CN101347685A - 使用微通道装置的纯化方法 - Google Patents
使用微通道装置的纯化方法 Download PDFInfo
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- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明涉及一种使用微通道装置的纯化方法,具体涉及从具有类似挥发性的化合物中除去杂质、形成超高纯度化合物的方法。该方法包括:在至少一个微通道装置中将至少一种目标化合物与至少一种杂质化合物分离;所述至少一种目标化合物和至少一种杂质化合物的相对挥发性小于或等于1.2;所述至少一种目标化合物所达到的纯度为99.99%。
Description
相关申请交叉引用
本申请根据35U.S.C.§119(e)要求2007年7月20日提交的美国临时专利申请第60/961,370号和2008年2月12日提交的美国临时专利申请第61,065,473号的优先权。
技术领域
本发明涉及从相对挥发性等于或小于1.2的化合物中除去杂质、从而形成超高纯度化合物的方法。
背景技术
对于材料加工和应用中作为进料、中间体、溶剂或最终产品的超高纯度化合物尚存在许多尚未满足的需求。在本文中,超高纯度定义为纯度为下限10-10重量%(1ppt)至上限0.01重量%(100ppm)。这些化合物包括但不限于可蒸馏的有机物,包括单体,用于色谱应用(例如HPLC)的溶剂,可升华的固体,电子化学物质,以及分析试剂。
纯化化合物的常规方法包括蒸馏、结晶、萃取、吸收、加合纯化、质量选择性超离心、以及与蒸馏相结合的化学处理。这些方法和其它相关的方法,例如美国专利公开第US 2006/0016215 A1号中揭示的蒸馏法经常受到限制,因为所需化合物和杂质的沸腾性质接近,或者具有低的相对挥发性,而且杂质浓度低,传质驱动力低。具有低相对挥发性α(α=杂质蒸气压/所需化合物的蒸气压)等于或小于1.2的化合物特别难以通过采用蒸气/液体平衡的分级法进行纯化,而使得无法通过常规方法得到超高纯度的材料。另外,对采用现有方法可以达到的纯度水平经常存在经济限制。过高的基建成本或运作成本会限制可达到的纯度,这是因为会由于杂质和化合物的物理性质和/或化学性质造成无法接受的产率损失,能量输入或者工艺循环时间。
例如,可以使用芬斯克方程,基于组分的相对挥发性(α)和所需的纯度预测蒸馏所需的最少平衡级(stage)数。为了除去最成问题的接近沸点的杂质(α<1.2),级数,或等板高度(HETP)会超过50,100,甚至200,即使使用今天最先进的填料(HETP=0.05-0.20m),这也可能需要塔高>10米。对于许多应用,这种尺寸的塔会造成规模放大很困难,为可操作性带来困难,并且由于大量化合物的储存可能导致安全隐患。
因此,人们一直需要更经济而高效的对含有相对挥发性等于或小于1.2的杂质的化合物进行纯化的方法。
本发明通过利用微通道装置的优点,同时结合已知的用于纯化的技术,满足了上述需求。微通道装置提供了更佳的对工艺条件的控制、改进的安全性、以及从实验室研发到工业生产的投入市场的速度。这些装置极为适合用于试剂、溶剂、中间体或最终产物的纯化。微通道技术的优点基本是来源于装置中提供的小尺寸和高表面积,使得相之间具有高的交换速率。通过微通道尺寸(通常为1-1000微米),通过增加的毛细管效应和界面效应的重要性和减少传热和传质的距离,促进了纯化。这些装置中优良的传热和传质提供了相之间高的交换速率,还提供了更佳的温度控制,以获得更有效的纯化级,或者更低的等板高度(HETP),这使得固定的纯化装置几何结构可以具有更多的级,从而获得更高的纯度。此外,通过对热交换进行更佳的整合,获得改进的能量效率,从而可以获得较低的资本密集度和较低的操作成本。所述微通道装置还使得能够通过“叠加(numbering-up)”或仅仅将单独的通道重复许多次而进行生产规模放大,而不是像常规的规模放大那样通过增大反应器容器的尺寸来进行规模放大,通过本发明的方式可以满足市场的需求,同时不会造成性能损失,无需常规的规模放大研究而显著节约时间和成本。
