技术领域technical field
本发明属于色谱分离技术领域，特别涉及一种通用模拟移动床色谱分离装置。The invention belongs to the technical field of chromatographic separation, in particular to a general-purpose simulated moving bed chromatographic separation device.
背景技术Background technique
模拟移动床色谱(简称SMB)技术具有高分离度、高产率、高收率、高生产效率和连续自动运行机制，是高端分离手段。模拟移动床色谱装置由若干根尾首相接成循环回路的色谱柱组成，通过沿流动相的流动方向有次序地移动流动相进口与流出液出口的位置来模拟固定相与流动相的相对逆流流动，进而实现不同组分的分离。SMB工作模式包括设置参与分离的色谱柱数目、划分不同功能区、设置各区色谱柱，模拟移动床色谱分离原理决定了工作模式的多样性；并且工作模式是优化模拟移动床色谱分离首先考查的关键因素，但实际上的SMB设备大都受切换阀及其配套软件的制约采用较为固定的运行模式，同一台SMB设备难于实现多种不同模式之间的转换。Simulated Moving Bed Chromatography (SMB for short) technology is a high-end separation method with high resolution, high yield, high yield, high production efficiency and continuous automatic operation mechanism. The simulated moving bed chromatographic device is composed of several chromatographic columns whose tails are connected into a circulation loop. The relative countercurrent flow of the stationary phase and the mobile phase is simulated by sequentially moving the positions of the mobile phase inlet and the effluent outlet along the flow direction of the mobile phase. This allows for the separation of different components. The SMB working mode includes setting the number of chromatographic columns participating in the separation, dividing different functional areas, and setting chromatographic columns in each area. The principle of simulated moving bed chromatographic separation determines the diversity of working modes; and the working mode is the key to the optimization of simulated moving bed chromatographic separation. Factors, but in fact, most SMB equipment is restricted by the switching valve and its supporting software and adopts a relatively fixed operating mode. It is difficult for the same SMB equipment to realize the conversion between multiple different modes.
发明内容Contents of the invention
本发明提供一种通用模拟移动床色谱分离装置。该装置为在SMB体系中每个色谱柱安排11个二通阀，可以设置多种的工作模式，实现多组分分离。The invention provides a general simulated moving bed chromatographic separation device. The device arranges 11 two-way valves for each chromatographic column in the SMB system, and can set various working modes to realize multi-component separation.
一种模拟移动床装置，包括M根色谱柱，4≤M≤30，每根色谱柱入口和出口分别连接入口多通和出口多通，入口多通分别连接6条输入管路以及前一根色谱柱的循环管路，出口多通分别连接4条输出管路以及当前色谱柱的循环管路；所述的每根输入管路或输出管路分别与相应的输入总线或输出总线连接；原料液、洗脱液分别由相应的输入总线输入相应色谱柱的输入管路；所述的循环管路连接前一根色谱柱出口多通和当前色谱柱入口多通，使所有色谱柱通过循环管路尾首相连；除循环流出液以外的各种色谱柱流出液分别由相应色谱柱通过相应的输出管路输出到相应的输出总线；A simulated moving bed device, including M chromatographic columns, 4≤M≤30, the inlet and outlet of each chromatographic column are respectively connected to the inlet multi-pass and the outlet multi-pass, and the inlet multi-pass is respectively connected to 6 input pipelines and the previous one The circulation pipeline of the chromatographic column, the multi-way outlet is respectively connected to 4 output pipelines and the circulation pipeline of the current chromatographic column; each of the input pipelines or output pipelines is connected to the corresponding input bus or output bus respectively; the raw material The liquid and the eluent are respectively input into the input pipeline of the corresponding chromatographic column through the corresponding input bus; the circulation pipeline is connected with the multi-pass at the outlet of the previous chromatographic column and the multi-pass at the inlet of the current chromatographic column, so that all the chromatographic columns pass through the circulation tube The end of the road is connected first; the effluents of various chromatographic columns except the circulating effluent are respectively output from the corresponding chromatographic columns to the corresponding output buses through the corresponding output pipelines;
原料液、洗脱液存贮于相应的储液罐中；从输出总线流出的各种色谱柱流出液即模拟移动床的体系流出液存贮于相应的储液罐中；The raw material liquid and eluent are stored in the corresponding liquid storage tanks; the effluents of various chromatographic columns flowing out from the output bus, that is, the system effluents of the simulated moving bed, are stored in the corresponding liquid storage tanks;
每根色谱柱的输入管路、输出管路和循环管路上均设置二通阀；所述二通阀由电磁阀和止逆阀组成，并由PLC或单片机控制系统控制每个二通阀为开启或关闭状态；Two-way valves are arranged on the input pipeline, output pipeline and circulation pipeline of each chromatographic column; the two-way valve is composed of a solenoid valve and a check valve, and each two-way valve is controlled by a PLC or a single-chip microcomputer control system. on or off state;
所述色谱柱在-10℃～200℃范围内的恒温条件下工作；The chromatographic column works under constant temperature conditions within the range of -10°C to 200°C;
上述的模拟移动床装置，可以设置多区带SMB：如三带a-b-c、四带SMB：a-b-c-d，五带SMB：a-b-c-d-e六带至更多带，a、b、c、d、e指每带色谱柱数目，可以设置开环输入原料液或者洗脱液模式的模式，吸附区和慢组分精细分离区连续、洗脱区独立的模式，各区独立工作的顺序SMB运行模式。The above-mentioned simulated moving bed device can be equipped with multi-zone SMB: such as three-zone a-b-c, four-zone SMB: a-b-c-d, five-zone SMB: a-b-c-d-e six-zone to more zones, a, b, c, d, e refer to the chromatogram of each zone The number of columns can be set to open-loop input raw material solution or eluent mode, continuous adsorption zone and slow component fine separation zone, independent elution zone mode, and sequential SMB operation mode in which each zone works independently.
