具有吸附—分解NOx功能的多酸催化体系制备、调变及性能研究
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摘要
随着氮氧化物(NOx)排放总量的逐年增大及限制NOx排放的法律法规日益严格,国内外众多科研机构加大了对NOx去除的研究。在NOx去除的众多方法中,直接催化分解法由于无还原剂消耗、不产生二次污染、工艺简单等优点而成为NOx去除的研究热点之一。杂多化合物(HPCs)由于其独特的晶体结构及催化性能而被广泛应用于各催化领域,将HPCs用于NOx去除的已有研究多局限于杂多酸(HPAs)对NOx的吸附及催化还原,而关于催化分解的研究较少,且研究最多的HPAs仅为Keggin结构磷钨酸(HPW),然而对于庞大的HPCs家簇来说,HPW的相关研究只是其冰山一角。由此本文制备了一系列Keggin、 Dawson结构杂多酸、杂多酸的稀土盐与铯盐以及负载型杂多酸,用于开拓杂多化合物催化分解NOx的新领域。研究主要内容为以下五个方面。
一、制备了以锗为中心原子的杂多酸催化剂H4GeW12O40(HGeW)、 H5GeW11VO40(HGeWV)、H5GeMo11VO40(HGeMoV)及H5GeW9Mo2VO40(HGeWMoV),通过IR表征确认了其Keggin杂多酸结构,并首次研究了其对NOx的吸附、脱附及催化分解性能。吸附实验结果表明,所制备的催化剂均具有吸附NOx的能力,在最佳吸附温度230℃时,各催化剂对NOx吸附效率及吸附容量的大小顺序为：HGeW> HGeWV> HGeWMoV> HGeMoV,其中HGeW对NOx的吸附效率及容量分别为80%与16.2mg NOx/g;通过IR表征发现NOx主要以[H+(NO2-,NO+)]形式吸附于杂多酸的二级结构中,此外有少量NOx以亚硝酰基(N0·)形式吸附。吸附于HGeW的NOx可通过升温热脱附与降温通水蒸汽反取代脱附两种方式进行脱附,后者由于有水蒸汽及时补充了杂多酸二级结构中NOx脱除而产生的空位,因而可以实现HGeW的重复使用。通过程序升温分解一质谱检测(TPD-MS)研究了NOx的催化分解,首次发现了NOx存杂多酸催化分解中O2的产生：考察了杂多酸中杂原子与中心原子对NOx催化分解的影响,结果发现以Ge为杂原子的杂多酸的催化活性高于P为杂原子的杂多酸,多原子为w的杂多酸对NOx的转化率高于多原子为Mo的杂多酸,但含W杂多酸的N2选择性却低于含Mo杂多酸,此外,V取代后杂多酸的催化活性低于取代前：分别考察了升温速率及气速对NOx催化分解的影响,结果发现高的升温速率与低的气速均有利于NOx转化率的增大,然而升温速率过高时或气速过低时N2选择性均有所下降。
二、制备并通过IR、XRD、TGA表征了Dawson型磷钨酸H6P2W18O62(HP2W),并首次将其用于NOx的吸附、脱附及分解研究。吸附实验结果表明：HP2W对NOx的吸附效率高于HPW,且最佳吸附温度为200℃；考察了吸附过程中气速对NOx吸附的影响,结果发现气速越高HP2W对NOx的吸附效率越低；考察了杂多酸中结晶水对NOx吸附的影响,结果发现杂多酸中存在两种形式结晶水,即松散结合的沸石水与通过化学键结合的质子水,其中沸石水对NOx的吸附有不利影响,而杂多酸中质子水的量决定了其对NOx的吸附容量；通过在氧化、还原及惰性氛围下对HP2W进行200、300及400℃煅烧以考察预处理对其吸附NOx性能的影响,结果发现不同氛围的预处理对HP2W吸附NOx的性能无明显的影响,且高温条件预处理由于造成HP2W质子型结晶水的损失,从而导致其对NOx的吸附能力的下降。通过升温热脱附方式及降温通水蒸汽反取代方式研究了NOx在HP2W的脱附情况,发现了与Keggin结构HGeW相同的脱附结果,即通水蒸气反取代的脱附方式可实现杂多酸的重复使用。通过TPD-MS研究了HP2W对NOx的分解性能,结果发现Dawson结构磷钨酸对NOx的分解能力较Keggin结构低,通过红外分析发现,其原因是由于Dawson结构HP2W所吸附的NOx多以NO及N203形式存在,仅少量NOx以质子化的亚硝酸鎓离子(HNO)+的形式存在,而亚硝酸鎓离子是降低N-O键能促进NOx分解的关键。
三、通过结晶反应及机械掺杂法制备出LnL (Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Yb, Y, Lu, Ho, Er, Tb, Dy, Tm; L=PW11O40)型稀土磷钨酸盐、LnL2型K8H3[Eu(PW11O39)2]以及磷钨酸铯盐Cs3-xHxPW12O40(x=0,0.5,1,1.5,2,2.5,3)催化剂,研究了上述催化剂对NOx的吸附及催化分解性能。LnL型稀土磷钨酸盐对NOx的吸附实验结果表明,LnL对NOx的吸附效率及容量均较低,且其对NOx吸附效率的顺序为：GdPW> PrPW> YPW> SmPW=CePW> LaPW> YbPW> NdPW> EuPW,对NOx吸附容量的顺序为：LaPW> GdPW> YPW> PrPW> CePW> NdPW> YbPW> SmPW> EuPW。通过机械研磨法制备出LnPW与HPW等质量掺杂的复合催化剂LnPW/HPW,并对其进行NOx吸附实验,结果表明该催化剂对NOx的吸附能力比掺杂HPW前有较大提高。通过快速升温的方式对所吸附的NOx进行催化分解,结果表明,含稀土元素的复合催化剂对NOx的分解性能均高于单纯的HPW,其催化分解NOx为氮气的活性顺序为：YPW/HPW> TmPW/HPW> YbPW/HPW> PrPW/HPW> TbPW/HPW> SmPW/HPW> LuPW/HPW> EuPW/HPW> LaPW/HPW> CePW/HPW> ErPW/HPW> GdPW/HPW> DyPW/HPW> HoPW/HPW> NdPW/HPW。研究了EuPW与HPW不同掺杂比所制备的EuPW/HPW催化剂对NOx的吸附与分解性能,结果表明,在复合催化剂中HPW主要起吸附NOx作用,EuPW主要起催化分解NOx作用,因此高HPW含量的催化剂具有高的NOx吸附能力,高EuPW含量的催化剂具有高的NOx分解能力。通过向EuPW/HPW催化剂中掺杂碳纳米管(CNTs),研究了微波辅助下NOx的催化分解。结果表明,提高CNTs掺杂量可促进NOx的分解。通过对比等质量掺杂HPW的LnL型与LnL2型稀土磷钨酸对NOx的吸附性能,发现由于LnL2型催化剂中K离子的存在,使其具有较大的比表面积,因此可以更好的分散HPW提高其比表面积,进而使其较LnL型掺杂具有更高的NOx吸附效率。采用TPD-MS技术对比研究了HPW、EuPW/HPW及K8H3[Eu(PW11O39)2]/HPW对NOx的分解性能,结果发现,由于稀土杂多酸盐的掺杂,EuPW/HPW对NOx催化分解性能高于HPW,而LnL2型催化剂K8H3[Eu(PW11039)2]中由于杂多化合物中缺位结构与碱土金属K的存在,使分解产生的氧原子被缺位结构及K原子所捕获而无法脱离催化剂表面,从而造成氧阻抑,因此导致LnL2型杂多酸盐具有低的NOx分解性能。