发明内容
在本发明中提供了一种制备超高纯度的化合物的方法,该方法包括:
在至少一个微通道装置中将至少一种目标化合物与至少一种杂质化合物分离;
所述至少一种目标化合物和至少一种杂质化合物的相对挥发性等于或小于1.2;
另外,其中至少一种目标化合物所得的纯度为99.99%。
具体实施方式
在本文中,“微通道装置”表示具有三维结构(用于流体流动的通道或空间)的微结构化的装置(通常是,但是并非排它性),垂直于流动方向的尺寸通常为0.1-5,000微米,更具体来说为10-1000微米。
有许多种用于本发明的微通道装置的制造技术和构建材料。一些构建材料包括但不限于金属、聚合物、硅、陶瓷和玻璃。下表1显示了一些可用于各种微通道装置的制造技术:
表1
金属 | 聚合物 | 硅 | 陶瓷 | 玻璃 |
机械微加工 | 模塑 | 光刻 | 陶瓷注塑 | 各向同性蚀刻 |
激光微加工 | 注塑 | 各向异性干蚀刻 | 带材浇铸 | 可光刻玻璃的微结构化 |
湿法化学蚀刻 | 热压纹 | 深度活性离子蚀刻(deep reactiveion etching) | 立体光刻 | 激光图案化 |
选择性激光熔融 | 聚合物激光微加工 | 各向异性湿蚀刻 | 涂层和泡沫体 | |
填隙(shims) | 微型立体光刻 | 各向同性蚀刻 |
任选地,本发明的微通道装置包括芯结构(wick structure)。所述芯结构有助于增大界面交换面积以及将液体和蒸气相保持在装置中不连续的区域,以便将可能降低性能的回混现象最小化。所述芯结构可以是本领域技术人员目前已知的任意种类。本发明的微通道装置的HETP可以为小于5厘米至小于0.25厘米。在一些实施方式中,所述微通道装置的HETP小于0.05厘米。
上述微通道装置能够提高传热和传质,因此是有用的。传热和传质会通过其中构建微通道装置并进行运作的构型或方式来获得提高。平整的通道壁有助于提高传热和传质。通道壁上的其它结构特征,例如凹槽、织构和图案都有助于提高装置的传热和传质,使得装置更为高效。对于任何包含至少一种目标化合物和至少一种杂质化合物,且杂质化合物的相对挥发性等于或小于1.2的材料,可通过使得样品材料通过微通道装置而进行分离。在本文中,“目标化合物”指任意试图达到预定的纯化后纯度水平的化合物。在本文中,“杂质化合物”表示任意与目标化合物混合、且希望与目标化合物相分离的材料。在本发明中,存在将要与至少一种杂质化合物相分离的至少一种目标化合物。本发明的目标是将至少一种目标化合物与至少一种杂质化合物相分离,使得所得目标化合物的纯度至少为99.9999%,至少为99.999%,或者至少为99.99%。单独使用微通道装置、或者将这些装置与其它已知的纯化技术结合利用,可以达到这种水平的纯度。
所述微通道装置可以单独使用或者与其它已知的纯化技术结合使用。一类技术是吸附纯化或化学纯化,例如通过温度变换吸附进行加合纯化。可以将选择性吸附剂或形成加合物的路易斯碱(例如胺、膦或醚)负载在微通道表面上,提供极高的交换面积以接触含杂质的物流。可以为传热流体的流动提供其它的微通道,以便为装置进行精确的温度控制,以便在吸附和脱附步骤之间进行有效的调节和循环。所述微通道装置可与化学纯化工艺(例如使用离子性液体作为纯化剂的那些)结合使用。作为举例说明,通过以下方式对金属有机化合物进行纯化:将含杂质的金属有机化合物与离子性液体混合,对所得的混合物进行加热,然后分离和隔离超高纯度的金属有机化合物。该方法可以与微通道装置结合使用,以显著减少目标金属有机化合物中的金属杂质、有机杂质和有机金属杂质。相对于使用常规纯化法的结果,该组合性的方法提供了含硅杂质含量减小的金属有机化合物,从而满足半导体工业中所要求的严格的纯度标准(所有杂质<10ppb)。
