吳 強(qiáng), 趙 立, 武美霞, 姚偉峰

(1.上海電力學(xué)院環(huán)境工程與化學(xué)學(xué)院,上海 200090；2.山西大同大學(xué)化學(xué)與環(huán)境工程學(xué)院,山西大同 037009)

以納米炭纖維為模板浸漬制備V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑

吳 強(qiáng)1, 趙 立1, 武美霞2, 姚偉峰1

(1.上海電力學(xué)院環(huán)境工程與化學(xué)學(xué)院,上海 200090；2.山西大同大學(xué)化學(xué)與環(huán)境工程學(xué)院,山西大同 037009)

以SiO2纖維為宏觀基體材料,首先采用化學(xué)氣相沉積法制備納米炭纖維,然后以納米炭纖維作模板將納米多孔Al2O3固化在SiO2纖維上,以此得到Al2O3-SiO2纖維復(fù)合載體材料,最后采用浸漬法制得V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑?？疾霽2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑對炭黑顆粒氧化反應(yīng)的催化性能。結(jié)果表明,該類催化劑能明顯降低炭黑顆粒的起燃溫度,可以有效地降低柴油車尾氣中炭黑顆粒的排放,具有潛在的實(shí)際應(yīng)用前景。

SiO2纖維；納米炭纖維；模板法；V2O5-K2SO4系催化劑；炭黑顆粒

Foundation item:National Natural Science Foundation of China(21107069,21103106)；Scientific Research Foundation for the Returned Overseas Chinese Scholars,State Education Ministry (Z-2013-002)； Shanghai Pujiang Program (12PJ1403800)；Innovation Program of Shanghai Municipal Education Commission(14ZZ153)；Open Project of Shanghai Key Laboratory of Rare Earth Functional Materials(Z-2011-050)；Scientific Research Foundation for the Returned Scholars of Shanghai University of Electric Power(K-2011-004)；085 Engineering Project of Smart Grid Energy Storage Technology of Shanghai University of Electric Power(C-8209-11-551).

Author introduction:WU Qiang,Ph.D.,Associate Professor,E-mail:qiangwu@shiep.edu.cn

1 前言

汽油機(jī)和柴油機(jī)是汽車最主要的動(dòng)力源,而柴油機(jī)以其低油耗、高功率、高可靠性和耐久性的優(yōu)勢,逐漸成為車用動(dòng)力的首選。但是,柴油車尾氣排放的炭黑顆粒已引起嚴(yán)重的環(huán)境污染,因此控制和消除柴油車尾氣炭黑顆粒的排放具有十分重要的意義［1-3］。采用氧化型催化劑將炭黑顆粒氧化成CO2是目前減少炭黑顆粒污染的最直接有效的排放后處理方法［4-6］。V2O5-K2SO4系催化劑具有低共熔點(diǎn)且易流動(dòng)的特性,易于實(shí)現(xiàn)炭黑顆粒與催化劑緊密接觸,因而具有優(yōu)異的催化氧化炭黑顆粒的反應(yīng)性能,并已受到廣泛關(guān)注［7,8］。但這類催化劑難以大量并均勻地涂層負(fù)載在有序結(jié)構(gòu)的宏觀基體材料上如蛭石、水滑石、棒狀纖維、蜂窩陶瓷體以及多孔陽極氧化鋁膜(AAO)。因此,研發(fā)具有高質(zhì)量和高性能催化劑的新工藝和新技術(shù)仍是研究重點(diǎn)。