研究了磷钨酸铯盐催化剂对NOx的吸附及催化分解性能,结果表明,由于磷钨酸铯盐的高比表面积,有利于HPW在其上的分散及对NOx的吸附,CS3-xHxPW12O40对NOx吸附效率的递变顺序为：Cs,H2PW> Cs1.5H1.5PW> Cs2H1PW> Cs2.5H0.5PW> Cs0.5H2.5PW;通过TPD-MS技术研究了磷钨酸铯盐催化剂中HPW与Cs3PW不同掺杂比对催化分解NOx性能的影响,结果表明,由于碱金属Cs对O的吸附能力,导致催化剂分解所产生的氧无法由催化剂上脱除,进而造成催化剂活性下降,且Cs3PW掺杂量越多,催化剂对NOx的分解性能越差。
四、将碳纳米管载体分别经混酸与硝酸蒸汽预处理并在不同温度下煅烧,随后分别采用浸渍法及机械研磨法负载磷钨酸,制备出HPW/CNTs催化剂,首次对比考察了上述催化剂对NOx的吸附与分解效果。在空速为10000h-1、吸附温度为200℃的条件下,以0.5g催化剂对1000ppm的NOx进行吸附实验,结果表明,以硝酸蒸汽预处理且经300℃煅烧后的CNTs为载体,采用机械研磨负载法制备的催化剂HPW/CNTs对NO、的吸附率与吸附能力最高,分别为54%与16.6mg NOx/g·h。对吸附NOx后的催化剂体系进行了催化分解NO、的TPD-MS研究,结果表明,所吸附的NO、在快速升温过程中发生分解,首次发现了过程中氧的产生,分解产物包括N2、O2及N2O。采用电阻炉快速加热与微波辐射两种方式分别对吸附的NOx进行催化分解,结果表明,微波功率为700W时,NOx分解为N2的收率为33.3%,高于电阻炉以150℃/min快速升温的N2收率。使用过的催化剂通水蒸汽后可实现再生,对再生后的催化剂进行循环使用研究,结果表明,再生后的催化剂吸附与催化分解NO、的性能未有明显下降。
五、分别以微波辅助法及水热合成法将NH4PW原位合成并固载于USY沸石笼,制备出“瓶中船”型催化剂NH4PW-USY,进而以NOx为氧化剂氧化去除NH4PW-USY中的NH4+得到H+,由此首次制备出沸石笼中只含有HPW的“瓶中船”型催化剂HPW-USY,并研究了该催化剂对NOx的吸附、脱附及分解性能。通过IR、XRD及孔径孔容表征发现微波辅助法在NH4PW-USY的制备中,具有不破坏沸石笼结构及高效率等特点而优于水热合成法。由于还原剂NH4PW高度分散于USY,“瓶中船”型催化剂NH4PW-USY具有高的还原NOx能力,其对NOx的去除效率高达65%,高于单纯的USY及NH4PW对NOx的去除率,分别为5%与50%。NH4PW-USY与NOx完全反应后,通过IR及Py-IR证实了HPW-USY被成功制备。考察了HPW-USY对NOx的吸附与脱附,发现其吸附容量可达2.7mg NOx/g,吸附饱合NOx后,可采用降温通水蒸汽的方式实现脱附。吸附NOx后刘HPW-USY进行TPD-MS测试,分解过程中发现了O2的产生,催化剂HPW-USY对NOx的转化率与N2选择性分别为64.9%与74.3%,均高于单纯HPW催化剂对NOx的转化率与N2选择性。
More and more research institutions pay close attention to nitrogen oxides (NOx) abatement, due to the increasing NOx emission and the introduction of more rigorous environmental laws. NOx catalytic decomposition has been one of the most attractive methods, for no reducing agent is consumed and pollution-free N2and O2are the only products. Heteropoly compounds (HPCs) have been widely used in the catalytic reaction because of its special crystal structure and catalytic properties. The application of HPCs on NOx elimination have been researched for many years, however, they are mainly used as NOx absorbent or used in NOx catalytic reduction. Keggin type phosphotungstic acid (HPW) is the most studied HPCs, while there are many HPCs that have not been explored in NOx abatement. In this thesis, novel Keggin and Dawson type heteropoly acids (HPAs), the lanthanide complexes and cesium salt of HPW and the supported catalyst were prepared and used in the NOx adsorption and decomposition. The content of this thesis contains the following five parts.
I) NOx Adsorption-Decomposition on Keggin Type Heteropoly Acids Containing Germanium
Four kinds of keggin stucture HPAs employing germanium as central atom, including tungstogermanic heteropoly acid (abbr. HGeW), tungstovanadogermanic heteropoly acid H5GeW11V040(abbr. HGeWV), molybdovanadogermanic heteropoly acid H5GeMo11V040(abbr. HGeMoV) and molybdotungstovanadogermanic heteropoly acid H5GeW9Mo2V04o (abbr. HGeWMoV) were first applied as catalysts to remove NOx in lean exhaust gas, and they were synthesized and characterized by IR measurements. The adsorption tests showed that at the optimum adsorption temperature of230℃, the synthesized catalysts showed excellent NOx adsorption ability in the following order:HGeW> HGeWV> HGeWMoV> HGeMoV, and among which HGeW had the highest