CN111659141A - Falling film distillation system for separating dichloromethane and white oil - Google Patents
Falling film distillation system for separating dichloromethane and white oil Download PDFInfo
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Abstract
本发明涉及二氯甲烷和白油分离用的降膜式蒸馏系统,其包括蒸馏塔和蒸发器,蒸馏塔包括上塔身和下塔身;蒸发器包括分别设置在上塔身顶部和底部且与上塔身周向内壁构成闭合蒸发腔的上管板和下管板、多根蒸发管、以及蒸汽供应组件,其中多根蒸发管之间相互隔开设置,且多根蒸发管的上端口与进液管相连通、下端口与下塔身所形成腔体相连通;蒸馏系统还包括能够与出气管相连通的气液分离器。本发明采用降膜式蒸发器,物料停留时间短,蒸汽工作压力小且蒸汽耗量低,同时蒸发后的白油浓缩液温度低、色泽浅、纯度高,蒸发出的二氯甲烷气体经过分离和后续冷凝分水后,二氯甲烷中白油含量20ppm以内。
The present invention relates to a falling film distillation system for dichloromethane and white oil separation, which comprises a distillation column and an evaporator, wherein the distillation column includes an upper column body and a lower column body; The upper tube plate and the lower tube plate, a plurality of evaporation tubes, and a steam supply assembly that form a closed evaporation chamber with the circumferential inner wall of the upper tower body, wherein the plurality of evaporation tubes are spaced apart from each other, and the upper ports of the plurality of evaporation tubes are It is communicated with the liquid inlet pipe, and the lower port is communicated with the cavity formed by the lower tower body; the distillation system also includes a gas-liquid separator which can be communicated with the gas outlet pipe. The invention adopts a falling film evaporator, the material residence time is short, the steam working pressure is small and the steam consumption is low, and the evaporated white oil concentrate has low temperature, light color and high purity, and the evaporated dichloromethane gas is separated after separation. After the subsequent condensation and water separation, the content of white oil in dichloromethane is within 20ppm.
Description
技术领域technical field
本发明属于蒸馏领域,具体涉及一种二氯甲烷和白油分离用的降膜式蒸馏系统。The invention belongs to the field of distillation, and in particular relates to a falling film distillation system for the separation of methylene chloride and white oil.
背景技术Background technique
目前,在油品精制领域,湿法锂电池隔膜生产工艺中需要回收二氯甲烷、白油,其中多采用白油作为成孔剂,成膜后用二氯甲烷将其中的白油萃取出来,形成了二氯甲烷和白油混合液,混合液中含5%白油,及95%二氯甲烷。该工艺中白油和二氯甲烷大量使用,因此对混合液进行分离处理,从而对二氯甲烷和白油进行回收和循环使用,是降低锂电池隔膜的生产成本的关键。At present, in the field of oil refining, dichloromethane and white oil need to be recovered in the production process of wet-process lithium battery diaphragm. Among them, white oil is mostly used as a pore-forming agent, and the white oil is extracted with dichloromethane after film formation. A mixture of dichloromethane and white oil was formed, and the mixture contained 5% white oil and 95% dichloromethane. In this process, a large amount of white oil and dichloromethane are used, so the separation and treatment of the mixed liquid, so as to recover and recycle the dichloromethane and the white oil, is the key to reducing the production cost of the lithium battery separator.
国内有的采用蒸馏方法,以分离和提纯二氯甲烷和白油,塔顶轻相为分离出二氯甲烷,釜底液为分离出的白油,其主要不足是:会使混合液中的轻组分部分发生氧化,破坏白油结构,对微量水分等极性物质的清除效果不好,白油中二氯甲烷含量过高等,另外蒸汽耗量较高,使得能量过大,二氯甲烷气体温度高,增加冷凝器的冷凝负荷,造成循环水量增大,白油温度过高,白油色泽加深,在脱色时白土用量会提高,增加生产成本,产品指标不好,冷凝后二氯甲烷中白油含量高达400ppm,成品白油中二氯甲烷含量也高达500ppm。Some domestic use distillation methods to separate and purify dichloromethane and white oil, the light phase at the top of the tower is the separated dichloromethane, and the bottom liquid is the separated white oil. The light components are partially oxidized, destroying the structure of the white oil, and the removal effect of polar substances such as trace moisture is not good. The content of dichloromethane in the white oil is too high. High gas temperature will increase the condensation load of the condenser, resulting in an increase in the amount of circulating water, excessive white oil temperature, and deepening of the white oil color. The content of medium white oil is as high as 400ppm, and the content of methylene chloride in finished white oil is also as high as 500ppm.