近年來,模板法因其具有簡便、經(jīng)濟(jì)、重復(fù)性高以及產(chǎn)品的形貌、結(jié)構(gòu)、尺寸取向可控等諸多優(yōu)點(diǎn)而廣泛應(yīng)用于納米材料的制備工藝。納米炭纖維是一種具有潛在應(yīng)用前景的模板材料,它可以通過工藝簡單、成本低廉的化學(xué)氣相沉積(CVD)法來制備。納米炭纖維不僅具有低密度、高比強(qiáng)度、高導(dǎo)電和導(dǎo)熱性、強(qiáng)耐腐蝕和耐高溫等性能,同時(shí)還兼具缺陷數(shù)量少、比表面積大和結(jié)構(gòu)致密等優(yōu)點(diǎn),因而在催化劑和催化劑載體、高效吸附劑、復(fù)合材料以及新材料制備等領(lǐng)域具有廣泛的應(yīng)用前景［9-12］。近年來,利用納米炭纖維模板可以制備出多種形貌可控的新型多孔功能復(fù)合材料,該類材料具有很強(qiáng)的吸附和催化性能［9-12］。

筆者采用納米炭纖維模板技術(shù)先將纖維狀納米多孔Al2O3固化在有序結(jié)構(gòu)的宏觀基體材料SiO2纖維上得到復(fù)合材料,再將Al2O3-SiO2纖維復(fù)合材料作為載體涂層負(fù)載相應(yīng)的活性組分 V2O5-K2SO4,進(jìn)而得到V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑。通過優(yōu)化制備條件,最終可以得到高質(zhì)量有序結(jié)構(gòu)宏觀基體與微觀顆粒復(fù)合的多孔材料,該類材料具有較強(qiáng)的吸附和催化性能,可以克服催化反應(yīng)中使用傳統(tǒng)納米粉末催化劑所帶來的各種弊端(如壓力降和熱傳遞問題、以及接觸效率低和催化劑難于分離等),能更為有效地降低柴油車尾氣中炭黑顆粒的排放,因而具有潛在的應(yīng)用前景。

2 實(shí)驗(yàn)

2.1 SiO2纖維上制備納米炭纖維

采用化學(xué)氣相沉積法在有序結(jié)構(gòu)的宏觀基體材料上合成納米炭纖維:以SiO2纖維作為有序結(jié)構(gòu)宏觀基體材料,采用Ni金屬作催化劑活性組分(催化劑質(zhì)量分?jǐn)?shù)為基體材料的1%),CH4氣體作為碳源,氣體流量為20mL/min,反應(yīng)溫度為550℃,常壓下反應(yīng)2 h即得到固化在 SiO2纖維上的納米炭纖維。

2.2 Al2O3-SiO2纖維復(fù)合載體的制備

采用納米炭纖維模板法制備Al2O3-SiO2纖維復(fù)合載體:將上述得到的固化在SiO2纖維上的納米炭纖維浸漬在濃度為0.3 mol/L Al(NO3)3前驅(qū)液中5min,然后抽濾以去除其表面過剩溶液,后經(jīng)300℃干燥1h,重復(fù)上述浸漬和干燥過程3次；最后在空氣中600℃下焙燒6h去除納米炭纖維模板,得到Al2O3-SiO2纖維復(fù)合載體。

2.3 V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑的制備

在80℃水浴和攪拌條件下將一定量NH4VO3和草酸溶解于去離子水中,然后繼續(xù)向溶液中緩慢地加入一定量的K2SO4,攪拌溶解后直至得到深藍(lán)色溶液,其中NH4VO3∶草酸∶K2SO4∶去離子水的配比為3.2mol∶3.2 mol∶1.6 mol∶1 L；將Al2O3-SiO2纖維復(fù)合載體浸漬在上述所得的深藍(lán)色溶液中1h,隨后樣品在烘箱中120℃ 條件下烘干5h,然后取出置于馬弗爐中,馬弗爐以10℃/min的升溫速率由室溫升至350℃焙燒24 h后冷卻到室溫得到V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑。