NOx adsorption efficiency and capacity of80% and16.2mg NOx/g. Two new IR absorption bands at2210and1851cm-1appeared after NOx being adsorbed on HGeW, the latter band was observed for the first time on HPAs adsorbed NOx, and was assigned to nitrosyl radical (NO-). Experiments on NOx desorption and the reusability of absorbent were carried out on HGeW by increasing oven temperature and cooling in wet air. The results showed that NOx could be desorbed through both two methods and the reusability of HGeW could be realized by the latter method. Temperature-programmed desorption-mass spectroscopy (TPD-MS) was carried out to investigate the decomposition of NOx on the synthesized catalysts and and purchased phosphotungstic acid (HPW) and for the first time, the formation of O2was observed on all of the catalysts mentioned above, and the decomposition products were comprised of N2, O2and N2O. The effect of heteroatom and polyatom on NOx decomposition was investigated, and the result showed that heteroatom Ge was superior to P, polyatom W was superior to Mo for NOx transformation, while it was inferior to Mo as for N2selectivity, and after substitute by V the catalytic activity would decrease. The effects of heating rate and gas velocity on NOx decomposition were investigated and the results showed that increasing the heating rate and decreasing the gas velocity promoted the NOx transformation, however, too high heating rate and too low gas velocity decreased the N2selectivity.
Ⅱ) NOx Adsorption-Aecomposition on Dawson Type Phosphotungstic Acid
The Dawson type phosphotungstic heteropolyacid (HP2W) was synthesized and characterized by IR, XRD and TGA measurements. NOx adsorption, desorption and decomposition were explored on HP2W. The influences of temperature, gas velocity, crystal water and pretreatment of HP2W on NOx adsorption were examined, the results showed that the NOx adsorption optimum temperature was200℃, the NOx adsorption efficiency had an inverse relationship with gas velocity, and the maximum NOx adsorption efficiency of78%was observed at the gas velocity of5000-1h. Two types of crystal water were observed on HP2W, among which the physical adsorbed water hindered the NOx adsorption, while the chemical adsorbed water improved it. After pretreated in the atmosphere of oxygen, hydrogen and nitrogen individually, the HP2W showed no significant difference on NOx adsorption. NOx desorption by improving temperature and cooling in wet air were comparatively studied, and the result was the same as that of HgeW explored in I), that is to say, desorption by cooling in wet air had a better performance for the reusability of HP2W could be realized through this method. TPD-MS was taken to investigate the NOx decomposition on Dawson type HP2W. Compared with Keggin type HPW, Dawson type phosphotungstic acid had lower catalytic activity, and the reason was attributed to the fact that less NOx was adsorbed on the second crystal structure of HP2W in the form of (HNO)+, which would improve the NOx decomposition by weakening the N-O bond.
