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(jí)：班級(jí)：學(xué)生：學(xué)生：學(xué)號(hào)：學(xué)號(hào)： 指導(dǎo)老師：指導(dǎo)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(jiǎn)介o 固相微萃取涂層研制的重要性o 碳納米管簡(jiǎn)介o 碳納米管在分離科學(xué)領(lǐng)域的運(yùn)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(biāo)準(zhǔn)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(yīng)機(jī)理o涂層制備條件優(yōu)化o涂層熱穩(wěn)定性評(píng)價(jià)涂層反應(yīng)機(jī)理：涂層反應(yīng)機(jī)

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(yīng)催化下發(fā)生水解反應(yīng)C2H5OSiOC2H5OC2H5OC2H5H2OTFAHOSiOHOHOHC2H5OH(2)TEOS(2)TEOS的水解產(chǎn)物發(fā)生縮聚反應(yīng)的水解產(chǎn)物發(fā)生縮聚反應(yīng)HOSiOHOHOHOSiOOOSiOOO()n(n+1)(3)KH-550(3)KH-550修飾碳納米管發(fā)生水解反應(yīng)修飾碳納米管發(fā)生水解反應(yīng)CONHCH2CH2SiOC2H5OC2H5OC2H5+CONHCH2CH2SiOHOHOHH2OC2H5OH(4)(4)羥基硅油化學(xué)鍵合到形成的溶膠羥基硅油化學(xué)鍵合到形成的溶膠- -凝膠網(wǎng)絡(luò)中凝膠

3、網(wǎng)絡(luò)中OSiOOOSiOOO()nHOSiCH3CH3OSiCH3CH3OSi()mCH3CH3OHSiCH3CH3OSiCH3CH3OSi()mCH3CH3OHOSiOOOSiOOO()n(5)(5)形成的有機(jī)無(wú)機(jī)復(fù)合物化學(xué)鍵合到碳納米管表面形成的有機(jī)無(wú)機(jī)復(fù)合物化學(xué)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(fù)

4、合涂層化學(xué)鍵合到石英纖維表面碳納米管羥基硅油復(fù)合涂層化學(xué)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(píng)價(jià)涂層熱穩(wěn)定性評(píng)價(jià)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(shí)驗(yàn)制備的KH550修飾的碳納米管