CN1206690A - 从卤化氢中除去水分的组合物和方法 - Google Patents

从卤化氢中除去水分的组合物和方法 Download PDF

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CN1206690A
CN1206690A CN98103093A CN98103093A CN1206690A CN 1206690 A CN1206690 A CN 1206690A CN 98103093 A CN98103093 A CN 98103093A CN 98103093 A CN98103093 A CN 98103093A CN 1206690 A CN1206690 A CN 1206690A
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麦肯齐·E·金
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Abstract

提供了一种从卤化氢流体中有效地除去水分的组合物,该组合物包括卤化镁涂布的大孔含碳基材。通过使卤化氢流体与卤化镁涂布的大孔含碳基材充分接触,并从涂布基材分离流体实现了有效地除去水分。

Description

从卤化氢中除去水分的组合物和方法
本发明涉及一种从卤化氢中除去水分的组合物和方法。
目前，卤化氢气体或液体以高纯无水组合物的形式使用。无水卤化氢通常用于半导体工业，如清洗反应器管和接受器(susceptors)，以及作为生产微电路的蚀刻剂。
在这些应用中，要求在引入最终使用环境之前从如氯化氢的卤化氢中高效地除去蒸汽或液态水分。氯化氢通常是气体，有时以液体的形式加压输送。氯化氢在615 pisg下变为液体。含水氯化氢是强腐蚀性的，因此，需要频繁更换与之接触的管线、管道、阀门等。在清洗接受器时，即清洗所加工晶片的支承结构时，在氯化氢中存在水会引起在接受器上形成新的氧化物，这与需要进行的清洗作用相矛盾。在蚀刻应用中，含水氯化氢是半导体生产环境中不必要的水分污染源，可能导致在这种环境下生产的微电路片产品有缺陷，甚至对其所希望的用途来说是无用的。
在现有技术中，用于从氯化氢中除去水分的方法是使用吸附水分的分子筛。用这种方法生产高纯度氯化氢的困难是氯化氢与水在分子筛的吸附点上的竞争。其结果是，在分子筛接触步骤的流出物中不可能获得所需的低残水值，即体积浓度为10ppm的数量级，或更低。
过去用硫酸或磷酸处理氯化氢以生产脱水氯化氢。然而，这种脱水方法所连带的缺点是向氯化氢中加入了硫和磷，加入的这些元素在前述的半导体生产中是极不需要的污染物。
曾经也提议用负载在氧化铝上的氯化镁来除去从卤化氢中除去水分。但发现，当加压氯化氢如液态形式的氯化氢与之接触时，氧化铝与氯化氢反应形成三氯化铝颗粒，堵塞氯化氢所通过来进行其纯化的过滤器，所以这种纯化材料不是所希望的。
此外，在氧化铝上形成氯化镁包括许多步骤，其中首先用溶液涂布氧化铝，如15重量％的溶于己烷溶剂的二丁基镁。溶剂在加热时由于蒸发而被除去。通过加热到约250℃二丁基镁在氧化铝上转化为二氢化镁。然后，氧化铝上的二氢化镁与浓盐酸接触转化为氯化镁。之后，这一组合物才用于从卤化氢中除去水分。
溴化氢是卤化氢的另一例子，在半导体生产中要求基本上完全无水。溴化氢在电子工业中用作晶片的蚀刻剂和接受器的清洗剂。在这些应用中，在溴化氢中存在的水杂质会导致前面提到的与氯化氢在类似应用中产生的同样缺点。此外，当溴化氢用作晶片的蚀刻剂时，当溴化氢中含有即使是极少量的水汽，也会产生浊雾(hazing)。
现有技术试图用磷酸作为干燥剂从溴化氢中除去水。这一方法对除去水污染物通常是有用的，但是会有向溴化氢中加入磷的缺点，在讲到氯化氢时提到了这一问题，在半导体生产中磷是一种重要的污染物。
因此，希望提供一种从卤化氢中除去水分的组合物和方法，它们不产生如颗粒的污染副产物。此外，还希望提供一种或从气态或从液态卤化氢中高效地除去水分的组合物和方法。另外，还希望提供这样一种组合物，与形成现有类似组合物的方法相比，这种组合物能以简单的方法来形成。
本发明提供了一种从卤化氢流体中除去水分的组合物，包括大孔含碳载体，在该载体上沉积了氯化镁或溴化镁的卤化镁。首先使二丁基镁的溶液与载体混合以用二丁基镁涂布载体表面，从而使卤化镁沉积在大孔含碳载体的表面。然后，在非反应性环境中通过蒸发除去形成溶液的溶剂。此后，涂布的载体与卤化氢流体接触将二丁基镁转化为卤化镁。这一方法避免了形成二氢化镁。
在使用中，涂布了卤化镁的载体与卤化氢流体充分接触以从卤化氢流体中基本完全除去水分。卤化氢流化和卤化镁中的卤素与要防止污染的流体中的卤素相同。
附图简要说明如下：
图1说明了本发明的应用。
图2是说明本发明的组合物从氮中除水容量的傅立叶变换红外光谱图。
图3是说明本发明组合物从HCl中除水容量的傅立叶变换红外光谱图。
本发明的组合物包括用卤化镁涂布的大孔含碳载体，其平均孔径大于约100埃，高至约100μm，优选在约20-约1000之间。合适的含碳载体，由例如聚合的树脂热解形成。代表性的合适的载体是由热解磺化苯乙烯／二乙烯基苯大网状离子交换树脂形成，且由例如US5，094，754所公开，在这里引入作为参考。这些含碳载体可以从Rohm and Haas Company，Philadelphia PA以注册商标AMBERSORB购得。