2.4 表征

采用X-射線衍射(XRD)測定樣品結(jié)構(gòu)形態(tài),儀器為Rigaku D/Max-2500型X-射線衍射儀,Cu靶K α射線(λ＝0.154 05 nm)。樣品形貌由JSM-7400F(JEOL)型場發(fā)射掃描電鏡(SEM)和Hitachi JEM-2000FX(JEOL)型透射電鏡測試。BET比表面積由AUTOSORB-3儀器測定。催化性能測試采用熱重-差熱分析測試方式,所用儀器為 Rigaku Thermo Plus TG 8120熱重分析儀,其中催化劑與炭黑顆粒保持質(zhì)量比為1∶10,經(jīng)混合研磨后放置于熱重-差熱分析儀的坩堝中,反應(yīng)體系以10℃/min的升溫速率由室溫升至700℃觀察熱重曲線的變化,該過程中持續(xù)通入空氣作為氧化劑,流量控制為30mL/min。另取相同質(zhì)量比的α-Al2O3和炭黑顆?；旌衔镒鲗φ諏?shí)驗(yàn),其他條件保持一致。

3 結(jié)果與討論

3.1 SiO2纖維上納米炭纖維的制備與表征

筆者前期研究結(jié)果表明,通過控制化學(xué)氣相沉積反應(yīng)的條件可以有效地調(diào)控納米炭纖維的生成,并且反應(yīng)溫度為550℃,CH4氣體流量為20mL/min,常壓下反應(yīng)2 h所制納米炭纖維適宜作為模板材料［10-12］,采用上述化學(xué)氣相沉積反應(yīng)的條件制備納米炭纖維模板。圖1(a)是化學(xué)氣相沉積前SiO2纖維的SEM照片,可以看出SiO2纖維呈長棒狀且表面較光滑,直徑約5.0μm。圖1(b)是化學(xué)氣相沉積后SiO2纖維表面生成納米炭纖維的SEM照片,可以看出納米炭纖維(厚度約為4.0μm)均勻且大量負(fù)載在SiO2纖維上,具有纖維狀結(jié)構(gòu)并且互相交織。

圖1 (a)SiO2纖維及(b)SiO2纖維上生成納米炭纖維的SEM照片F(xiàn)ig.1 SEM images of(a)pure silica fiber and(b)carbon nanofibers formed on silica fiber.

由圖2可以看出,納米炭纖維的直徑為30-80nm,Ni粒子位于納米炭纖維的頂部,這表明納米炭纖維的生成機(jī)理遵循“頂端生長模式”［10］。

圖2 納米炭纖維的TEM照片F(xiàn)ig.2 TEM image of carbon nanofibers.

3.2 Al2O3-SiO2纖維復(fù)合載體的制備與表征

筆者前期研究結(jié)果表明,納米炭纖維模板法可以實(shí)現(xiàn)快速且高效地在宏觀基體材料上涂層附載大量的單金屬或復(fù)合金屬氧化物,并且在納米炭纖維模板去除后,所生成的物質(zhì)將具備與納米炭纖維模板相似的形貌。考慮到這里所制V2O5-K2SO4復(fù)合載體催化劑主要用于炭黑氧化反應(yīng)的催化性能的實(shí)驗(yàn)研究,因此不能直接采用納米炭纖維模板法制備相應(yīng)的V2O5-K2SO4復(fù)合載體催化劑,主要存在以下兩點(diǎn)原因:一是采用空氣中直接燒除納米炭纖維模板時(shí),其焙燒溫度必須高于600℃；二是 V2O5-K2SO4系催化劑具有低共熔點(diǎn),在制備過程中其焙燒溫度不能高于400℃。因?yàn)楫?dāng)焙燒溫高于上述400℃時(shí),所制產(chǎn)物會(huì)不均勻并且出現(xiàn)大塊聚結(jié)現(xiàn)象。而當(dāng)焙燒溫低于上述400℃時(shí),納米炭纖維模板不能被完全燒掉,它會(huì)明顯影響后續(xù)的炭黑氧化反應(yīng)的催化性能。

基于以上原因,本研究先采用納米炭纖維模板法將納米多孔 Al2O3固化在 SiO2纖維上得到Al2O3-SiO2纖維復(fù)合載體材料,再采用浸漬法制備V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑。圖3是采用納米炭纖維模板法所制Al2O3-SiO2纖維復(fù)合載體的 SEM照片。由圖3可以看出,納米多孔Al2O3可以大量并均勻的涂層附載在SiO2纖維上,其層厚約為2.5μm,并且保留了納米炭纖維模板的形貌。

