CN1079676A - 催化多相反应器 - Google Patents
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Abstract
一种用于进行连续多相催化剂反应例如转化合
成气成为高级烃燃料的反应器。经可透气的板15
将气体反应物引入到包括产物和细分散的催化剂的
油浆16中,通过包括过滤板22的过滤器设备13将
液体产物与剩余的油浆分离。通过过滤器设备中的
恒位面设备23使越过过滤板22产生一个压差。该
压差使过滤板22内的滤液32的高度保持低于油浆
16的高度,通过引入气体组分作为气泡流使油浆16
保持在搅拌的稳定状态下。横过过滤板22的压差
的波动避免了过滤板堵塞,并且滤液32和油浆16
上面的气体空间28、29是连通的。
Description
本发明涉及用于进行连续多相催化反应的反应器,该反应器特别(但不是专门地)用于通过费-托型合成反应将由甲烷转化生成合成气催化转化成烃燃料的反应。适用于该设备的其他反应体系包括用于制备石油化学品、由合成气制备氧化物的各种油浆反应以及脱氢反应。
三相催化反应体系被用于许多化学方法中,并且其在石油化学工业中的应用出现了增加的趋势。在使用中的三相体系中,机械搅拌的、环形及泡罩塔油浆反应器含有悬浮于液体中的细小催化剂颗粒。在大多数应用中,液体必须与油浆分离,以除去液体产物,或用于催化剂再生,在液体是惰性介质的情况下,有时由于降解或杂质的聚焦而必须置换该液体。
由于低的传质和耐热,机械搅拌的油浆反应器特别适用于间歇过程,这些特征也使它们适合于实验室中的反应动力学的测量。然而,这种类型的反应器的严重缺点和限制是在任何连续操作中很难分离催化剂颗粒。
工业上,仅仅机械搅拌的反应器用于由棉子、大豆、玉米、葵花子等得到的油的双键的加氢。由于使用镍催化剂,产物包括人造奶油、催化加氢植物油、皂和脂膏。根据脂油的低扩散性和高粘度来选择反应器。由于不用过滤就可得到完全没有催化剂的产物这样的优点,所以已经提出固定床操作。许多其他加氢反应也是在搅拌的反应器中进行,例如硝基化合物的加氢。
因为避免使用机械移动部件,所以泡罩塔油浆反应器的操作是简单的。由于低的扩散阻力和有效的传热的结合,所以这些反应器对许多工业过程是有吸引力的。然而,固-液分离通常是在反应器的外面在精细过滤和沉降系统中进行,催化剂油浆将循环到反应器,有时要用油浆泵来循环。因此,在泡罩塔油浆反应器的连续操作中可能遇到严重的问题。
由于世界石油资源的减少,所以使用天然气作为能源就变得更有吸引力,并且使天然改质成为高级烃燃料的方法的重要性正在增加。
因此,本发明的一个目的是提供一种可进行多相催化反应的连续方法的反应器,该反应器没有现有技术的这些缺点。
本发明的一个特殊的目的是提供这样一种反应器,该反应器非常适用于在H2中转化天然气成为合成气再成为柴油燃料。
根据本发明,提供了一种固/液油浆反应设备,其包括:用来容纳油浆的反应器;与油浆接触并确定滤液区的过滤器,该过滤器分离油浆并具有一个滤液产物的出口;用来产生一个横过过滤器的平均压差的设备;用来产生平均压差上下升降或波动的设备;以及用于将气体反应物或其他组分以气泡形式加入到油浆中的设备。
这样一种系统相当简单然而有效,通常认为特别成问题的分离步骤是在不是非常复杂的情况下和在适当的操作条件下进行,并且过滤器是自身清洗的。
优选的是,该压差是由浸在反应器油浆中的过滤器产生的静压所产生的。优选的是,油浆反应器中油浆上面的空间和滤液段中的滤液上面的空间之间的联通避免了产生的压差超过相应的静压。上述两个空间的联通可通过在油浆部分和滤液部分之间延伸并与每个部分相通的管子来实现。压力的升降和波动可通过反应器中油浆的湍流运动来产生。压力的升降和波动也许可以通过对滤液部分的共振作用优选通过管子来传递或增强。
优选的是,横过过滤器的压差的升降或波动的振幅或大小大约与静压差的平均值是相同的或更大。优选的是横过过滤器的平均压差应保持在相当低的水平,一般小于5毫巴(500Pa)。气体接触管除了起到油浆上面的气相和过滤器的内部之间的联通作用外,还提供了一个简易的气体。放出管路,该气体已穿过过滤器薄膜,另外已截留在滤液部分。
气体产物或组分可用任何常规方法放出,例如通过反应器的分开的出口或简单地通过管而放出。进行的实验得到如果气体接触管关闭或严重阻塞,则过滤器也将迅速变得阻塞起来。当然,该接触管将限制横过过滤器的压力降,因此避免了不希望的和破坏性的压力聚积,另外,当反应器内部和出口端之间存在相当大的压力降时,可能会发生上述的压力的聚积。