进一步的，上述的模拟移动床装置，可选择SMB参与分离的色谱柱数目，即：在所述装置中参与分离过程的色谱柱为N根，3≤N≤M；N根色谱柱通过循环管路尾首相连，形成回路。Further, in the above-mentioned simulated moving bed device, the number of chromatographic columns that SMB participates in the separation can be selected, that is: there are N chromatographic columns participating in the separation process in the device, 3≤N≤M; N chromatographic columns pass through the circulation pipe The end of the road is connected head-to-head to form a loop.
进一步的，上述的模拟移动床装置，将一条输出总线与一条输入总线连接，构成截取管路。Further, in the above-mentioned simulated moving bed device, an output bus is connected with an input bus to form an intercepting pipeline.
进一步的，上述的模拟移动床装置，可以实现截取部分流出液并连续回流精制，打开当前输出流出液的色谱柱的与所述截取管路相连的输出管路二通阀和该柱的后一根色谱柱的与所述截取管路相连的输入管路二通阀，构成回流管路，并且在回流管路上设置输送泵；Further, the above-mentioned simulated moving bed device can intercept part of the effluent and continuously reflux and refine it, and open the two-way valve of the output pipeline connected to the interception pipeline of the chromatographic column currently outputting the effluent and the latter of the column. An input pipeline two-way valve connected to the intercepting pipeline of a chromatographic column constitutes a return pipeline, and a delivery pump is arranged on the return pipeline;
或者在截取管路中设置1个三通和1台输送泵，所述三通的一个口用于输出流出液，同时打开当前输出流出液的色谱柱的与所述截取管路相连的输出管路二通阀和该柱的后一根色谱柱的与所述截取管路相连的输入管路二通阀，同样构成回流管路；Or set a tee and a delivery pump in the interception pipeline, one port of the tee is used to output the effluent, and simultaneously open the output pipe of the chromatographic column that is currently outputting the effluent connected to the interception pipeline The input pipeline two-way valve connected with the intercepting pipeline of the last chromatographic column of the post and the two-way valve of the column also constitute the return pipeline;
并且，上述两种构成回流管路的方式中，在当前色谱柱的回流管路开通时，将当前色谱柱循环管路关闭。Moreover, in the above two ways of forming the return pipeline, when the return pipeline of the current chromatography column is opened, the circulation pipeline of the current chromatography column is closed.
或者，上述的模拟移动床装置，可以实现截取部分流出液并反馈给进样入口或洗脱液入口，打开当前输出流出液的色谱柱的与所述截取管路相连的输出管路二通阀和除该柱的后一根色谱柱之外任意一根色谱柱的与所述截取管路相连的输入管路二通阀，构成绕过管路；Alternatively, the above-mentioned simulated moving bed device can intercept part of the effluent and feed it back to the sample inlet or eluent inlet, and open the two-way valve of the output pipeline connected to the interception pipeline of the chromatographic column that currently outputs the effluent And the two-way valve of the input pipeline connected to the interception pipeline of any chromatographic column except the last chromatographic column of the column, constitutes a bypass pipeline;
所述绕过管路中设置0～1台输送泵。0-1 delivery pumps are set in the bypass pipeline.
进一步的，上述的模拟移动床装置，可以设置同步或异步切换模式，针对同一个工作模式，在切换周期内，通过控制系统分时间段设置进口、出口位置，调整各个功能区带的长度即各带色谱柱数目。Further, the above-mentioned simulated moving bed device can be set in a synchronous or asynchronous switching mode. For the same working mode, within the switching cycle, the inlet and outlet positions are set by the control system in time periods, and the lengths of each functional zone are adjusted. with column number.
进一步的，上述的模拟移动床装置，所述的M根色谱柱依次排列的序号为：Z1、Z2、Z3、Z4、Z5、…、Z(n-1)、Zn、Z(n+1)、…、ZM，则在所述的N根色谱柱中，排在两端的相邻色谱柱尾首相连，其它相间隔的色谱柱尾首相连，色谱柱尾首相连即为所述循环管路，所有循环管路等长；Further, in the above-mentioned simulated moving bed device, the sequential numbers of the M chromatographic columns are: Z1, Z2, Z3, Z4, Z5, ..., Z(n-1), Zn, Z(n+1) , ..., ZM, in the N chromatographic columns, the adjacent chromatographic columns arranged at both ends are connected end to end, and other spaced chromatographic columns are connected end to end, and the end to end connection of the chromatographic columns is the circulation pipeline , all circulation lines are of equal length;
N为偶数时，N根色谱柱的连接方式为：Z1、Z3、Z5、…、Z(N-3)、Z(N-1)、ZN、Z(N-2)、Z(N-4)、…、Z4、Z2、Z1，即：按奇数增大的方向，奇数色谱柱尾首相连至一端Z(N-1)，Z(N-1)与ZN尾首相连，然后，按偶数减小方向，偶数色谱柱尾首相连至另一端Z2，Z2与Z1尾首相连，构成N根色谱柱的回路，为“麻花式”尾首相连；When N is an even number, the connection methods of N chromatographic columns are: Z1, Z3, Z5, ..., Z(N-3), Z(N-1), ZN, Z(N-2), Z(N-4 ), ..., Z4, Z2, Z1, that is: according to the direction of odd number increase, the end of the odd-numbered chromatographic column is connected to one end Z(N-1), Z(N-1) is connected to the end of ZN, and then, according to the even number In the decreasing direction, the even-numbered chromatographic columns are connected end-to-end to the other end Z2, and Z2 and Z1 are connected end-to-end to form a loop of N chromatographic columns, which is a "twist-style" end-to-end connection;
N为奇数时，N根色谱柱的连接方式为：Z1、Z3、Z5、…、Z(N-4)、Z(N-2)、ZN、Z(N-1)、Z(N-3)、…、Z4、Z2、Z1，即：按奇数增大的方向，奇数色谱柱尾首相连至一端ZN，ZN与Z(N-1)尾首相连，然后，按偶数减小方向，偶数色谱柱尾首相连至另一端Z2，Z2与Z1尾首相连，构成N根色谱柱的回路，为“麻花式”尾首相连；When N is an odd number, the connection methods of N chromatographic columns are: Z1, Z3, Z5, ..., Z(N-4), Z(N-2), ZN, Z(N-1), Z(N-3 ), ..., Z4, Z2, Z1, that is: according to the direction of odd number increase, the end of the odd number column is connected to one end ZN, ZN is connected to the end of Z(N-1), and then, according to the direction of even number decrease, the even number The end of the chromatographic column is connected to the other end Z2, and Z2 and Z1 are connected end to end to form a loop of N chromatographic columns, which is "twist style" end to end connection;
采用“麻花式”尾首相连的方式连接管线，能够使循环管路的被循环的液体有近似的输送过程，避免扩散差异。The "twist-style" end-to-end connection of the pipeline can make the circulating liquid in the circulation pipeline have an approximate delivery process and avoid diffusion differences.