3.3 V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑的制備與表征

由圖4可知,V2O5-K2SO4均勻地涂層附載在Al2O3-SiO2纖維復(fù)合載體上,其層厚約為3.5 μm。經(jīng)計(jì)算,V2O5-K2SO4擔(dān)載量(質(zhì)量分?jǐn)?shù))為62.0%。BET比表面積測定V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑的比表面積為36.5 m2/g。可以推斷,與表面光滑的SiO2纖維相比,Al2O3-SiO2纖維復(fù)合載體因其具備纖維狀納米多孔結(jié)構(gòu),因而可提供更多V2O5-K2SO4涂層附載的空間,制備出高質(zhì)量有序結(jié)構(gòu)宏觀基體與微觀顆粒復(fù)合的多孔材料。該類材料將具有較強(qiáng)的吸附和催化性能,可以克服催化反應(yīng)中使用傳統(tǒng)納米粉末催化劑所帶來的多種弊端,因而具有潛在的應(yīng)用前景。

圖3 納米炭纖維模板法所制Al2O3-SiO2纖維復(fù)合載體SEM照片:(a)低分辨率下和(b)高分辨率下Fig.3 SEM images of Al2O3/silica fiber composites using carbon nanofibers template method:(a)low magnification and(b)high magnification.

圖4 V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑的SEM照片:(a)低分辨率下、(b)中分辨率下和(c)高分辨率下Fig.4 SEM images of V2O5-K2SO4supported over Al2O3/silica fiber composites by wet impregnation method:(a)low magnification,(b)mild magnification and(c)high magnification.

由圖5中XRD譜圖對比可知,采用浸漬法制得的V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑具有比較明顯的V2O5特征吸收峰(15.1°、21.5°、26.0°),同時(shí)XRD譜圖中出現(xiàn)了很強(qiáng)的K2SO4的特征吸收峰(24.0°、29.5°、31.0°、37.8°),與文獻(xiàn)［13］報(bào)道結(jié)果一致。這表明K2SO4的添加能夠提高 V2O5在 Al2O3-SiO2纖維復(fù)合載體上的分散度,使得V2O5在Al2O3-SiO2纖維復(fù)合載體上均勻分布,從而可提高催化活性相的有效比表面積。

3.4 催化性能測試分析

以炭黑顆粒催化燃燒反應(yīng)作為探針考察所制復(fù)合催化劑的催化活性。圖6是V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑催化燃燒炭黑顆粒的TG-DTA曲線。

圖5 V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑的XRD譜圖Fig.5 XRD patterns of V2O5-K2SO4supported over Al2O3/silica fiber composites.

圖6 V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑催化燃燒炭黑顆粒的TG-DTA曲線Fig.6 TG-DTA curves of V2O5-K2SO4supported over Al2O3-silica fiber composites mixed with carbon black.

另取用商品α-Al2O3粉末催化燃燒炭黑顆粒的實(shí)驗(yàn)作對比。商品α-Al2O3粉末催化燃燒炭黑顆粒時(shí),其起燃溫度約為500℃,達(dá)到50%轉(zhuǎn)化率時(shí)為600℃。而對于V2O5-K2SO4/復(fù)合載體催化劑,其起燃溫度約為350℃,達(dá)到50%轉(zhuǎn)化率時(shí)為450℃,這證明了V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑能明顯降低炭黑顆粒的起燃溫度,可以有效地降低柴油車尾氣中炭黑顆粒的排放,具有潛在的實(shí)際應(yīng)用前景。關(guān)于其催化反應(yīng)機(jī)理,對于V2O5-K2SO4/ Al2O3-SiO2纖維復(fù)合催化劑來說,K2SO4的作用主要是使V2O5在Al2O3-SiO2纖維復(fù)合載體上產(chǎn)生均勻分布,從而可提高催化活性相的有效比表面積。同時(shí)V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑是一種宏觀基體與微觀微粒相復(fù)合的多孔材料,并且在炭黑顆粒的催化氧化反應(yīng)過程中,V2O5-K2SO4系催化劑具有低共熔點(diǎn)且易流動(dòng)的特性,更易于實(shí)現(xiàn)炭黑顆粒與催化劑的緊密接觸,因而具有優(yōu)異的催化氧化炭黑顆粒的反應(yīng)性能。