Ⅲ) NOx Adsorption-Decomposition on Salts of Phosphotungstic Acid
LnL (Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Yb, Y, Lu, Ho, Er, Tb, Dy, Tm; L=PW11O40), LnL2type K8H3[Eu(PW,,039)2] and Cs3-xHxPW1204o(x=0,0.5,1,1.5,2,2.5,3) were prepared and used for NOx adsorption and decomposition. The adsorption results showed that NOx adsorption efficiency and capacity on LnL were lower, and for the NOx adsorption efficiency, LnL exhibited the following order: GdPW> PrPW> YPW> SmPW=CePW> LaPW> YbPW> NdPW> EuPW, while for the adsorption capacity the order was:LaPW> GdPW> YPW> PrPW> CePW> NdPW> YbPW> SmPW> EuPW. After doped with HPW, the NOx adsorption ability of LnL/HPW was improved significantly. The NOx decomposition on LnL/HPW was explored by rapid heating, and the results showed that the catalytic decomposition of NOx on LnL/HPW were superior than that of HPW, and for the N2yeild the catalytic activity followed the order:YPW/HPW> TmPW/HPW YbPW/HPW> PrPW/HPW> TbPW/HPW> SmPW/HPW> LuPW/HPW> EuPW/HPW> LaPW/HPW> CePW/HPW> ErPW/HPW> GdPW/HPW> DyPW/HPW> HoPW/HPW> NdPW/HPW. The effects of doping ratio between EuPW and HPW on adsorption and decomposition of NOx were studied. The results showed that HPW played the role of NOx adsorbent while EuPW as catalyst for decomposition of NOx, and more HPW in EuPW/HPW contributed to higher NOx adsorption efficiency and capacity, while more EuPW contributed to high NOx transformation and N2selectivity. Microwave was introduced to NOx decomposition on the catalyst of EuPW/HPW/CNTs, and the result showed that the decomposition of NOx was related to ratio of CNTs, and more CNTs improved the NOx decomposition. Compared with LnL type EuPW/HPW, the LnL2type K8H3[Eu(PW11O39)2]/HPW had higher NOx adsorption efficiency for the K ion increased the special surface thus improved the HPW dispers on K8H3[Eu(PW11O39)2], while the NOx decomposition on K8H3[Eu(PW11O39)2]/HPW was inferior to that of EuPW/HPW for the defect site and K ion on K8H3[Eu(PW11O39)2] captured O and inhibited the O removal from catalyst. NOx adsorption and decomposition on Cs3_xHxPW12O040were studied, the adsorption results showed that due to the high special surface of CS3PW, and the Cs3_xHxPW12O40exhibited fine NOx adsorption ability with the following order: CS1H2PW> Cs1.5H1.5PW> Cs2H1PW> Cs2.5H0.5PW> Cs0.5H2.5PW. TPD-MS was taken on Cs,H2PW and Cs2H1PW to investigate the effect of ratio between Cs3PW and HPW on NOx decomposition, the result showed that because the alkalis metal Cs had the O adsorption ability and O inhibited the NOx catalytic decomposition, so the more Cs, the less decomposition activity on CS3-XHxPW12O40.
Ⅳ) NOx Adsorption-Decomposition on H3PW12O40/CNTS
A series of HPW/CNTs catalysts were prepared by impregnation and mechanical grinding methods. For this purpose, CNTs was pre-treated separately by nitric acid vapor, mixture of nitric acid and sulphuric acid, and subsequently calcined. The performances of catalysts on NOx adsorption-decomposition were studied.0.5g catalyst was used to adsorb1000ppm NOx under the space velocity of1000h-1at200℃, and the results showed that the catalyst prepared by mechanical grinding methods supporting HPW on CNTs pretreated by nitric acid vapor and calcined at300℃had the highest NOx adsorption efficiency and capacity of54%and16.6mg NOx/g·h, respectively. TPD-MS was carried out on the catalyst adsorbed NOx, and the result showed that N2, O2and N2O were formed during rapid heating, among which O2was observed for the first time. Two modes of decomposition were employed, and one was by electric oven at a ramping rate of150℃/min, and the other was by microwave oven. Compared to the mode of the former, the latter has higher N2yield with a N2yield up to33.3%corresponding to the power of microwave oven being700W. The catalyst used can be reusable by water vapor reactivation, and the recycling results showed that there were no significant performance degradation for NOx adsorption and catalytic decomposition.
V) NOx Adsorption-Decomposition on "Ship in Bottle" Type HPW-USY
To synthesis pure HPW encaged in USY zeolite (HPW-USY), NH4PW encaged in the USY (NH4PW-USY) was firstly prepared by the methods of microwave radiation and hydrothermal synthesis. FT-IR, XRD, BET, pore size and pore volume measurements indicated that microwave radiation method was superior to hydrothermal synthesis in the preparation of NH4PW-USY. Then NH4PW-USY was used to reduce NOx, and accompanied with the consumption of NH4+and formation of H+, NH4PW-USY was turned into HPW-USY simultaneously, which was confirmed by FT-IR and in site pyridine adsorption IR. NOx adsorption-desorption behavior on HPW-USY was studied. The NOx adsorption capacity was2.7mg NOx/g, and the adsorbed NOx was desorbed when the temperature was decreased to ca.100℃in wet air. TPD-MS was carried out on HPW-USY adsorbed NOx to explore the performance of catalytic decomposition NOx. For the first time, O2production was observed a little latter than the formation of N2O and N2, the NOx conversion was64.9%and N2selectivity was74.3%on HPW-USY, which was higher than pure HPW.