发明内容SUMMARY OF THE INVENTION
本发明所要解决的技术问题是克服现有技术的不足,提供一种全新的二氯甲烷和白油分离用的降膜式蒸馏系统。The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a brand-new falling film distillation system for the separation of dichloromethane and white oil.
为解决上述技术问题,本发明采取如下技术方案:In order to solve the above-mentioned technical problems, the present invention adopts the following technical solutions:
一种二氯甲烷和白油分离用的降膜式蒸馏系统,其包括蒸馏塔和蒸发器,蒸馏塔沿着竖直方向延伸,且包括上塔身和下塔身,其中进液管位于上塔身的顶部,出液管位于下塔身的底部,出气管位于下塔身的侧上部;A falling film distillation system for separation of methylene chloride and white oil, comprising a distillation column and an evaporator, the distillation column extends along a vertical direction, and includes an upper column body and a lower column body, wherein a liquid inlet pipe is located on the upper At the top of the tower body, the liquid outlet pipe is located at the bottom of the lower tower body, and the air outlet pipe is located at the upper side of the lower tower body;
蒸发器设置在上塔身内,且包括分别设置在上塔身顶部和底部且与上塔身周向内壁构成闭合蒸发腔的上管板和下管板、两端部与上管板和下管板贯穿连通且沿着上塔身的高度方向延伸的多根蒸发管、以及向上塔身所形成蒸发腔提供蒸汽的蒸汽供应组件,其中多根蒸发管之间相互隔开设置,且多根蒸发管的上端口与进液管相连通、下端口与下塔身所形成腔体相连通;The evaporator is arranged in the upper tower body, and includes an upper tube sheet and a lower tube sheet, which are respectively arranged at the top and bottom of the upper tower body and form a closed evaporation chamber with the circumferential inner wall of the upper tower body, and the two ends are connected with the upper tube sheet and the lower tube. A plurality of evaporating tubes connected through the plate and extending along the height direction of the upper tower body, and a steam supply assembly for supplying steam to an evaporation cavity formed by the upper tower body, wherein the plurality of evaporating tubes are spaced apart from each other, and the plurality of evaporation tubes The upper port of the pipe is communicated with the liquid inlet pipe, and the lower port is communicated with the cavity formed by the lower tower body;
蒸馏系统还包括能够与出气管相连通的气液分离器。The distillation system also includes a gas-liquid separator that can communicate with the gas outlet pipe.
优选地,蒸发器还包括设置在上塔身内且用于蒸发管定位的定型板、用于吊装下管板的固定拉杆,其中定型板至少有一块,且每一块定型板与上塔身内壁之间形成供蒸汽流动的通道,固定拉杆与蒸发管平行设置,且上端部固定在定型板上、下端部固定在下管板上。定型板和固定拉杆的设置,不仅能够实现蒸发管在蒸发腔内的定位;而且定型板形成的蒸汽流动通道,改善蒸汽在蒸汽腔内的流动性,以确保蒸发效果。Preferably, the evaporator further comprises a shaping plate arranged in the upper tower body and used for positioning the evaporation tubes, and a fixed tie rod used for hoisting the lower tube plate, wherein there is at least one shaping plate, and each shaping plate is connected to the inner wall of the upper tower body. A channel for steam flow is formed between the two, the fixed pull rod is arranged in parallel with the evaporation tube, the upper end is fixed on the setting plate, and the lower end is fixed on the lower tube plate. The setting of the shaping plate and the fixed tie rod can not only realize the positioning of the evaporation tube in the evaporation chamber; but also the steam flow channel formed by the shaping plate can improve the fluidity of the steam in the steam chamber to ensure the evaporation effect.
根据本发明的一个具体实施和优选方面,定型板有多块,每一块定型板均水平设置,且具有能够贴合在上塔身内壁的贴合侧边、以及与对应侧上塔身内壁断开形成通道的断开侧边,其中多块定型板沿着蒸发管的长度方向上下间隔分布,且所形成的多个通道相对错开设置。在此,通过错开的通道,不仅能够充分的实现蒸汽与蒸发管的接触实现混合液的间接加热,而且能够形成稳定的蒸汽流向,有利于混合的蒸发。According to a specific implementation and preferred aspect of the present invention, there are a plurality of shaping plates, each of which is arranged horizontally, and has a fitting side that can fit on the inner wall of the upper tower body, and has a side edge that is cut off from the inner wall of the upper tower body on the corresponding side. The broken sides of the channel are formed by opening, wherein a plurality of shaping plates are distributed up and down along the length direction of the evaporation tube, and the formed channels are relatively staggered. Here, through the staggered channels, not only can the contact between the steam and the evaporation tube be fully realized to realize the indirect heating of the mixed liquid, but also a stable steam flow direction can be formed, which is beneficial to the evaporation of the mixture.