反应装置可包括将脉冲压力施加给滤液区,或者直接施加给滤液、或者施加给滤液上面的气体空间的设备。优选的是,该脉冲压力是通过汽缸中的往复活塞的作用而提供。该设备可代替上述管子或作为附件。
优选的是,过滤器是以过滤器单元的形式以内部确定滤液区,并且其包括一个过滤器滤芯以将滤液区和油浆区分开。优选的是,过滤器滤芯通常是圆筒形的,并且在使用中其轴心通常是垂直的,尽管其与垂直面可倾斜10°或30°。过滤器滤芯可以位于反应容器中或反应容器的分支部分中,在该反应容器中使至少部分油浆相循环。优选的是,过滤器滤芯包括一个细网状的筛,螺旋绕制的细丝,细的垂直细丝或烧结的金属颗粒。过滤器滤芯材质和催化剂优选是这样选择的,以致过滤器滤芯中的最大孔或孔径与催化剂粒径具有相同的数量级。催化剂粒径优选不小于孔径的一半。然而,催化剂粒径可大于孔径为相同量级或更小的最大孔径。用于加入气体反应物或组分的设备可包括优选位于反应器底部的任何合适的设备,例如泡罩塔板,许多喷嘴、多孔塔板等。反应物可以是例如来自天然气转化的CO和H,产物可以是甲醇和高级烃类。
压力升降值可以大约为压差,例如为压差的10至200%,压差的实际值可以是1至1000毫巴,优选2至50毫巴。
压力升降可通过反应器中油浆的湍流流动和/或过滤器滤芯外边的气泡上升来提供,这些气泡本身可以产生湍流流动状态。
反应器优选装有液体反应物或组分的入口和/或出口。过滤器单元设备完全或部分地装有滤液,因此,过滤器单元设备的出口可与该过滤器单元设备的顶部上面的滤液部分的管子连接。另外,滤液部分的出口可以包括一个用于测定滤液部分中滤液高度的管子。过滤器单元设备可以是可垂直调整的,优选的滤液高度可根据反应器来调节。
优选的是,反应器装有传热设备,该传热设备可包括许多垂直安装的用于循环传热介质的管子。
当然,反应器可包括许多过滤单元。
本发明特别适用于将天然气(甲烷)转化成高级烃燃料的方法,该方法包括先将甲烷燃烧转化生成一氧化碳和氢,用费-托合成法将CO和H催化转化成高级烃燃料例如液体石蜡,然后分离和/或裂化这些产物以生成所需范围烃类。
当用这种方法生产柴油燃料时,该柴油燃料在其质量和性能方面都比常规柴油优越的多。首先,它不含有硫。这一点从环境角度来说是重要的。其次,它具有很高的十六烷值,因此,能够与低级柴油馏分掺和以生产满足高级范围标准的产品。第三,它实际上不含有当燃烧时产生油烟的有害化合物,并且几乎不需要添加剂在低温下使用也没有问题。
本发明可用各种方式实施,下面参考附图用实施例的方式对一些实施方案进行说明。
图1是用于进行本发明方法的三相油浆反应器的剖面简图;
图2是显示达到压力波动的另一种系统的反应器部分的简化的剖面简图;
图3、4和5是类似于图2的显示调节横过过滤器的压差的三种方式的示意图;和
图6和7是另外两种实施方案。
图1中的反应器11包括确定反应器11的外壳12和在外壳12中的过滤器设备13。外壳12的底部有一个气体入口14,在合成气转化过程中该气体入口可构成反应物入口。在气体入口14的上面有气体输送设备如可透气的多孔板15,该板支撑着反应器11中的油浆16,在外壳12的顶部有一个气体出口17。气体出口17由节流阀或阀18控制。该外壳还有一个油浆的入口19和出口21。
过滤器设备13包括一个与油浆16接触的通常为垂直的圆筒形过滤器滤芯22,该过滤器滤芯是以细网状的筛子形式,虽然其另外可以包括螺旋绕制的金属细丝、烧结的金属颗粒或窄的分开的细的垂直细丝。其安装一个立管23形式的恒位面设备,它的上端在过滤器设备13顶部以下。管23通到滤液出口24,其依次通到收集器25并到出口阀26。管27从管23的顶部之上的过滤器设备13内的空间28延伸到油浆16之上的反应器11顶部之内的空间29。管27上的开口31连接两个空间28和29。
在操作时,气体反应物通过入口14和板15引入到反应容器11。反应物在油浆16中形成气泡,气泡向上通过过滤设备13。油浆16由液相反应产物和细分散形式的催化剂组成。气体反应物当它们与催化剂接触时就反应,因此加入到油浆中的产物中。
同时,该产物通过过滤器滤芯22形成没有催化剂的产物滤液32。所有气体产物和未反应的反应物可以通过出口17排出,然后进行处理和/或循环。产物滤液32通过恒位面设备23和出口24离开过滤器设备13,并收集到收集器25中以控制连续或周期性排出。
油浆16和产物滤液32之间的液面差由恒位面设备确定,使越过过滤器滤芯22形成压差,这有助于输送该液体产物通过过滤器滤芯22。