一、制备了以锗为中心原子的杂多酸催化剂H4GeW12O40(HGeW)、 H5GeW11VO40(HGeWV)、H5GeMo11VO40(HGeMoV)及H5GeW9Mo2VO40(HGeWMoV),通过IR表征确认了其Keggin杂多酸结构,并首次研究了其对NOx的吸附、脱附及催化分解性能。吸附实验结果表明,所制备的催化剂均具有吸附NOx的能力,在最佳吸附温度230℃时,各催化剂对NOx吸附效率及吸附容量的大小顺序为：HGeW> HGeWV> HGeWMoV> HGeMoV,其中HGeW对NOx的吸附效率及容量分别为80%与16.2mg NOx/g;通过IR表征发现NOx主要以[H+(NO2-,NO+)]形式吸附于杂多酸的二级结构中,此外有少量NOx以亚硝酰基(N0·)形式吸附。吸附于HGeW的NOx可通过升温热脱附与降温通水蒸汽反取代脱附两种方式进行脱附,后者由于有水蒸汽及时补充了杂多酸二级结构中NOx脱除而产生的空位,因而可以实现HGeW的重复使用。通过程序升温分解一质谱检测(TPD-MS)研究了NOx的催化分解,首次发现了NOx存杂多酸催化分解中O2的产生：考察了杂多酸中杂原子与中心原子对NOx催化分解的影响,结果发现以Ge为杂原子的杂多酸的催化活性高于P为杂原子的杂多酸,多原子为w的杂多酸对NOx的转化率高于多原子为Mo的杂多酸,但含W杂多酸的N2选择性却低于含Mo杂多酸,此外,V取代后杂多酸的催化活性低于取代前：分别考察了升温速率及气速对NOx催化分解的影响,结果发现高的升温速率与低的气速均有利于NOx转化率的增大,然而升温速率过高时或气速过低时N2选择性均有所下降。
二、制备并通过IR、XRD、TGA表征了Dawson型磷钨酸H6P2W18O62(HP2W),并首次将其用于NOx的吸附、脱附及分解研究。吸附实验结果表明：HP2W对NOx的吸附效率高于HPW,且最佳吸附温度为200℃；考察了吸附过程中气速对NOx吸附的影响,结果发现气速越高HP2W对NOx的吸附效率越低；考察了杂多酸中结晶水对NOx吸附的影响,结果发现杂多酸中存在两种形式结晶水,即松散结合的沸石水与通过化学键结合的质子水,其中沸石水对NOx的吸附有不利影响,而杂多酸中质子水的量决定了其对NOx的吸附容量；通过在氧化、还原及惰性氛围下对HP2W进行200、300及400℃煅烧以考察预处理对其吸附NOx性能的影响,结果发现不同氛围的预处理对HP2W吸附NOx的性能无明显的影响,且高温条件预处理由于造成HP2W质子型结晶水的损失,从而导致其对NOx的吸附能力的下降。通过升温热脱附方式及降温通水蒸汽反取代方式研究了NOx在HP2W的脱附情况,发现了与Keggin结构HGeW相同的脱附结果,即通水蒸气反取代的脱附方式可实现杂多酸的重复使用。通过TPD-MS研究了HP2W对NOx的分解性能,结果发现Dawson结构磷钨酸对NOx的分解能力较Keggin结构低,通过红外分析发现,其原因是由于Dawson结构HP2W所吸附的NOx多以NO及N203形式存在,仅少量NOx以质子化的亚硝酸鎓离子(HNO)+的形式存在,而亚硝酸鎓离子是降低N-O键能促进NOx分解的关键。
三、通过结晶反应及机械掺杂法制备出LnL (Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Yb, Y, Lu, Ho, Er, Tb, Dy, Tm; L=PW11O40)型稀土磷钨酸盐、LnL2型K8H3[Eu(PW11O39)2]以及磷钨酸铯盐Cs3-xHxPW12O40(x=0,0.5,1,1.5,2,2.5,3)催化剂,研究了上述催化剂对NOx的吸附及催化分解性能。LnL型稀土磷钨酸盐对NOx的吸附实验结果表明,LnL对NOx的吸附效率及容量均较低,且其对NOx吸附效率的顺序为：GdPW> PrPW> YPW> SmPW=CePW> LaPW> YbPW> NdPW> EuPW,对NOx吸附容量的顺序为：LaPW> GdPW> YPW> PrPW> CePW> NdPW> YbPW> SmPW> EuPW。通过机械研磨法制备出LnPW与HPW等质量掺杂的复合催化剂LnPW/HPW,并对其进行NOx吸附实验,结果表明该催化剂对NOx的吸附能力比掺杂HPW前有较大提高。通过快速升温的方式对所吸附的NOx进行催化分解,结果表明,含稀土元素的复合催化剂对NOx的分解性能均高于单纯的HPW,其催化分解NOx为氮气的活性顺序为：YPW/HPW> TmPW/HPW> YbPW/HPW> PrPW/HPW> TbPW/HPW> SmPW/HPW> LuPW/HPW> EuPW/HPW> LaPW/HPW> CePW/HPW> ErPW/HPW> GdPW/HPW> DyPW/HPW> HoPW/HPW> NdPW/HPW。研究了EuPW与HPW不同掺杂比所制备的EuPW/HPW催化剂对NOx的吸附与分解性能,结果表明,在复合催化剂中HPW主要起吸附NOx作用,EuPW主要起催化分解NOx作用,因此高HPW含量的催化剂具有高的NOx吸附能力,高EuPW含量的催化剂具有高的NOx分解能力。通过向EuPW/HPW催化剂中掺杂碳纳米管(CNTs),研究了微波辅助下NOx的催化分解。结果表明,提高CNTs掺杂量可促进NOx的分解。通过对比等质量掺杂HPW的LnL型与LnL2型稀土磷钨酸对NOx的吸附性能,发现由于LnL2型催化剂中K离子的存在,使其具有较大的比表面积,因此可以更好的分散HPW提高其比表面积,进而使其较LnL型掺杂具有更高的NOx吸附效率。采用TPD-MS技术对比研究了HPW、EuPW/HPW及K8H3[Eu(PW11O39)2]/HPW对NOx的分解性能,结果发现,由于稀土杂多酸盐的掺杂,EuPW/HPW对NOx催化分解性能高于HPW,而LnL2型催化剂K8H3[Eu(PW11039)2]中由于杂多化合物中缺位结构与碱土金属K的存在,使分解产生的氧原子被缺位结构及K原子所捕获而无法脱离催化剂表面,从而造成氧阻抑,因此导致LnL2型杂多酸盐具有低的NOx分解性能。