优选地,多个通道上下间隔,且左右相对错位分布,固定拉杆有两根,且分别将位于通道同侧的定型板和底部的下管板固定串接。Preferably, a plurality of channels are spaced up and down, and are distributed in relative dislocation from left to right, and there are two fixed tie rods, which respectively connect the shaping plate on the same side of the channel and the lower tube plate at the bottom in series.
优选地,二氯甲烷和白油混合液自蒸发管的上部向下流动,蒸汽腔内的蒸汽流向与混合液流向相同,且蒸汽在蒸汽腔内流动并形成负压。不仅能最佳化实现混合液的蒸发,而且在负压下进一步提高气液分离的效果。Preferably, the mixture of dichloromethane and white oil flows downward from the upper part of the evaporation tube, the steam in the steam chamber flows in the same direction as the mixture, and the steam flows in the steam chamber and forms a negative pressure. It can not only optimize the evaporation of the mixed liquid, but also further improve the effect of gas-liquid separation under negative pressure.
根据本发明的又一个具体实施和优选方面,气液分离器为旋液分离器,且位于下塔身外,其中旋液分离器入口与出气管相连通。According to yet another specific implementation and preferred aspect of the present invention, the gas-liquid separator is a hydrocyclone, and is located outside the lower tower body, wherein the inlet of the hydrocyclone is communicated with the gas outlet pipe.
根据本发明的又一个具体实施和优选方面,降膜式蒸馏系统还包括与进液管连通且处于上管板上方的分液腔,该分液腔包括位于上管板上方的分液盘、围设在分液盘周边的围板、以及将围板与上塔身相连接的连接件,其中围板的上端部敞开设置,进液管的下端部伸入分液腔中,分液盘上开设有能够将混合液体均匀分流至下方对应上管口的分流孔。在此,通过分液腔的设置,便于实现混合液体均匀流向每根蒸发管。According to yet another specific implementation and preferred aspect of the present invention, the falling film distillation system further includes a liquid separation chamber connected to the liquid inlet pipe and positioned above the upper tube plate, the liquid separation chamber comprising a liquid separation tray positioned above the upper tube plate, A coaming plate surrounding the perimeter of the liquid separator, and a connecting piece connecting the coaming plate to the upper tower body, wherein the upper end of the coaming plate is open, the lower end of the liquid inlet pipe extends into the liquid separator chamber, and the liquid separator tray The upper part is provided with a distribution hole which can distribute the mixed liquid evenly to the lower corresponding upper nozzle. Here, through the arrangement of the liquid separation chamber, it is convenient to realize the uniform flow of the mixed liquid to each evaporation tube.
优选地,分流孔有多个且分为多组,每一分流孔组对应下方一根蒸发管的上管口的周向分布,且每组分流孔的孔心所形成圆形的圆心设置在下方对应的上管口的中心线上,其中圆形的直径大于上管口的管径,自每组分流孔流出的混合液体分别从下方对应的上管口的周边贴合蒸发管的内壁向下流动。由每组分流孔和蒸发管的对应设置,使得自分流孔流出的液体能够自上管口的周向并贴合蒸发管的内壁下流,以提高蒸发效率。Preferably, there are multiple distribution holes and are divided into multiple groups, each group of distribution holes corresponds to the circumferential distribution of the upper nozzle of an evaporation tube below, and the center of the circle formed by the center of each group of distribution holes is set at On the center line of the corresponding upper nozzle at the bottom, the diameter of the circle is larger than the diameter of the upper nozzle, and the mixed liquid flowing out from each group of flow holes is attached to the inner wall of the evaporation tube from the periphery of the corresponding upper nozzle below. flow down. Due to the corresponding arrangement of each group of flow holes and evaporation tubes, the liquid flowing out from the flow separation holes can flow down from the circumference of the upper nozzle and fit the inner wall of the evaporation tube, so as to improve the evaporation efficiency.
进一步的,多根蒸发管呈环形阵列的方式依次间隔布满在上管板和下管板之间,多组分流孔与多根蒸发管一一对应设置,且相邻两根蒸发管的上管口所对应的两组分流孔之间供用一个分流孔。通过蒸发管的布局,以便于每组分离孔位置的定位,从而达到均匀分流的效果。Further, a plurality of evaporation tubes are arranged in an annular array between the upper tube plate and the lower tube plate, and the multi-component flow holes are arranged in one-to-one correspondence with the plurality of evaporation tubes, and the upper parts of the adjacent two evaporation tubes are arranged at intervals. A shunt hole is provided between the two groups of flow holes corresponding to the nozzle. The layout of the evaporation tubes facilitates the positioning of the positions of each group of separation holes, so as to achieve the effect of even distribution.
