化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2009年
7期
969-974
,共6页
张明华%彭树华%何建平%王军民%巩沛鑫%王克
張明華%彭樹華%何建平%王軍民%鞏沛鑫%王剋
장명화%팽수화%하건평%왕군민%공패흠%왕극
羟丙基瓜尔胶%对甲苯磺酸-乙酸酐%摩尔取代度%TEMPO氧化
羥丙基瓜爾膠%對甲苯磺痠-乙痠酐%摩爾取代度%TEMPO氧化
간병기과이효%대갑분광산-을산항%마이취대도%TEMPO양화
hydropropyl guar gum%mixed p-toluenesulfonic-acetic anhydride%molar substitution degree%TEMPO-mediated oxidation
本文探索了表征羟丙基瓜尔胶(HPG)中羟丙基摩尔取代度(MS)以及取代位置的化学方法.当反应温度为110℃、反应时间为14h以及HPG中羟基与对甲苯磺酸-乙酸酐摩尔比为1:3.5时,用对甲苯磺酸-乙酸酐化学法和气相色谱法可准确测定HPG的羟丙基MS,与1H-NMR测定结果相对误差小于10%.在pH=10.30和0℃的条件下,瓜尔胶的伯羟基被2,2,6,6-四甲基哌啶氮--氧化物(TEMPO)-NaClO-NaBr体系选择性氧化成羧基,由此可表征羟丙基链段的取代位置.
本文探索瞭錶徵羥丙基瓜爾膠(HPG)中羥丙基摩爾取代度(MS)以及取代位置的化學方法.噹反應溫度為110℃、反應時間為14h以及HPG中羥基與對甲苯磺痠-乙痠酐摩爾比為1:3.5時,用對甲苯磺痠-乙痠酐化學法和氣相色譜法可準確測定HPG的羥丙基MS,與1H-NMR測定結果相對誤差小于10%.在pH=10.30和0℃的條件下,瓜爾膠的伯羥基被2,2,6,6-四甲基哌啶氮--氧化物(TEMPO)-NaClO-NaBr體繫選擇性氧化成羧基,由此可錶徵羥丙基鏈段的取代位置.
본문탐색료표정간병기과이효(HPG)중간병기마이취대도(MS)이급취대위치적화학방법.당반응온도위110℃、반응시간위14h이급HPG중간기여대갑분광산-을산항마이비위1:3.5시,용대갑분광산-을산항화학법화기상색보법가준학측정HPG적간병기MS,여1H-NMR측정결과상대오차소우10%.재pH=10.30화0℃적조건하,과이효적백간기피2,2,6,6-사갑기고정담--양화물(TEMPO)-NaClO-NaBr체계선택성양화성최기,유차가표정간병기련단적취대위치.
An improved chemical method for the determination of the molar substitution degree and substitution position of hydropropyl guar gum has been described.The hydropropyl groups are totally cleaved from modified guar gum at 110℃ in the presence of excess mixed p-toluenesulfonic-acetic anhydride for 14 hours,and the products entirely hydrolyzed into 1,2-dihyroxypropane at pH=11 in an hour.Quantifying the mass of the reaction products derived from the hyropropyl groups,the molar substitution degree of the substituted-hydropropyl guar gum can be exactly estimated,and the relative error of the method is less than 10% compared with the result of the 1H-NMR.Only primary hydroxyl groups can be oxidized to carboxyl groups by use of TEMPO-mediated oxidation,and that is applied for characterizing the substitution position of hydropropyl guar gum.