4 結(jié)論

以SiO2纖維為宏觀基體材料,采用化學(xué)氣相沉積法在其表面可制備出納米炭纖維,提供一種有序結(jié)構(gòu)定向催化生長納米炭纖維的技術(shù)。采用納米炭纖維模板法和浸漬法的復(fù)合方法,并優(yōu)化實(shí)驗(yàn)條件可以得到 V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑。研究表明V2O5-K2SO4/Al2O3-SiO2纖維復(fù)合催化劑能明顯降低炭黑顆粒的起燃溫度,可以有效地降低柴油車尾氣中炭黑顆粒的排放,具有潛在的實(shí)際應(yīng)用前景。

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［1］ Mordkovich V Z,Baxendale M,Yoshimura S,et al.Intercalation into nanotubes.Carbon,1996,34(10):1301-1303.

［2］ Lovell D R.Carbon and High-Performance Fibers Directory.5th ed.,London:Chapman&Hall,1991:66.

［3］ Mochida I,Korai Y.Chemical characterization and preparation of the carbonaceous mesophase.In:Bacha J D,Newman J W,White J L, eds.Petroleum-Derived Carbons.Washington DC:ACS,1986,29-31.

［4］ Su J,Li G,Hao Z.The research and application of copper impregnated coarse-grain graphite throat.23rd Int′l Biennial Conference on Carbon,Extended Abstract and Program,July 18-23,Pennsylvania 1997,256-258.

［5］ Shigeki T,Jinichi M,Hiroshi H.Manufacture of mesocarbon microbeads.JP 61-222913,1986.

［6］ Jones L E.The Effect of Boron on Carbon Fiber Microstructure and Reactivity.Ph.D.Thesis.Penn State University,University Partk, PA 1987.

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Synthesis of Al2O3-silica fibers supported on a V2O5-K2SO4catalyst used for soot combustion

WU Qiang1, ZHAO Li1, WU Mei-xia2, YAO Wei-feng1
(1.College of Environmental and Chemical Engineering,Shanghai University of Electric Power,Shanghai200090,China; 2.College of Chemical and Environmental Engineering,Shanxi Datong University,Datong 037009,China)

An Al2O3-silica fiber support was prepared by first impregnating a Al(NO3)3solution on a silica fiber mat on which sacrificial carbon nanofibers had been formed by chemical-vapor deposition,followed by burning in air.The support was further impregnated with a solution containing NH4VO3and K2SO4to prepare the Al2O3-silica fiber supported V2O5-K2SO4catalyst.The catalyst can greatly decrease the combustion temperature of soot by around 200℃,which is promising for decreasing soot emission in diesel-powered vehicles.

Silica fiber；Carbon nanofibers；Template method；V2O5-K2SO4catalysts；Soot

O643.3

A

2015-03-15;

2015-08-15

國家自然科學(xué)基金(21107069,21103106);教育部留學(xué)回國人員科研啟動(dòng)基金(Z-2013-002);上海市浦江人才計(jì)劃(12PJ1403800);上海市教育委員會(huì)科研創(chuàng)新項(xiàng)目(14ZZ153);稀土功能材料上海市重點(diǎn)實(shí)驗(yàn)室開放課題(Z-2011-050);上海電力學(xué)院海外引進(jìn)人才科研啟動(dòng)項(xiàng)目(K-2011-004);上海電力學(xué)院085工程項(xiàng)目“智能電網(wǎng)儲(chǔ)能技術(shù)”(C-8209-11-551).

吳 強(qiáng),博士,副教授.E-mail:qiangwu@shiep.edu.cn

1007-8827(2015)05-0445-06