可以预期,在这些条件之下,催化剂会堵塞过滤器滤芯,但是,发现只要压差不太大,就不会出现这种情况。引入的反应物与气体空间28、29连通一起,并结合反应器容器11中通常的湍流状态,可导致横过过滤器滤芯22的压差波动,这样依次使液体流波动通过过滤器滤芯22,起到抑制堵塞的作用。这种情况可以通过使气泡运动通过过滤器滤芯22的表面而得以加强。
另一实施方案示于图2。在这种情况下,过滤器设备41没有连接反应器中的空间28和29(未画出)的管27,代替的是气缸和活塞组合体42连到空间28。通过往复活塞产生脉动压力,使横过过滤器滤芯22的压差形成所需的波动。当然,这种安排可以连同图1所示的实施方案使用。油浆和滤液上面的空间之间的连通可以通过一个带有限制压力脉冲传递到油浆上面的空间的油门或节流阀的管(未画出)来提供,另外,该管往往会消除往复的活塞的净影响。尽管如此,该管还会控制该静压差。
恒位面设备23可以制成是可调的,以便提供一个高于越过过滤器滤芯22的压差的控制范围。可以达到这个作用的三种方式示于图3、4和5中。
在图3的过滤器设备51中,把立管52和管53以相对于过滤器设备51可滑动的形式安装。在图4的过滤器设备61中,立管62以相对于过滤器设备61可滑动的形式安装,但管63相对于过滤器设备61而固定。在图5的过滤器设备中,管73固定,而立管72可滑动地装在一个固定的套筒74中。于是,滤液32的高度当其升高或降低时保持与过滤器设备71相对固定。
图3-5所示的各种变形可以与图1或图2所示的实施方案相组合。
在图6所示的反应器81中,过滤器设备83的出口84有一个向上的弯管85,以保证过滤器设备83充满液体。在图7所示的反应器91中,有一个管97把反应器中的气体空间与滤液连通。出口管94延伸到过滤器设备93的底部,出口管94和反应器中的空间之间有一个任意的连通管96。该连通管96往往会防止任何虹吸效应,并允许留在滤液中的任何气体溢出。另外,过滤器设备93要充满滤液。
在所有说明性的实施方案中,反应器的几何形状、连通设备(例如管27)和滤液截面可以改变大小,以便通过猛烈的类共振效应使压力波动最佳化。
现在用下面的实施例进一步说明本发明,实施例是用实验室规模进行的。
实施例1
将一根直径4.8cm,高约2m的不锈钢管装满烃液体和细粉状催化剂,该管按油浆泡罩塔通过鼓气泡到油浆中的方法操作。
过滤器设备放在反应器的上部。过滤器设备用Company pressmetall Krebs
ge GmbH生产的SiRa不锈钢烧结的金属圆筒R20型制成。过滤器设备的外径为2.5cm,高度为25cm,平均孔径为20μm。
在该特殊试验中,反应器中装入油浆,油浆由聚α-烯烃液体和约10%(重)细粉状氧化铝载钴催化剂组成,催化剂粒径为30-150μm。让气泡通过液体使催化剂保持悬浮状态。该气体是H2、Co和N2的不同组成的混合物,并以表观气体速度为4cm/S加入。反应器中的温度是230℃,压力是30巴(3×106帕)。
油浆中滤液的高度调节到阀以上约一半的位置。
反应器中费-托反应形成的液体通过过滤器设备回收。另外,加到反应器中的聚α-烯烃液体也通过过滤器设备回收。回收的液体为320-2.5g/h,其取决于液体产物的形成速度和烃液体的加入速度。该试验持续约400小时,通过过滤器设备回收的液体总量为30升。在试验中反应器中液体的量是固定的,没有观察到液体中有什么颜色表明存在固体颗粒。
实施例2
在直径22cm,高2.5m的玻璃管中装入烃液体C Monsa-nto传热流体,MCS 2313)和细氧化铝粉(平均粒径约75μm),氧化铝的含量为约15%(重)。按油浆泡罩塔(SBC)用气体鼓泡通过油浆的方法操作该管。
过滤器设备在油浆相上面的气体空间和产物相上面的气体空间之间没有连通管,该过滤器设备是放在SBC的上部。过滤器设备是用Sintermefallwerk Rrebs
ge GmbH生产的SiKa fil10不锈钢烧结的金属圆筒制成。该烧结圆筒外径为2.5cm,高为20cm,平均孔径为10μm。
在该特定的试验中,油浆面控制在烧结圆筒的顶部,测定SBC中的压力幅度是6毫巴,越过烧结金属壁的压降大约为3-4毫巴(300-400帕)。油浆的温度为20℃,压力是1巴(105帕),气体速度约为6cm/S。
在实验开始,通过烧结金属圆筒的滤液流速为约1000毫升/分。4小时后,流速降到0,由于在油浆一边的烧结金属壁堵塞。
