CN1735677A - 去除烃流中的杂质 - Google Patents

去除烃流中的杂质 Download PDF

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CN1735677A
CN1735677A CN02804895.4A CN02804895A CN1735677A CN 1735677 A CN1735677 A CN 1735677A CN 02804895 A CN02804895 A CN 02804895A CN 1735677 A CN1735677 A CN 1735677A
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J·S·里德
T·希马恩斯基
S·T·米歇尔
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Saint Gobain Ceramics and Plastics Inc
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Abstract

本发明提供了一种用于纯化烃料去除其中金属杂质的方法，包括使烃流通过包含氧化铝以及相对较少量的氧化钙和氧化镁的介质。

Description

去除烃流中的杂质
本申请源自另一重要发现，这种介质可以用来从烃流中去除金属类杂质。
发明背景
本发明涉及用吸附剂材料处理烃流，以有效地除去经常存在于烃流中造成麻烦的金属组分。
重整所产生的烃流中通常含有金属杂质，其形式包括金属有机化合物、金属无机化合物或金属本身。这类金属杂质可能会引发严重问题，例如催化剂失活、加工设备中使用的金属性质退化、环境污染、有毒污染等。迫切希望从烃流中去除这些杂质，以避免或者减轻此类影响。
发明概述
本发明提供一种用于去除烃流中金属杂质的方法，包括使烃流接触吸附剂介质，该吸附剂介质包含重量百分数50到96％的氧化铝以及重量百分数50到4％的碱土金属氧化物，所述碱土金属氧化物选自氧化钙和氧化镁，CaO∶MgO重量比从90∶10到50∶50，其BET表面积至少为100米2/克。优选在20℃到450℃的温度使烃流与介质接触，更优选在250℃到350℃的温度进行。
根据本发明从石油流中用介质去除的金属包括铅、铜、铝、硅、铁、铬、锌、镁、镍、钠、钙、钒、汞、磷和镁。一般原则上，烃流含有碳原子在5个及5个以上的烃。
术语“介质”在这里用来表示具有上述组成、形状为颗粒、球形、棒形或其它有足够孔隙率(通过表面积来反映)的陶瓷材料，使金属杂质通过物理作用被捕集在介质的孔隙内、吸附在介质的孔表面、或更为普遍的是与介质材料发生化学反应产生出的组分再也不会被这些杂质原属的烃流所输送。
为了产生本发明的介质，原来以化学计量加入的组分重量被调整为经焙烧制得本发明介质后残留的氧化物的重量，在此基础上计算各组分的比例。
从下表可见，这通常给出了相当精确的转换。
  勃姆石  CaCO3   MgCO3      Al2O3   CaO   MgO
  90  8.2   1.8   92.2   6.6   1.2
  60  36   4   65.9   31.1   3.0
  96  3.6   0.4   97.1   2.6   0.3
  96  2.0   2.0   97   1.6   1.4
头三个配方采用了白云灰岩，第4个配方用的是普通白云石。可以看到，从前体材料到最终焙烧产品，相对比例没有非常显著的变化。
介质可以根据实际应用采取任何所需形状。例如，可以是短棒形、颗粒形、空芯圆柱形、环形、鞍形，等等。美国专利USP5,304,423介绍了一种特别有用的形状。可供选用的各种形状介质可以呈配置在床内的带有多个通道的整体形式。但是，这种整体结构介质对于本发明基本目标的应用中并非优选。
据信，从烃流中除去金属的主要机理是基于金属与介质间的反应。当金属和介质在非极性液体(烃流)中都呈极性时，加速了金属在介质表面上的吸附。加热会加速这一过程。通过除去化学作用所保留的杂质可以恢复介质的活性。这可以通过将包含活性下降的介质的床用热(例如，约150℃)蒸气反冲(back-flushing)来进行。通过蒸气处理连续进行8小时左右除去杂质的过程就基本完成了。在进行重新活化之前，要求采用烃类溶剂，比如甲苯或XYSOL(加拿大Calgary的Trysol Canada Ltd.出品)等富含芳烃的溶剂去除吸附在介质孔隙中的残留重烃，该过程优选加热到300℃左右进行。
业已发现，在溶剂清洗与蒸气处理之间采用热甲醇(例如，150℃)清洗会有助于清除残油、并有助于蒸气渗入孔隙。在蒸气中加入部分甲醇也能达到相同效果。甲醇特别有效，但是，据信任何低分子量醇，如乙醇或(正或异)丙醇可以替代。
