CN102652034A - 从裂化气中除去汞 - Google Patents

从裂化气中除去汞 Download PDF

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CN102652034A
CN102652034A CN2010800556648A CN201080055664A CN102652034A CN 102652034 A CN102652034 A CN 102652034A CN 2010800556648 A CN2010800556648 A CN 2010800556648A CN 201080055664 A CN201080055664 A CN 201080055664A CN 102652034 A CN102652034 A CN 102652034A
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mercury
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cus
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V·I·卡纳兹雷夫
J·K·格拉瓦拉
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Honeywell UOP LLC
Universal Oil Products Co
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Abstract

本发明提供从饱和烃和不饱和烃的混合物如裂化气中除去汞。首先将气体包含在除去水和汞的可再生吸附床中，然后使用于吸附床的再生料流通过包含硫化铜的非可再生床以扑捉汞。令人惊讶地，发现再生料流中的乙炔不与硫化铜反应产生爆炸性的乙炔铜。

Description

从裂化气中除去汞
以前国家申请的优先权要求
本申请要求2009年12月15日提交的美国申请No.61/286,437的优先权。
发明背景
本发明涉及一种从烃料流中除去汞的方法。更具体而言，本发明涉及从包含大比例不饱和烃的烃料流中除去汞。
元素汞和汞化合物污染原油衍生的烃料流和天然气。由于汞对健康的影响以及汞导致含铝热交换器腐蚀的不利影响，将汞从烃料流中除去是重要的。汞与铝结合导致机械故障和泄漏。此外，在乙炔转化器和其他不饱和烃转化器中，汞可使包括氢化催化剂的一些催化剂中毒。由于没有确定可忍受的汞的水平，理想的是除去汞直至可得分析能力不能检测的水平。这是低于1ppt(part per trillion)的水平。
许多汞除去技术是可得的，它们的应用在非反应性进料如饱和烃和馏分的情况下是简单的。但是，由于产生高反应性的副产物，乙烯工业提出了一个挑战。蒸汽裂化器熔炉裂化饱和烃并产生大比例的不饱和烃，大多数为烯烃，但是也有一些乙炔及其同系物。由于烃聚合和焦炭形成，这些不饱和烃可使用于汞除去的固体吸附剂物质失活。此外，已知乙炔系烃与铜和银结合形成爆炸性的炔化物，所述乙炔系烃通常用作用于汞除去的固体物质中的活性成分。因此，必须特别考虑以从裂化气料流或包含或可能包含乙炔系烃的其它料流中除去汞。
尽管铜化合物如铜氧化物和硫化物已经用于从某些烃中除去痕量汞，但是由于爆炸性炔化物的潜在形成，可能包含炔类的不饱和烃的处理证明是非常困难的。现在已经发现该问题的解决方法。
发明概述
本发明提供从包含任何量的炔化物前体的气体料流中除去汞，所述炔化物前体包括乙炔或乙炔系烃。特别地，本发明提供通过将脱水和汞除去结合总体遏制裂化气中的汞。用包含再生汞清除剂如UOP的HgSiv再生汞清除吸附剂的分子筛将裂化气脱水。然后在乙烯装置的分离部分中将不含水和汞的裂化气烃分离。将一部分脱甲烷塔顶馏分(DMO)作为用于脱水单元的再生剂返回。然后将留在脱水单元中的DMO再生剂冷却，并直接将其送入一个或多个非可再生汞除去床中，所述非可再生汞除去床包含能够除去汞而不会形成爆炸性炔化物或将硫化铜还原成硫化亚铜(作为汞清除剂的一种形式的惰性物且还更可能产生爆炸性炔化物)或过度老化的复合CuS-氧化铝多孔物质。由于除去的汞水平是小的，非可再生床可长时间使用而不用更换吸附剂。
发明详述
本发明可以用于处理包含乙炔或乙炔系烃的烃类。通常，在待处理的烃中可以存在0.1%的所述前体。然而，重要的是考虑由于可能随时间积累，任何量的炔化物可能是个问题。烃料流可以来自裂化气或裂化制备乙烯的料流。
确认通过共形成多孔碱性碳酸铜和氧化铝粉末，随后热处理形成的复合珠，然后用S处理以生产CuS-氧化铝复合物而制备的材料在用乙炔处理时不具有形成炔化铜的倾向。因此，该材料适合用作用于从裂化气再生料流中除去汞的清除剂。该材料特征在于具有通过共附聚作用产生的大晶体。此外，以上述方式生产的CuS-氧化铝复合物具有抵抗通过再生剂中存在的氢气将CuS活性相还原产生Cu2S的倾向。后一化合物不适合作为汞清除剂。最后，CuS-氧化铝复合物抵制劣化，因为其不促进再生剂的活性组分与导致焦化、残余物沉积和孔阻塞的材料的反应。这些不利因素可使得汞清除剂在使用时无效。
在本发明中使用的复合材料包含5-60重量%的CuS，优选10-55重量%的CuS，更优选20-45重量%的CuS，最优选40重量%的CuS。此外，优选复合材料包含10ppm至2重量%的氯离子，更优选50ppm至1重量%的氯离子。
对于裂化气和再生气体，几种不同气体料流的分析显示于下表中。该分析没有显示汞和一些其它杂质的水平。
表
Figure BDA00001741514200031
为了测试本发明中使用的硫化铜吸附剂和确定其是否与乙炔反应而形成炔化铜，在严格条件下进行如下试验。如上所述，通常在裂化气中存在0.5%的乙炔，在再生气体中存在0.1%的乙炔。在我们的试验中，在100%乙炔下测试吸附剂以模拟极端条件。将硫化铜吸附剂试样研磨以增加暴露于乙炔的表面积。然后在1大气压和室温下将试样暴露于100%乙炔下24小时。然后将乙炔从试样中抽空，并用氮气吹扫。然后使用红外光谱法检测试样的炔化铜。如果没有发现炔化铜，则认为材料用作吸附剂是安全的。在整个珠或研磨的硫化铜吸附剂暴露24小时之后，没有任何放热过程的迹象。此外，在40℃下在干乙炔中暴露硫化铜吸附剂1周之后，没有任何形成炔化铜的迹象。此外，在设计模拟吸附剂长时间暴露于乙炔的加速试验中，在1周之后，仍没有任何形成炔化物的迹象。