研究了磷钨酸铯盐催化剂对NOx的吸附及催化分解性能,结果表明,由于磷钨酸铯盐的高比表面积,有利于HPW在其上的分散及对NOx的吸附,CS3-xHxPW12O40对NOx吸附效率的递变顺序为：Cs,H2PW> Cs1.5H1.5PW> Cs2H1PW> Cs2.5H0.5PW> Cs0.5H2.5PW;通过TPD-MS技术研究了磷钨酸铯盐催化剂中HPW与Cs3PW不同掺杂比对催化分解NOx性能的影响,结果表明,由于碱金属Cs对O的吸附能力,导致催化剂分解所产生的氧无法由催化剂上脱除,进而造成催化剂活性下降,且Cs3PW掺杂量越多,催化剂对NOx的分解性能越差。
四、将碳纳米管载体分别经混酸与硝酸蒸汽预处理并在不同温度下煅烧,随后分别采用浸渍法及机械研磨法负载磷钨酸,制备出HPW/CNTs催化剂,首次对比考察了上述催化剂对NOx的吸附与分解效果。在空速为10000h-1、吸附温度为200℃的条件下,以0.5g催化剂对1000ppm的NOx进行吸附实验,结果表明,以硝酸蒸汽预处理且经300℃煅烧后的CNTs为载体,采用机械研磨负载法制备的催化剂HPW/CNTs对NO、的吸附率与吸附能力最高,分别为54%与16.6mg NOx/g·h。对吸附NOx后的催化剂体系进行了催化分解NO、的TPD-MS研究,结果表明,所吸附的NO、在快速升温过程中发生分解,首次发现了过程中氧的产生,分解产物包括N2、O2及N2O。采用电阻炉快速加热与微波辐射两种方式分别对吸附的NOx进行催化分解,结果表明,微波功率为700W时,NOx分解为N2的收率为33.3%,高于电阻炉以150℃/min快速升温的N2收率。使用过的催化剂通水蒸汽后可实现再生,对再生后的催化剂进行循环使用研究,结果表明,再生后的催化剂吸附与催化分解NO、的性能未有明显下降。
五、分别以微波辅助法及水热合成法将NH4PW原位合成并固载于USY沸石笼,制备出“瓶中船”型催化剂NH4PW-USY,进而以NOx为氧化剂氧化去除NH4PW-USY中的NH4+得到H+,由此首次制备出沸石笼中只含有HPW的“瓶中船”型催化剂HPW-USY,并研究了该催化剂对NOx的吸附、脱附及分解性能。通过IR、XRD及孔径孔容表征发现微波辅助法在NH4PW-USY的制备中,具有不破坏沸石笼结构及高效率等特点而优于水热合成法。由于还原剂NH4PW高度分散于USY,“瓶中船”型催化剂NH4PW-USY具有高的还原NOx能力,其对NOx的去除效率高达65%,高于单纯的USY及NH4PW对NOx的去除率,分别为5%与50%。NH4PW-USY与NOx完全反应后,通过IR及Py-IR证实了HPW-USY被成功制备。考察了HPW-USY对NOx的吸附与脱附,发现其吸附容量可达2.7mg NOx/g,吸附饱合NOx后,可采用降温通水蒸汽的方式实现脱附。吸附NOx后刘HPW-USY进行TPD-MS测试,分解过程中发现了O2的产生,催化剂HPW-USY对NOx的转化率与N2选择性分别为64.9%与74.3%,均高于单纯HPW催化剂对NOx的转化率与N2选择性。
More and more research institutions pay close attention to nitrogen oxides (NOx) abatement, due to the increasing NOx emission and the introduction of more rigorous environmental laws. NOx catalytic decomposition has been one of the most attractive methods, for no reducing agent is consumed and pollution-free N2and O2are the only products. Heteropoly compounds (HPCs) have been widely used in the catalytic reaction because of its special crystal structure and catalytic properties. The application of HPCs on NOx elimination have been researched for many years, however, they are mainly used as NOx absorbent or used in NOx catalytic reduction. Keggin type phosphotungstic acid (HPW) is the most studied HPCs, while there are many HPCs that have not been explored in NOx abatement. In this thesis, novel Keggin and Dawson type heteropoly acids (HPAs), the lanthanide complexes and cesium salt of HPW and the supported catalyst were prepared and used in the NOx adsorption and decomposition. The content of this thesis contains the following five parts.
