CN1328485A - 连续进行气-液、液-液或气-液-固反应的反应器 - Google Patents
连续进行气-液、液-液或气-液-固反应的反应器 Download PDFInfo
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Abstract
本发明涉及一种结构形式为高的圆柱并用作实施气-液、液-液或气-液-固反应的反应器(1),它有在上反应器区安置的方向朝下的射流喷嘴(2),经喷嘴送入原料和反应混合物;优选在下反应器区有排出口(3),反应混合物经此排出口经外循环以泵(P)重新送入射流喷嘴(2),在反应器(1)中安置同心导管(4),该导管延伸除反应器端头外的反应器(1)的整个长度,其截面面积为反应器(1)的截面面积的十分之一到二分之一的范围内;在导管(4)上端之上的射流喷嘴(2),优选按相距八分之一到一个导管直径定位或者浸入导管(4)的深度达数个导管直径;在环形空间组合有换热器,特别是两底之间焊接换热管的换热器,这些换热管宜与导管平行布置。
Description
本发明涉及一种连续进行气-液、液-液或气-液-固-反应的反应器;方法及其用途。
在多种化学过程中,气-液传质和导热效率是速度决定步骤。为了改善相界面的传质,曾建议对这类反应采用喷射器,即利用高速液体射流的动能使气相吸入和分散。通过高的能量引入,在喷射器中形成高湍流和大剪切力,其结果使气体分散为很小的气泡,即在单位体积内形成很大的气-液界面。文献曾经报导,喷射器单位体积内的相界面值为40000-70000m2/m3,而除喷射器外的所有体系中只有500-2500(参见Chem.Eng.Sei.(化学工程科学)卷47,No.13/14pp35577,1992)。
采用喷射器进行气-液反应或气-液-固-反应的设备的例子如DE-A-4323687报导的回路-文丘里-反应器与通过相应的聚硝基化合物的催化氢化的制造芳香双胺或聚胺的连续过程相组合。在回路文丘里-反应器的一端安置喷射器,即带固定排列的脉冲交换管和扩散器的双物流射流喷嘴,其中液态的泵送混合物与气态的反应剂(氢)发生接触。喷射器通过气-液相分离界面以一定的结构长度浸入液体之中。在喷射器本身中,气体分散效率高,然而在其余的反应器体积内并不如此,而在流动行为和停留时间方面具有纯粹的气泡柱特性。在这除喷射器外的反应体积内的不规则的小空间和大空间的涡旋使悬浮态的催化剂传质效率较低。反应器中的气体含量的调节主要取决于物料的性质,较低程上还取决于初始分散。释放的反应热将通过用泵进行循环的外换热器导出。
EP-A-263 935报导了实施强放热反应的搅拌釜式反应器,其中释放的热经场式管换热器在其产生处就地导出。场管换热器系指具有平行双套管管束的换热器,其中突出于反应器空间的外管端是封闭的,而内管的相应端却是开口的,这样,热载体经过安置在反应器之外的导入空间流入内管,而经内管和外管之间的空间以及导出空间流出。它们的特征是传热面积和反应空间体积的比值高,因而对于释放的反应热的导出将很有效。但这个方法的缺点是不能保证相的良好混合,其结果使不可控制的副反应增强,效率降低,冷却表面被树脂状化合物和/或催化剂组分覆盖。
因此,本发明的目的在于提供一种气-液、液-液或气-液-固反应用的反应器,这种反应器保证在整个反应器体积内有剧烈的相混合,从而能提高经济性和改进空间-时间-产率。
在一个实施方案中,本发明的目的是保证反应器在很大程度上是等温的,即保证反应器的高度方向上的温度梯度很小。
其次,本发明的目的是提出一种应用本发明反应器进行气-液、液-液、或气-固-反应的连续方法。
本发明从一种用于气-液、或气-液-固-反应器出发,该反应器的结构形式是高的圆柱形,上反应器区布置方向朝下的射流喷嘴,经喷嘴送入原料和反应混合物,而在下反应器区宜有抽出口,反应混合物经抽出口和藉助泵经外回路重新送入射流喷嘴。
