萘、甲基萘在Ni_2P/SiO_2及Pd-Pt/SiO_2-Al_2O_3催化剂上的加氢研究
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摘要
随着世界优质原油储量的日渐枯竭,原油供应已有明显重质化、劣质化的趋势。另一方面,为缓解原油供应紧张的局面,煤焦油、页岩油、油砂沥青等非常规能源被认为是很有潜力的石油补充能源。然而不论是重质劣质原油还是煤焦油、页岩油、油砂沥青,都含有大量芳烃,过多的芳烃会降低燃料的燃烧性能并造成环境污染,深度脱芳烃已经成为清洁燃料生产的一个重要课题。在现有的脱芳烃技术中,加氢脱芳烃是最有效的。目前工业上加氢脱芳烃多采用传统的过渡金属硫化物催化剂,此类催化剂活性较低,已不能适应深度脱除大量稠环芳烃的需要。贵金属催化剂的加氢脱芳烃性能好,但对硫敏感,极易中毒失活。因此,需要开发活性更高的加氢脱芳烃催化剂,或改善贵金属的抗硫性。另外,目前关于含硫物质对加氢过程影响的研究很多,而关于含氮物质对加氢脱芳烃反应及催化剂影响的研究较少。针对这些问题,本论文选取油品中较有代表性的芳烃：萘及α、β-甲基萘作为模型化合物,尝试将新型催化材料磷化镍应用于上述芳烃的加氢反应,考察了其加氢脱芳烃性能,探讨了其加氢机理及含氮化合物(喹啉)在反应中对其造成的影响,并用XRD、TEM、N2吸附、CO化学吸附、Py-IR和XPS等表征手段对催化剂进行了表征。还按不同Pd/Pt摩尔比制备了一系列Pd-Pt贵金属催化剂,将Pd/Pt摩尔比与催化剂抗硫性能进行了关联。研究内容和主要结果包括：
用原位还原法制备了Si02负载的Ni2P催化剂,考察了不同Ni/P摩尔比和负载量对催化剂芳烃加氢活性的影响。结果表明,当Ni/P摩尔比为1.25、负载量为30 wt%时催化剂活性最高。在该催化剂上,萘的转化率最高可达100%,十氢萘选择性最高可达92.1%；α、p-甲基萘的转化率最高可达96.0%和99.0%,1-甲基十氢萘和2-甲基十氢萘选择性最高可达27.0%和82.6%,各项指标均高于相同质量的硫化态Ni-W催化剂。通过计算得到,温度为340℃时,萘加氢生成四氢萘的反应速率常数k1为0.80 min-1,四氢萘加氢生成十氢萘的反应速率常数k2为0.84 min-1,两步加氢的反应速率常数之比kR(=k1/k2)为0.95。Ni2P/SiO2催化剂的活性位具有使顺式十氢萘异构生成反式十氢萘的活性。
α、β-甲基萘对活性位的吸附能力要远高于萘,α-甲基萘的吸附能力又略高于p-甲基萘。喹啉及其加氢中间产物对活性位强烈的竞争吸附会强烈抑制萘的加氢,萘则会阻碍四氢喹啉加氢生成十氢喹啉。二苯并噻吩的加入会导致萘转化率降低,这要归因于S在催化剂表面上的不可逆吸附。
用浸渍法制备了Si02-Al203负载的Pd-Pt (Pd:Pt=1:1; 1:4; 4:1)双金属催化剂,比较了其芳烃加氢性能及抗硫性。结果表明,Pd-Pt (Pd:Pt=4:1)催化剂上的芳烃转化率和完全加氢产物生成率最高。在该催化剂上,萘转化率最高可达98.2%,十氢萘选择性最高可达93.6%,α、β-甲基萘转化率最高可达97.5%和98.2%,1-甲基十氢萘和2-甲基十氢萘选择性最高可达18.5%和73.0%。萘在单金属Pd、Pt及Pd-Pt (Pd:Pt=4:1)三种催化剂上的加氢速率顺序为υpd-Pt(4:1)>υpd>υpt。反应物中加入二苯并噻吩后,Pd-Pt (Pd:Pt=4:1)仍有最高的芳烃加氢活性。
With world high-quality crude oil reserves being depleted, the crude oil reserves have a trend of becoming heavier and degraded. On the other hand, in order to alleviate oil shortages, the coal tars, shale oils and oil sand asphalts are considered as potential supplements of crude oils. However, the coal tars, shale oils and oil sand asphalts contain large amounts of aromatics. Excessive aromatics not only lower the combustibility of fuels, but also produce hazardous particulates and cause environmental pollution. Hence, deeply removing aromatics has become increasingly important. Hydrodearomatization (HDA) is the most effective way to remove aromatics. Petroleum industry today mostly uses the transition metal sulfide catalysts, but the activity of this type of catalyst is too low to adapt for deeply removing large quantities of polynuclear aromatics. Noble metal catalysts have high HDA activities, but they are liable to be poisoned by sulfides in liquid fuels. As a result, the new catalyst which has higher HDA activity must be developed; also, the sulfur resistance of noble metal must be improved. On the other hand, although there are a lot of research works about the effects of S-containing compounds on hydrogenation and HDA, the research works about the effects of N-containing compounds on HDA and catalyst are rare. In order to solve these problems, naphthalene andα/β-methylnaphthalene were chosen as the model compounds of liquid fuels. The new catalytic material nickel phosphide was applied in hydrogenation of the aromatics which were mentioned previously, the HDA activity of nickel phosphide was studied; the reaction mechanism and the effects of N-containing compound (quinoline) on catalyst were investigated, too. The catalysts were characterized by XRD, TEM, N2 adsorption, CO chemisorption, Py-IR, and XPS. A series of Pd-Pt bimetallic catalysts with different Pd/Pt molar ratios were prepared, and the relationship between Pd/Pt molar ratio and catalyst's sulfur resistance was studied. The main contents and results are as follows:
A series of Ni2P/SiO2 catalysts with different Ni/P molar ratio and loading in the oxidic precursors were prepared by an in-situ reduction method. Their catalytic performances were evaluated in aromatics hydrogenation. The optimal initial Ni/P ratio is 1.25 and the optimal loading of NiO and P2O5 is 30 wt%. On this catalyst, the naphthalene conversion is up to 100%, the selectivity to decalin is up to 92.1%; theα/β-methylnaphthalene conversions are up to 96.0% and 99.0%, the selectivity to 1-methyldecalin and 2-methyldecalin are up to 27.0% and 82.6%. These values are all higher than those on sulfided Ni-W catalyst. The reaction rate constant of naphthalene yield tetralin k1 is 0.80 min-1, the reaction rate constant of tetralin yield decalin k2 is 0.84 min-1, the ratio of k1/k2 is 0.95. Cis-decalin can be isomerized to trans-decalin on active sites of Ni2P/SiO2.
The competitive adsorptions ofα-andβ-methylnaphthalene hinder naphthalene hydrogenation, and naphthalene has negligible effects onα/β-methylnaphthalene hydrogenation. The adsorptive capacities ofα-andβ-methylnaphthalene are far higher than that of naphthalene, and the adsorptive capacity ofα-methylnaphthalene is a little higher than that ofβ-methylnaphthalene. Quinoline and its hydrogenation intermediate products hinder naphthalene hydrogenation, while naphthalene hinders tetrahydroquinoline yielding decahydroquinoline. The addition of dibenzothiophene leads to a decline of naphthalene conversion, which may be attributed to irreversible adsorption of S on catalyst surface.
Bimetallic Pd-Pt (Pd:Pt=1:1;1:4;4:1) catalysts supported on SiO2-Al2O3 were prepared by immersion method. Their hydrogenation activities and sulfur resistances were analyzed and compared. Results showed that, the Pd-Pt (Pd:Pt=4:1) catalyst showed the highest activity and selectivity to full hydrogenation products. On this catalyst, the naphthalene conversion and selectivity to decalin are up to 98.2% and 93.6%, respectively,α-andβ-methylnaphthalene conversions are up to 97.5% and 98.2%, the selectivity to 1-methyldecalin and 2-methyldecalin are up to 18.5% and 73.0%. The order of naphthalene hydrogenation rate on Pd, Pt and Pd-Pt (Pd:Pt=4:1) follow the sequence:υPd-Pt(4:1)>υPd>υPt. The hydrogenation activity of Pd-Pt (Pd:Pt=4:1) catalyst is still the highest in the presence of dibenzothiophene.
用原位还原法制备了Si02负载的Ni2P催化剂,考察了不同Ni/P摩尔比和负载量对催化剂芳烃加氢活性的影响。结果表明,当Ni/P摩尔比为1.25、负载量为30 wt%时催化剂活性最高。在该催化剂上,萘的转化率最高可达100%,十氢萘选择性最高可达92.1%；α、p-甲基萘的转化率最高可达96.0%和99.0%,1-甲基十氢萘和2-甲基十氢萘选择性最高可达27.0%和82.6%,各项指标均高于相同质量的硫化态Ni-W催化剂。通过计算得到,温度为340℃时,萘加氢生成四氢萘的反应速率常数k1为0.80 min-1,四氢萘加氢生成十氢萘的反应速率常数k2为0.84 min-1,两步加氢的反应速率常数之比kR(=k1/k2)为0.95。Ni2P/SiO2催化剂的活性位具有使顺式十氢萘异构生成反式十氢萘的活性。
α、β-甲基萘对活性位的吸附能力要远高于萘,α-甲基萘的吸附能力又略高于p-甲基萘。喹啉及其加氢中间产物对活性位强烈的竞争吸附会强烈抑制萘的加氢,萘则会阻碍四氢喹啉加氢生成十氢喹啉。二苯并噻吩的加入会导致萘转化率降低,这要归因于S在催化剂表面上的不可逆吸附。
用浸渍法制备了Si02-Al203负载的Pd-Pt (Pd:Pt=1:1; 1:4; 4:1)双金属催化剂,比较了其芳烃加氢性能及抗硫性。结果表明,Pd-Pt (Pd:Pt=4:1)催化剂上的芳烃转化率和完全加氢产物生成率最高。在该催化剂上,萘转化率最高可达98.2%,十氢萘选择性最高可达93.6%,α、β-甲基萘转化率最高可达97.5%和98.2%,1-甲基十氢萘和2-甲基十氢萘选择性最高可达18.5%和73.0%。萘在单金属Pd、Pt及Pd-Pt (Pd:Pt=4:1)三种催化剂上的加氢速率顺序为υpd-Pt(4:1)>υpd>υpt。反应物中加入二苯并噻吩后,Pd-Pt (Pd:Pt=4:1)仍有最高的芳烃加氢活性。
With world high-quality crude oil reserves being depleted, the crude oil reserves have a trend of becoming heavier and degraded. On the other hand, in order to alleviate oil shortages, the coal tars, shale oils and oil sand asphalts are considered as potential supplements of crude oils. However, the coal tars, shale oils and oil sand asphalts contain large amounts of aromatics. Excessive aromatics not only lower the combustibility of fuels, but also produce hazardous particulates and cause environmental pollution. Hence, deeply removing aromatics has become increasingly important. Hydrodearomatization (HDA) is the most effective way to remove aromatics. Petroleum industry today mostly uses the transition metal sulfide catalysts, but the activity