优选地,进液管的下端部位于分液盘的上方,且在进液管的下端部还设有喷淋头,其中二氯甲烷和白油混合液自喷淋头流出流量大于自分流孔流出的流量。这样一来,在分液腔内应该形成有一定液位高度,以确保液体自每一个分流孔均匀流出。Preferably, the lower end of the liquid inlet pipe is located above the liquid separator, and the lower end of the liquid inlet pipe is also provided with a spray head, wherein the outflow of the mixture of dichloromethane and white oil from the spray head is greater than the self-splitting hole outgoing traffic. In this way, a certain liquid level should be formed in the liquid distribution chamber to ensure that the liquid flows out from each distribution hole evenly.
此外,降膜式蒸馏系统还包括自上管板的顶部向上延伸的上隔板、自下管板的底部向下延伸的下隔板、以及自下塔身的底部向上延伸且与下隔板对齐设置的延伸板,其中上隔板将上塔身分隔成两个或多个混合液进料区,分液腔对应设有在混合液进料区内,进液管与分液腔一一对应设置,且每一个分液腔对应设有一根进液管;下隔板对应将下塔身的上部分隔成与混合液进料区一一对应的气相区,且下隔板与对齐的延伸板之间隔开设置,气相区下延至延伸板顶部,两个或多个气相区自下隔板和延伸板的隔开处相连通设置,出气管位于气相区且位于延伸板的侧上方;延伸板将下塔身的下部分隔成与气相区相对应的液相区,且每一个液相区对应设有一根出液管。这样设置的目的:就是为了实现多次进出蒸馏塔内且在进入不同蒸发区进行蒸馏工艺的实施,以确保蒸馏效果。In addition, the falling film distillation system also includes an upper baffle extending upward from the top of the upper tube sheet, a lower baffle extending downward from the bottom of the lower tube sheet, and extending upward from the bottom of the lower column body and connected to the lower baffle Aligned extension plates, wherein the upper partition divides the upper tower body into two or more mixed liquid feeding areas, the liquid separation chamber is correspondingly arranged in the mixed liquid feeding area, and the liquid inlet pipe and the liquid separation chamber are one by one. Correspondingly arranged, and each liquid separation chamber is correspondingly provided with a liquid inlet pipe; the lower baffle separates the upper part of the lower tower body into a gas phase area corresponding to the mixed liquid feeding area, and the lower baffle is aligned with the extension The plates are spaced apart, the gas phase zone extends down to the top of the extension plate, two or more gas phase zones are communicated and arranged from the space between the lower partition plate and the extension plate, and the gas outlet pipe is located in the gas phase zone and above the side of the extension plate; The plate divides the lower part of the lower tower body into liquid phase areas corresponding to the gas phase area, and each liquid phase area is correspondingly provided with a liquid outlet pipe. The purpose of this setting is to implement the distillation process in and out of the distillation column multiple times and enter different evaporation zones to ensure the distillation effect.
由于以上技术方案的实施,本发明与现有技术相比具有如下优点:Due to the implementation of the above technical solutions, the present invention has the following advantages compared with the prior art:
本发明采用降膜式蒸发器,物料停留时间短,蒸汽工作压力小且蒸汽耗量低,同时蒸发后的白油浓缩液温度低、色泽浅、纯度高,蒸发出的二氯甲烷气体经过分离和后续冷凝分水后,二氯甲烷中白油含量20ppm以内,此外,结构简单,实施方便。The invention adopts a falling film evaporator, the material residence time is short, the steam working pressure is small, and the steam consumption is low, and at the same time, the evaporated white oil concentrate has low temperature, light color and high purity, and the evaporated dichloromethane gas is separated after separation. After water separation with subsequent condensation, the content of white oil in dichloromethane is within 20 ppm, and in addition, the structure is simple and the implementation is convenient.