I) NOx Adsorption-Decomposition on Keggin Type Heteropoly Acids Containing Germanium
Four kinds of keggin stucture HPAs employing germanium as central atom, including tungstogermanic heteropoly acid (abbr. HGeW), tungstovanadogermanic heteropoly acid H5GeW11V040(abbr. HGeWV), molybdovanadogermanic heteropoly acid H5GeMo11V040(abbr. HGeMoV) and molybdotungstovanadogermanic heteropoly acid H5GeW9Mo2V04o (abbr. HGeWMoV) were first applied as catalysts to remove NOx in lean exhaust gas, and they were synthesized and characterized by IR measurements. The adsorption tests showed that at the optimum adsorption temperature of230℃, the synthesized catalysts showed excellent NOx adsorption ability in the following order:HGeW> HGeWV> HGeWMoV> HGeMoV, and among which HGeW had the highest NOx adsorption efficiency and capacity of80% and16.2mg NOx/g. Two new IR absorption bands at2210and1851cm-1appeared after NOx being adsorbed on HGeW, the latter band was observed for the first time on HPAs adsorbed NOx, and was assigned to nitrosyl radical (NO-). Experiments on NOx desorption and the reusability of absorbent were carried out on HGeW by increasing oven temperature and cooling in wet air. The results showed that NOx could be desorbed through both two methods and the reusability of HGeW could be realized by the latter method. Temperature-programmed desorption-mass spectroscopy (TPD-MS) was carried out to investigate the decomposition of NOx on the synthesized catalysts and and purchased phosphotungstic acid (HPW) and for the first time, the formation of O2was observed on all of the catalysts mentioned above, and the decomposition products were comprised of N2, O2and N2O. The effect of heteroatom and polyatom on NOx decomposition was investigated, and the result showed that heteroatom Ge was superior to P, polyatom W was superior to Mo for NOx transformation, while it was inferior to Mo as for N2selectivity, and after substitute by V the catalytic activity would decrease. The effects of heating rate and gas velocity on NOx decomposition were investigated and the results showed that increasing the heating rate and decreasing the gas velocity promoted the NOx transformation, however, too high heating rate and too low gas velocity decreased the N2selectivity.
Ⅱ) NOx Adsorption-Aecomposition on Dawson Type Phosphotungstic Acid
The Dawson type phosphotungstic heteropolyacid (HP2W) was synthesized and characterized by IR, XRD and TGA measurements. NOx adsorption, desorption and decomposition were explored on HP2W. The influences of temperature, gas velocity, crystal water and pretreatment of HP2W on NOx adsorption were examined, the results showed that the NOx adsorption optimum temperature was200℃, the NOx adsorption efficiency had an inverse relationship with gas velocity, and the maximum NOx adsorption efficiency of78%was observed at the gas velocity of5000-1h. Two types of crystal water were observed on HP2W, among which the physical adsorbed water hindered the NOx adsorption, while the chemical adsorbed water improved it. After pretreated in the atmosphere of oxygen, hydrogen and nitrogen individually, the HP2W showed no significant difference on NOx adsorption. NOx desorption by improving temperature and cooling in wet air were comparatively studied, and the result was the same as that of HgeW explored in I), that is to say, desorption by cooling in wet air had a better performance for the reusability of HP2W could be realized through this method. TPD-MS was taken to investigate the NOx decomposition on Dawson type HP2W. Compared with Keggin type HPW, Dawson type phosphotungstic acid had lower catalytic activity, and the reason was attributed to the fact that less NOx was adsorbed on the second crystal structure of HP2W in the form of (HNO)+, which would improve the NOx decomposition by weakening the N-O bond.