进一步的，上述的模拟移动床装置，所述M根色谱柱的排列方式为一字排列、环形排列或者矩形排列等方式时，“麻花式”尾首相连方便，循环管线等长。Further, in the above-mentioned simulated moving bed device, when the arrangement of the M chromatographic columns is in-line arrangement, circular arrangement or rectangular arrangement, the "twisted pattern" is convenient for end-to-end connection, and the circulation pipelines are of equal length.
进一步的，上述的模拟移动床装置，可设置多种工作模式同时工作，将N根色谱柱的模拟移动床分解为2套模拟移动床体系，即：L根色谱柱尾首相连组成一套模拟移动床，3≤L≤(N-3)，剩余(N-L)根色谱柱尾首相连组成另外一套模拟移动床，2套模拟移动床体系为独立运行模式、并联运行模式或者串联运行模式。Further, the above-mentioned simulated moving bed device can be set to work in multiple working modes at the same time, and the simulated moving bed of N chromatographic columns is decomposed into two sets of simulated moving bed systems, that is, L chromatographic columns are connected head-to-head to form a set of simulated moving beds. Moving bed, 3≤L≤(N-3), the remaining (N-L) chromatographic columns are connected head-to-head to form another set of simulated moving bed, and the two sets of simulated moving bed systems are in independent operation mode, parallel operation mode or series operation mode.
进一步的，上述的模拟移动床装置，断开2套模拟移动床之间的连接管线，能够构成数套不同模拟移动床体系，数套模拟移动床体系为独立运行模式、并联运行模式或者串联运行模式。Further, the above-mentioned simulated moving bed device can form several sets of different simulated moving bed systems by disconnecting the connecting pipeline between two sets of simulated moving beds, and several sets of simulated moving bed systems can be operated in independent operation mode, parallel operation mode or series operation model.
进一步的，上述的模拟移动床装置，将所有色谱柱设置于一个区域，所有二通阀设置于另外一个区域，对色谱柱区域进行控温。Further, in the above-mentioned simulated moving bed device, all chromatographic columns are set in one area, and all two-way valves are set in another area to control the temperature of the chromatographic column area.
进一步的，上述的模拟移动床装置，输入总线上配备过滤器、在线脱气机，循环管路上配备流量计，输出总线上配备流量计、溶液浓度和纯度的检测器。Further, the above-mentioned simulated moving bed device is equipped with a filter and an online degasser on the input bus, a flow meter on the circulation pipeline, and a flow meter and a detector for solution concentration and purity on the output bus.
进一步的，上述的模拟移动床装置，与工作模式无关的管路均可在相应的多通或三通处用堵头密封，以延长相关二通阀寿命。Further, in the above-mentioned simulated moving bed device, the pipelines irrelevant to the working mode can be sealed with plugs at the corresponding multi-way or three-way positions, so as to prolong the service life of the related two-way valves.
与现有技术相比，本发明的优势在于：Compared with the prior art, the present invention has the advantages of:
1、本装置具有多种功能：设置SMB参与分离的色谱柱数目；设置多区带SMB：如三带a-b-c、四带SMB：a-b-c-d，五带SMB：a-b-c-d-e，六带至更多带，a、b、c、d指每带色谱柱数目；设置区带间连续运行或独立运行模式；设置开环进样与取样的模式；设置同步或异步切换模式；截取部分流出液并反馈给进样入口或洗脱液入口；多种工作模式同时工作；完成多组分分离等。1. This device has multiple functions: set the number of chromatographic columns for SMB to participate in the separation; set multi-zone SMB: such as three-zone a-b-c, four-zone SMB: a-b-c-d, five-zone SMB: a-b-c-d-e, six-zone to more zones, a, b, c, d refer to the number of chromatographic columns in each zone; set the continuous operation or independent operation mode between the zones; set the open-loop sampling and sampling mode; set the synchronous or asynchronous switching mode; intercept part of the effluent and feed it back to the injection inlet Or eluent inlet; multiple working modes work at the same time; complete multi-component separation, etc.
2、二通阀操作灵活，容易维护。2. The two-way valve is flexible in operation and easy to maintain.
3、管线连接方便。3. The pipeline connection is convenient.
4、阀与色谱柱分区放置，可以对色谱柱整体控温。4. The valve and the chromatographic column are placed in partitions, which can control the overall temperature of the chromatographic column.
附图说明Description of drawings
图1是一种8根色谱柱的模拟移动床装置示意图，该模拟移动床为一个回路，八个区带，1-1-1-1-1-1-1-1，分离三组分强吸附组分A、中等吸附组分B和弱吸附组分C。Fig. 1 is a schematic diagram of a simulated moving bed device with 8 chromatographic columns, the simulated moving bed is a loop, eight zones, 1-1-1-1-1-1-1-1, three components are separated Adsorbing component A, moderately adsorbing component B and weakly adsorbing component C.
图2是一种8根色谱柱的模拟移动床装置示意图，该模拟移动床为一个回路，六个区带，1-1-2-1-1-2，分离三组分A、B和C。与工作模式无关的管路可在相应的多通或三通处用堵头密封。Fig. 2 is a schematic diagram of a simulated moving bed device with 8 chromatographic columns, the simulated moving bed is a loop, six zones, 1-1-2-1-1-2, separate three components A, B and C . Pipelines that have nothing to do with the working mode can be sealed with plugs at the corresponding multi-way or tee.