Claims (9)

1.一种从包含饱和烃和不饱和烃的混合物的气态烃料流中除去汞杂质的方法，所述方法包括：
a)提供包含元素汞的流体料流；
b)将所述流体料流供入包含所述汞优先吸附在其上的吸附剂的可再生固定吸附床中，由此吸附汞，建立汞质量传递前沿和回收提纯的产物流出物；
c)在汞质量传递前沿突破之前终止向所述可再生床的流动；
d)通过使清洗解吸剂穿过而再生所述可再生床，由此在再生流出物料流中将汞解吸并从所述床中除去；
e)将所述再生流出物料流供入包含含氧化铝和硫化铜的复合物的非可再生固定吸附床中，以从所述再生流出物料流中除去汞。
2.根据权利要求1的方法，其中所述清洗解吸剂为来自乙烯装置分离部分的脱甲烷塔顶料流的一部分。
3.根据权利要求1的方法，其中所述不饱和烃不与所述硫化铜反应形成炔化物。
4.根据权利要求1的方法，其中所述复合物包含5-60重量%的CuS。
5.根据权利要求1的方法，其中所述复合物包含10-55重量%的CuS。
6.根据权利要求1的方法，其中所述复合物包含20-45重量%的CuS。
7.根据权利要求1的方法，其中所述复合物包含40重量%的CuS。
8.根据权利要求1的方法，其中所述复合物包含10ppm至2重量%的氯离子。
9.根据权利要求1的方法，其中所述复合物包含20ppm至1重量%的氯离子。
CN2010800556648A 2009-12-15 2010-12-10 从裂化气中除去汞 Pending CN102652034A (zh)

Applications Claiming Priority (3)

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US28643709P 2009-12-15 2009-12-15
US61/286,437 2009-12-15
PCT/US2010/059804 WO2011081836A2 (en) 2009-12-15 2010-12-10 Mercury removal from cracked gas

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