Ⅲ) NOx Adsorption-Decomposition on Salts of Phosphotungstic Acid
LnL (Ln=La, Ce, Pr, Nd, Sm, Eu, Gd, Yb, Y, Lu, Ho, Er, Tb, Dy, Tm; L=PW11O40), LnL2type K8H3[Eu(PW,,039)2] and Cs3-xHxPW1204o(x=0,0.5,1,1.5,2,2.5,3) were prepared and used for NOx adsorption and decomposition. The adsorption results showed that NOx adsorption efficiency and capacity on LnL were lower, and for the NOx adsorption efficiency, LnL exhibited the following order: GdPW> PrPW> YPW> SmPW=CePW> LaPW> YbPW> NdPW> EuPW, while for the adsorption capacity the order was:LaPW> GdPW> YPW> PrPW> CePW> NdPW> YbPW> SmPW> EuPW. After doped with HPW, the NOx adsorption ability of LnL/HPW was improved significantly. The NOx decomposition on LnL/HPW was explored by rapid heating, and the results showed that the catalytic decomposition of NOx on LnL/HPW were superior than that of HPW, and for the N2yeild the catalytic activity followed the order:YPW/HPW> TmPW/HPW YbPW/HPW> PrPW/HPW> TbPW/HPW> SmPW/HPW> LuPW/HPW> EuPW/HPW> LaPW/HPW> CePW/HPW> ErPW/HPW> GdPW/HPW> DyPW/HPW> HoPW/HPW> NdPW/HPW. The effects of doping ratio between EuPW and HPW on adsorption and decomposition of NOx were studied. The results showed that HPW played the role of NOx adsorbent while EuPW as catalyst for decomposition of NOx, and more HPW in EuPW/HPW contributed to higher NOx adsorption efficiency and capacity, while more EuPW contributed to high NOx transformation and N2selectivity. Microwave was introduced to NOx decomposition on the catalyst of EuPW/HPW/CNTs, and the result showed that the decomposition of NOx was related to ratio of CNTs, and more CNTs improved the NOx decomposition. Compared with LnL type EuPW/HPW, the LnL2type K8H3[Eu(PW11O39)2]/HPW had higher NOx adsorption efficiency for the K ion increased the special surface thus improved the HPW dispers on K8H3[Eu(PW11O39)2], while the NOx decomposition on K8H3[Eu(PW11O39)2]/HPW was inferior to that of EuPW/HPW for the defect site and K ion on K8H3[Eu(PW11O39)2] captured O and inhibited the O removal from catalyst. NOx adsorption and decomposition on Cs3_xHxPW12O040were studied, the adsorption results showed that due to the high special surface of CS3PW, and the Cs3_xHxPW12O40exhibited fine NOx adsorption ability with the following order: CS1H2PW> Cs1.5H1.5PW> Cs2H1PW> Cs2.5H0.5PW> Cs0.5H2.5PW. TPD-MS was taken on Cs,H2PW and Cs2H1PW to investigate the effect of ratio between Cs3PW and HPW on NOx decomposition, the result showed that because the alkalis metal Cs had the O adsorption ability and O inhibited the NOx catalytic decomposition, so the more Cs, the less decomposition activity on CS3-XHxPW12O40.
Ⅳ) NOx Adsorption-Decomposition on H3PW12O40/CNTS
A series of HPW/CNTs catalysts were prepared by impregnation and mechanical grinding methods. For this purpose, CNTs was pre-treated separately by nitric acid vapor, mixture of nitric acid and sulphuric acid, and subsequently calcined. The performances of catalysts on NOx adsorption-decomposition were studied.0.5g catalyst was used to adsorb1000ppm NOx under the space velocity of1000h-1at200℃, and the results showed that the catalyst prepared by mechanical grinding methods supporting HPW on CNTs pretreated by nitric acid vapor and calcined at300℃had the highest NOx adsorption efficiency and capacity of54%and16.6mg NOx/g·h, respectively. TPD-MS was carried out on the catalyst adsorbed NOx, and the result showed that N2, O2and N2O were formed during rapid heating, among which O2was observed for the first time. Two modes of decomposition were employed, and one was by electric oven at a ramping rate of150℃/min, and the other was by microwave oven. Compared to the mode of the former, the latter has higher N2yield with a N2yield up to33.3%corresponding to the power of microwave oven being700W. The catalyst used can be reusable by water vapor reactivation, and the recycling results showed that there were no significant performance degradation for NOx adsorption and catalytic decomposition.
V) NOx Adsorption-Decomposition on "Ship in Bottle" Type HPW-USY
To synthesis pure HPW encaged in USY zeolite (HPW-USY), NH4PW encaged in the USY (NH4PW-USY) was firstly prepared by the methods of microwave radiation and hydrothermal synthesis. FT-IR, XRD, BET, pore size and pore volume measurements indicated that microwave radiation method was superior to hydrothermal synthesis in the preparation of NH4PW-USY. Then NH4PW-USY was used to reduce NOx, and accompanied with the consumption of NH4+and formation of H+, NH4PW-USY was turned into HPW-USY simultaneously, which was confirmed by FT-IR and in site pyridine adsorption IR. NOx adsorption-desorption behavior on HPW-USY was studied. The NOx adsorption capacity was2.7mg NOx/g, and the adsorbed NOx was desorbed when the temperature was decreased to ca.100℃in wet air. TPD-MS was carried out on HPW-USY adsorbed NOx to explore the performance of catalytic decomposition NOx. For the first time, O2production was observed a little latter than the formation of N2O and N2, the NOx conversion was64.9%and N2selectivity was74.3%on HPW-USY, which was higher than pure HPW.
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