图3是一种8根色谱柱的模拟移动床装置示意图，该模拟移动床为一个回路，四个区带，2-2-2-2，分离二组分A、B。Fig. 3 is a schematic diagram of a simulated moving bed device with 8 chromatographic columns. The simulated moving bed is a circuit with four zones, 2-2-2-2, to separate two components A and B.
图4是一种8根色谱柱的模拟移动床装置示意图，该模拟移动床为一个回路，六个区带，1-1-2-1-1-2，其中第一带独立且梯度洗脱，分离三组分A、B和C。Figure 4 is a schematic diagram of a simulated moving bed device with 8 chromatographic columns, the simulated moving bed is a loop, six zones, 1-1-2-1-1-2, wherein the first band is independent and gradient elution , to separate the three components A, B and C.
图5是一种8根色谱柱的模拟移动床装置示意图，执行顺序色谱分离，4根色谱柱参与分离，各带独立运行，或分离四段馏分A、B、C和W，或用梯度洗脱。Figure 5 is a schematic diagram of a simulated moving bed device with 8 chromatographic columns, performing sequential chromatographic separation, 4 chromatographic columns participate in the separation, and each band operates independently, or separates four sections of fractions A, B, C and W, or uses gradient washing take off.
图6是一种8根色谱柱的模拟移动床装置示意图，该模拟移动床为“麻花式”尾首相连。Fig. 6 is a schematic diagram of a simulated moving bed device with 8 chromatographic columns, and the simulated moving bed is connected end to end in a "twist style".
图7是一种8根色谱柱的模拟移动床装置示意图，该模拟移动床为“麻花式”尾首相连，两个1-1-2模拟移动床回路，串联分离组分A、B和C。Figure 7 is a schematic diagram of a simulated moving bed device with 8 chromatographic columns. The simulated moving bed is connected head-to-head in a "twist style", and two 1-1-2 simulated moving bed circuits are used to separate components A, B and C in series. .
其中，Zn：第n根色谱柱，n：色谱柱序号，Lmi：输入或输出总线，m＝1代表输入，m＝2代表输出，i为输入或输出总线序号，Lnmi：第n根色谱柱输入/输出管路；Vnmi：Lnmi的二通阀，Tn：循环管路二通阀；Among them, Zn: the nth chromatographic column, n: the serial number of the chromatographic column, Lmi: the input or output bus, m=1 represents the input, m=2 represents the output, i is the serial number of the input or output bus, Lnmi: the nth chromatographic column Input/output pipeline; Vnmi: two-way valve of Lnmi, Tn: two-way valve of circulation pipeline;
F：原料液储液罐，D或Dq：洗脱液D或洗脱液Dq储液罐，q：洗脱液序号，A：分离组分A储液罐，B：组分B储液罐，C：组分C储液罐，W：组分W储液罐，Pi：第i条输入总线的输送泵。F: raw material liquid storage tank, D or Dq: eluent D or eluent Dq liquid storage tank, q: eluent serial number, A: separated component A liquid storage tank, B: component B liquid storage tank , C: liquid storage tank of component C, W: liquid storage tank of component W, Pi: delivery pump of the i-th input bus.
具体实施方式Detailed ways
以下以8根色谱柱模拟移动床装置为实施例对本发明作进一步的详细描述。The present invention will be further described in detail below by taking 8 chromatographic columns simulated moving bed device as an example.
实施例1Example 1
一种模拟移动床装置，包括8根相同的色谱柱，第n根色谱柱Zn入口和出口分别连接入口多通和出口多通，入口多通分别连接6条输入管路和前一根色谱柱的循环管路T(n-1)，出口多通分别连接4条输出管路和当前色谱柱的循环管路Tn，共11条管路；原料液、洗脱液分别被相应的输送泵经由输入总线泵入各自的输入管路；循环管路连接前一根色谱柱Z(n-1)出口和当前色谱柱Zn入口，使所有色谱柱尾首相连；除循环流出液以外的各种色谱柱流出液分别经由各自的输出管路汇入相应的输出总线；原料液、洗脱液存贮于相应的储液罐中；从输出总线流出的溶液即模拟移动床的体系流出液存贮于相应的储液罐中；色谱柱的所有输入管路、所有输出管路和所有循环管路均设置二通阀；色谱柱在室温下工作；二通阀由电磁阀和止逆阀组成，由PLC或单片机控制系统控制所有二通阀各自的工作状态，或开或关。具体运行步骤通过各个二通阀的开、关状态体现，在此，仅叙述色谱柱的开通状态，关闭状态不赘述，色谱柱循环管路二通阀只用出口方向设置的Tn表示。A simulated moving bed device, including 8 identical chromatographic columns, the inlet and outlet of the nth chromatographic column Zn are respectively connected to the inlet multi-pass and the outlet multi-pass, and the inlet multi-pass is respectively connected to 6 input pipelines and the previous chromatographic column The circulation pipeline T(n-1), the multi-way outlet is respectively connected to 4 output pipelines and the circulation pipeline Tn of the current chromatographic column, a total of 11 pipelines; the raw material liquid and the eluent are respectively passed by the corresponding delivery pump The input bus pumps into their respective input pipelines; the circulation pipeline connects the outlet of the previous chromatographic column Z(n-1) and the inlet of the current chromatographic column Zn, so that all chromatographic columns are connected end to end; The column effluents are connected to the corresponding output bus through their respective output pipelines; the raw material liquid and eluent are stored in the corresponding liquid storage tanks; the solution flowing out from the output bus, that is, the system effluent of the simulated moving bed, is stored in the In the corresponding liquid storage tank; all input pipelines, all output pipelines and all circulation pipelines of the chromatographic column are equipped with two-way valves; the chromatographic column works at room temperature; the two-way valve is composed of a solenoid valve and a check valve. The PLC or single-chip microcomputer control system controls the respective working states of all two-way valves, either on or off. The specific operation steps are reflected by the open and closed states of each two-way valve. Here, only the open state of the chromatographic column is described, and the closed state is not described in detail. The two-way valve of the chromatographic column circulation pipeline is only represented by Tn set in the outlet direction.