介质的制备方法包括以下步骤：a)将50到97％重量百分数的水合氧化铝组分，如勃姆石，与50到3％重量百分数的10∶1到50∶50的碳酸钙—碳酸镁混合物混合成水浆混合物，其中勃姆石和碳酸盐混合物的量基于浆料中的含固量计算；
b)加酸使浆料胶溶；
c)将胶溶后浆料挤出形成所需介质形状；及
d)干燥去水，然后在650℃到850℃的温度焙烧定型。
例如，水合氧化铝组分可以选择任何市售勃姆石产品，其分子式通常给定为AlOOH或者更准确地表示成Al2O3·H2O。
碳酸钙和碳酸镁混合物通常取自白云石粉末，优选白云灰岩粉末，后者是白云石(其中钙和镁金属原子的数量基本相同)和方解石的混合物，并以方解石为主，另外还有几个百分点的硅、铁等杂质。当在焙烧步骤中进行煅烧时，该混合物分解成相应的氧化物。因此，从理论上说，可以在勃姆石浆中掺入氧化物或氢氧化物来制备本发明的产物。然而，这样可能需要更多的酸使浆料胶溶，所以并非优选。
为了有助于碳酸盐在勃姆石溶胶中的分散，较佳的是采用平均粒径50微米左右或更细的粉末。特别适合的是一种市售白云灰岩，由National Lime andStone Company用Bucyrus Microfine的商品名销售(99％通过325目筛)。这种材料中碳酸钙与碳酸镁的重量比大约是6∶1。
为了使浆料(基本上是勃姆石溶胶中含有钙/镁组分的分散体)胶溶而加入的酸，可以是能胶溶这种溶胶的任何一种公知酸。因为焙烧会造成酸的分解，所以要避免使用硝酸、盐酸、硫酸等无机酸，强有机酸，如乙酸，甲酸更好，被用于胶溶化。胶溶化的溶胶实际上变成了稳定的凝胶体，可以通过挤出等成形方法制得其形状在干燥和焙烧过程中得以保持的成形物。优选添加足够量的酸使pH值降到5或5以下。
成形物干燥所进行的条件优选是去除水分而不破坏其形状。这意味着在大约100℃相对较低的温度进行干燥(尽管在大多数情况下可以再升温高达50℃)，虽然通常10-24小时的干燥周期已满足要求，但可延长到两天。
干燥后成形物的焙烧时间可以足够长，以使其从相应的碳酸盐形成氧化钙和氧化镁，并排除所有结合的水分，把勃姆石转变成其它中间同质异晶体的γ型氧化铝或无定形体。然而，较佳的是焙烧不要在会导致形成α型或者烧结的条件下进行，因为这会造成孔隙损失使氧化铝变成活性低的形式。因此，优选焙烧温度是最高温度500到800℃，焙烧周期直到不再有重量下降为止。一般，在焙烧温度时加热30分钟到5个小时就足以基本上分解所有的碳酸盐并排掉所有的结合水分。
焙烧产物的表面积至少为100米2/克，例如超过200米2/克，优选在200到250米2/克之间。
优选实施方式的说明
下面结合非限制性实施例对本发明作进一步说明，这些例子说明了本发明介质在从烃流中有效去除污染物的能力。
在下面的实施例中，采用ICP进行分析，由加拿大的Metro Tech System Ltd.of Calgary进行各种元素的识别。
实施例1到4都用了API比重为48含有各种不同量金属污染物的烃流。该烃流泵入长25厘米直径1.27厘米填充了8克介质的经加热的不锈钢管柱。在每个例子中介质有以下的性质。所得介质的BET表面积测定为219米2/克，表观孔隙率78.5％，吸收水103.4％，表观比重3.54克/立方厘米、材料密度0.76克/立方厘米。材料分析显示92.2％重量的氧化铝，6.6％重量的氧化钙和1.2％重量的氧化镁。
实施例1
首轮中含有24ppm铁、2ppm锌、2ppm铅的烃流以3.1毫升/分的流速通过上述介质。初始温度保持在273.9℃，60小时之后温度升高到301.7℃，120小时后温度再升高到315.6℃。经过设定时间后除去金属的量，以该元素在烃流中ppm的百分数示于下表1。
表1
  小时   铅   铁   锌
  6   100   87   100
  12   100   85   100
  24   24   81   100
  36   14   88   100
  48   38   95   100
  60*   100   98   100
  72   100   98   100
  84   100   100   100
  96   33   96   100
  108   39   97   100
  120*   38   100   100
  132   39   100   100
  144   39   100   100
  156   96   99   100
  162   100   96   100
  174   78   91   100
  186   100   100   100
  198   83   93   100
  200   91   99   100
