CN1090042C - 液体脱气:设备和方法 - Google Patents

液体脱气:设备和方法 Download PDF

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CN1090042C
CN1090042C CN97111519A CN97111519A CN1090042C CN 1090042 C CN1090042 C CN 1090042C CN 97111519 A CN97111519 A CN 97111519A CN 97111519 A CN97111519 A CN 97111519A CN 1090042 C CN1090042 C CN 1090042C
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K·乔
黄晓燕
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Abstract

本发明涉及供在温度高于(＞)60℃、压力高于或等于(≥)40磅/英寸2表压的液体脱气的微孔膜接触器。该接触器具有适于承受温度高于(＞)60℃、液体压力高于或等于(≥)40磅/英寸2表压的时间多于或等于(≥)30天不会产生塌陷也不会产生明显的孔收缩或孔封闭的微孔中空纤维膜。该膜有一外壳包封。

Description

液体脱气:设备和方法
本发明涉及采用微孔中空纤维膜接触器使液体脱气。
液体脱气是指完全地或有控制地从液体中除去溶解的或夹带的气体。在某些生产过程中所用的液体要求是超纯的。这些超纯液体不含或基本不含无机物质，如铁，离子及气体。通过反渗透法常可达到除去这些无机  物和离子的目的。然而，反渗透法不能除去溶解的或夹带的气体。最通常的溶解或夹带的气体是主要成分为氮气、氧气和二氧化碳的空气。
以前，已经采用膜接触器如中空纤维膜接触器来脱除溶解或夹带的气体。这类接触器采用了壁厚小于或等于约30微米的聚丙烯微孔中空纤维膜。然而，这类接触器只能脱除约1℃-约60℃液体中的气体，例如见Hoechst Celanese Corporation的LIQUI-CELExtra-Flow4英寸×28英寸膜接触器。虽然在该温度下除去气体是可行的，但随着某些工业部门对超纯液体要求的提高，需要研究更有效的脱气技术。采用传统的接触器的话，因传统接触器不能承受更高的温度，因而液体脱气受上述温度的限制。在温度约60-85℃脱气更激烈的情况下，中空纤维将会塌陷使接触器失效。因此，需要一种能在更高温度下作业的接触器。
在半导体工业中，制备半导体芯片的硅片表面是用超纯水清洗的。而超纯水中如果有任何污染物，即使是溶解的或夹带的气体(一般为空气)也会对芯片产生有害的影响。因此，需要有超纯水源。
日本专利申请No.52-143213(1977年11月28日申请)公开了壁厚分别为30微米和27微米的聚烯烃(如聚乙烯和聚丙烯)中空纤维。该中空纤维可用作尤其是气体分离膜(从一种气体中分离另一种气体的方法)。该聚烯烃是晶态的和成核的，成核剂是苯甲酸钠。中空纤维被称作是具有“形状稳定性”的，这可理解为具有较低的收缩率。
本发明涉及温度高于(＞)60℃、压力高于或等于(≥)40磅/英寸2表压下液体脱气的微孔膜接触器。该接触器的微孔中空钎维膜在经受液体温度高于60℃、液体压力高于或等于40磅/英寸2表压、时间长于或等于(≥)30天的情况下不会塌陷也不会产生明显的孔收缩或孔封闭。该纤维膜有外壳包封。
为了说明本发明，在附图中绘出了目前优选的一种形态；然而，应当理解本发明并不限于附图所绘的这种严格的排布和装置。
图1是液体脱气工艺示意图。
图2是接触器的剖视图。
参照图1，图中绘出了液体脱气流程10。流程10中采用膜接触器12(下面做更详细讨论)。流程10为逆流形态，但本发明并不限于此。接触器12一般包括液体通道(Shell side)和气体通道(tube side)。含夹带或溶解气体的液体14优选地导入接触器12的液体通道，吹扫气体16(或真空或两者吹扫气/真空)优选地导入接触器12的气体通道。已脱除气体的水18从接触器12排出，同时吹扫气体16也从接触器12中移走。一般技术熟练人员容易理解通过改变流动速率(或压力)、温度和构成液体和气体通道材料的组成，能对气体通过膜的输送量按要求进行设定。在本发明中，水是能脱气的一种液体。通常，液体12，当为水时，其最低温度高于约60℃，该液体的最高温度低于液体的沸点，但优选不高于80℃(如果该液体是水)。进入接触器的液体压力应高于约40磅/英寸2表压至高达约120磅/英寸2表压，但优选不高于约85磅/英寸2表压。中空纤维膜在60℃、40磅/英寸2表压或高于60℃和40磅/英寸2表压时应具有好的尺寸稳定性。好的尺寸稳定性是指至少应能经得起塌陷和/或阻止明显的孔收缩或孔封闭。明显的孔收缩或孔封闭是指有数量相当多的孔有任何缩小或堵塞，以致膜输送气体的能力大大地降低(即至少降低50％)。