当在设备中进行类似的试验时,其中用一段管作为连接管连通气体空间,开始的流速基本保持在整个试验的相同值上。
Claims (23)
1、固/液油浆反应设备,其包括用于容纳油浆区中的油浆(16)的反应容器(11);和用于将气体组分以气泡形式加入到油浆中的设备,其特征在于:包括一个与油浆(16)接触的确是与油浆区分开的滤液区的过滤器,并且该过滤器有一个滤液产物(32)的出口(23);产生横过该过滤器的平均压差的设备;和引起平均压差上下升降或波动的设备。
2、根据权利要求1的反应设备,其特征在于压差是由浸于反应器油浆中的过滤器(13)产生的静压所产生的。
3、根据权利要求1或2的反应设备,其特征在于压力的升降或波动是由油浆区中的油浆(16)的湍流运动所产生的。
4、根据上述任一权利要求的反应设备,其特征在于油浆区上面的气体空间(29)与滤液区中的滤液(32)连通或与滤液区(32)上面的任何气体空间(28)连通。
5、根据权利要求4的反应设备,其特征在于所述的连通是由在油浆区和滤液区之间延伸并与这两个区相通的管(27)提供。
6、根据上述任一权利要求的反应设备,其特征在于横过过滤器(13)的压差的升降或波动幅度大约与平均值相同或更大。
7、根据上述任一权利要求的反应设备,其特征在于还包括一个气体产物或组分离开反应容器(11)的出口(17)。
8、根据上述任一权利要求的反应设备,其特征在于提供向滤液区施加脉冲压力的设备(42)。
9、根据权利要求8的反应设备,其特征在于所述的脉冲压力是由气缸(42)中往复的活塞的作用而提供的。
10、根据上述任一权利要求的反应设备,其特征在于过滤器(13)通常是圆筒形并且在使用中其轴心通常是垂直的。
11、根据上述任一权利要求的反应设备,其特征在于过滤器(13)位于反应容器(11)中。
12、根据权利要求1至7之一的反应设备,其特征在于过滤器(13)安装在反应容器(11)的分枝设备中,其中使至少部分油浆相循环。
13、根据上述任一权利要求的反应设备,其特征在于过滤器(13)是以过滤器单元的形式内部确定滤液区,并且该过滤器包括分开滤液区和油浆区的过滤器滤芯(32)。
14、根据上述任一权利要求的反应设备,其特征在于过滤器滤芯(22)包括细网状的筛子、螺旋绕制的细丝、细的垂直细丝或烧结的金属颗粒。
15、根据上述任一权利要求的反应设备,其特征在于用于加入气体反应物或组分的设备包括在反应容器(11)的底部的多孔板(15)。
16、根据上述任一权利要求的反应设备,其特征在于反应容器(11)装有可任意含有分散的颗粒物质如细分散的催化剂的液体反应物或组分的入口(19)和/或出口(21)。
17、根据上述任一权利要求的反应设备,其特征在于过滤器(13)准备全部或部分充装滤液产物。
18、根据权利要求17的反应设备,其特征在于滤液区的出口包括一个用来确定滤液区(32)中滤液高度的管子(23)。
19、根据上述任一权利要求的反应设备,其特征在于滤液高度可根据反应容器(11)来调节。
20、根据上述任一权利要求的反应设备,其特征在于过滤器(13)安装为可垂直调节的。
21、根据上述任一权利要求的反应设备,其特征在于反应容器(11)装有传热设备。
22、根据权利要求21的反应设备,其特征在于传热设备是由供传热介质循环的许多垂直安装的管子提供。
23、根据上述任一权利要求的反应设备,其特征在于反应容器中有许多过滤器。
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-
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- 1992-02-25 GB GB929203958A patent/GB9203958D0/en active Pending
-
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- 1993-02-24 DE DE69309910T patent/DE69309910T2/de not_active Expired - Lifetime
- 1993-02-24 MY MYPI93000333A patent/MY111389A/en unknown
- 1993-02-24 WO PCT/NO1993/000030 patent/WO1993016795A1/en active IP Right Grant
- 1993-02-24 US US08/021,898 patent/US5407644A/en not_active Expired - Lifetime
