CN1260229A - 反应性蒸馏 - Google Patents
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Abstract
反应性蒸馏在带有填料(2)的蒸馏塔(1)中进行,该填料(2)至少部分设计作为催化剂载体(23)。形成不同密度的两相的流体(3,4)流经填料。内体积流量(300)针对较浓稠流体(3)而设定,其值位于某一特征值(a)附近的区间(Ⅰ)内,这个值与该较浓稠流体的停留时间分布有关:对该特征值,停留时间分布的方差(s)－作为内体积流量的函数－采用最小值;在所述区间的边界,内体积流量与特征值相差不超过30%,优选不超过10%。
Description
本发明涉及按照权利要求1的前序部分所述的反应性蒸馏，还涉及反应性蒸馏的使用以及实施反应性蒸馏的填料蒸馏塔。
反应性蒸馏是指一种过程，其中在塔里进行催化反应，同时存在蒸馏过程。此处的塔可以是填料蒸馏塔。蒸馏塔的填料通常包含大量含有固体的局部空间(partial spaces)以及在这些局部空间之间的空腔，空腔和局部空间大致沿塔轴或与塔轴成一定角度的方向延伸，在含有催化活性物质的填充床的情况下都会形成局部空间。较浓稠的流体在填充床局部空间中以某一体积流量(被称为内体积流量)流动。较不浓稠的流体通过空腔反向流动。填充床局部空间被可透过流体的壁界定。一方面在填充床中发生催化反应，另一方面，两种流体间发生传质。
在反应性蒸馏中会出现不希望的副产物，其浓度取决于运行参数。通常需要对产物进行处理，出现副产物愈多处理起来愈复杂愈费资金。因此，有利的是要以转变的副产物尽可能少的方式选择运行参数。不过每单位体积填料达到尽可能大的反应性蒸馏生产率也是目标所在。为了达到这一点，必须以，可用于反应的整个填料表面全被较浓稠的流体包覆(浸湿)，为条件。从US-A 5 120 403中可了解反应性蒸馏，其中，填料被液相浸没，气相和液相一起形成泡沫，在填料中移动。
本发明目的是提供实施反应性蒸馏的另一种方法，使副产物产量最小，或至少接近可能的最小值，而待生产的产品尽可能高。该目的借助权利要求1中说明的反应性蒸馏实现。
在带填料的蒸馏塔中进行反应性蒸馏。填料至少有一部分是催化剂载体形式的，形成不同密度的两相的流体流经填料。内体积流量是针对较浓度流体而言，其值大小处于某一特征值区间内，该特征值与该较浓稠流体的停留时间分布有关：对特征值来说，停留时间分布的方差-作为内体积流量的函数-采用最小值；在所说的区间的边界点，内体积流量同特征值之间相差不超过30％，优选不超过10％。
从属权利要求涉及本发明的优选实施方案。权利要求8的主题是根据本发明的方法的运用，权利要求9是针对相应的填料蒸馏塔。
以下将参考附图描述本发明，图中：
图1塔的下端部分，借助此部分可进行反应性蒸馏；
图2进行反应性蒸馏的填料的一部分；
图3说明停留时间分布的曲线图；
图4实验测定的说明停留时间分布的方差对内体积流量的依存关系的曲线图，
图5类似垫片的填料件的壁部分；
图6带有圆柱形填料件的载体结构；以及
图7两种填料结构的部分填料。
图1中的塔1包含填料2，如专利说明书EP 0 640 385(＝P.6592)中所了解的。填料2包括填料单元2′，这些单元以架子状排列，是由指向主流方向10的层2″堆积起来的，层2″基本由圆柱形填料件23形成。在填料件23之间，流道彼此交叉，且彼此不封闭。填料件23铺成栅格状载体结构，图1中没有示出。相邻的填料单元2′在每种情况下都是互相错置成90度角。套筒12构成参与反应性蒸馏的流体3和4的偏向流动障碍(见图2)。
参考图2和3，现解释一下为说明本发明所需的反应性蒸馏的几个方面。形成不同密度的两相的流体3和4，沿平行于塔轴的z轴方向彼此反向流经填料2。填料2包含空腔24和局部空间23，它们大致沿塔轴延伸，或者与轴成一定角度定向。局部空间23在填充床20的各种情况下都能形成，特别是作为催化活性物质载体的颗粒的浇注主体。局部空间23由壁22界定，壁22可透过流体3和4。这些壁22，例如，可由线栅(以织物，网状物、纤网形式)制造。流体3以内体积流量300流经填充床20，箭头30指的是流体3含有的物质分子运动的途径。通过在点21处(在填充床20内)的反应，初始物质转为所希望的产物或不希望的副产物(箭头30′)。在由壁22形成的填充床20的表面发生流体3和4之间的传质，通过这种传质可以实现蒸馏。
