SbSn金属间化合物的结构和对石油改性研究
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摘要
随着经济的发展,工农业对原油的需求量越来越大,而原油的品质越来越差,硫和重金属含量不断增高,给后续处理工艺带来很大的麻烦,同时也加剧了环境的污染。另一方面,世界各国对环保的要求越来越高,对原油产品中硫含量的限制越来越苛刻。这两方面的矛盾促使了原油加工中脱硫技术的发展。寻求经济高效的脱硫技术一直是原油加工工业中的一个热点,开发新的脱硫材料和脱硫工艺是一件很有意义的工作。
本文以Sb、Sn为原料,采用不同的非平衡凝固方法和条件来制备SbSn金属间化合物,借助于差示扫描量热(DSC)、X射线衍射(XRD)、X射线光电子能谱(XPS)、俄歇电子能谱(AES)等现代分析手段对制备的材料进行了表征。考察了制备出的材料对原油中沥青质、硫和重金属等杂质的脱除效果。主要内容如下:
1.对熔体的过热处理进行了研究,使用DSC表征了Sn和Sb混合物在升温过程中的变化,结果表明:1:1的锡-锑混合物在超过熔点完全转化为液相以后会在900℃附近发生液相微观结构变化,锡单质也会在970℃附近存在着液相结构的转变。不同熔融温度下制备出的材料的结构并不相同,由750℃下熔融快冷制备出的SbSn颗粒为六方晶体,由950℃下熔融快冷制备出的SbSn颗粒为三方晶体。根据标准图谱提供的金属间化合物SbSn的空间点群和晶格参数,用Materials Studio 3.0.1建立了SbSn的单晶胞空间结构图,并计算出了相应的XRD图,计算图与实测图有一致性。不同熔融温度下制备出材料的表面成分和锑元素的价态有所不同,电压30V,电流400A,淬速30m/s的条件下制备出的材料与950℃下熔融快冷制备出的材料的晶体结构一致,并且表面是富锑的,锑的价态是以+3价为主;电压20V,电流20A,淬速30m/s的条件下制备出的材料与750℃下熔融快冷制备出的材料的晶体结构一致,表面是富锡的,锑的价态是以零价态为主。
2.以沥青质的的脱出率作为评价标准,来确定原油乳化液的最佳配制条件。研究结果表明最优的乳化液配制条件为:表面活性剂为油包水型,含量在0.15%以上,水含量在35%～40%之间。
3.研究了不同的工艺条件对材料的结构和脱硫性能的影响。对于原油乳化液脱硫过程来说,研究结果表明:不同熔融温度下制备出的材料的脱硫性能不同,
With the development of economy, crude oil plays a more and more important role in the agriculture and industry, but the quality of crude oil is becoming poor, and the content of sulfur and heavy metal is increasing continuously, which brings trouble to the follow-up process of crude oil, and polluted the environment badly. On the other hand, the standards of international community to environmental protection trend towards more strict, and the prescriptive value of the sulfur content in crude oil products are becoming lower and lower. The causes from the above two sides urged the development of the desulfurization technology. Developing a new technology of desulfurization is a focus in the crude oil processing industry, and finding a new desulfurization material and process is a very meaningful work.
Intermetallic compound SbSn was prepared by using different non-equilibrium solidification methods and conditions using Sb and Sn as raw materials. The prepared materials were analyzed and characterized by modern analytical techniques, such as DSC, XRD, XPS, and AES etc. The effection of decreasing the contents of asphaltene, S and heavy metal in crude oil by using the prepared materials was investigated. The following results have been obtained.