解决方案的特征在于,在反应器中安置一同心导管,该导管基本上延伸除反应器端面之外的整个反应器长度,而其戴面面积占反应器截面面积的十分之一到二分之一;该喷嘴安置在导管上端上面,其距离为八分之一的导管直径至导管直径,或者浸入该导管,其深度可达数个导管直径;并且在环形空间组合换热器,特别是在上底和下底间有焊接换热管的换热器,该换热管宜与导管平行布置。
由此发现,基本上或完全排除了传质限制和传热限制,从而使整个反应在纯动力学控制下进行。
本发明的解决方案是使绝大部分反应混合物呈一种向内的循环流,而只有少量用于循环流运行所必需的反应混合物由外部泵送,这种解决方案有利于节能。
在整个反应器体积中,流动条件是非常明确的,即是说,反应器的重要设计数据:流速、气体含量、反混、混合时间和停留时间特性皆能足够准确地掌握,因此,本发明的反应器可直接放大。
术语射流喷嘴按众所周知系指一种沿流动方向呈锥形的管;射流喷嘴可设计为三物料或双物料的喷嘴,亦可能设计成脉冲交换管和扩散器或者设计成单物料喷嘴。
在利用单物料喷嘴时,可补充将一种或多种气态反应物导入反应器顶部的气体空间或经过适宜的设备,优选经过一根或多根,特别是1-3根环管导入导管和反应器内壁之间的环形空间,该设备有许多孔,该孔特别是分布在下反应器空间或沿反应器的高度上分布。气体导入亦可在挡板之下或直接进入单物料喷嘴上面的气体空间。通过鼓泡产生的驱动支持对内循环流动。
反应混合物的排出口原则上可布置在每个任意的反应器高度上,优选布置在下反应区,特别优选布置在反应器底。部分反应混合物藉助泵经排出口抽出,还可经固体物,特别是悬浮的催化剂的分离(例如采用横流过滤器)之后重新送入反应器上部的射流喷嘴。
术语导管系指直立圆柱形反应器中同心安置的内管,该内管几乎占据了整个反应器的长度,但反应器端部除外。导管的上端总是被液体覆盖,即应位于上气体分离空间以下,而且该空间按照本发明应占反应器总体积的3-15%,特别是反应器总体积的5-7%。导管的上端应与方向朝下的并优选同导管一样垂直安置的射流喷嘴保持距离。通过喷嘴/导管与内部充满液位的相对位置可调节反应混合物中的气体含量。
射流喷嘴优选到达气-液分离界面区。在这种情况下反应体积中气体含量可通过内液位在一定限度内的升高或下降进行变化。例如喷嘴通过内液位的升高浸入液体,这样反应混合物中的气体含量将取较小的值,相反通过内液位的降低至射流喷嘴口以下则可将较大量的气体抽入反应体积。
导管所具有的截面宜为反应器截面的十分之一到二分之一的范围内。导管的下端终止在反应器区的下端,优选终止在反应器圆柱形端区。
在导管和反应器内壁之间的环形空间中有一换热器成为其一体化的组成部分,特别是在两底之间有焊接换热管的换热器,其换热管平行于导管布置。通过这种方式特别保证用于有大热效应反应的反应器的高等温性,即是说,沿反应器高度的温度梯度很小,因为反应热在其产生的地方即被导出。而且相对外循环冷却来说此过程的安全性得到改善,因为反应器冷却甚至在外循环的泵发生事故时亦能照样进行。在冷却水供应发生事故时,冷却还能进行到换热器中的全部冷却水蒸发为止。
同时可能在环形空间组合另一种结构的换热器,特别是场式管-换器热。
优选方式的反应器所具有的细长比,即长度(1)与直径(d)之比,为3-10,优选6-10。反应器能有高的细长比是基于有朝向的内部的循环流动。高的细长比的后果可使反应器体积中的气体含量随反应器中液体的内液位的小变动而变动,因为通过这种方式射流喷嘴和气-液-分离界面的相对位置发生变化。
导管和反应器的直径之比优选在0.25-0.5范围内,特别优选0.28-0.33范围内。
在优选方案中,在下反应器区,即在导管的下端之下,优选相距1-2个导管直径处以基本垂直于导管的方式安置挡板。挡板的形状宜为盘形,其直径大于导管的直径,小于反应器的内径,其厚度宜通过所选的金属材料的机械强度确定,即在大约5-10mm范围内。挡板的功能除折流之外还在于避免气泡夹带于入外回路并使泵受到损害。