流体3中包含的分子在填充床20中有不同的停留时间。在点z＝0，时间t＝0，被带入填充床20中的分子-参见图3-在稍后时间t＝t1，位于点z＝z1的附近，两条点划线301和302表示分子流经填充床20途径的散射区域。在时间点t＝t1处分子的位置z的频率分布以钟形曲线31给出，用函数曲线C＝C(z；t＝t1)作定量说明。如果在填充床20的较低端-即在z＝z2-记录到受监视的分子的出现(这些分子是在t＝0时同时加入到填充床20的)，那么将得到钟形曲线32：c′＝c′(t，z＝z2)。对于该曲线32，可以确定一个方差s，此方差s随内体积流量300而变化。受监视分子可以是，例如，离子，其浓度可以在填充床底端z＝z2处作为导电率的测量结果而确定。
测量依赖于内体积流量300的方差s可获得曲线33，它有一最小值：见图4。在内体积流量的特征值a处，对应于s的最小值，副产物的产量同样也最小。在比a小得多的内体积流量处，填充床20将出现流体3的滞流，因而出现停留时间部分偏高，其结果是曲线32加宽，因而方差s增大。在内体积流量比a大得多的情况，在由壁22形成的填充床20的表面将出现液体旁流。流体从催化活性填充床20流过，但几乎不与其接触。流体3停留时间部分偏高，同样导致曲线32的加宽以及方差s的增大。
对于要进行的反应性蒸馏的预定生产率，当以内体积流量采用特征值a的方式设计塔的尺寸时，将得到理想的工艺过程。在位于a值附近的限制区间I中，对这个a值的偏差不会对此方法产生明显不利：在此区间I的边界处内体积流量3以与特征值a相差至多约30％，当然优选差值为10％或更小。
进行反应性蒸馏的另一种合适填料可从专利说明书EP 0 631 813(＝p.6579)中获知。形成平行铺设层的填料件23成形为垫片状并由两个可透过流体的壁22′和22″组成：见图5。填料件23的内部空间含有带催化活性物质的颗粒200。在壁22′和22″中的平行通道25，其轮廓呈凸纹形式，形成了内部空间。这些通道25彼此交叉且相互不封闭。在填料件23的边缘，它们被隔离，作为壁22′和22″的轮廓成形结果，在相互交叉彼此不封闭的相邻层之间同样都会产生似通道的空腔。
图6表示另一种适宜填料，可从已经命名为EP 0640385中获知。以折线形叠合的表面51和52的静止混合结构5用作填料件23的载体结构。由这种折线状形成的全部或其余的单独通道在各种情况下都含一个填料件23。一般说来，在载体结构5处还会形成一薄层较浓稠流体。借此，可用于蒸馏的表面扩大了。
为了得到用于蒸馏的更大表面，可以下面的方式设计填料2：见图7。在塔中，第一类区和第二类区6和7在塔轴方向上以交替顺序布置。在第一类区6中，包含填料结构5(对照图6)，其中，两种流体间只发生传质。在第二类区7中包含填料结构5′和23，其中发生反应性蒸馏。区6和7的长度可以改变以获得不同大小的可用表面。
反应性蒸馏的产量对填料蒸馏塔是预定的。塔填料的容量必须根据本发明以下面方式设计：为塔操作提供的内体积流量，一方面主要与预定产量相符，另一方面其值位于特征值a附近的所说的区间I内。
根据本发明的反应性蒸馏可用于，例如酯，醚和醇的生产或分解。其他应用可以是烯烃或芳烃化合物的选择性水解，而且还可用于异构化。
用于说明根据本发明的反应性蒸馏的一个例子：
甲基-叔丁基醚(MTBE)的合成可在带有催化活化填料的反应性蒸馏中进行(对照EP-A 0 396 650)。其中，来自带有甲醇的C4物流中的异丁烯转为MTBE。此过程中可用酸性离子交换树脂作催化剂。除了主反应，还主要出现三个副反应。一方面C4物流可含有痕量水，异丁烯与其反应生成叔丁醇；另一方面，异丁烯与自身反应生成二异丁烯；此外还发生甲醇浓缩生成二甲醚的反应。一种反应物大量过剩或缺少其他反应物时会出现所说的后两种副反应。
在借助催化活性填料操作的反应性蒸馏中，内体积流量小会出现液相的滞流，因而在塔反应区的不同的位置停留时间会部分偏高。在这些滞留区，一种反应物过量或在缺少由反应引起的其他反应物时，发生所说副反应的程度会增加。在内体积流量超过区间I的上限的情况，应该说是可以避免滞留区的，但转化率会显著降低。
在根据本发明的反应性蒸馏中，塔的内体积流量以下方式设置：液相均匀地流过催化活性固体；在催化活性固体床中避免滞留区，催化剂因而全部浸湿，所述副反应可都会得到抑制。
Claims (10)
1.蒸馏塔(1)中的反应性蒸馏，该塔包含至少一部分是设计作为催化载体(23)的填料(2)，还包含形成流经该填料的不同密度的两相的流体(3，4)，其特征在于：内体积流量(300)针对较浓稠流体(3)设置，其值位于某一特征值(a)附近的区间(I)内，该特征值与较浓稠流体的停留时间分布(32)有关；对这一特征值而言，停留时间分布的方差(s)-作为内体积流量的函数-采用最小值；在所述区间的边界，内体积流量与该特征值相差不超过30％，优选10％。
