广西大学学报(自然科学版)
廣西大學學報(自然科學版)
엄서대학학보(자연과학판)
JOURNAL OF GUANGXI UNIVERSITY (NATURAL SCIENCE EDITION)
2014年
3期
498-506
,共9页
蔡国瑞%项双龙%姜宏%熊春荣
蔡國瑞%項雙龍%薑宏%熊春榮
채국서%항쌍룡%강굉%웅춘영
椰壳活性炭%酚羟基%硅烷接枝%反应介质
椰殼活性炭%酚羥基%硅烷接枝%反應介質
야각활성탄%분간기%규완접지%반응개질
coconut shell activated carbon%phenolic hydroxyl%silane grafting%reaction medium
椰壳活性炭接枝含胺基的硅烷偶联剂对于固载生物酶、金属有机络合物及离子液体催化剂具有重要意义。为探究反应介质对椰壳活性炭接枝硅烷偶联剂的影响,采用正交实验分析法,将椰壳活性炭经硝酸氧化后,在4种不同极性和介电常数的反应介质中接枝硅烷偶联剂。结果表明:椰壳活性炭经硝酸氧化可提高表面含氧官能团含量,硝酸浓度为20wt%时,活性炭表面酚羟基含量达到0.329 mmol/g,酚羟基/羧基酯基比达到最大值1.259;通过FT-IR、XPS及N2物理吸附-脱附等手段表征了接枝硅烷偶联剂后的样品,结果表明,非极性反应介质中硅烷接枝效果优于极性反应介质,介电常数小也有利于硅烷化。在非极性甲苯中,硅烷偶联剂3-胺丙基三甲氧基硅烷、3-氯丙基三甲氧基硅烷及氯苄基三氯硅烷在氧化后椰壳活性炭上的接枝量分别为42.3%、45.2%、23.0%,说明介电常数较小的非极性反应介质甲苯为硅烷偶联反应的最佳溶剂。
椰殼活性炭接枝含胺基的硅烷偶聯劑對于固載生物酶、金屬有機絡閤物及離子液體催化劑具有重要意義。為探究反應介質對椰殼活性炭接枝硅烷偶聯劑的影響,採用正交實驗分析法,將椰殼活性炭經硝痠氧化後,在4種不同極性和介電常數的反應介質中接枝硅烷偶聯劑。結果錶明:椰殼活性炭經硝痠氧化可提高錶麵含氧官能糰含量,硝痠濃度為20wt%時,活性炭錶麵酚羥基含量達到0.329 mmol/g,酚羥基/羧基酯基比達到最大值1.259;通過FT-IR、XPS及N2物理吸附-脫附等手段錶徵瞭接枝硅烷偶聯劑後的樣品,結果錶明,非極性反應介質中硅烷接枝效果優于極性反應介質,介電常數小也有利于硅烷化。在非極性甲苯中,硅烷偶聯劑3-胺丙基三甲氧基硅烷、3-氯丙基三甲氧基硅烷及氯芐基三氯硅烷在氧化後椰殼活性炭上的接枝量分彆為42.3%、45.2%、23.0%,說明介電常數較小的非極性反應介質甲苯為硅烷偶聯反應的最佳溶劑。
야각활성탄접지함알기적규완우련제대우고재생물매、금속유궤락합물급리자액체최화제구유중요의의。위탐구반응개질대야각활성탄접지규완우련제적영향,채용정교실험분석법,장야각활성탄경초산양화후,재4충불동겁성화개전상수적반응개질중접지규완우련제。결과표명:야각활성탄경초산양화가제고표면함양관능단함량,초산농도위20wt%시,활성탄표면분간기함량체도0.329 mmol/g,분간기/최기지기비체도최대치1.259;통과FT-IR、XPS급N2물리흡부-탈부등수단표정료접지규완우련제후적양품,결과표명,비겁성반응개질중규완접지효과우우겁성반응개질,개전상수소야유리우규완화。재비겁성갑분중,규완우련제3-알병기삼갑양기규완、3-록병기삼갑양기규완급록변기삼록규완재양화후야각활성탄상적접지량분별위42.3%、45.2%、23.0%,설명개전상수교소적비겁성반응개질갑분위규완우련반응적최가용제。
Grafting silane with amine group is very meaningful for coconut shell activated carbon ( AC) to immobilized enzyme, metal complex and ionic liquid. In order to study the effect of reaction medium on silylation of the oxidated AC, four reaction media with different polarity and dielectric constant were investigated by orthogonal test. The results demonstrated that the content of oxygen-containing functional groups was greatly improved on coconut shell AC after oxidization by HNO3 . When nitric acid concentration was 20 wt%, Bohm titration showed that the phenolic hydroxyl con-tent was 0. 329 mmol/g, and the molar ratio of phenolic hydroxyl to carboxyl group reached a maxi-mum value of 1. 259, which was further verified by FT-IR and XPS. The samples after grafting si-lane were characterized using FT-IR, XPS and N2 adsorption-desorption. The results shown that non-polar solvent was more beneficial for silylation than polar solvent. In addition, low dielectric constant of solvent was also preferential to graft silane. In toluene, the contents of 3-aminopropyltri-methoxysilane, 3-chloropropyltrimethoxysilane and chlorobenzyl trichlorosilane on the oxidated coco-nut shell AC were 42.3%, 45.2% and 23.0%, respectively. In conclusion, toluene with a low di-electric constant is the best reaction medium for silylation of coconut shell AC.