离子性液体通常是在低温下为液体的盐,熔点低于100℃。许多离子性液体在室温下保持液相,被称为室温离子性液体。离子性液体完全由离子组成,通常由大体积有机阳离子和无机阴离子组成。由于这些化合物中的高库仑作用力,离子性液体实际上没有蒸气压。
任意合适的离子性液体均可用于本发明。用于离子性液体中的示例性的阳离子包括但不限于烃基铵阳离子、烃基鏻阳离子、烃基吡啶鎓阳离子、以及二烃基咪唑鎓阳离子,分别见下面的第I-IV类所示。可用于该离子性液体的示例性的阴离子包括但不限于氯代金属酸根阴离子(chlorometalateanion),氟代硼酸根阴离子,例如四氟硼酸根阴离子以及烃基取代的氟代硼酸根阴离子,以及氟代磷酸根阴离子,例如六氟磷酸根阴离子和烃基取代的氟代磷酸根阴离子。示例性的氯代金属酸根阴离子包括但不限于氯代铝酸根阴离子,例如四氯铝酸根阴离子和氯代三烷基铝酸根阴离子,氯代镓酸根阴离子,例如氯代三甲基镓酸根和四氯代镓酸根,氯代铟酸根阴离子,例如四氯铟酸根和氯代三甲基铟酸根。
第I类:烃基取代的卤化铵 第II类:烃基取代的卤化鏻
R=烃基 R=烃基
第III类烃基取代的卤代吡啶鎓 第IV类烃基取代的卤代咪唑鎓
在上述的第I-IV类式中,R=H,(C1-C10)烷基,例如甲基、乙基、丙基、丁基、戊基、己基和辛基;芳烷基,例如苄基;烯基,例如烯丙基;芳基,例如苯基;或者二(C1-C6)烷基氨基(C1-C10)烷基,例如二甲基氨基甲基,二甲基氨基乙基,二甲基氨基丙基和二乙基氨基丙基,X是卤素,例如氯。各R基团可以是相同或不同的。
基于微通道装置技术的其它纯化法,例如蒸馏、汽提、萃取和吸附,提供所需的提高的传热和传质,以得到超高纯度的产品(ppm,ppb,ppt)。这些纯化法还提供了传递级的强化(intensification of transfer stage),这是解决对具有类似沸点(相对挥发性,0.8<α<1.2)的流体混合物进行纯化而达到高纯度的问题所需的。有益的操作条件包括一定的温度和压力,使得液相中的一种或多种流体组分能够发生相变,生成蒸气相或者吸附在吸附剂上的吸附相。这些条件可包括温度为-25℃至250℃,压力为0.1Pa至10MPa。进料的杂质含量可为流体混合物的1ppm至最高10重量%,甚至50重量%。
所述微通道装置可用来纯化各种化合物。本发明化合物的杂质通常相对蒸发性小于1.5,难以通过常规的蒸馏法纯化。更优选的是,所述化合物中杂质的相对挥发性为α≤1.2。单体之类的可蒸馏的有机物可用来合成用于高级用途的聚合物,在这些用途中,需要超高的纯度,以满足对于食品、药物、或人类健康护理应用的严格的产品要求。这些应用可包括用于药物递送的药用装置,人类健康护理诊断用品,可植入人体的装置,以及用于生物、药物或营养化合物(nutraceutic compound)的纯化/生产的离子交换树脂。一种得到超高纯度聚合物产品的方式是减少起始单体中的杂质。
用于高纯度单体的其它应用包括生产低挥发性有机物含量(VOC)的丙烯酸类乳胶漆。具体来说,源自丙烯酸丁酯的低VOC漆的生产需要除去单体中接近沸点的杂质,作为一种减少最终产品中残余VOC的方式。低VOC漆的特征是挥发性杂质含量等于或小于100ppm。一种特别麻烦的接近沸点的杂质是二丁基醚(沸点=140℃),其沸点接近丙烯酸丁酯(沸点=145℃),相对挥发性α=1.20。通过使用目前常规的蒸馏塔进行的丙烯酸丁酯的纯化需要很高的基建投资和高的运作成本。本发明的方法以远为高效和节约成本的方式制得了纯度更高的产品。
超高纯度的单体能够特别有效地用来生产用于包括光刻和光电子领域的用途的特殊聚合物。在一些实施方式中,需要除去一种单体的光学异构体,以得到所需的聚合物性质。
