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WP/γ-Al2O3催化剂的制备、表征及加氢脱硫和加氢脱氮活性 总被引:1,自引:0,他引:1
Two series of WP/Al2O3 catalyst precursors with WP mass loading in the range 18.5%-37.1% were prepared using the impregnation method and mixing method, respectively, and the catalysts were then obtained by temperature-programmed reduction of supported tungsten phosphate (precursor of WP/Al2O3 catatlysts) in H2 at 650℃ for 4h. The catalysts were characterized by XRD, BET, TG/DTA, XPS and 31p MAS-NMR. The activities of these catalysts were tested in the hydrodenitrogenation (HDN) of pyridine and hydrodesulfurization (HDS) of thiophene at 340℃ and 3.0MPa. The results showed that owing to the stronger interaction of the support with the active species, the precursor of WP/Al2O3 catalyst was more difficultly phosphided and a greater amount of W species was in a high valence state W6 on the surface of the catalyst prepared by the impregnation method than that by the mixing method. 31p MAS-NMR results indicated that 31p shift from 85% H3PO4 of 2.55 × 10-4 for WP and 2.57 × 10-4 for WP/γ-Al2O3 catalysts prepared by mixing method. Such WP/Al2O3 catalysts showed higher HDN activities and lower HDS activities than those prepared by the impregnation method under the same loading of WP.WP/γ-Al2O3 catalysts with weak interaction between support and active species were favorable for HDN reaction while the WP/γ-Al2O3 catalysts with strong interaction were favorable for HDS reaction. 相似文献
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作为现今柴油脱硫的主流,加氢催化脱硫得到了极广泛的应用,对国内外加氢催化脱硫技术及催化剂进行了简要介绍及展望,指出在发展氧化脱硫、生物脱硫的同时,不要忽略对加氢脱硫的进一步研究和改进。 相似文献
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考察了催化裂化(FCC)汽油中硫化物和模型硫化物在OTA(Olefin To Aromatics)催化剂上的催化转化性能.结果表明FCC汽油硫化物总脱硫率为86.3 %,其中,硫醚和四氢噻吩的转化率都达到100 %,硫醇硫转化率96.6 %,噻吩硫转化率78.8 %,烷基噻吩转化率85.8 %,苯并噻吩转化率81.4 %.3-甲基噻吩在OTA催化剂上的转化产物中含有小分子(噻吩),异构硫化物(2-甲基噻吩),以及大分子异构硫化物(如2,5-二甲基噻吩、2,4-二甲基噻吩和2,3-二甲基噻吩).烷基噻吩和苯并噻吩硫化物在OTA催化剂上脱硫反应网络一方面含有直接加氢脱硫反应,另一方面经历歧化、异构化和裂解等反应. 相似文献
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原油的劣质化和环保法规的日益严格使馏分油的加氢精制技术面临严峻挑战,近年来,磷化镍(Ni2P)由于具有优异的加氢脱硫和加氢脱氮性能已成为新型催化加氢材料研究的焦点。本文综述了Ni2P的制备、表征和催化性能方面的研究进展。磷化氢还原法、次磷酸盐还原法和氢气等离子体还原法可在较低温度下制备高活性Ni2P催化剂。扫描透射电镜表明Ni2P(0001)表面有Ni3P和Ni3P2两种可能的终端结构。Ni3P终端的Ni是四方锥型结构,有解离H吸附;而Ni3P2终端的Ni是四面体型结构,无解离H吸附,这表明四方锥型的Ni活性点具有高反应活性。从目前的研究看,Ni2P是具有潜在应用前景的一种新型加氢精制催化材料。 相似文献
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考察了成型时拟薄水铝石和合金粉的比例、胶溶剂硝酸质量分数,水粉比及焙烧温度对骨架镍催化剂侧压强度的影响,采用XRD和TG-DTA等手段对催化剂进行表征。结果表明,催化剂侧压强度随着拟薄水铝石和合金粉的比例、胶溶剂硝酸质量分数、水粉比以及焙烧温度的提高呈现先增加后减小的规律,在拟薄水铝石与合金粉质量比1.5、胶溶剂硝酸质量分数6%和水粉比0.21 mL.g-1条件下成型,860℃空气中焙烧,得到侧压强度最好的催化剂,以苯乙烯、甲基苯乙烯加氢为探针反应,对催化剂的加氢性能进行评价,结果表明,在反应压力2 MPa、温度80℃、原料空速2 h-1和V(H2)∶V(油)=300∶1条件下,苯乙烯与甲基苯乙烯在考察的500 h运转周期内,转化率接近100%,且催化剂活性保持稳定。 相似文献
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以碳酸镁、活性炭为原料,采用浸渍法制备了一系列MgO/C-CoPcS脱硫醇催化剂。研究了活性组分磺化酞菁钴(CoPcS)负载量和n(Mg)∶n(C)对催化剂活性的影响。通过XRD和BET对催化剂进行表征。实验结果表明, n(Mg)∶n(C)=0.2,CoPcS负载质量分数为1%时,催化剂活性最高。CoPcS的加入对催化剂的晶型没有影响;随着n(Mg)∶n(C)增加,MgO特征峰加强,比表面积降低。制备了n(Mg)∶n(C)=0.2,磺化酞菁钴负载质量分数为1%的MgO/C-CoPcS催化剂,进行了微型固定床反应实验。空速为2 h-1条件下,反应超过750 h,转化率保持在99%以上。 相似文献
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以具有较低热膨胀系数和较好抗热冲击性的堇青石蜂窝状陶瓷为载体、Fe-Mo/ZSM-5为活性组分制备了蜂窝状催化剂,研究了表面活性剂、载体和涂覆方法等条件对蜂窝状催化剂性能及其催化活性的影响。采用XRD、FT-IR、BET和SEM等技术对蜂窝状催化剂的体相结构、表面离子形态等进行了表征和研究。结果表明,以羧甲基纤维素为表面活性剂、美国康宁公司的堇青石蜂窝状陶瓷为载体和超声波法涂覆的蜂窝状催化剂具有最佳的催化活性,300 ℃时NOx催化转化率达100%,且随着温度的升高保持不变。 相似文献