参看图2，比较详细地展示了一个典型的接触器12。接触器12可根据美国专利5264171、5284584和5352171制造，每一专利内容都已列入本文供参考。接触器12通常包括壳体30和多根管子32。管子32优选是微孔中空纤维。中心管34沿壳体30的纵向轴放置。中心管34是根多孔管，因此液体可进入中心管或从管中流出。隔板36固定在中心管34两端的中间。壳体30、管子固定板38和管子32的外表面被规定为液体通道40。液体通道40装有进口42和出口44。通过液体通道40的物料流用箭头46指示。管子32的内部或内腔规定为气体通道48的一部分。气体通道48装有进口50和出口52。接触器12不限于上述结构。
微孔中空纤维32优选由壁厚超过30微米(更优选超过35微米，最优选大于或等于(≥)50微米)；孔隙率低于80％(更优选低于60％，最优选约20％)；Gurley数大于1(更优选大于100，最优选约300)；泡点高于或等于25磅/英寸2表压(更优选高于100磅/英寸2表压、最优选高于200磅/英寸2表压)，以及90℃无载荷、60分钟的收缩率低于5％(优选约2％或更低)的聚烯烃材料制成。
聚烯烃指由简单烯烃衍生的一类热塑性聚合物。典型的聚烯烃包括(但不限于)聚乙烯、聚丙烯、聚甲基戊烯、聚乙烯的共聚物、聚丙烯的共聚物、聚甲基戊烯的共聚物以及它们的混合物。优选的聚烯烃是聚丙烯，下文将作详细讨论。
聚丙烯优选的是结晶的，且其结晶温度高于或等于125℃。为了获得这种结晶聚丙烯，优选是有晶核的。有核的或有成核剂是指常常通过向聚合物添加一种物质而引发的促进晶核形成作用。优选的成核剂可选自苯甲酸钠或山梨醇乙酸酯或它们的混合物。优选的成核剂是苯甲酸钠。优选的是向聚合物添加约2400ppm成核剂。有核材料至少在两方面是有利的。第一，结晶均匀性较好因而有较高的热稳定性。第二，结晶均匀性较好因而能降低聚合物的“蠕变”或孔的闭合或孔的收缩趋向。
聚丙烯的熔体流动指数(ASTM D1238-85)大于0.1克/10分钟，优选大于1克/10分钟，最优选范围为0.1-20克/10分钟。
关于聚烯烃树脂的选择，人们应当考虑通常存在于所有市售商品树脂中的添加剂体系或稳定剂，因为某些稳定剂能引起孔的封闭或孔的收缩和/或在纤维表面结皮。例如，由0.05％BHT(丁基化的羟基甲苯或2，6-二-叔丁基-4-甲基苯酚)、0.12％(Irganox 1010，Ciba GeigyCorp.提供)四〔亚甲基(3，5-二-丁基-γ-羟基氢化肉桂酸酯)〕甲烷和32ppm硬脂酸钙组成的稳定剂会引起孔隙完全堵塞并在纤维表面形成表皮。据信从聚合物中渗出的稳定剂会堵塞孔隙并会复盖纤维表面。另一方面，由600ppm受阻酚(Ethyl 330，Ethyl Corp.提供)和1000ppm亚磷酸盐(Orgafox，Ciba Ciegy Corp提供)组成的稳定剂对孔隙或纤维表面没有影响。基于上述，提出下列选择稳定剂的准则：不会迁移的稳定剂是优选的，这种稳定剂可具有高分子量和/或含长碳氢基的侧链(如非极性的、化学性质方面与聚烯烃更相容)，并且稳定剂用量较低(所以迁移物质较少)。
根据本发明制造的模制品在温度高于约60℃、压力高于40磅/英寸2表压条件下能继续运行超过30天。
下述是制造根据本发明微孔中空纤维的优选工艺过程。树脂是聚丙烯(Fina pp 3362，Fina Co.提供)。挤出温度为210℃，挤出速度为100米/分，纺丝张力为21克。考虑到成核剂(约2400ppm苯甲酸钠)，纤维不必进行快速骤冷。在纤维纺丝后进行拉伸。纺成的纤维的外径为332微米，壁厚为55微米。在150℃退火热处理。然后，对纤维作10％冷拉伸、50％热拉伸(142℃)，其后进行20％松驰(142℃)。制得的纤维具有下述性能：外径325微米，内径215微米，壁厚55微米，Gurley数250秒/米2，泡点250磅/英寸2，收缩率1.2％，形状比1.02，抗拉强度460克，及断裂伸长率220％。
此处所列所有测定数值都是按照常规工业标准测定的(如相当的ASTM方法)，并对下列数值作更详细的讨论。
Gurley-“Gurley”是指空气流通过微孔中空纤维壁时阻力的量度。空气流所受阻力(如用Gurley透气度测定仪测定)，是在恒定的12.2英寸水柱压力下，测定10毫升空气通过一平方英寸样品所需的时间(秒)。测量值以“秒/英寸2”报告，并标准化为一平方英寸的数值。
泡点-“泡点”是中空纤维测定的大孔直径和综合孔径的量度。试验是以约一英尺中空纤维用加压氮气在甲醇浴中进行的。开始时氮气压力为15磅/英寸2表压，并以每秒约5-10磅/英寸2表压增加。当出现15条气泡流(streamer)时计算测量的结果。本文中泡点是以磅/英寸2表压报告的，泡点与孔大小(微米)用下式相关联：
(微米)＝6.56/(磅/英寸2表压，甲醇浴中)
孔隙率-“孔隙率”是中空纤维内孔体积和表观孔径分布的量度。孔隙率是按照ASTM D-2873-89所述步骤测定的。
本发明可以在不超出本发明精神和基本特征的条件下以其它形式来实施，因此，应该参阅作为说明本发明范围的所附权利要求书，而不仅限于上述说明。

