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문장희 ( Moon Jang Hee ),김정호 ( Kim Jeong Ho ),배도규 ( Bae Do Gyu ),신봉섭 ( Shin Bong Seop ) 한국잠사학회 2001 한국잠사곤충학회지 Vol.43 No.2
STMP로 피브로인을 인산화 시키는 반응에서, 처리 조건별로 실험하여 적정 조건을 구하였고, 인이 결합되는 위치를 규명하기 위해 FT-IR과 ³¹P NMR분석을 행했고, 인산화된 견 피브로인의 특성을 평가하여 다음과 같은 결론을 얻었다. 1. 견 피브로인을 STMP로 인산화 시킬 때, 알칼리도가 클수록, 처리 온도가 높을수록 인산화 정도가 증가되었다. 2. 처리시간에 따른 인산화 정도는 1 hr까지는 급격하게 증가하였고, 1 hr 이후에는 서서히 증가되어 비교적 단시간에 인산화가 많이 진행되었다. 3. STMP 농도에 따른 인산화 정도는 50%까지는 급격히 증가되지만, 100% 이상에서는 증가가 미약하였다. 4. 인산화된 견 피브로인의 FT-IR 분석에서, 각 시료는 α-helix에 가까운 형태이었고, 아미노기에 의한 인산화 반응 (phosphoramidation)은 고려되지 않았다. 5. ³¹P NMR 분석 결과에서는 인산화가 polyphosphate 형태로 되어 있다는 것을 알 수 있었다. To improve the functional properties as food, silk fibroin was phosphorylated with STMP. In the phosphorylation reaction of silk fibroin, the degree of phosphorylation was increased with high alkali index and treatment temperature. Depending on treatment time and concentration of STMP it was rapidly increased up to 1hr. and 50%, but slowly above that time and 100%. It was indicated in the results of FT-IR analysis and (31)P NMR spectroscopy of phosphorylated fibroin that it had a close a-helix and poly-phosphate structure. The more phosphorylation of fibroin made more turbidity, foam expansion and foam stability, but less solubility. Emulsifying activity was increased up to P100, but slightly decreased above P100 and emulsifying stability was constantly increased on the progressing of phosphorylation.
辛奉燮,南重熙 한국잠사학회 1991 한국잠사곤충학회지 Vol.33 No.2
The treatments of methacrylamide on silk fibers were studied in aqueous solution using potassium persulfate as an initiator, and suitable conditions of reaction were determined for weighing of silk fibers. The results obtained were summarized as follows; The weight of MAA-treated silk fibers increased with monomer concentration. The adequate concentration of potassium persulfate was found to be 1.7%. Maximum weight increase was shown at initial pH 3.8 of reaction liquor controlled by buffer solution.
辛奉燮,南重熙 한국잠사학회 1994 한국잠사곤충학회지 Vol.36 No.1
The effects of some sodium phosphates as auxiliary agents were studied on the blockade of hardness for silk degumming. In this work, four kinds of sodium phosphates were tested and the results were obtained yhrough masking effects of metallic ions, difference of pH values and boil-off ratio. The degumming of calcium ingredient was analyzed by means of atomic absorption spectrophotometer and degumming test of cocoon shell was performed in the presence of calcium ingredient and sodium phosphates added to soap solution. In the view of the effects of sodium phosphates on calcium hardness, tetrasodium pyrophosphate(TSPP) and sodium phosphate dibasic(SPD) masked calcium ions more than sodium phosphate monobasic(SPM) and sodium hexametaphosphate(SHP). SHP and TSPP have excellent abilities of masking ferrous ions. The pH values of TSPP solution is higher than others, but lower than soap solution. The pH values were differently measured one another among the sodium phosphates but the boil-off ratio was increased in case of sodium phosphate with high pH value.
辛奉燮,南重熙 한국잠사학회 1992 한국잠사곤충학회지 Vol.34 No.1
Treatment of vinyl monomers onto silk fiber modifies the properties of the original silk fiber considerably. This field has been the subject of investigation by many workers using chemical and radiation initiation. Many studies on the reaction conditions, polymerization mechanism, physical properties and practical performances of methacrylamide-treated silk fiber have been continued. However, the polymerization mechanism has not been clearly reveated yet and this remains ambiguously whether the grafting is formed on fiber or not. In general, it has been accepted that free radicals were formed and vinyl monomers were polymerized in silk fibroin by graft polymerization mechanism, while active sties were varied by the types of monomer and initiator as well as by the reaction conditions. On the other hand, there is another argument on polymerization mechanism, in which monomers are polymerized and impregnated in the internal side of the fiber by homopolymerization. Though a large number of analytical methods are used to examine the polymerization mechanism of methacrylamide-treated silk fiber, the results on the basis of thermal analysis are merely reported in this paper. In differential scanning calorimetry (DSC) analysis, the thermal decomposition behaviors of the methacrylamide-treated silk fibers were determined and compared to those of the controlled silk fibers. DSC curves obtained from the methacrylamide-treated silk fibers showed double peaks at around 290°C (A peak) and 320°C (B peak) which are attributed to the thermal decomposition of the methacrylamide polymer and silk fibroin fiber, respectively. The temperature of A and B peak shifted to higher value with the increase of add-on. Also, the moisture regain of the treated silk fibers increased with add-on.