图1所示的模拟移动床装置具体为：设有一个回路，八个区带，1-1-1-1-1-1-1-1，分离三组分，分别为强吸附组分A、中等吸附组分B和弱吸附组分C；The simulated moving bed device shown in Figure 1 is specifically as follows: there is a loop, eight zones, 1-1-1-1-1-1-1-1, three components are separated, which are the strong adsorption component A , medium adsorption component B and weak adsorption component C;
在该装置中，原料液于储液罐F中由输液泵P1泵入输入总线L11，洗脱液于储液罐D中由输液泵P2泵入输入总线L12，分离后组分A经输出总线L24进入储液罐A，组分B经输出总线L23进入储液罐B，组分C经输出总线L22进入储液罐C；In this device, the raw material liquid is pumped into the input bus L11 by the infusion pump P1 in the liquid storage tank F, the eluent is pumped into the input bus L12 by the infusion pump P2 in the liquid storage tank D, and the separated component A passes through the output bus L24 enters the liquid storage tank A, component B enters the liquid storage tank B through the output bus L23, and component C enters the liquid storage tank C through the output bus L22;
连接其中的一条输出总线和其中的一条输入总线，构成截取管路，L24-L16、L23-L15、L22-L14、L21-L13；Connect one of the output buses and one of the input buses to form interception pipelines, L24-L16, L23-L15, L22-L14, L21-L13;
在截取管路L24-L16中设置一个三通和一台流动相输送泵P6，三通的一个口输出该截取管路的体系流出液A，打开当前输出流出液A的色谱柱Z1的与截取管路L24-L16相连的输出管路二通阀V124和后一根色谱柱Z2的与截取管路L24-L16相连的输入管路二通阀V216，开通截取管路，同时关闭色谱柱Z1流出液A循环管路T1，形成色谱柱Z1与色谱柱Z2之间的流出液A回流管路；Set a tee and a mobile phase delivery pump P6 in the interception pipeline L24-L16, one port of the tee outputs the system effluent A of the interception pipeline, open the chromatographic column Z1 that currently outputs the effluent A and intercept The two-way valve V124 of the output pipeline connected with the pipeline L24-L16 and the two-way valve V216 of the input pipeline connected with the interception pipeline L24-L16 of the next chromatographic column Z2 open the interception pipeline and close the outflow of the column Z1 at the same time The liquid A circulation pipeline T1 forms the effluent A return pipeline between the chromatographic column Z1 and the chromatographic column Z2;
在截取管路L23-L15和L22-L14同理设置，形成色谱柱Z3与色谱柱Z4之间的流出液B回流管路，以及色谱柱Z7与色谱柱Z8之间的流出液C回流管路；The interception pipelines L23-L15 and L22-L14 are similarly set to form the effluent B return pipeline between the chromatographic column Z3 and the chromatographic column Z4, and the effluent C return pipeline between the chromatographic column Z7 and the chromatographic column Z8 ;
在截取管路L21-L13中设置1台流动相输送泵P3，打开当前输出A、B混合物流出液的色谱柱Z5的与截取管路L21-L13相连接的输出管路二通阀V521和色谱柱Z3的与截取管路L21-L13相连接的输入管路二通阀V313，形成色谱柱Z5与色谱柱Z3之间的流出液AB的绕过管路。Set up a mobile phase delivery pump P3 in the interception pipeline L21-L13, open the output pipeline two-way valve V521 connected to the interception pipeline L21-L13 and the chromatographic The two-way valve V313 of the input pipeline connected to the intercepting pipeline L21-L13 of the column Z3 forms a bypass pipeline for the effluent AB between the chromatographic column Z5 and the chromatographic column Z3.
该装置的工作模式具体为：The working mode of the device is specifically:
Z1：V112和V124开，用洗脱液D洗脱组分A，固定相再生，组分A流出液一部分流入储液罐A，一部分通过回流管路L24-L16回流至Z2；Z1: V112 and V124 are opened, component A is eluted with eluent D, and the stationary phase is regenerated. Part of the effluent of component A flows into liquid storage tank A, and part of it flows back to Z2 through the return line L24-L16;
Z2：V216和T2开，组分A与B精细分离；Z2: V216 and T2 are separated, components A and B are finely separated;
Z3：V313和V323开，组分A、B被吸附并分离，组分A、B混合液由绕过管路L21-L13提供，组分B流出液一部分流入储液罐B，一部分通过回流管路L23-L15回流至Z4；Z3: V313 and V323 open, components A and B are adsorbed and separated, the mixed solution of components A and B is provided by bypassing the pipeline L21-L13, part of the effluent of component B flows into the liquid storage tank B, and part of it passes through the return pipe Road L23-L15 returns to Z4;
Z4：V415和T4开，回收组分B，流动相再生；Z4: V415 and T4 are opened, component B is recovered, and the mobile phase is regenerated;
Z5：V521和T5开，洗脱组分A、B混合物，固定相再生，A、B混合物流出液一部分经绕过管路L21-L13流入Z3，一部分通过回流管路L23-L15回流至Z6；Z5: V521 and T5 open, the mixture of components A and B is eluted, the stationary phase is regenerated, part of the effluent of the mixture of A and B flows into Z3 through the bypass pipeline L21-L13, and part of it flows back to Z6 through the return pipeline L23-L15;
Z6：T6开，组分A、B混合物和组分C精细分离；Z6: T6 open, component A, B mixture and component C are finely separated;
Z7：V711和V722开，原料液的A、B、C被吸附并分离，组分C流出液一部分流入储液罐C，一部分通过回流管路L22-L14回流至Z8；Z7: V711 and V722 open, A, B, and C of the raw material liquid are adsorbed and separated, part of the effluent of component C flows into the liquid storage tank C, and part of it flows back to Z8 through the return line L22-L14;
Z8：V814和T8开，回收C组分，流动相再生。Z8: V814 and T8 are opened, component C is recovered, and the mobile phase is regenerated.