附图说明Description of drawings
下面结合附图和具体的实施例对本发明做进一步详细的说明。The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
图1为本发明的蒸馏系统的结构示意图;Fig. 1 is the structural representation of the distillation system of the present invention;
图2为图1中局部结构示意图(蒸馏塔和蒸发器);Fig. 2 is the partial structure schematic diagram (distillation tower and evaporator) in Fig. 1;
图3为图2中蒸发器的结构放大示意图;Fig. 3 is the structural enlarged schematic diagram of the evaporator in Fig. 2;
图4为图2中蒸馏塔上部的结构放大示意图;Fig. 4 is the structural enlargement schematic diagram of distillation column upper part among Fig. 2;
图5为图4中右侧分液腔的俯视示意图;Fig. 5 is the top view schematic diagram of the right liquid separation chamber in Fig. 4;
其中:1、蒸馏塔;10、上塔身;11、下塔身;1a、进液管;1b、出液管;1c、出气管;Among them: 1, distillation tower; 10, upper tower body; 11, lower tower body; 1a, liquid inlet pipe; 1b, liquid outlet pipe; 1c, gas outlet pipe;
2、蒸发器;20、上管板;21、下管板;22、蒸发管;23、蒸汽供应组件;230、蒸汽进口;231、蒸汽凝结水出口;24、定型板(折流板);24a、贴合侧边;24b、断开侧边;t、通道;25、固定拉杆;2. Evaporator; 20. Upper tube sheet; 21. Lower tube sheet; 22. Evaporation tube; 23. Steam supply assembly; 230. Steam inlet; 231. Steam condensate outlet; 24. Forming plate (baffle plate); 24a, fit the side edge; 24b, disconnect the side edge; t, channel; 25, fix the pull rod;
3、气液分离器;3. Gas-liquid separator;
4、分液腔;40、分液盘;40a、分流孔;k、分流孔组;41、围板;42、连接件;4. Separation chamber; 40. Separation plate; 40a, shunt hole; k, shunt hole group; 41, enclosure plate; 42, connecting piece;
5、上隔板;6、下隔板;7、延伸板;h1、h2,混合液进料区;q1、q2,气相区;y1、y2,液相区;8、喷淋头。5. Upper baffle; 6. Lower baffle; 7. Extension plate; h1, h2, mixed liquid feeding area; q1, q2, gas phase area; y1, y2, liquid phase area; 8, shower head.
具体实施方式Detailed ways
为使本申请的上述目的、特征和优点能够更加明显易懂,下面结合附图对本申请的具体实施方式做详细的说明。在下面的描述中阐述了很多具体细节以便于充分理解本申请。但是本申请能够以很多不同于在此描述的其它方式来实施,本领域技术人员可以在不违背本申请内涵的情况下做类似改进,因此本申请不受下面公开的具体实施例的限制。In order to make the above objects, features and advantages of the present application more clearly understood, the specific embodiments of the present application will be described in detail below with reference to the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application. However, the present application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the connotation of the present application. Therefore, the present application is not limited by the specific embodiments disclosed below.
在本申请的描述中,需要理解的是,术语“中心”、“纵向”、“横向”、“长度”、“宽度”、“厚度”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”、“顺时针”、“逆时针”、“轴向”、“径向”、“周向”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本申请和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本申请的限制。In the description of this application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", " Back, Left, Right, Vertical, Horizontal, Top, Bottom, Inner, Outer, Clockwise, Counterclockwise, Axial , "radial", "circumferential" and other indicated orientations or positional relationships are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the application and simplifying the description, rather than indicating or implying the indicated device or Elements must have a particular orientation, be constructed and operate in a particular orientation and are therefore not to be construed as limitations on this application.
此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括至少一个该特征。在本申请的描述中,“多个”的含义是至少两个,例如两个,三个等,除非另有明确具体的限定。In addition, the terms "first" and "second" are only used for descriptive purposes, and should not be construed as indicating or implying relative importance or implying the number of indicated technical features. Thus, a feature delimited with "first", "second" may expressly or implicitly include at least one of that feature. In the description of the present application, "plurality" means at least two, such as two, three, etc., unless expressly and specifically defined otherwise.
在本申请中,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”、“固定”等术语应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或成一体;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通或两个元件的相互作用关系,除非另有明确的限定。对于本领域的普通技术人员而言,可以根据具体情况理解上述术语在本申请中的具体含义。In this application, unless otherwise expressly specified and limited, the terms "installed", "connected", "connected", "fixed" and other terms should be understood in a broad sense, for example, it may be a fixed connection or a detachable connection , or integrated; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between the two elements, unless otherwise specified limit. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific situations.