另外,用于电子材料应用的超高纯度单体和溶剂可包含各种有机化合物,例如取代的丙烯酸酯和甲基丙烯酸酯、丙酮、MTBE、PGMEA、环己酮和DMF。这些单体和溶剂用来生产用于集成电路的硅芯片制造的光刻聚合物和辅助产品。计算机芯片制造商还使用许多种溶剂、螯合剂和清洁溶液,例如蚀刻后残余物去除剂,从而在制造过程中清洗硅晶片。超高纯度产品标准要求在芯片加工的所有方面使用超高纯度的材料。
所述微通道装置还可以与一种或多种其它的纯化法结合,形成混合纯化法,以绕过在溶解性或蒸气-液体平衡中的组成或热力学障碍,或者通过其它方式阻碍达到高纯度产品的障碍。这些障碍包括但不限于萃取蒸馏、共沸蒸馏、抽提结晶、薄膜渗透/蒸馏、反渗透/蒸馏、反应蒸馏、催化蒸馏、汽提蒸馏和本领域技术人员已知的其它混合纯化法。
在萃取蒸馏中,通过加入溶剂或其它加入的物流,与至少一种组分选择性地发生作用,增大至少一种组分的相对挥发性,改变进料组分的相对挥发性,使得易于分离和纯化。无论所需的产物是作为塔顶产品或塔底产品回收,对溶剂的选择都是很重要的。对溶剂的选择由待纯化的化合物的性质决定,可包括一定范围的材料,例如水、有机烃类和离子性液体。加入的溶剂通常在独立的溶剂回收塔中回收,循环到萃取蒸馏塔中。所述微通道装置可用于萃取蒸馏塔、溶剂回收塔、或者用于这两者。微通道装置提供的分离效率的改进(较低的HETP)有助于克服较高循环比造成的纯度的限制,所述较高的循环比会稀释浓度,降低常规塔中萃取溶剂的效率。
在共沸蒸馏中,加入溶剂以产生或改变与一种或多种进料组分的组成窄点(compositional pinch point)。在第一个塔中制得的作为塔顶或塔底产品的共沸混合物被输送到第二个塔,在第二个塔中,通过加入溶剂破坏共沸混合物,所需的纯化的物流作为富集的产物回收。对混合的溶剂/进料物流进行进一步的处理,回收溶剂,将其再循环到第二个(共沸蒸馏)塔,弃去来自第一个塔的副产品/杂质。
在抽提结晶法中,加入溶剂来改变两种或更多种溶质的相对溶解度,以进行结晶过程。这可包括改变阻碍纯相形成的组成共晶,或者改变对温度不敏感的溶解度曲线,该种曲线会使得无法通过调节温度而很容易地分离和隔离纯的物质。通过蒸馏回收和循环溶剂,以影响溶解性性质。高效微通道蒸馏提供了一种独特的方法来确保再循环中包含高纯度的溶剂,这有助于提高结晶工艺的效率,减少溶剂流的流动和与之相关的成本。
在薄膜和/或反渗透蒸馏混合纯化系统中,蒸馏塔与薄膜分离装置联机,以提高纯化工艺的效用。在一个实施方式中,可以首先使得进料流通过薄膜进行处理,浓缩进料流并减小下游蒸馏塔的尺寸。在第二个实施方式中,可以使来自蒸馏塔的产物通向薄膜装置,用于二次纯化或抛光步骤。
Claims (9)
1.一种制备超高纯度化合物的方法,该方法包括:
在至少一个微通道装置中将至少一种目标化合物与至少一种杂质化合物分离;
所述至少一种目标化合物和至少一种杂质化合物的相对挥发性小于或等于1.2;另外,所述至少一种目标化合物所达到的纯度为99.99%。
2.如权利要求1所述的方法,其特征在于,所述至少一个微通道装置是微通道蒸馏装置。
3.如权利要求1所述的方法,其特征在于,在至少一个微通道装置中进行的纯化是通过温度变换吸附进行的。
4.如权利要求1所述的方法,其特征在于,还包括至少一个具有芯结构的微通道装置。
5.如权利要求1所述的方法,其特征在于,所述微通道装置的等板高度(HETP)小于5厘米。
6.如权利要求1所述的方法,其特征在于,以所述至少一种目标化合物和至少一种杂质化合物的总量为基准计,所述至少一种杂质的含量减小到小于100ppm。
7.如权利要求1所述的方法,其特征在于,所述至少一个微通道装置与至少一个另外的纯化法结合使用。
8.如权利要求1所述的方法,其特征在于,所述达到的纯度为99.99%的目标化合物被用于电子材料应用。
9.如权利要求7所述的方法,其特征在于,所述达到的纯度为99.99%的目标化合物被用于电子材料应用。