本发明还提出一种在上述反应器中实施气-液或气-液-固-反应的连续方法,其中反应混合物的绝大部分,相当于外部泵送反应混合物体积流的2-30倍,优先5-10倍的内循环流从上向下流过导管,并从下向上流过导管和反应器内壁之间的环形空间。内循环流系指反应混合物在反应器内部的一种循环;它由安置在上反应器区的,朝下的射流喷嘴产生的液体射流驱动。这种朝下的液体射流在导管中产生一种向下的物流,该物流在离开导管之后在下反应器区折流并在导管和反应器内壁之间的环形空间向上流动。在导管的上端液体通过驱动射流重新被吸入,与此射流混合并再次向下折流。循环流动可通过向导管和反应器内壁之间的环形空间添加一种或多种气态反应剂以充分利用气体的浮力来促进。
以气泡形式在两相物流中存在的循环气体通过液体射流在导管的上端即近射流喷嘴处分散,通过这种方式达到很高的传质系统和单位体积内很高的相界面。其次,通过液体射流,该气体从上反应器区的气体分离空间被吸入并分散。
本发明的设备和方法适用于特别强放热的气-液、液-液或气-液-固-反应,尤其适用于悬浮催化氢化、有机氧化、乙氧基化、丙氧基化或羟醛缩合。
将本发明的方法和设备用于上述反应可得到较好空间-时间产率、缓和反应条件,特别是对压力以及有时对温度、减小反应体积、通过节能降低加工费用、还可能降低投资费用以及改进安全。
下面将根据附图和实施例对本发明作较详细的阐述。
唯一的附图表示通过本发明的反应器1的长度方向的剖面,在上反应器区有射流喷嘴2,原料和反应混合物经喷嘴送入,在下反应器区有排出口3,反应混合物经此排出口藉助于泵P经外循环重新送入射流喷嘴2。在反应器1中安置同心导管4,该导管延伸除反应器端头外的大部分反应器长度。附图表明,在导管4下端之下宜装挡板7。同样宜装换热器,该换热器在图中为所谓的场示管-换热器,它带有冷却剂K的导入空间5和导出空间5’以及换热管6。按照另一优选实施方案,换热器的形式可为两底间焊接换热管的换热器,换热管宜平行于导管4安置。
实施例子
图1所示的反应器的反应体积约为0.05m3,它具有36根平行安置的场示管,这些场示管总的冷却面积约为2.5m3,进入的冷水流约为1m3/h,温度约为35℃,藉助于剂量泵将30.3kg/h的丙醛在75℃下以快速流动的混合物中送入反应器,该混合物约含84%的丙酸,大约15%的丙醛和最大为1%的副产物,特别是有机酸和醇类。通过同时加入31Nm3/h的空气,将反应器的压力调到23bar。为了保持循环流动,将2.5m3/h的体积物流转入外部产品循环。在射流喷嘴中的压力比反应器压力大3bar,其比动力输入约为5kW/m3。
反应几乎在等温条件下进行,因为反应热在其产生处即被导出。反应器下面三分之一处的最高温度为76℃。
38.8kg/h的反应混合物分物流被连续导出,其组成为84%丙酸,大约15%丙醛和小于1%副产物,特别是有机酸和醇类。这相当于空间-时间产率为650kg/m3h。未转化的丙醛可用加热装置,特别是蒸馏分离或者在由两个相互串联的本发明的反应器组成的级联中并附加采用反应管的条件下继续反应。丙醛的总转化率在采用两个本发明反应器级联的情况下为98.7%,选择性约为96%。
Claims (8)
1.一种结构形式为高的圆柱并用作实施气-液、液-液或气-液-固反应的反应器(1),它有在上反应器区安置的方向朝下的射流喷嘴(2),经喷嘴送入原料和反应混合物;优选在下反应器区有排出口(3),反应混合物经此排出口经外循环以泵(P)重新送入射流喷嘴(2),其特征在于,在反应器(1)中安置同心导管(4),该导管延伸除反应器端头外的反应器(1)的整个长度,其截面面积为反应器(1)的截面面积的十分之一到二分之一的范围内;在导管(4)上端之上的射流喷嘴(2),优选按相距八分之一到一个导管直径定位或者浸入导管(4)的深度达数个导管直径;在环形空间组合有换热器,特别是两底之间焊接换热管的换热器,这些换热管宜与导管平行布置。
2.权利要求1的反应器(1),其特征在于,射流喷嘴(2)为单物料喷嘴;有时还装有导入一种或多种气态反应剂的设备,优选为一根或多根,特别是1-3根环管,它具有许多特别在下反应器区或沿反应器高度分布的孔,该设备安置在导管(4)和反应器内壁之间的环形空间内。
3.权利要求1的反应器(1),其特征在于,射流喷嘴作为三物料或双物料喷嘴构成。
