CN101186839A - 使用氧化铝作为有机金属硅络合物的捕获物质 - Google Patents

使用氧化铝作为有机金属硅络合物的捕获物质 Download PDF

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CN101186839A
CN101186839A CNA2007101929585A CN200710192958A CN101186839A CN 101186839 A CN101186839 A CN 101186839A CN A2007101929585 A CNA2007101929585 A CN A2007101929585A CN 200710192958 A CN200710192958 A CN 200710192958A CN 101186839 A CN101186839 A CN 101186839A
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C·尼德茨
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Abstract

本发明涉及一种在1000℃下煅烧后含有至少80重量％的氧化铝的固体上捕获气相或液相中的有机硅络合物的方法。氧化铝的总孔隙体积大于30ml/100g，直径为70或更大的孔隙中的孔隙体积部分大于10ml/100g，比表面积大于10m2/g。

Description

使用氧化铝作为有机金属硅络合物的捕获物质
本发明涉及一种用于有机金属硅络合物捕获(capture)物质的方法。这些络合物可能存在于通常流经催化剂的气流或液流中。如果催化剂没有保护，其随后可能中毒并且其性能(活性和/或选择性)会过早降低。
本发明方法中的处理进料是汽油馏分，优选来自裂化装置的汽油馏分，更优选主要来源于催化裂化装置的汽油。处理过的汽油也可以是来自例如蒸汽裂化、焦化或减粘裂化过程等不同转化过程的汽油的混合物，或者甚至是直接来源于蒸馏石油产品得到的汽油。
硅通常是许多催化应用(加氢，Prime G+等)中的主要有害物。试验表明除了通常谈到的硅，必须对不同类型的硅加以区别：
●称为无机硅的硅通常是存在来自于耐火材料粒的碎屑的结果。其物理上是存在的，但是看来似乎并不影响所涉及的催化剂的活性或选择性；
●通常称为有机硅的硅来源于有机金属络合物，其可以与置于下游的催化剂反应并不可逆转地使催化剂中毒。在上游添加通常基于聚硅氧烷的消泡剂在该现象中起着重要的作用。
本发明表明使用氧化铝可以通过反应性吸收有效地将有机硅络合物保留在氧化铝表面。本发明也表明使用特殊的氧化铝更为有利，也就是说其对于所述的络合物具有优异的捕获潜力。
在本文中，数值表示为以重量计的％和ppm。
从而，本发明涉及一种在于1000℃下煅烧后含有至少80重量％的氧化铝的固体上捕获气相或液相中的有机硅络合物的方法，。氧化铝的总孔隙体积(TPV)大于30ml/100g，优选大于45ml/100g，更优选大于50ml/100g，更为优选大于55ml/100g。
直径为70或更大的孔隙中(在下文中称为V70A)的孔隙体积部分大于10ml/100g，优选大于15ml/100g，更优选大于25ml/100g，更为优选大于35ml/100g，高度优选大于45ml/100g，甚至更优选大于55ml/100g。
该氧化铝的比表面积大于10m2/g，优选大于20m2/g，更优选大于30m2/g，甚至大于50m2/g或甚至大于70m2/g。
在特定的催化剂操作条件下有时可以观察到由不希望的聚合引起的胶质形成问题，并且这个问题也存在于保护性捕获物质中。为此，在本发明的特定实施方式中，比表面积可小于300m2/g，优选小于200m2/g，更优选小于150m2/g。
可以通过例如凝胶沉淀法之类的传统方法或通过例如三水铝石之类的氧化铝氢氧化物的快速脱水获得用作制备氧化铝的原材料的粉末。氧化铝随后进行干燥操作并可选择地进行煅烧；后者可以在200℃和1200℃之间、优选300℃和1000℃之间的温度下进行。
氧化铝可以是任何本领域技术人员已知的常规形态：粉末、珠粒、压出物、碎料、整料等。优选珠粒和压出物。珠粒的尺寸(相当于珠粒的直径)因而在0.5-10mm的范围内，优选在0.7-8mm的范围内，更优选在0.8-5mm的范围内。压出物形状可为圆柱状或多叶状(polylobed)，实心或空心。其尺寸(相当于其长度)在0.5-5mm的范围内，优选在0.7-3mm的范围内。需要注意术语“尺寸”指珠粒的直径和压出物的长度。一般来讲，在研究中术语“尺寸”指的是型材的最大尺寸。
当使用氧化铝珠粒时，其可以通过成型、通过氧化铝的悬浮液或水分散体或者以由有机相、水相和表面剂或乳化剂构成的乳液形式存在的碱性铝盐溶液的落滴凝结(drop coagulation)而获得。
氧化铝珠粒也可以通过利用例如旋转造粒机或滚筒的旋转技术聚集氧化铝粉末获得。随后可获得具有受控尺寸和孔隙分布的珠粒，其整体通常在聚集步骤中生成。
氧化铝压出物可以通过研磨然后挤出氧化铝基材料获得，所述材料可以通过快速脱水三水铝石和/或沉淀一种或多种氧化铝凝胶获得。
在成型之后，对氧化铝进行多种处理以提高其机械性能，例如通过将其保存在具有受控湿度的气氛中、随后进行煅烧、然后可选择地使用一种或多种无机和/或有机酸溶液浸渍氧化铝而进行的熟化，和在封闭气氛中进行的水热处理。通常在处理后对氧化铝进行干燥和煅烧。
在本发明的一个特定实施方案中，氧化铝可以掺杂一种或多种选自碱金属、碱土金属和稀土的元素。所述掺杂元素的总含量小于20重量％，优选小于10重量％，更优选在500ppm-5重量％的范围内。掺杂物可以在成型操作之前、之中和/或之后加入。
在掺杂的辅助元素的累计量以重量计超过5000ppm的情况下，吸收剂的总孔隙体积大于30ml/100g，更为优选大于35ml/100g，比表面积大于20m2/g，优选在30-300m2/g的范围内，更优选在30-200m2/g的范围内。V70A大于10ml/100g，优选大于15ml/100g，更优选大于25ml/100g，更为优选大于35ml/100g，更加优选大于45ml/100g，或甚至大于55ml/100g。
优选的掺杂物是钠、钾、钙、镁和镧。更优选选择钠和镧。高度优选镧。
下述实施例说明了本发明，而非对本发明范围的限制。
实施例1
反应在体积为600ml的包含工作溶液的烧杯中进行并且利用被石蜡包裹的表面皿使反应不受环境大气影响。按原状(不压碎)对固体进行研究并将其置于三角架上的烧杯中以避免由磁力搅拌器引起的不希望的耗损。所有试验在大气压下的环境温度中进行。有机金属络合物为聚甲基氢化硅氧烷((CH3)3SiO[(CH3)HSiO]nSi(CH3)3)；其溶于环己烷中。
反应在环境温度和大气压下利用6.3g固体和200ml含有以重量计5000ppm聚甲基氢化硅氧烷的环己烷溶液进行。
相应于一次试验的每一个点，使用叠加法利用ICP(电感耦合等离子体)对固体进行分析。
如下所述进行ICP分析：试样在加热板上使用H2SO4-H3PO4混合物通过快速酸侵蚀进行溶解。进行ICP测定时所选择的峰值为λ＝288.158nm。
叠加法如下组成：制备待分析试样的相同试样，加合每个所分析的元素增加的浓度。利用相同的基质和恒定的最终体积获得增加的标准尺度。对试样的分析得到一条标准曲线。曲线与横坐标的交叉点确定为所述轴的原点，从而确定出试样中元素的浓度。
利用重量分析法检测溶液的滴定度：所得到的物料平衡是一致的。在封闭的试管中侵蚀固体试样进行测试然后进行重量分析所产生的结果与ICP分析所得到的结果非常接近。
在使用氢氟酸侵蚀之后进行硅的重量分析。通过蒸发含有过量氢氟酸的溶液可除去所有的二氧化硅，并且通过重量差异测定硅的量。
本研究中所使用的氧化铝在表1中给出，所得到的结果在图1和图2中给出。
  氧化铝 A     B     C     D     E     F
  外形 珠粒     珠粒     珠粒     压出物     珠粒     珠粒
  直径(mm) 2-5     2-4     1.8-3.15     1.2     2-5     2-5
  比表面积(m2/g) 332 73 189 275 321 341
  孔隙总体积(ml/100g) 39.7 63.9 66.7 64.2 43.2 42.7
  V70A(ml/100g) 23.4 60.9 62.5 53.5 6.1 30.9
图1表示出作为暴露于溶液的时间的函数的固体中所分析的硅的量(以重量％计)。
图2表示出反应3小时后固体中所分析的硅的量(以重量％计)。
由图2显示，捕获物质E(不按照本发明)的V70A为6.1ml/100g，其在捕获硅时没有捕获物质A-D和F(按照本发明)有效。
实施例2：掺杂氧化铝
在氧化铝A成型后分别用氢氧化钠和硝酸镧干浸渍而得到氧化铝G和H。在450℃下煅烧后，G和H分别具有2.1重量％和0.9重量％的Na2O和La2O3含量。在与其它氧化铝(实施例1)相同的条件下测试，反应3小时后，G和H所捕获的硅分别为0.75重量％和0.82重量％。
在氧化铝F成型后用氢氧化钠干浸渍得到氧化铝I。在450℃下煅烧后，I中的Na2O含量为1.7重量％。在与其它上述氧化铝(实施例1)相同的条件下测试，反应3小时后，I捕获的硅为0.91重量％。