在本申请中,除非另有明确的规定和限定,第一特征在第二特征“上”或“下”可以是第一和第二特征直接接触,或第一和第二特征通过中间媒介间接接触。而且,第一特征在第二特征“之上”、“上方”和“上面”可是第一特征在第二特征正上方或斜上方,或仅仅表示第一特征水平高度高于第二特征。第一特征在第二特征“之下”、“下方”和“下面”可以是第一特征在第二特征正下方或斜下方,或仅仅表示第一特征水平高度小于第二特征。需要说明的是,当元件被称为“固定于”或“设置于”另一个元件,它可以直接在另一个元件上或者也可以存在居中的元件。当一个元件被认为是“连接”另一个元件,它可以是直接连接到另一个元件或者可能同时存在居中元件。本文所使用的术语“垂直的”、“水平的”、“上”、“下”、“左”、“右”以及类似的表述只是为了说明的目的,并不表示是唯一的实施方式。In this application, unless otherwise expressly stated and defined, a first feature "on" or "under" a second feature may be in direct contact with the first and second features, or the first and second features indirectly through an intermediary touch. Also, the first feature being "above", "over" and "above" the second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is level higher than the second feature. The first feature being "below", "below" and "below" the second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature has a lower level than the second feature. It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it can be directly on the other element or an intervening element may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical", "horizontal", "upper", "lower", "left", "right" and similar expressions used herein are for the purpose of illustration only and do not represent the only embodiment.
参见图1,按照本实施例二氯甲烷和白油分离用的降膜式蒸馏系统,其包括蒸馏塔1和蒸发器2、以及气液分离器3。Referring to FIG. 1 , according to the present embodiment, a falling film distillation system for separating methylene chloride and white oil includes a
具体的,蒸馏塔1沿着竖直方向延伸,且包括上塔身10和下塔身11,其中进液管1a位于上塔身10的顶部,出液管1b位于下塔身11的底部,出气管1c位于下塔身11的侧上部。Specifically, the
本例中,蒸馏塔1呈柱状,且截面呈圆形。In this example, the
结合图2所示,蒸发器2设置在上塔身10内,且包括分别设置在上塔身10顶部和底部且与上塔身10周向内壁构成闭合蒸发腔的上管板20和下管板21、两端部与上管板20和下管板21贯穿连通且沿着上塔身10的高度方向延伸的多根蒸发管22、向上塔身所形成蒸发腔提供蒸汽的蒸汽供应组件23、设置在上塔身10内且用于蒸发管22定位的定型板24、用于吊装下管板21的固定拉杆25。As shown in FIG. 2 , the
多根蒸发管22之间相互隔开设置,且多根蒸发管22的上端口与进液管1a相连通、下端口与下塔身11所形成腔体相连通。The plurality of
具体的,多根蒸发管22呈环形阵列的方式依次间隔布满在上管板20和下管板21之间。Specifically, a plurality of evaporating
蒸汽供应组件23,为常规部件,包括蒸汽进口230和蒸汽凝结水出口231、以及蒸汽发生器、用于将蒸汽发生器与蒸汽进口连通的蒸汽管道。The
结合图3所示,定型板24(也可以叫做折流板)有多块,且每一块定型板24与上塔身10内壁之间形成供蒸汽流动的通道t,固定拉杆25与蒸发管22平行设置,且上端部固定在定型板24上、下端部固定在下管板21上。定型板和固定拉杆的设置,不仅能够实现蒸发管在蒸发腔内的定位;而且定型板形成的蒸汽流动通道,改善蒸汽在蒸汽腔内的流动性(形成折流),以确保蒸发效果。As shown in FIG. 3 , there are multiple shaping plates 24 (also called baffles), and a channel t for steam flow is formed between each shaping
本例中,每一块定型板24均水平设置,且具有能够贴合在上塔身10内壁的贴合侧边24a、以及与对应侧上塔身10内壁断开形成通道t的断开侧边24b,其中多块定型板24沿着蒸发管22的长度方向上下间隔分布,且所形成的多个通道t相对错开设置。在此,通过错开的通道,不仅能够充分的实现蒸汽与蒸发管的接触实现混合液的间接加热,而且能够形成稳定的蒸汽流向,有利于混合的蒸发。In this example, each of the setting
本例中,多个通道t上下间隔,且左右相对错位分布,固定拉杆25有两根,且分别将位于通道t同侧的定型板24和底部的下管板21固定串接。这样一来,蒸发管定位安装更加稳定。In this example, a plurality of channels t are spaced up and down, and are relatively dislocated from left to right. There are two fixed
同时,二氯甲烷和白油混合液自蒸发管22的上部向下流动,蒸汽腔内的蒸汽流向与混合液流向相同。最佳化实现混合液的蒸发。At the same time, the mixed liquid of dichloromethane and white oil flows downward from the upper part of the
本例中,二氯甲烷和白油之间的沸点差(二氯甲烷沸点低,39.8℃,白油的沸点高,350℃以上),在混合液体加入蒸馏塔之前可进行预热,只要蒸发管内混合液温度大于或等于39.8℃时候,使混合液分离出气相的二氯甲烷和液相的白油,因此,蒸发腔内的蒸汽温度和蒸发管内混合液体的稳定温差较小,这样蒸汽的用量明显变小。In this example, the difference in boiling point between dichloromethane and white oil (low boiling point of dichloromethane, 39.8 °C, high boiling point of white oil, above 350 °C), can be preheated before the mixed liquid is added to the distillation column, as long as it evaporates When the temperature of the mixed liquid in the tube is greater than or equal to 39.8 °C, the mixed liquid is separated from the dichloromethane in the gas phase and the white oil in the liquid phase. Therefore, the vapor temperature in the evaporation chamber and the stable temperature difference of the mixed liquid in the evaporation tube are small, so that the vapor The dosage is significantly reduced.