*表示温度升高。
实施例2
200个小时以后管柱用甲苯清洗，照上述方法用蒸气再生。本轮在315°C进行，流速仍为3.1毫升/分。烃流中杂质含量和类型与实施例1相同。结果见表2，各栏示出的是除去元素的ppm百分数。
表2
  小时   铅   铁   锌
  6   100   100   100
  12   100   100   100
  24   100   100   100
  36   100   100   100
  48   100   100   100
  60   100   100   100
  72   100   100   100
  84   100   100   100
  96   100   100   100
  108   100   100   100
  120   100   100   100
  132   100   100   100
  144   100   100   100
  156   100   100   100
  162   100   100   100
实施例3
实施例2进行162个小时以后，换成含有以下金属杂质的烃流：
铁-116ppm；锌-2ppm；铅-3ppm；铝-223ppm；镁-49ppm；钠-38ppm；钙-57ppm；锰-1ppm。
本轮在实施例2的条件下继续进行24小时。在12小时和24小时取出的样品显示各时间段上的杂质都是100％的被去除了。
实施例4
本例探讨了温度对于各种元素杂质去除的影响。使用的还是前面实施例的相同试验设备，但是，介质更新了，烃流含有：汞-6ppm；铜-2.6ppm；铁-8.9ppm；锌-0.1ppm；磷-8.2ppm。烃流的流速继续保持3.1毫升/分，在以下表3所示的温度变化过程流动6小时。
表3
  小时  1   3  5  6
  温度(℃)  110   210  280  280
  汞  50％   66％  77％  85％
  铜  81％   96％  100％  100％
  铁  0％   30％  100％  100％
  锌  100％   100％  100％  100％
  磷  100％   100％  100％  100％
实施例5
本例的评估是在中试装置中进行的，使用要进行再加工的烃流。其API比重为45-50，水含量是1-10％，含固量1-3％。除去底部水分和沉淀物后，烃流被泵入通过两个热交换器及一个管线加热器，从而把温度升高到248.9C到315.6℃之间。然后，使热流通过含有大约1.87米3(66立方英尺)的与上述实施例相同的介质的床。烃流的处理量每天在25到38之间。烃流的压力为517kN/m2到620kN/m(75到90psi)，在此压力下至少50-60％的烃流量是蒸气状态。蒸气流被分离出来，不通过介质床。蒸气和流过液体床的液体组分然后合并起来送往分馏塔。加工总量到2300桶后，除去的金属百分数如下：
磷-98％；钠-72％；铁-95％；铝-97％；铜-92％；锌-99％；钙-94％；镁-98％；硅-77％；铅-49％；铬-89％。
在处理了1900桶后的取样中含有铁、钙、钠、镁、铝、硅、磷。经过床后，所去除的这些元素的百分数如下：
钙-90％；钠-73％；镁-98％；铝-95％；铁-92％；硅-15％；磷-96％。
实施例6
本例中的烃流是Northern Alberta原油，含有锌、镍、钠和钒。来自该烃流的一份样品和10克与上述实施例相同的介质放到压热反应釜中。压热反应釜在689kN/m2(100psi)氮气压力下加热到300℃。30分钟后对样品进行分析，发现45％的镍、21％的钠、76％的钠和24％的钒被除去。

Claims (5)

1.一种用于去除烃流中的金属的方法，其特征在于，包括使烃流接触吸附剂介质，该吸附剂介质包含重量百分数50到97％的氧化铝以及重量百分数50到3％的选自氧化钙和氧化镁的碱土金属氧化物，其中氧化钙与氧化镁的重量比从10∶1到50∶50，所述介质的BET表面积至少为100米2/克。
2.如权利要求1所述的方法，其特征在于，所述吸附剂介质的表观孔隙率在60到80％。
3.如权利要求1所述的方法，其特征在于，所述介质包含少于1％的其它金属或金属氧化物杂质。
4.如权利要求1所述的方法，其特征在于，所述去除杂质的过程在20℃到450℃的温度进行。
5.如权利要求4所述的方法，其特征在于，所述去除杂质的过程在250℃到350℃的温度进行。
CN02804895.4A 2001-02-13 2002-01-24 去除烃流中的杂质 Pending CN1735677A (zh)

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