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Guida Sun Cuiqing Li Zhijun Zhou Fengyan Li 《Frontiers of Chemical Engineering in China》2008,2(2):155-164
Supported tungsten phosphide catalysts were prepared by temperature-programmed reduction of their precursors (supported phospho-tungstate
catalysts) in H2 and characterized by X-ray diffraction (XRD), BET, temperature-programmed desorption of ammonia (NH3-TPD) and X-ray photoelectron spectroscopy (XPS). The reduction-phosphiding processes of the precursors were investigated
by thermogravimetry and differential thermal analysis (TG-DTA) and the suitable phosphiding temperatures were defined. The
hydrodesulfurization (HDS) and hydrodenitrogenation (HDN) activities of the catalysts were tested by using thiophene, pyridine,
dibenzothiophene, carbazole and diesel oil as the feedstock. The TiO2, γ-Al2O3 supports and the Ni, Co promoters could remarkably increase and stabilize active W species on the catalyst surface. A suitable
amount of Ni (3%–5%), Co (5%–7%) and V (1%–3%) could increase dispersivity of the W species and the BET surface area of the
WP/γ-Al2O3 catalyst. The WP/γ-Al2O3 catalyst possesses much higher thiophene HDS and carbazole HDN activities and the WP/TiO2 catalyst has much higher dibenzothiophene (DBT) HDS and pyridine HDN activities. The Ni, Co and V can obviously promote the
HDS activity and inhibit the HDN activity of the WP/γ-Al2O3 catalyst. The G-Ni5 catalyst possesses a much higher diesel oil HDS activity than the sulphided industrial NiW/γ-Al2O3 catalyst. In general, a support or promoter in the WP/γ-Al2O3 catalyst which can increase the amount and dispersivity of the active W species can promote its HDS and HDN activities. 相似文献
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以介孔分子筛SBA-15为载体,制备一系列不同La含量的La-Ni2P/SBA-15催化剂前驱体,将La-Ni2P/SBA-15前驱体涂覆在预处理的整体式载体堇青石上,在H2气氛程序升温还原,制备不同La含量的La-Ni2P/SBA-15/堇青石整体式催化剂。对合成的催化剂进行X射线衍射和N2吸附-脱附结构表征,并评价对二苯并噻吩的加氢脱硫活性。结果表明,Ni2P存在于所有的La-Ni2P/SBA-15/堇青石整体式催化剂中,且随着La含量的增加,La-Ni2P/SBA-15/堇青石整体式催化剂的比表面积和孔体积均有一定程度的提高,催化活性也提高。对于Ni2P/SBA-15/堇青石整体式催化剂,在300 ℃和380 ℃时,二苯并噻吩加氢脱硫转化率仅为27.2%和91.3%;而1.5%La-Ni2P/SBA-15/堇青石催化剂在300 ℃和380 ℃时,二苯并噻吩转化率分别为36.8%和96.3%,显示出较好的二苯并噻吩加氢脱硫活性。La-Ni2P/SBA-15/堇青石整体式催化剂在对二苯并噻吩的加氢脱硫过程中,以直接脱硫和加氢脱硫两种脱硫方式同时进行,并且以直接脱硫为主。 相似文献
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采用溶胶-凝胶法制备了TiO2-Al2O3复合载体, 以柠檬酸(CA)为络合剂采用浸渍法制备了Ni2P负载的TiO2-Al2O3复合载体催化剂, 并用 X 射线衍射(XRD)、N2吸附比表面积(BET)测定技术对催化剂的结构和性质进行了表征, 考察了载体焙烧温度、催化剂焙烧温度、还原温度、还原压力对其进行的二苯并噻吩(DBT)加氢脱硫(HDS)性能的影响。结果表明, 升高载体焙烧温度有利于催化剂表面上活性物种的分散, 但焙烧温度过高会导致催化剂烧结, 适宜的载体焙烧温度为550℃。当还原温度为500~550℃时, 磷化镍主要以Ni12P5相形式存在, 且随着还原温度的升高, Ni12P5的衍射峰强度逐渐增强, 还原温度为700℃时, 可得到单一的Ni2P物相。载体焙烧温度为550℃, 催化剂焙烧温度为500℃, 还原温度为700℃, 常压还原制备的Ni2P/TiO2-Al2O3催化剂具有最好的活性。在360℃、3.0MPa、氢油体积比500、液时体积空速2.0h-1的条件下, 反应4h时, DBT转化率为99.5 %。 相似文献
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通过变温陈化步骤,采用水热结晶法制备TS-1分子筛。改变陈化步骤,得到一系列粒径不同的TS-1分子筛,并探究粒径对丙烯醇环氧化反应催化性能的影响。采用FT-IR、UV-Vis、BET、XRD和SEM等表征TS-1分子筛催化剂晶相,结果表明,不同条件制得的TS-1分子筛具有相同的MFI结构,Ti大部分以骨架钛形式存在,也有少量锐钛矿相Ti O2存在。随着反应温度的升高,TS-1粒径逐渐增大。通过后续催化反应发现,TS-1分子筛催化剂的催化活性改变不大,这可能是由于催化剂中活性位点的数目变化不大。从催化剂分离实验可以看出,随着粒径的增大,催化剂回收率从82.4%增至95.3%。 相似文献