本例中,气液分离器3为旋液分离器,且位于下塔身11外,其中旋液分离器入口与出气管1c相连通。In this example, the gas-
至于旋液分离器为本领域常规产品,可通过直接外购的手段获取,而且主要是将二氯甲烷气体中的白油分离出来。As for the hydrocyclone, it is a conventional product in the field, which can be obtained by means of direct outsourcing, and mainly separates the white oil in the methylene chloride gas.
同时,旋液分离器产生约为0.074Mpa的微负压,将气相区内的气态二氯甲烷吸入旋液分离器进行气液分离。At the same time, the hydrocyclone separator generates a slight negative pressure of about 0.074Mpa, and the gaseous dichloromethane in the gas phase area is sucked into the hydrocyclone separator for gas-liquid separation.
结合图4所示,降膜式蒸馏系统还包括与进液管1a连通且处于上管板20上方的分液腔4、自上管板20的顶部向上延伸的上隔板5、自下管板21的底部向下延伸的下隔板6、以及自下塔身11的底部向上延伸且与下隔板6对齐设置的延伸板7。As shown in FIG. 4 , the falling film distillation system also includes a
具体的,上隔板5、下隔板6和延伸板7均为一块,这样一来,上隔板5将上塔身10分隔成两个混合液进料区h1、h2;下隔板6对应将下塔身11的上部分隔成与混合液进料区h1、h2一一对应的两个气相区q1、q2;延伸板7将下塔身11的下部分隔成与气相区q1、q2相对应的两个液相区y1、y2。Specifically, the
本例中,分液腔4有两个且分别设置在两个混合液进料区h1、h2中,进液管1a与分液腔4一一对应设置,且每一个分液腔4对应设有一根进液管1a。In this example, there are two liquid-separating
分液腔4包括位于上管板20上方的分液盘40、围设在分液盘40周边的围板41、以及将围板41与上塔身10相连接的连接件42,其中围板41的上端部敞开设置,进液管1a的下端部伸入分液腔4中,分液盘40上开设有能够将混合液体均匀分流至下方对应上管口的分流孔40a。The liquid-separating
结合图5所示,分流孔40a有多个且分为多组,每一分流孔组k对应下方一根蒸发管22的上管口的周向分布,且每组分流孔的孔心所形成圆形的圆心设置在下方对应的上管口的中心线上,其中圆形的直径大于上管口的管径,这样一来,自每组分流孔流出的混合液体分别从下方对应的上管口的周边贴合蒸发管22的内壁向下流动,以提高蒸发效率,确保蒸发效果。As shown in FIG. 5 , there are
本例中,下隔板6与对齐的延伸板7之间隔开设置,这样一来,气相区下延至延伸板7顶部,两个气相区q1、q2自下隔板6和延伸板7的隔开处相连通设置,这样设置的好处就是,不管是经过左侧还是右侧蒸发管流出的气体和液体,其中气体部分会浮设在气相区q1、q2,并在一侧出气管1c的导引下,能够将气体送入旋液分离器中,进一步完成二氯甲烷气体中白油的分离。In this example, the
同时,由底部延伸板7将下塔身11的下部分隔成与气相区q1、q2相对应的液相区y1、y2,且每一个液相区y1、y2对应设有一根出液管1b,在此,申请人解释一下为什么底部还要分成两个液相区y1、y2,其主要原因是:能够分别对应的实现自上方蒸发管22中分离后白油的收集。这样一来,当左侧进液管1a通入混合液经过蒸发后,混合液分离出气相的二氯甲烷和液相的白油,其中气相的二氯甲烷自出气管送入旋液分离器中将气态二氯甲烷中含有的白油进行分离,至于蒸发后液相的白油自左侧的出液管1b排出,此时,排出的白油可自蒸馏塔1顶部右侧的进液口进入右侧的蒸发管22中,实现白油的二次蒸馏,二次蒸馏后分离出气相的二氯甲烷送入旋液分离器中进行气液分离,二次蒸馏后的液相白油自右侧出液管1b排出,然后会白油进行冷却处理,即可以完成二氯甲烷和白油分离。At the same time, the lower part of the
本例中,每根进液管1a的下端部位于分液盘40的上方,且在进液管1a的下端部还设有喷淋头8,其中二氯甲烷和白油混合液自喷淋头8流出流量大于自分流孔40a流出的流量。这样一来,在分液腔内应该形成有一定液位高度,以确保液体自每一个分流孔均匀流出。In this example, the lower end of each liquid inlet pipe 1a is located above the
此外,本实施例采用上述的蒸馏系统,且经过二次蒸馏后,成品白油中二氯甲烷含量:≤0.008%(80ppm);二氯甲烷中白油含量:≤0.002%(20ppm);成品白油中含水:≤0.02%。而,现有设备中上述指标一般最好只能达到:成品白油中二氯甲烷含量:≤0.05%(500ppm);二氯甲烷中白油含量:≤0.04%(400ppm)。因此,采用本申请的蒸馏系统,能够大幅度改善白油和二氯甲烷分离的效果,确保达到白油中二氯甲烷含量低,二氯甲烷中白油含量低的技术目的。In addition, this embodiment adopts the above-mentioned distillation system, and after secondary distillation, the content of methylene chloride in the finished white oil: ≤0.008% (80ppm); the content of white oil in methylene chloride: ≤0.002% (20ppm); the finished product Water in white oil: ≤0.02%. However, the above-mentioned indicators in the existing equipment can generally only be achieved: the content of methylene chloride in the finished white oil: ≤ 0.05% (500ppm); the content of white oil in the methylene chloride: ≤ 0.04% (400ppm). Therefore, by adopting the distillation system of the present application, the separation effect of white oil and dichloromethane can be greatly improved, and the technical purpose of low content of dichloromethane in white oil and low content of white oil in dichloromethane can be ensured.
