Title ナイロン66のATR法による赤外スペクトル測定実験 Sub Title An experiment with infrared absorption spectra measurement of Nylon-66 by ATR method. Author 大場, 茂(Oba, Shigeru) 向井, 知大(Mukai, Tomohiro) Publisher 慶應義塾大学日吉紀要刊行委員会 Publication year 2014 Jtitle 慶應義塾大学日吉紀要. 自然科学 (The Hiyoshi review of natural science). No.56 (2014. 9) ,p.21- 34 Abstract 慶應義塾大学日吉キャンパスにおける文系学生を対象とした化学実験のテーマの1 つとして, ナイロン66 の合成と染色に関する実験を2000 年以前から行っている。合成後のナイロンについて, 機器分析の1 つとして, ATR 法(全反射減衰分光法)による赤外スペクトル測定を2008 年から開始した。それは, 吸収される赤外線のエネルギーから, 化合物に含まれている官能基を簡単に同定できるというメリットがある。本稿では, その背景ならびに実験準備上の注意を述べる。また, すべての吸収帯の帰属についても文献を調べ, 環状単量体のデータとも比較して検討した。なお, アジポイルクロリドの溶媒としてヘキサンを用いているが, これとヘキサメチレンジアミンの水酸化ナトリウム溶液との界面重合により生成したナイロン66 の糸が弱いのは, 重合度ならびに結晶化度が低いためである。冷延伸法によりナイロンの糸を強化 できることが知られているが, ナイロン66 は熱安定性が悪いため, 空気中での溶融紡糸が困難であることを確認した。 Notes 研究ノート Genre Departmental Bulletin Paper URL https://koara.lib.keio.ac.jp/xoonips/modules/xoonips/detail.php?koara_id=AN10079809-2014093 0-0021 慶應義塾大学学術情報リポジトリ(KOARA)に掲載されているコンテンツの著作権は、それぞれの著作者、学会または出版社/発行者に帰属し、その権利は著作権法によって 保護されています。引用にあたっては、著作権法を遵守してご利用ください。 The copyrights of content available on the KeiO Associated Repository of Academic resources (KOARA) belong to the respective authors, academic societies, or publishers/issuers, and these rights are protected by the Japanese Copyright Act. When quoting the content, please follow the Japanese copyright act. Powered by TCPDF (www.tcpdf.org)
, (Mukai, Tomohiro) Publisher
Publication year 2014 Jtitle . (The Hiyoshi review of natural
science). No.56 (2014. 9) ,p.21- 34 Abstract 1 ,
66 2000 , 1 , ATR ()2008 , , , , , , , 66 , , 66 ,
Notes Genre Departmental Bulletin Paper URL
https://koara.lib.keio.ac.jp/xoonips/modules/xoonips/detail.php?koara_id=AN10079809-2014093
(KOARA)/
The copyrights of content available on the KeiO Associated
Repository of Academic resources (KOARA) belong to the respective
authors, academic societies, or publishers/issuers, and these
rights are protected by the Japanese Copyright Act. When quoting
the content, please follow the Japanese copyright act.
Powered by TCPDF (www.tcpdf.org)
66 ATR
An Experiment with Infrared Absorption Spectra Measurement of
Nylon-66 by ATR method.
Shigeru OHBA and Tomohiro MUKAI
1 66 2000 1 ATR 2008 66 66
Hiyoshi Review of Natural Science Keio University No. 56,
21-342014
223-8521 4-1-1Research and Education Center for Natural Sciences,
Keio University, Hiyoshi 4-1-1, Kohoku-ku, Yokohama 223-8521,
Japan. 102-8160 2-17-1Present Address, Science Research Center,
Hosei University, Fujimi 2-17-1, Chiyoda- ku, Tokyo 102-8160,
Japan. [Received Feb. 1, 2014]
22
1
2
2-1 66
66 H2NCH26NH2 HOOCCH24COOH 11 1 12 X
66X P1 2 C12H22N2O2 1 Z13α23 a4.87b5.26c17.15α50.5β76γ63.5° 4 c
N-H…O ac 2 a 2 b
23
66 ATR
4 66 265200 Brill Brill α5 6 7
230 66 8 220 2509
1 66
O
C
O
2 ) 6
NH 3
2 66 3[C12H22N2O2]n P1Z1 c N-H…O ac 2 b
24
2-2 66 Morgan
1959 101112 ClOCCH24 COCl 2 66 3
10
610 1 1 6 ClOCCH28COCl 10
3 66 NaOH
H 2 N
H H
C Cl
3-2
66 265 280 300 66 300 14 66
4
4-1 116.21 25 g
0.5 M NaOH 430 ml 183.03 25 g 480 ml / 1.76 2 3 11
4-2 215
C=O 1700 cm1 C=O 100 cm1 8 C=O 2 66 3 16 66
1718 IR SDBSWeb19 Gaussian 09 20
1420 1470 cm1 CH2 scissoring CH2
29
21 66
IR 40 240 30 1.090 1.240 g/cm3 66 3
EtC=ONH-CH26-NH-C=O-CH24-C=ONH-Pr IR 936 cm1 C-CO C-C trans 1144
cm1 C-C gauche 22IR 1 2324 3 11 3 1742 cm1
1633 cm1 6 66 IR 25 3 IR 66 26 66 1730 cm1 C=O 66 1501713 cm1
27
8C=O 2
R
C
N
H
O
R
R
C
N+
H
O-
R
30
No. 562014
27 C=O1725 1700 cm1 2 3 1742 cm1 28 IR 1694 1742 cm1 C=O29
5
66 ,
3 66
cm1a
cm119
3301s 3081w 2930s 2857m 1742w 1633vs 1536vs 1473m 1464m 1416m 1372w
1275m 1200m 1180w 1146w 1041w 935m 686s
N-H21
N-H 21
2 N-HC-N 21
CH2 scissoringnext to NH22
not adjacent to amide22
next to CO22
CH2 twist-wagging 21
CH2 wagging 21
C-C skeletal22
3307vs 3072m 2961s 2853s
1672vs 1563vs 1474m 1467m 1435s 1328w 1369m 1276m 1285m 1206m1229m
1164s 1119w 1053w1070w 950w 692s
avs: very strong, s: strong, m: middle, w: weak.
31
ε- 6 1114 260
5-2
1111214 adipoyl chloride → chloride
301 1 ec chlorid
acetate 30
acetatechloride 31
5-3
CO2
H2O CH2NH2COOH3 H2SO4
32
4 CO2
2368 cm1668 cm1
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