4.权利要求1-3之一的反应器(1),其特征在于,细长比1/d为3-10,优选6-10。
5.权利要求1或4之一的反应器(1),其特征在于,导管(4)的直径和反应器(1)直径之比在0.25-0.5范围内,特别优选在0.28-0.33范围内。
6.权利要求1-5之一的反应器(1),其特征在于,在导管(4)下端之下的反应器区安置挡板(6),优选以相距约为一个导管直径定位。
7.一种用于在权利要求1-6之一的反应器中实施气-液或气-液-固-反应的连续方法,其特征在于,主要部分反应混合物,即相当于外部泵送的反应混合物体积流的2-30倍,优选5-10倍以内循环流动的方式从上向下流过导管(4),并从下向上流过导管(4)和反应器内壁之间的环形空间。
8.权利要求1-6之一的设备或权利要求8的方法在特强放热的气-液或气-液-固反应中的应用,优选用于氢化、氧化、乙氧基化、丙氧基化、加氢甲酰基化或羟醛缩合。
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CN104826558A (zh) * | 2015-05-15 | 2015-08-12 | 北京神雾环境能源科技集团股份有限公司 | 用于乙炔选择性加氢制乙烯的浆态床反应器及反应系统 |
CN108473406A (zh) * | 2015-12-22 | 2018-08-31 | 巴斯夫欧洲公司 | 圆柱状反应器及其用于连续氢甲酰化的用途 |
CN108473406B (zh) * | 2015-12-22 | 2021-10-15 | 巴斯夫欧洲公司 | 圆柱状反应器及其用于连续氢甲酰化的用途 |
CN106636650A (zh) * | 2016-12-12 | 2017-05-10 | 中南民族大学 | 旋流鼓泡塔三相反应器 |
CN106636650B (zh) * | 2016-12-12 | 2019-04-26 | 中南民族大学 | 旋流鼓泡塔三相反应器 |
US10363535B1 (en) | 2018-04-18 | 2019-07-30 | Shanghai Yankuang Energy R&D Co., Ltd. | Gas-liquid-solid three-phase slurry bed industrial reactor capable of achieving continuous operation |
CN110411269A (zh) * | 2018-04-27 | 2019-11-05 | 赢创德固赛有限公司 | 用于控制反应器的温度的设备 |
CN111167385A (zh) * | 2020-01-10 | 2020-05-19 | 天津大学 | 利用醛原料和空气制备酸的喷射型气液反应器 |
CN113209930A (zh) * | 2021-05-26 | 2021-08-06 | 中国海洋石油集团有限公司 | 一种醛缩合反应设备及反应方法 |
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EP1140349B1 (de) | 2002-08-07 |
WO2000030743A1 (de) | 2000-06-02 |
DE59902306D1 (de) | 2002-09-12 |
US6838061B1 (en) | 2005-01-04 |
DE19854637A1 (de) | 2000-05-31 |
KR20010110300A (ko) | 2001-12-12 |
JP4891480B2 (ja) | 2012-03-07 |
JP2002530189A (ja) | 2002-09-17 |
CN1191882C (zh) | 2005-03-09 |
EP1140349A1 (de) | 2001-10-10 |
KR100634922B1 (ko) | 2006-10-17 |
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