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2008
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- 2008-07-09 TW TW097125849A patent/TW200914123A/zh unknown
- 2008-07-16 EP EP08160505A patent/EP2020258A2/en not_active Withdrawn
- 2008-07-16 EP EP12150399A patent/EP2439208A1/en not_active Withdrawn
- 2008-07-18 KR KR1020080069861A patent/KR20090009733A/ko not_active Application Discontinuation
- 2008-07-21 CN CNA2008101429540A patent/CN101347685A/zh active Pending
- 2008-07-21 CN CNA2008101429555A patent/CN101348499A/zh active Pending
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- 2010-09-24 KR KR1020100092928A patent/KR20100114864A/ko not_active Application Discontinuation
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113521784A (zh) * | 2021-07-05 | 2021-10-22 | 内蒙古工业大学 | 一种微精馏热集成系统 |
CN113521784B (zh) * | 2021-07-05 | 2023-01-06 | 内蒙古工业大学 | 一种微精馏热集成系统 |
Also Published As
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US20110172452A1 (en) | 2011-07-14 |
EP2439208A1 (en) | 2012-04-11 |
TW200914123A (en) | 2009-04-01 |
EP2020258A2 (en) | 2009-02-04 |
US20100185003A1 (en) | 2010-07-22 |
EP2359922A1 (en) | 2011-08-24 |
JP2009035539A (ja) | 2009-02-19 |
CA2637118A1 (en) | 2009-01-20 |
KR20100114864A (ko) | 2010-10-26 |
EP2359923A1 (en) | 2011-08-24 |
US20100185002A1 (en) | 2010-07-22 |
US7919638B2 (en) | 2011-04-05 |
US7659414B2 (en) | 2010-02-09 |
US8101787B2 (en) | 2012-01-24 |
US7939684B2 (en) | 2011-05-10 |
US20090023940A1 (en) | 2009-01-22 |
KR20090009733A (ko) | 2009-01-23 |
CN101348499A (zh) | 2009-01-21 |
CA2637118C (en) | 2012-08-14 |
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