该卤化镁涂层是先使颗粒大孔含碳载体与二烷基镁化合物的溶液充分接触形成的，二烷基镁化合物的例子有二甲基、二乙基、二丁基和二丙基镁，优选二丁基镁。形成溶液的代表性的溶剂包括己烷、庚烷等。载体与溶液的接触通常是在约25℃-约70℃的温度下进行约1小时至约4小时。所到的涂布载体与溶液分离，通过如蒸发的方法除去多余的溶剂。蒸发可以通过加热到约55℃至约65℃的温度和惰性或非反应性气氛如氮气或惰性气体中进行。
在最后一个步骤中，涂布载体或是单独或是在如氮气的非反应性气氛中与卤化氢气体接触，其中卤化氢占该气体体积的约5％-100％。在这一最终步骤中，二烷基镁被转化成卤化镁。当涂布的载体用来干燥氯化氢流体时，使用卤化氢作为卤化氢。当涂布的载体用来干燥溴化氢流体时，使用溴化氢作为卤化氢。与卤化氢流体在一定温度下接触一段时间以使二烷基镁基本上完全转化为卤化镁。常用的接触时间是约1．1 min／ml树脂-约5．5 min／ml树脂，优选为约1．6 min／ml树脂-约5．5 min／ml树脂。常用的反应温度为约25℃-约240℃，优选为40℃-约60℃。
即使在高压下流体是液体的情况下，本发明组合物也能从卤化氢流体中除去水分，而不会形成污染卤化氢的反应产物，如颗粒的反应产物。而且，本发明组合物能够经得住在50℃和高至约1100 psig的压力下的高压液体卤化物。
卤化镁涂层足以使本发明组合物来从卤化氢流体中除去水分至低于约100 ppb，优选至低于约50 ppb，而不会明显堵塞载体的大孔。本发明组合物的特征在于水分吸附容量超过40升水／升涂布载体，优选超过60升水／升涂布载体。卤化镁的浓度至少超过约0．1摩尔卤化镁／升含碳载体，优选至少超过约1．2摩尔卤化镁／升含碳载体。
在使用中，本发明组合物可以与或是流动的流体流或是在容器中静止的卤化氢流体以某种方式充分接触，以使基本上所有的卤化氢与组合物接触。
参照图1，要干燥的卤化氢流体从室12的入口1引入。流体流过保留的玻璃料14进入本发明的涂布含碳颗粒床16，其中，水分被从流体中除去。然后，流体通过过滤器18和出口20去使用地点(未示出)。
下面的实施例用来说明而不是限制本发明。
实施例Ⅰ
这一实施例用来说明制备本发明的用氯化镁涂布的产品的方法。
在200ml 10％甲醇／水溶液中清洗200ml Ambersorb563含碳吸附剂。Ambersorb563是从Rohm and Haas Company，Philadelphia PA购得，其表面积为550m2／g，用氮孔度计测得的大孔隙率为0．23ml／g。倾出溶液，微珠再用甲醇漂洗三次。载体在空气中干燥直到能自由流动，然后注入到1000ml的圆筒中，从底部通入N2，同时圆筒被加热到100℃，经历约4小时，直到几乎除去了所有的水／甲醇，这时将圆筒的温度提高到240℃，经历15小时。在这一活化期间结束时，将载体冷却到60℃。加入足够量的二丁基镁在庚烷中的15％的溶液，充满碳空隙体积，然后，从圆筒的底部通入氮气流，吹出≈75％的庚烷。重复这一步骤，直到使庚烷中所有的二丁基镁都被加入。为了得到均匀的混合物和防止结块，搅拌是需要的。Ambersorb563含碳吸附剂上的二丁基镁保持在1 slpm、55℃的氮气流中一整天，然后将含碳吸附剂分离出来，放入手套箱(glove box)，并放进一个适合于处理有害气体的样品柱中。有含碳吸附剂的气体样品柱与一能流通无水HCl和氮气的气体支管连接。两倍过量的含5％HCl的氮气以15 psia和1000 sccm流过含碳吸附剂，这时用纯HCl 15 psia和1000 sccm流过含碳吸附剂30分钟，然后，容器用HCl加压到60 psia过夜。在接下来的一个上午，用1000 sccm的N2吹扫含碳吸附剂，样品柱被加热到240℃，经历52小时。用高压CO2吹扫会更有效。最终产品放出的总烃在26℃少于1 ppm。
实施例Ⅱ
这一实施例说明使用本发明产品从氮和HCl中除去水分。
进行实验以确定涂布的含碳吸附能否干燥氮气流。为了进行水的截留实验，使用常规卤化氢纯化器以500 sccm干燥N2或HCl气体。然后，HCl气体或是通过如图1所示的纯化装置或是旁路通过该纯化器。旁路气流代表水的背景含量。所得气流通过一个路径长为10米、温度为130℃的气体池以用于傅立叶转换红外分析装置(FT-IR)。按要求向100 sccm N2气流中加入四(45)PPM的水(总流量为600 sccm)。
FT-IR光谱的组成表明从N2中除去水的能力到达了小于100 ppb的水平。图2显示了FT-IR在1772 cm-1的三个FT-IR光谱，说明了本发明组合物从N2中截留水分的能力。
用常规纯化器和本发明组合物旁路干燥的N2称之为“干燥N2”。“水”表示旁路通过本发明组合物的湿(4PPM)N2气流，“新纯化器+水”表示通过实施例Ⅰ组合物的的湿N2。光谱清楚地表明“干燥N2”和“新纯化器+水”之间没有差别，说明了常规纯化器和本发明纯化器都能截留N2中的水分至相同水平(＜100 ppb)。
参看图3，本发明实施例Ⅰ的组合物具有能从HCl中除去水分至小于100 ppb的能力。图3显示了FT-IR在1772 cm-1的三个FT-IR光谱，说明了实施例Ⅰ的组合物从HCl中截留水分的能力。
用常规纯化器和本发明组合物Ⅰ旁路干燥的HCl称之为“干燥HCl”。“水”表示旁路通过实施例Ⅰ组合物的湿(4PPM)HCl气流，“新纯化器+水”表示通过实施例Ⅰ组合物的的湿HCl。光谱清楚地表明“干燥HCl”和“新纯化器+水”之间没有差别，说明了常规纯化器和实施例Ⅰ纯化器都能截留HCl中的水分至相同水平(＜100ppb)。