1. Melt superheat treatment was studied and the transformation of mixture of Sb and Sn with the temperature increasing was characterized by DSC. Result revealed that the mixture of Sb and Sn with a molar proportion of 1:1 has a change of liquid microstructure at about 900℃, which is far above the melting point of Sb or Sn, moreover Sn has a liquid micro structural change at about 970℃. The crystal structures of SbSn prepared at different melting temperatures were not the same. SbSn prepared by melting spraying quencher at the melting temperatures of 750℃is hexagonal crystal, while SbSn prepared at the melting temperatures of 950℃is trigonal crystal. According to the space lattice and crystal lattice parameters given by stand atlas of XRD, the monocrystalline space lattice model of SbSn was obtained using Materials Studio 3.0.1, and XRD pattern of it was calculated. The calculated
本文以Sb、Sn为原料,采用不同的非平衡凝固方法和条件来制备SbSn金属间化合物,借助于差示扫描量热(DSC)、X射线衍射(XRD)、X射线光电子能谱(XPS)、俄歇电子能谱(AES)等现代分析手段对制备的材料进行了表征。考察了制备出的材料对原油中沥青质、硫和重金属等杂质的脱除效果。主要内容如下:
1.对熔体的过热处理进行了研究,使用DSC表征了Sn和Sb混合物在升温过程中的变化,结果表明:1:1的锡-锑混合物在超过熔点完全转化为液相以后会在900℃附近发生液相微观结构变化,锡单质也会在970℃附近存在着液相结构的转变。不同熔融温度下制备出的材料的结构并不相同,由750℃下熔融快冷制备出的SbSn颗粒为六方晶体,由950℃下熔融快冷制备出的SbSn颗粒为三方晶体。根据标准图谱提供的金属间化合物SbSn的空间点群和晶格参数,用Materials Studio 3.0.1建立了SbSn的单晶胞空间结构图,并计算出了相应的XRD图,计算图与实测图有一致性。不同熔融温度下制备出材料的表面成分和锑元素的价态有所不同,电压30V,电流400A,淬速30m/s的条件下制备出的材料与950℃下熔融快冷制备出的材料的晶体结构一致,并且表面是富锑的,锑的价态是以+3价为主;电压20V,电流20A,淬速30m/s的条件下制备出的材料与750℃下熔融快冷制备出的材料的晶体结构一致,表面是富锡的,锑的价态是以零价态为主。
2.以沥青质的的脱出率作为评价标准,来确定原油乳化液的最佳配制条件。研究结果表明最优的乳化液配制条件为:表面活性剂为油包水型,含量在0.15%以上,水含量在35%～40%之间。
3.研究了不同的工艺条件对材料的结构和脱硫性能的影响。对于原油乳化液脱硫过程来说,研究结果表明:不同熔融温度下制备出的材料的脱硫性能不同,
With the development of economy, crude oil plays a more and more important role in the agriculture and industry, but the quality of crude oil is becoming poor, and the content of sulfur and heavy metal is increasing continuously, which brings trouble to the follow-up process of crude oil, and polluted the environment badly. On the other hand, the standards of international community to environmental protection trend towards more strict, and the prescriptive value of the sulfur content in crude oil products are becoming lower and lower. The causes from the above two sides urged the development of the desulfurization technology. Developing a new technology of desulfurization is a focus in the crude oil processing industry, and finding a new desulfurization material and process is a very meaningful work.
Intermetallic compound SbSn was prepared by using different non-equilibrium solidification methods and conditions using Sb and Sn as raw materials. The prepared materials were analyzed and characterized by modern analytical techniques, such as DSC, XRD, XPS, and AES etc. The effection of decreasing the contents of asphaltene, S and heavy metal in crude oil by using the prepared materials was investigated. The following results have been obtained.
1. Melt superheat treatment was studied and the transformation of mixture of Sb and Sn with the temperature increasing was characterized by DSC. Result revealed that the mixture of Sb and Sn with a molar proportion of 1:1 has a change of liquid microstructure at about 900℃, which is far above the melting point of Sb or Sn, moreover Sn has a liquid micro structural change at about 970℃. The crystal structures of SbSn prepared at different melting temperatures were not the same. SbSn prepared by melting spraying quencher at the melting temperatures of 750℃is hexagonal crystal, while SbSn prepared at the melting temperatures of 950℃is trigonal crystal. According to the space lattice and crystal lattice parameters given by stand atlas of XRD, the monocrystalline space lattice model of SbSn was obtained using Materials Studio 3.0.1, and XRD pattern of it was calculated. The calculated
引文
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