 합성에 관한 연구
태범석,이종일,박영우 ( Beom Seok Tae,Jong Il Lee,Young Woo Park ) 한국공업화학회 1995 공업화학 Vol.6 No.5
ADN의 전해합성에 대한 유화전해액 제조용 계면활성제의 종류 및 농도 전해반응을 위한 전류밀도 및 전해온도, 전극표면을 지나는 유화전해액의 속도 그리고 DSA 전극의 손상 등의 영향을 조사하였다. 계면활성제로 Tetraethylammonium chloride가 좋고 최소사용농도는 전해액의 0.15wt% 정도 이상이다. 전류밀도의 증가는 물의 전해에 의한 부반응으로 효율이 떨어지고 전해온도는 별 영향이 없다. 전해액의 속도증가는 유화전해액의 안정성을 향상시켜 효율을 높힌다. 양극인 DSA의 손상은 ADN 합성에 나쁘나 ADN의 파괴에 의한 부반응을 일으키지 않는다. The effect of surfactants and their concentration, current density, temperature, velocity of electrolyte and defection of dimensionally stable anode(DSA) were investigated for electrosynthesis of adiponitrile(ADN). Tetraethylammoniun chloride was found to be most suitable among the tested surfactants and its concentration should be at least 0.15wt% to electrolyte. Increment of current density had a worse effect on electrosynthesis of ADN due to the electrodecomposition of water, while reaction temperature had little effect in the tested temperature range. Increment of electrolyte velocity on the electrode had a favorable effects on the electrosynthesis of ADN, because of making more stable emulsified electrolyte. Defective DSA had worse effect on electrosynthesis of ADN, but did not induce side reactions such as decomposition of ADN.
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이종일,태범석,박영우 ( Jong Il Lee,Beom Seok Tae,Young Woo Park ) 한국공업화학회 1995 공업화학 Vol.6 No.4
Nylon 66의 precursor인 Adiponitrile(ADN)의 전해합성에 대한 전극재료, 유화액 제조를 위한 계면활성제 그리고 반응물인 AN의 전기화학적 특성들을 조사하였다. 양극재료로는 내식성과 낮은 산소발생 과전압을 갖는 Dimensional Stable Anode(DSA)가 좋다. 분극특성으로부터 Electrohydrodimerization(EHD) 반응은 초기에는 -1.2∼ -1.3V(vs. Hg/Hg₂Cl₂)에서 시작되나 시간이 경과함에 따라 양극과 음극 모두 전위의 변화가 일어나는 것으로 보아 실제로는 약 -7.8V(vs. Hg/Hg₂Cl₂)에서 ADN의 합성반응이 진행되는 것으로 생각된다. 계면활성제로 quaternary ammonium salts(QAS)는 대부분 적합하다. Electrosynthesis of adiponitrile (ADN), a precursor for Nylon 66, was investigated by characterization of the effect of electrode materials, additives, and reactant AN. DSA was used as a anode material, which is well known to the corrosion resitive and has low oxygen overvoltage. Polarization characteristics show that the initial step of EHD reaction occurs at about -1.2∼ -1.3V(vs Hg/Hg₂Cl₂), but the final ADN synthesis reaction appears to occur at about -7.8V(vs Hg/Hg₂Cl₂) looking at the electrode potential change along time. The quaternary ammonium salts were acceptable for the electrosynthesis of ADN.
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이종일,태범석,박영우 ( Jong Il Lee,Beom Seok Tae,Young Woo Park ) 한국공업화학회 1995 공업화학 Vol.6 No.5
수질의 부패나 공장내 용수를 사용하는 장치의 부식과 직접 관련이 있는 용존산소의 측정을 위하여 주로 이용되는 고가의 귀금속인 금과 대치할 수 있는 비교적 저렴한 금도금전극으로 용존산소의 환원 한계전류의 측정과 재현성을 검토하였다. 순도 99% 이상의 순금도금전극은 약 -0.5V(vs. Hg/Hg₂Cl₂)의 전극전위 부근에서 산소의 환원한계전류가 나타나며 합금도금전극은 -0.5∼-0.6V(vs. Hg/Hg₂Cl₂)로 유사하나 순금도금전극이 수소발생에 따른 전류의 영향이 작아 용존산소 측정에 합금도금전극보다 적합하다. 그리고 이들의 재현성이 상당히 좋으며 용존산소의 농도변화에 따른 산소환원반응에 의한 한계전류가 99% 이상의 직선 비례관계가 성립하여 산소전극으로 충분하다. Due to the high cost of precious gold material, relatively lower cost electroplated pure and gold alloy electrodes have been prepared and tested their compatibility and reproducibility by measuring limiting cathodic current of various dissolved oxygen concentration. Pure gold plated electrodes had the limiting cathodic current for dissolved oxygen at -0.5V(vs. Hg/Hg₂Cl₂) and gold alloy plated electrodes had it at -0.5∼-0.6V(vs. Hg/Hg₂Cl₂); however, the one was suitable than the other for disposable dissolved oxygen sensor, because the alloy deposited electrodes had higher effect on cathodic current for hydrogen evolution reaction. Both type of electrodes had the good reproducibility with respect to variation of dissolved oxygen concentration and the limiting cathodic current for dissolved oxygen was linear function of its various concentrations.
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Methanesulfonyl Chloride 의 전해불소화 반응 중 유해가스의 생성 및 제어
이종일,태범석,박영우 한국산업안전학회 1996 한국안전학회지 Vol.11 No.3
Synthesis of perfluoromethanesulfonyl fluoride(PFMSF) which is a valuable precursor of perfluoro-chemicals such as surface modifier and fine chemicals was studied by electrochemical fluorination (ECF). In order to determine the termination of preelectrolysis, it was carried to monitor the variation of current during preelectrolysis by means of constant cell voltage operation. In a batch cell, chronopotentiometric electrolysis and various chemical analysis such as GC, GC/MS and IC were used to understand the potential change of electrode and synthesis and control of hazardous gases products. Termination of preelectrolysis was determinated by measurement the current and/or detection of F₂ gas generation. And during the preelectrolysis, an amount of generated OF₂was shown that a lot of moisture was absorbed from air when a cell was filled with anhydrous hydrogen fluoride(AHF). Above 4V cell voltage. F₂ gas was generated and acted on any form of fluorinating agents. In the ECF of MSC (methane sulfonyl chloride) by constant current operation, the potential of anode was intimately relation with generation of SO₂F₂. Exchange of Cl to F was dominatly occured in a initial stage. There were various gaseous products including PFMSF as main product and C₄ compounds.
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