Claims (17)

1.供温度高于60℃、压力高于或等于40磅/英寸2表压条件下液体脱气的微孔膜接触器，包括适于承受温度＞60℃、液压压力≥40磅/英寸2表压、时间≥30天不会塌陷也不会产生明显的孔收缩或孔封闭的微孔中空纤维膜；和包封所述纤维膜的外壳，其中所述明显的孔收缩或孔封闭是指该膜输送气体的能力降低至少50％。
2.根据权利要求1的接触器，其中所述微孔中空纤维膜的壁厚至少50微米。
3.根据权利要求1的接触器，其中所述微孔中空纤维膜包括有核聚烯烃。
4.根据权利要求1的接触器，其中所述微孔中空纤维膜包括结晶温度≥125℃的聚丙烯。
5.根据权利要求4的接触器，其中所述聚丙烯的熔体流动指数为≥0.1克/10分钟。
6.根据权利要求3的接触器，其中所述成核剂选自苯甲酸钠或山梨醇乙酸酯或它们的混合物。
7.根据权利要求6的接触器，其中所述成核剂是苯甲酸钠。
8.供温度高于60℃、压力高于或等于40磅/英寸2表压液体脱气的微孔膜接触器，包括：
壁厚大于30微米、由有核聚烯烃制的微孔中空纤维膜；和
保护所述纤维膜的外套。
9.根据权利要求8的接触器，其中所述壁厚为至少50微米。
10.根据权利要求8的接触器，其中所述成核剂选自苯甲酸钠、山梨醇乙酸酯或它们的混合物。
11.根据权利要求10的接触器，其中所述成核剂是苯甲酸钠。
12.在温度等于60℃并且其中有溶解的或夹带气体的液体脱气的方法，包括如下步骤：
提供在高于60℃和40磅/英寸2表压下，具有好的尺寸稳定性的有核聚烯烃中空纤维膜的微孔膜接触器，此处好的尺寸稳定性是指至少能经得起塌陷和阻止明显的孔收缩，所述明显的孔收缩或孔封闭是指该膜输送气体的能力降低至少50％；及
通过使溶解的或夹带的气体透过纤维膜而使液体脱气。
13.在温度等于60℃、压力等于或高于40磅/英寸2表压下，使含有溶解或夹带气体的水的脱气方法，其步骤包括：
提供具有多个壁厚至少为50微米且结晶温度高于或等于125℃的聚丙烯中空纤维膜的微孔膜接触器；及
通过使溶解的或夹带的气体透过纤维膜而使水脱气。
14.一种膜，包括
由有核聚烯烃制造的壁厚大于30微米、孔隙率低于80％、Gurley数大于1的微孔中空纤维，所述聚烯烃的熔体流动指数大于0.1克/10分钟。
15.根据权利要求14的膜，其中聚烯烃选自聚乙烯、聚丙烯、聚甲基戊烯、聚乙烯共聚物、聚丙烯共聚物、聚甲基戊烯共聚物以及它们的混合物。
16.根据权利要求14的膜，其中聚烯烃是聚丙烯。
17.根据权利要求15的膜，其中聚丙烯的结晶温度≥125℃。
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