到达切换时间时，控制系统将工作模式沿流动相方向移至回路中下一根色谱柱，该过程反复进行，模拟固定相与流动相的相对逆流流动，经过吸附、脱附和精馏，实现3个组分分离。When the switching time is reached, the control system will move the working mode to the next chromatographic column in the loop along the direction of the mobile phase. This process is repeated to simulate the relative countercurrent flow of the stationary phase and the mobile phase. After adsorption, desorption and rectification, 3 components are separated.
图2所示的模拟移动床装置具体为：设有一个回路，六个区带，1-1-2-1-1-2，分离三组分A、B和C。The simulated moving bed device shown in Fig. 2 is specifically as follows: there is one circuit, six zones, 1-1-2-1-1-2, and three components A, B and C are separated.
在多通入口和三通的出口使用堵头密封，关闭与工作模式无关的管路Ln14和L22-14，同时将原L23-L15截取管路三通的出口用堵头密封，用P5输送D2洗脱液。Use a plug to seal the multi-way inlet and the outlet of the tee, close the pipelines Ln14 and L22-14 that have nothing to do with the working mode, and seal the outlet of the original L23-L15 intercepted pipeline tee with a plug, and use P5 to transport D2 eluent.
该装置的工作模式具体为：The working mode of the device is specifically:
Z1：V112和V124开，用洗脱液D1洗脱组分A，固定相再生，组分A流出液一部分流入储液罐A，一部分通过回流管路L24-L16回流至Z2；Z1: V112 and V124 are opened, component A is eluted with eluent D1, and the stationary phase is regenerated. Part of the effluent of component A flows into liquid storage tank A, and part of it flows back to Z2 through the return line L24-L16;
Z2：V216和T2开，组分A与B精细分离；Z2: V216 and T2 are separated, components A and B are finely separated;
Z3和Z4：V313、T3和V423开，组分A、B被吸附并分离，组分A、B混合液由绕过管路L21-L13提供，组分B流出液流入储液罐B；Z3 and Z4: V313, T3 and V423 open, components A and B are adsorbed and separated, the mixed solution of components A and B is provided by bypassing the pipeline L21-L13, and the effluent of component B flows into the liquid storage tank B;
Z5：V515、V521和T5开，用D2洗脱组分A和B，固定相再生，A和B混合物流出液一部分经绕过管路流入Z3，一部分循环至Z6；Z5: V515, V521 and T5 are opened, components A and B are eluted with D2, and the stationary phase is regenerated. Part of the effluent from the mixture of A and B flows into Z3 through the bypass pipeline, and part of it is recycled to Z6;
Z6：T6开，组分A、B混合物和组分C精细分离；Z6: T6 open, component A, B mixture and component C are finely separated;
Z7和Z8：V711、T7和V822开，原料液的A、B、C被吸附并分离，组分C流出液流入储液罐C。Z7 and Z8: V711, T7 and V822 open, A, B and C of the raw material liquid are adsorbed and separated, and the effluent of component C flows into the liquid storage tank C.
到达切换时间时，控制系统将工作模式沿流动相方向移至回路中下一根色谱柱，该过程反复进行，模拟固定相与流动相的相对逆流流动，经过吸附、脱附和精馏，实现3个组分分离。When the switching time is reached, the control system will move the working mode to the next chromatographic column in the loop along the direction of the mobile phase. This process is repeated to simulate the relative countercurrent flow of the stationary phase and the mobile phase. After adsorption, desorption and rectification, 3 components are separated.
图3所示的模拟移动床装置具体为：设有一个回路，2-2-2-2四个区带，分离二组分A、B。The simulated moving bed device shown in Fig. 3 is specifically: a circuit is provided, and four zones of 2-2-2-2 are used to separate two components A and B.
该装置的工作模式具体为：The working mode of the device is specifically:
Z1和Z2：V112、T1、V224开，用洗脱液D洗脱组分A，固定相再生，组分A流出液一部分流入储液罐A，一部分通过回流管路L24-L16回流至Z3；Z1 and Z2: Open V112, T1, V224, elute component A with eluent D, and regenerate the stationary phase, part of the effluent from component A flows into liquid storage tank A, and part of it flows back to Z3 through the return line L24-L16;
Z3和Z4：V316、T3、T4开，组分A与B精细分离；Z3 and Z4: V316, T3, T4 open, components A and B are finely separated;
Z5和Z6：V511、T5和V623开，组分A、B被吸附并分离，组分B流出液一部分流入储液罐B，一部分通过回流管路L23-L15回流回流至Z7；Z5 and Z6: V511, T5 and V623 open, components A and B are adsorbed and separated, part of the effluent of component B flows into the liquid storage tank B, and part of it flows back to Z7 through the return line L23-L15;
Z7和Z8：V715、T7和T8开，回收组分B，流动相再生；Z7 and Z8: V715, T7 and T8 are opened, component B is recovered, and the mobile phase is regenerated;
到达切换时间时，控制系统将工作模式沿流动相方向移至回路中下一根色谱柱，该过程反复进行，模拟固定相与流动相的相对逆流流动，经过吸附、脱附和精馏，实现2个组分分离。When the switching time is reached, the control system will move the working mode to the next chromatographic column in the loop along the direction of the mobile phase. This process is repeated to simulate the relative countercurrent flow of the stationary phase and the mobile phase. After adsorption, desorption and rectification, 2 components are separated.
针对2-2-2-2四个区带，把切换周期Ts依次分t1、t2、t3、t4时间段，For the four zones of 2-2-2-2, the switching period Ts is divided into t1, t2, t3, t4 time periods in turn,
t1：将组分B出口，沿流动相方向移至下一根色谱柱，切换周期为Ts；t1: Move the outlet of component B to the next chromatographic column along the direction of the mobile phase, and the switching period is Ts;
t2：将洗脱液入口，沿流动相方向移至下一根色谱柱，切换周期为Ts；t2: Move the eluent inlet to the next chromatographic column along the direction of the mobile phase, and the switching period is Ts;
t3：将组分A出口，沿流动相方向移至下一根色谱柱，切换周期为Ts；t3: Move the outlet of component A to the next chromatographic column along the direction of the mobile phase, and the switching period is Ts;
t4：将进料口，沿流动相方向移至下一根色谱柱，切换周期为Ts；t4: Move the feed port to the next chromatographic column along the direction of the mobile phase, and the switching period is Ts;
Ts：复原，2-2-2-2四个区带。Ts: Recovery, 2-2-2-2 four zones.