2.根据权利要求1的反应性蒸馏，其特征在于：塔(1)包含有填料(2)，该填料(2)包括许多含有固体物质的局部空间(23)和在所述局部空间之间的空腔(24)，空腔大致沿塔轴或与塔轴成一定角度的方向上延伸，每种情况下的所述局部空间都是由填充床形成的，该填充床包含有催化活性物质，这些填充床局部空间由可透过流体(3，4)的壁(22)界定。
3.根据权利要求2的反应性蒸馏，其特征在于：塔(1)中沿塔轴方向以交替次序布置有第一类区和第二类区(6，7)，第一类区中含有其中只发生两流体间传质的填料结构(5)，而第二类区则包含其中进行反应性蒸馏的填料结构(5′)。
4.根据权利要求2或3的反应性蒸馏，其特征在于：为实现反应性蒸馏而提供的填料(2)或填料结构(5′)是由沿塔轴方向定向的多层堆积起来的；每种情况下相邻两层都形成彼此交叉且彼此不封闭的似通道的空腔。
5.根据权利要求4的反应性蒸馏，其特征在于：每种情况下的各层都是由多个含有催化活性物质的填料件(23)形成的，该催化活性物质安置在载体结构(5)中；填料件主要是圆柱形的。
6.根据权利要求4的反应性蒸馏，其特征在于：每种情况下，各层都是由包括两个可透流体的壁的套筒状填料件(23)形成；填料件的内部空间是由包含催化活性物质(200)的平行通道形成，这些通道以壁(25)上的凸纹状轮廓的形式存在，这些通道彼此交叉且彼此不封闭，只在填料件的边缘被隔离开。
7.根据权利要求1-6中的任一个所述的反应性蒸馏用于酯，醚或醇的生产或分解。
8.根据权利要求1-6中的任一个所述的反应性蒸馏用于烯烃或芳烃族化合物的选择性水解。
9.根据权利要求1-6中的任一个所述的反应性蒸馏用于进行异构化。
10.用于实施根据权利要求1-6中任一个所述的反应性蒸馏的填料蒸馏塔(1)，其特征在于：对反应性蒸馏而言，产量是预定的；塔填料的容量以下面方式设计：为塔操作预定的内体积流量(300)，一方面大致与预定产量相应，另一方面位于特征值(a)附近的所述区间(I)内。
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| FR2807676B1 (fr) * | 2000-04-17 | 2002-07-12 | Inst Francais Du Petrole | Sous-ensemble polyfonctionnel assurant la mise en contact, la distribution de matiere et l'echange de chaleur et/ou de matiere d'au moins une phase gazeuse et d'au moins une phase liquide |
| EP1163952A1 (de) * | 2000-06-14 | 2001-12-19 | Sulzer Chemtech AG | Mikrokanäle enthaltendes Festbett angeordnet in einem rohrförmigen Reaktorteil |
| EP1549604B1 (en) | 2002-10-11 | 2011-07-13 | Akzo Nobel N.V. | A process for the preparation of monochloroacetic acid |
| FR2867697B1 (fr) * | 2004-03-16 | 2007-06-01 | Air Liquide | Structure de garnissage ondule-croise |
| CA2586971C (en) * | 2004-11-12 | 2013-07-23 | Velocys Inc. | Process using microchannel technology for conducting alkylation or acylation reaction |
| US9272965B2 (en) * | 2009-12-22 | 2016-03-01 | Catalytic Distillation Technologies | Process for the conversion of alcohols to olefins |