Claims (12)

1.一种用于在气相或液相中通过将固体与汽油馏分接触从而捕获存在于所述汽油馏分中的有机硅络合物的方法，所述固体在1000℃下煅烧后含有至少80重量％的氧化铝，所述氧化铝的总孔隙体积大于30ml/100g，直径为70或更大的孔隙中的孔隙体积部分大于10ml/100g，且比表面积大于10m2/g。
2.权利要求1所述的方法，其中氧化铝的总孔隙体积大于45ml/100g。
3.权利要求1或2所述的方法，其中氧化铝的以直径为70或更大的孔隙表示的体积大于25ml/100g。
4.权利要求1-3任意一项所述的方法，其中氧化铝的比表面积大于20m2/g。
5.权利要求1-4任意一项所述的方法，其中氧化铝的比表面积在70m2/g-200m2/g的范围内。
6.权利要求1-5任意一项所述的方法，其中氧化铝的以直径为70或更大的孔隙表示的体积大于45ml/100g。
7.权利要求1-6任意一项所述的方法，其中氧化铝掺杂有一种或多种选自碱金属、碱土金属和稀土的元素，所述掺杂元素的总量小于20重量％。
8.权利要求7所述的方法，其中氧化铝掺杂有一种或多种选自钠、钾、钙、镁和镧的元素。
9.权利要求8所述的方法，其中掺杂物是镧。
10.权利要求1-9任意一项所述的方法，其中氧化铝为珠粒或压出物的形式。
11.权利要求10所述的方法，其中氧化铝为尺寸在0.5-10mm范围内的珠粒形式。
12.权利要求10所述的方法，其中氧化铝为尺寸在0.5-5mm范围内的压出物形式。
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