上述过程重复进行，由此异步切换改变各带色谱柱数目即区带长度。The above process is repeated, thus asynchronously switching to change the number of chromatographic columns in each band, that is, the length of the zone.
图4所示的模拟移动床装置具体为：设置一个回路，六个区带，1-1-2-1-1-2，其中第一带独立且梯度洗脱，分离三组分A、B和C。The simulated moving bed device shown in Figure 4 is specifically: a circuit is set, six zones, 1-1-2-1-1-2, wherein the first zone is independent and gradient eluted, and the three components A and B are separated and C.
洗脱液D1于储液罐D1中由输液泵P2泵入输入总线L12，洗脱液D2于储液罐D2中由输液泵P4泵入输入总线L14，洗脱液D3于储液罐D3中由输液泵P5泵入输入总线L15，洗脱液D4于储液罐D4中由输液泵6泵入输入总线L16；L24、L23、L22输出总线的三通原截取管路出口处用堵头密封。The eluent D1 is pumped into the input bus L12 by the infusion pump P2 in the liquid storage tank D1, and the eluent D2 is pumped into the input bus L14 by the infusion pump P4 in the liquid storage tank D2, and the eluent D3 is pumped into the input bus L14 by the infusion pump P4 in the liquid storage tank D3 The infusion pump P5 is pumped into the input bus L15, and the eluent D4 is pumped into the input bus L16 by the infusion pump 6 in the liquid storage tank D4; the outlet of the three-way original interception pipeline of the L24, L23, and L22 output buses is sealed with a plug .
工作模式具体为：The specific working mode is:
Z1：V112、V114和V124开，用洗脱液D1和D2梯度洗脱组分A，固定相再生，组分A流出液流入储液罐A；Z1: V112, V114 and V124 open, gradient elution of component A with eluents D1 and D2, stationary phase regeneration, component A effluent flows into liquid storage tank A;
Z2：V215和T2开，用D3作流动相，精细分离组分A与B；Z2: Separate V215 and T2, use D3 as the mobile phase, and finely separate components A and B;
Z3和Z4：V313、T3和V423开，组分A、B被吸附并分离，组分A、B混合液由绕过管路L21-L13提供，组分B流出液流入储液罐B；Z3 and Z4: V313, T3 and V423 open, components A and B are adsorbed and separated, the mixed solution of components A and B is provided by bypassing the pipeline L21-L13, and the effluent of component B flows into the liquid storage tank B;
Z5：V516、V521和T5开，用D4洗脱组分A和B，固定相再生，A和B混合物流出液一部分经绕过管路流入Z3，一部分循环至Z6；Z5: V516, V521 and T5 are opened, components A and B are eluted with D4, and the stationary phase is regenerated. Part of the effluent from the mixture of A and B flows into Z3 through the bypass pipeline, and part of it is recycled to Z6;
Z6：T6开，组分A、B混合物和组分C精细分离；Z6: T6 open, component A, B mixture and component C are finely separated;
Z7和Z8：V711、T7和V822开，混合物A、B、C被吸附并分离，组分C流出液流入储液罐C。Z7 and Z8: V711, T7 and V822 open, the mixtures A, B and C are adsorbed and separated, and the effluent of component C flows into the liquid storage tank C.
图5所示的模拟移动床装置具体为：设置Z1～Z4共4根色谱柱参与分离，执行顺序色谱分离，各带独立运行，能够进行分离四段馏分A、B、C和W，或进行梯度洗脱。The simulated moving bed device shown in Figure 5 is specifically as follows: a total of 4 chromatographic columns Z1 to Z4 are set to participate in the separation, and sequential chromatographic separation is performed. Each band operates independently, and can separate the four sections of fractions A, B, C and W, or carry out Gradient elution.
洗脱液D1于储液罐D1中由输液泵P2泵入输入总线L12，洗脱液D2于储液罐D2中由输液泵P3泵入输入总线L13，洗脱液D3于储液罐D3中由输液泵P4泵入输入总线L14；分别由L24、L23、L22和L21输出组分A至储液罐A、组分B至储液罐B、组分C至储液罐C和组分W至储液罐W；L24、L23、L22输出总线的三通原截取管路出口处用堵头密封The eluent D1 is pumped into the input bus L12 by the infusion pump P2 in the liquid storage tank D1, the eluent D2 is pumped into the input bus L13 by the infusion pump P3 in the liquid storage tank D2, and the eluent D3 is in the liquid storage tank D3 Pumped into input bus L14 by infusion pump P4; output component A to liquid storage tank A, component B to liquid storage tank B, component C to liquid storage tank C and component W from L24, L23, L22 and L21 respectively To the liquid storage tank W; the outlet of the three-way original interception pipeline of L24, L23, L22 output bus is sealed with a plug
工作模式具体为：The specific working mode is:
Z1：V114、V124开，用洗脱液D1洗脱组分A，固定相再生，组分A流出液流入储液罐A；Z1: V114 and V124 are open, component A is eluted with eluent D1, the stationary phase is regenerated, and the effluent of component A flows into liquid storage tank A;
Z2：V213和V223开，用D2作流动相，精细分离组分B；Z2: V213 and V223 open, use D2 as mobile phase, finely separate component B;
Z3：V312和V322开，用D3作流动相，精细分离组分C；Z3: V312 and V322 open, use D3 as mobile phase, finely separate component C;
Z4：V411和V421开，进样液的组分A、B、C、W被吸附并分离，W流出液流入储液罐B；Z4: V411 and V421 open, components A, B, C, and W of the sample liquid are adsorbed and separated, and W effluent flows into the liquid storage tank B;
图6所示的模拟移动床装置具体为色谱柱的“麻花式”尾首相连。The simulated moving bed device shown in Fig. 6 is specifically a "twisted" end-to-end connection of chromatographic columns.