Claims (15)

1．一种适用于从卤化氢流体中除去水分的组合物，包括涂布了卤化镁的大孔含碳载体。
2．如权利要求1的组合物，其中，所述的卤化镁是氯化镁。
3．如权利要求1的组合物，其中，所述的卤化镁是溴化镁。
4．如权利要求1的组合物，其每升所述组合物的吸水能力超过约60升水。
5．如权利要求2的组合物，其每升所述组合物的吸水能力超过约60升水。
6．如权利要求3的组合物，其每升所述组合物的吸水能力超过约60升水。
7．一种从卤化氢流体中除去水分的方法，包括使所述流体与涂布了卤化镁的大孔含碳载体充分接触，并从所述涂布载体分离所述流体。
8．如权利要求7的方法，其中，所述的卤化镁是氯化镁。
9．如权利要求7的方法，其中，所述的卤化镁是溴化镁。
10．如权利要求7的方法，其中，所述的卤化氢是气体。
11．如权利要求8的方法，其中，所述的卤化氢是气体。
12．如权利要求9的方法，其中，所述的卤化氢是气体。
13．如权利要求7的方法，其中，所述的卤化氢是液体。
14．如权利要求8的方法，其中，所述的卤化氢是液体。
15．如权利要求9的方法，其中，所述的卤化氢是液体。
CN98103093A 1997-07-29 1998-07-29 从卤化氢中除去水分的组合物和方法 Expired - Lifetime CN1126711C (zh)

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CN109292736B (zh) * 2018-11-26 2020-04-10 浙江博瑞电子科技有限公司 一种电子级氯化氢气体中痕量水分的去除的设备和使用方法
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