综上,本例中的蒸馏系统,采用国内最先进的微负压降膜蒸发工艺,其特点是:To sum up, the distillation system in this example adopts the most advanced micro-negative pressure falling film evaporation process in China, and its characteristics are:
1)、物料停留时间短,蒸汽工作压力小,蒸汽耗量低;1) The material residence time is short, the steam working pressure is small, and the steam consumption is low;
2)、二氯甲烷气体温度低(50℃以下),不会对设备在长期使用时造成腐蚀,并且冷凝器的冷凝负荷小,循环用水量低,可降低生产成本;2) The temperature of methylene chloride gas is low (below 50 ℃), which will not cause corrosion to the equipment during long-term use, and the condensation load of the condenser is small, and the circulating water consumption is low, which can reduce the production cost;
3)、蒸发后白油浓缩液的温度低、色泽浅、纯度高,脱色时白土添加量减少,降低生产成本;3) After evaporation, the temperature of the white oil concentrate is low, the color is light, and the purity is high, and the amount of white clay added during decolorization is reduced, which reduces the production cost;
4)、蒸发后的二氯甲烷气体,先经高效闪发捕集再经冷凝器冷凝后的二氯甲烷液体纯度高,再进行分水,因此,可获得二氯甲烷中白油的含量20ppm以内。4) The evaporated dichloromethane gas is firstly captured by high-efficiency flashing and then condensed by the condenser. The dichloromethane liquid has high purity, and then water is separated. Therefore, the content of white oil in dichloromethane can be obtained as 20ppm within.
以上对本发明做了详尽的描述,其目的在于让熟悉此领域技术的人士能够了解本发明的内容并加以实施,并不能以此限制本发明的保护范围,且本发明不限于上述的实施例,凡根据本发明的精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围。The present invention has been described in detail above, and its purpose is to enable those skilled in the art to understand the content of the present invention and implement it, and cannot limit the scope of protection of the present invention by this, and the present invention is not limited to the above-mentioned embodiments, All equivalent changes or modifications made according to the spirit of the present invention shall be included in the protection scope of the present invention.
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CN212308890U (en) * | 2020-06-28 | 2021-01-08 | 太仓市宝马油脂设备有限公司 | Falling film distillation system for separating dichloromethane and white oil |
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Denomination of invention: Falling film distillation system for separating dichloromethane and white oil Granted publication date: 20250429 Pledgee: Bank of Jiangsu Co.,Ltd. Suzhou Branch Pledgor: TAICANG BAOMA OILS & FATS EQUIPMENT Co.,Ltd. Registration number: Y2025980018673 |