- 1993-02-24 RU RU94040725A patent/RU2120820C1/ru active
- 1993-02-24 AU AU36495/93A patent/AU664429B2/en not_active Expired
- 1993-02-24 AT AT93905652T patent/ATE151662T1/de not_active IP Right Cessation
- 1993-02-24 DZ DZ930018A patent/DZ1665A1/fr active
- 1993-02-24 EP EP93905652A patent/EP0627958B1/en not_active Expired - Lifetime
- 1993-02-24 CA CA002130660A patent/CA2130660C/en not_active Expired - Lifetime
- 1993-02-24 CN CN93103456A patent/CN1037414C/zh not_active Expired - Lifetime
- 1993-02-24 DK DK93905652.9T patent/DK0627958T3/da active
- 1993-09-19 SA SA93140197A patent/SA93140197B1/ar unknown
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101940903A (zh) * | 2010-05-04 | 2011-01-12 | 姚光纯 | 一种通过脉冲压力波来改善催化反应的工艺方法 |
CN106179167A (zh) * | 2016-07-26 | 2016-12-07 | 西北大学 | 一种具有强化传热的气‑固相连续反应装置 |
CN106179167B (zh) * | 2016-07-26 | 2019-06-21 | 西北大学 | 一种具有强化传热的气-固相连续反应装置 |
CN113289507A (zh) * | 2021-05-10 | 2021-08-24 | 内蒙古旭阳新材料有限公司 | 一种湿铝粉生产设备及方法 |
CN113289507B (zh) * | 2021-05-10 | 2023-02-03 | 内蒙古旭阳新材料有限公司 | 一种湿铝粉生产设备及方法 |
Also Published As
Publication number | Publication date |
---|---|
DE69309910T2 (de) | 1997-07-24 |
CN1037414C (zh) | 1998-02-18 |
AU3649593A (en) | 1993-09-13 |
NO943121D0 (no) | 1994-08-24 |
RU2120820C1 (ru) | 1998-10-27 |
EP0627958B1 (en) | 1997-04-16 |
SA93140197B1 (ar) | 2006-11-12 |
US5407644A (en) | 1995-04-18 |
AU664429B2 (en) | 1995-11-16 |
NO300119B1 (no) | 1997-04-14 |
CA2130660C (en) | 2004-03-30 |
ATE151662T1 (de) | 1997-05-15 |
DZ1665A1 (fr) | 2002-02-17 |
CA2130660A1 (en) | 1993-08-26 |
NO943121L (no) | 1994-08-24 |
RU94040725A (ru) | 1996-07-27 |
GB9203958D0 (en) | 1992-04-08 |
DK0627958T3 (da) | 1997-10-27 |
DE69309910D1 (de) | 1997-05-22 |
MY111389A (en) | 2000-03-31 |
WO1993016795A1 (en) | 1993-09-02 |
EP0627958A1 (en) | 1994-12-14 |
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