碳納米管固相微萃取涂層研制答辯

1、碳納米管固相微萃取涂層研制碳納米管固相微萃取涂層研制 班級：班級：學生：學生：學號：學號： 指導老師：指導老師：本論文的主要內(nèi)容：本論文的主要內(nèi)容：o1. 前言o2. 材料與方法o3. 結(jié)果與分析o4. 結(jié)論1. 1. 前言前言o 固相微萃取技術(shù)簡介o 固相微萃取涂層研制的重要性o 碳納米管簡介o 碳納米管在分離科學領(lǐng)域的運用o 碳納米管固相微萃取涂層研制情況2. 2. 材料與方法材料與方法o 儀器o 試劑與材料o 固相微萃取探頭的制備o 標準溶液配制o 固相微萃取操作o 氣象色譜條件3. 3. 結(jié)果與分析：結(jié)果與分析：o涂層反應機理o涂層制備條件優(yōu)化o涂層熱穩(wěn)定性評價涂層反應機理：涂層反應機

2、理：(1) TEOS(1) TEOS前驅(qū)體在前驅(qū)體在TFATFA催化下發(fā)生水解反應催化下發(fā)生水解反應C2H5OSiOC2H5OC2H5OC2H5H2OTFAHOSiOHOHOHC2H5OH(2)TEOS(2)TEOS的水解產(chǎn)物發(fā)生縮聚反應的水解產(chǎn)物發(fā)生縮聚反應HOSiOHOHOHOSiOOOSiOOO()n(n+1)(3)KH-550(3)KH-550修飾碳納米管發(fā)生水解反應修飾碳納米管發(fā)生水解反應CONHCH2CH2SiOC2H5OC2H5OC2H5+CONHCH2CH2SiOHOHOHH2OC2H5OH(4)(4)羥基硅油化學鍵合到形成的溶膠羥基硅油化學鍵合到形成的溶膠- -凝膠網(wǎng)絡中凝膠

3、網(wǎng)絡中OSiOOOSiOOO()nHOSiCH3CH3OSiCH3CH3OSi()mCH3CH3OHSiCH3CH3OSiCH3CH3OSi()mCH3CH3OHOSiOOOSiOOO()n(5)(5)形成的有機無機復合物化學鍵合到碳納米管表面形成的有機無機復合物化學鍵合到碳納米管表面SiC H3C H3OSiC H3C H3OSi()mC H3C H3O HOSiOOOSiOOO()nCON HCH2C H2SiO HO HO HCON HC H2CH2SiH4CH3CH3OSiCH3CH3O()mOSiOOOSiOOO()nH OO HSiH3CC H3O H(6)(6)碳納米管羥基硅油復

4、合涂層化學鍵合到石英纖維表面碳納米管羥基硅油復合涂層化學鍵合到石英纖維表面CONHCH2CH2SiH4CH3CH3OSiCH3CH3O()mOSiOOOSiOOO()nHOOHSiH3CCH3OHOHOH石 英 纖 維CONHCH2CH2SiH4CH3CH3OSiCH3CH3O()mOSiOOOSiOOO()nO HOHSiH3CCH3OH(石 英 纖 維 )碳 納 米 管碳 納 米 管（7 7）去活化試劑）去活化試劑PMHSPMHS掩蔽涂層表面殘余的硅羥基掩蔽涂層表面殘余的硅羥基CNHOCH2CH2SiOHOHOSiOOOSiOOOSiCH3CH3OSiCH3CH3OSiCH3CH3OH碳

5、納 米 管石 英 纖 維（）n()mCH3SiOCH3HSiCH3CH3OSiCH3CH3OSiCH3CH3CH3()()pq+CH3SiOHSiCH3OSiCH3CH3OSiCH3CH3CH3()()pqCNHOCH2CH2SiOHO HOSiOOOSiOOOSiCH3CH3OSiCH3CH3OSiCH3CH3OH碳 納 米 管石 英 纖 維（）n()m涂層制備條件的優(yōu)化：涂層制備條件的優(yōu)化：NapFhuoreneAcePhe02000004000006000008000001000000120000014000001600000Peak area 0.2mg/ml KH550-MWCNTs

6、-COOH 0.4mg/ml KH550-MWCNTs-COOH 0.6mg/ml KH550-MWCNTs-COOH 0.8mg/ml KH550-MWCNTs-COOHNapPhuoreneAcePhe020000040000060000080000010000001200000140000016000001800000Peak area 0.6mg/ml KH550-MWCNTs-COOH PDMS PA PDMS/DVBabcdefg0200000400000600000800000100000012000001400000160000018000002000000Peak area

7、0.2mg/ml KH550-MWCTs-COOH 0.4mg/ml KH550-MWCTs-COOH 0.6mg/ml KH550-MWCTs-COOH 0.8mg/ml KH550-MWCTs-COOHabcdefgh0100000020000003000000400000050000006000000Peak area 0.2mg/ml KH550-MWCNTs-COOH 0.4mg/ml KH550-MWCNTs-COOH 0.6mg/ml KH550-MWCNTs-COOH 0.8mg/ml KH550-MWCNTs-COOHabcdefgh0100000020000003000000400000050000006000000Peak area 0.2mg/ml KH550-MWCNTs-COOH PDMS PA PDMS/DVB涂層熱穩(wěn)定性評價涂層熱穩(wěn)定性評價1002003004005006007008005060708090100dM/dT100200300400500600700800-0.20-0.18-0.16-0.14-0.12-0.10-0.08-0.06-0.04-0.020.00 %Initail MassTemperature(oC)4.4.結(jié)論結(jié)論 本實驗制備的KH550修飾的碳納米管