of this type of catalyst is too low to adapt for deeply removing large quantities of polynuclear aromatics. Noble metal catalysts have high HDA activities, but they are liable to be poisoned by sulfides in liquid fuels. As a result, the new catalyst which has higher HDA activity must be developed; also, the sulfur resistance of noble metal must be improved. On the other hand, although there are a lot of research works about the effects of S-containing compounds on hydrogenation and HDA, the research works about the effects of N-containing compounds on HDA and catalyst are rare. In order to solve these problems, naphthalene andα/β-methylnaphthalene were chosen as the model compounds of liquid fuels. The new catalytic material nickel phosphide was applied in hydrogenation of the aromatics which were mentioned previously, the HDA activity of nickel phosphide was studied; the reaction mechanism and the effects of N-containing compound (quinoline) on catalyst were investigated, too. The catalysts were characterized by XRD, TEM, N2 adsorption, CO chemisorption, Py-IR, and XPS. A series of Pd-Pt bimetallic catalysts with different Pd/Pt molar ratios were prepared, and the relationship between Pd/Pt molar ratio and catalyst's sulfur resistance was studied. The main contents and results are as follows:
A series of Ni2P/SiO2 catalysts with different Ni/P molar ratio and loading in the oxidic precursors were prepared by an in-situ reduction method. Their catalytic performances were evaluated in aromatics hydrogenation. The optimal initial Ni/P ratio is 1.25 and the optimal loading of NiO and P2O5 is 30 wt%. On this catalyst, the naphthalene conversion is up to 100%, the selectivity to decalin is up to 92.1%; theα/β-methylnaphthalene conversions are up to 96.0% and 99.0%, the selectivity to 1-methyldecalin and 2-methyldecalin are up to 27.0% and 82.6%. These values are all higher than those on sulfided Ni-W catalyst. The reaction rate constant of naphthalene yield tetralin k1 is 0.80 min-1, the reaction rate constant of tetralin yield decalin k2 is 0.84 min-1, the ratio of k1/k2 is 0.95. Cis-decalin can be isomerized to trans-decalin on active sites of Ni2P/SiO2.
The competitive adsorptions ofα-andβ-methylnaphthalene hinder naphthalene hydrogenation, and naphthalene has negligible effects onα/β-methylnaphthalene hydrogenation. The adsorptive capacities ofα-andβ-methylnaphthalene are far higher than that of naphthalene, and the adsorptive capacity ofα-methylnaphthalene is a little higher than that ofβ-methylnaphthalene. Quinoline and its hydrogenation intermediate products hinder naphthalene hydrogenation, while naphthalene hinders tetrahydroquinoline yielding decahydroquinoline. The addition of dibenzothiophene leads to a decline of naphthalene conversion, which may be attributed to irreversible adsorption of S on catalyst surface.
Bimetallic Pd-Pt (Pd:Pt=1:1;1:4;4:1) catalysts supported on SiO2-Al2O3 were prepared by immersion method. Their hydrogenation activities and sulfur resistances were analyzed and compared. Results showed that, the Pd-Pt (Pd:Pt=4:1) catalyst showed the highest activity and selectivity to full hydrogenation products. On this catalyst, the naphthalene conversion and selectivity to decalin are up to 98.2% and 93.6%, respectively,α-andβ-methylnaphthalene conversions are up to 97.5% and 98.2%, the selectivity to 1-methyldecalin and 2-methyldecalin are up to 18.5% and 73.0%. The order of naphthalene hydrogenation rate on Pd, Pt and Pd-Pt (Pd:Pt=4:1) follow the sequence:υPd-Pt(4:1)>υPd>υPt. The hydrogenation activity of Pd-Pt (Pd:Pt=4:1) catalyst is still the highest in the presence of dibenzothiophene.
引文
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