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Trinitrotoluene의 환원반응에서 가스크로마토그래피 모니터링을 이용한 2,6-diamino-4-nitrotoluene의 합성
김형석,유재철,김호기,김새롬,최근배,정원복,서원준,김진석,Kim, Hyoung-Sug,Yu, Jae Chul,Kim, Ho Gi,Kim, Sae Rom,Choi, Keun Bae,Jung, Won Bok,Seo, Won Jun,Kim, Jin-Seuk 한국군사과학기술학회 2014 한국군사과학기술학회지 Vol.17 No.2
In this research, we investigated synthetic method of 2,6-DANT that can be used as a chain extender of urethane/urea and epoxy materials in a demilitarization method via chemical transformations considering environmental, economical aspects and stability of process. We was able to identify through GC monitoring that 2,4-DANT and 2,6-DANT were produced when we inject 'hydrazine monohydrate 3.3 eq. by TNT 1 eq.' with a fine metering pump for 30 minutes and then, reflux for an additional 2 hours. We was able to isolate only 2,6-DANT(99.3% purity and 45.0% yield) from mixture of 2,4-DANT and 2,6-DANT through the separating and refining methods using 2,6-DANT solubility in methanol and crystallinity of 2,6-DANT.
실시간 In-situ IR을 이용한 Glycidyl Azide Monomer(GAM)의 양이온중합 반응속도 연구
김형석,김관영,강신춘,노시태,김진석,유재철,최근배,Kim, Hyoung-Sug,Kim, Kwan-Yung,Kang, Shin-Choon,Noh, Si-Tae,Kim, Jin-Seuk,Yu, Jae-Chul,Choi, Keun-Bae 한국군사과학기술학회 2009 한국군사과학기술학회지 Vol.12 No.2
We synthesized glycidyl azide monomer(GAM) as a monomer for polymerization of glycidy azide polymer(GAP) which is a promising energetic prepolymer for a plastic-bonded explosive. Using quantitative real-tim in-situ infrared(in-situ IR) spectroscopy, kinetic study on the cationic ring opening polymerization of GAM was carried out. The reaction rate was obtained from monitoring the change of ether C-O stretching band($1050cm^{-1}$) in series IR spectra. The reaction was in accordance with the first-order reaction law for each of reaction temperature at 100/1 mole ratio of [GAM]/[$BF_3*etherate$]. In the ring opening polymerization of GAM, with ratio of [GAM]/[$BF_3*etherate$] to equal 100/1 at various temperature, the activation parameters obtained from the evaluation of kinetic data were ${\Delta}H^*$=14.34kcal/mol, ${\Delta}S^*=-12.31cal/mol{\cdot}K$ and $E_a$=14.89kcal/mol.