| PL235394B1 (pl) * | 2017-09-29 | 2020-07-13 | Losentech Spolka Z Ograniczona Odpowiedzialnoscia | Kolumna do procesów wymiany masy i ciepła, zwłaszcza destylacji reaktywnej |
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| WO1990002603A1 (de) * | 1988-09-02 | 1990-03-22 | Gebrüder Sulzer Aktiengesellschaft | Vorrichtung zur durchführung katalysierter reaktionen |
| US5108550A (en) * | 1990-02-06 | 1992-04-28 | Koch Engineering Company, Inc. | Catalyst system for distillation reactor |
| EP0466954A1 (en) * | 1990-07-17 | 1992-01-22 | CHEMICAL RESEARCH & LICENSING COMPANY | Catalytic distillation |
| JP2846975B2 (ja) * | 1991-07-10 | 1999-01-13 | 日本原子力研究所 | 反応蒸留用固体酸触媒 |
| EP0631813B1 (de) * | 1993-06-30 | 1998-01-07 | Sulzer Chemtech AG | Katalysierender Festbettreaktor |
| DE59308587D1 (de) * | 1993-08-26 | 1998-06-25 | Sulzer Chemtech Ag | Packung mit katalytischen oder adsorbierenden Mitteln |
| KR960022419A (ko) * | 1994-12-29 | 1996-07-18 | 김준웅 | 반응증류를 이용하여 메틸아세테이트로부터 초산과 메탄올을 제조하는 방법 및 장치 |
| US5961815A (en) * | 1995-08-28 | 1999-10-05 | Catalytic Distillation Technologies | Hydroconversion process |
| DE19624130A1 (de) * | 1996-06-17 | 1997-12-18 | Basf Ag | Verfahren zur katalytischen Destillation |
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| US20030124038A1 (en) | 2003-07-03 |
| ATE242029T1 (de) | 2003-06-15 |
| DE59905823D1 (de) | 2003-07-10 |
| EP1013325B1 (de) | 2003-06-04 |
| BR9905921A (pt) | 2000-09-26 |
| ES2200489T3 (es) | 2004-03-01 |
| TW452500B (en) | 2001-09-01 |
| ZA997521B (en) | 2000-06-07 |
| CZ9904683A3 (cs) | 2001-08-15 |
| CA2288312C (en) | 2004-01-06 |
| KR20000062215A (ko) | 2000-10-25 |
| CN1158125C (zh) | 2004-07-21 |
| PL337271A1 (en) | 2000-07-03 |
| EP1013325A1 (de) | 2000-06-28 |
| SG74756A1 (en) | 2000-08-22 |
| CA2288312A1 (en) | 2000-06-22 |
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