这里仅考虑色谱柱间循环管路的设置方式，未考虑工作状态。8根色谱柱依次排列的序号为：Z1、Z2、Z3、Z4、Z5、Z6、Z7、Z8，设定N根色谱柱参与分离过程，3≤N≤8，N＝8时色谱柱的连接方式为：Z1、Z3、Z5、Z7、Z8、Z6、Z4、Z2、Z1，即：两端Z7与Z8尾首相连、Z2与Z1尾首相连，其它间隔色谱柱尾首相连，构成8根色谱柱的回路；当选择参与分离的色谱柱数目时，这种循环管路等长，且连接方式操作简单，如：当N＝6时或将N＝8时色谱柱的连接方式转换为N＝6时，将Z5循环管路连在Z6入口端即可，连接回路为：Z1、Z3、Z5、Z6、Z4、Z2、Z1，即：两端Z5与Z6尾首相连、Z2与Z1尾首相连，其它间隔色谱柱尾首相连，构成6根色谱柱的回路；当N＝7时或将N＝8时色谱柱的连接方式转换为N＝7时，将Z6循环管路连在Z7入口端即可，连接回路为：Z1、Z3、Z5、Z7、Z6、Z4、Z2、Z1，即：两端Z7与Z6尾首相连、Z2与Z1尾首相连，其它间隔色谱柱尾首相连，构成7根色谱柱的回路；Here, only the setting method of the circulation pipeline between the chromatographic columns is considered, and the working status is not considered. The serial numbers of the 8 chromatographic columns are: Z1, Z2, Z3, Z4, Z5, Z6, Z7, Z8, set N chromatographic columns to participate in the separation process, 3≤N≤8, and the connection of chromatographic columns when N=8 The method is: Z1, Z3, Z5, Z7, Z8, Z6, Z4, Z2, Z1, that is: Z7 and Z8 at both ends are connected head-to-head, Z2 and Z1 are connected head-to-head, and other interval chromatographic columns are connected head-to-head to form 8 columns The loop of the chromatographic column; when the number of chromatographic columns involved in the separation is selected, the length of the circulation pipeline is equal, and the connection method is easy to operate, such as: when N=6 or when N=8, the connection method of the chromatographic column is converted to N = 6, just connect the Z5 circulation pipeline to the Z6 inlet, the connection circuit is: Z1, Z3, Z5, Z6, Z4, Z2, Z1, that is: both ends of Z5 and Z6 are connected at the end, and Z2 and Z1 are connected at the end. First connected, other interval chromatographic columns connected end to end to form a loop of 6 chromatographic columns; when N=7 or when the connection mode of the chromatographic columns when N=8 is converted to N=7, connect the Z6 circulation pipeline to the Z7 The inlet port is enough, the connection circuit is: Z1, Z3, Z5, Z7, Z6, Z4, Z2, Z1, that is: both ends Z7 and Z6 are connected end to end, Z2 and Z1 are connected end to end, and other interval chromatographic columns are connected end to end , forming a loop of seven chromatographic columns;
通过这种循环管路的设置，能够容易的将本实施例的装置构成多套移动床，例如，N＝8时，将Z3循环管路连在Z4入口端，将Z6循环管路连在Z5入口端，即可构成两套各4根柱的移动床，两套移动床体系能够设置成独立运行(可以是不同流动相、不同固定相、不同原料液)，并联运行，或者串联运行。Through the setting of this circulation pipeline, the device of this embodiment can be easily formed into multiple sets of moving beds. For example, when N=8, the Z3 circulation pipeline is connected to the Z4 inlet port, and the Z6 circulation pipeline is connected to the Z5 circulation pipeline. At the inlet end, two sets of moving beds with 4 columns each can be formed. The two sets of moving bed systems can be set to operate independently (can be different mobile phases, different stationary phases, and different raw material solutions), parallel operation, or series operation.
图7所示的模拟移动床装置具体为：色谱柱的“麻花式”尾首相连，两个1-1-2模拟移动床回路，串联分离组分A、B和C。The simulated moving bed device shown in Figure 7 is specifically: the "twisted" end-to-end connection of the chromatographic column, two 1-1-2 simulated moving bed circuits, and the separation of components A, B and C in series.
洗脱液D1于储液罐D1中由输液泵P2泵入输入总线L12，洗脱液D2于储液罐D2中由输液泵P5泵入输入总线L15。L23、L22输出总线的三通原截取管路出口处用堵头密封。The eluent D1 is pumped into the input bus L12 by the infusion pump P2 in the liquid storage tank D1, and the eluent D2 is pumped into the input bus L15 by the infusion pump P5 in the liquid storage tank D2. The outlets of the original interception pipelines of the tees of the L23 and L22 output buses are sealed with plugs.
工作模式具体为：The specific working mode is:
第一个回路连接顺序为：Z1、Z3、Z4、Z2和Z1；The first loop connection sequence is: Z1, Z3, Z4, Z2 and Z1;
Z1：V112和V124开，用洗脱液D1洗脱组分A，固定相再生，组分A流出液一部分流入储液罐A，一部分经回流管路L24-L16回流至Z3；Z1: V112 and V124 are opened, component A is eluted with eluent D1, and the stationary phase is regenerated. Part of the effluent of component A flows into liquid storage tank A, and part of it flows back to Z3 through the return line L24-L16;
Z3：V316和T3开，组分A与B精细分离；Z3: V316 and T3 open, components A and B are finely separated;
Z4和Z2：V413、T4和V223开，组分A、B被吸附并分离，组分A、B混合液由绕过管路L21-L13提供，组分B流出液流入储液罐B；Z4 and Z2: V413, T4 and V223 open, components A and B are adsorbed and separated, the mixed solution of components A and B is provided by bypassing the pipeline L21-L13, and the effluent of component B flows into the liquid storage tank B;
第二个回路连接顺序为：Z5、Z7、Z8、Z6和Z5。The second loop connection sequence is: Z5, Z7, Z8, Z6 and Z5.
Z5：V515、V521和T5开，用D2洗脱组分A和B，固定相再生，A和B混合物流出液一部分经绕过管路流入Z4，一部分循环至Z7；Z5: V515, V521 and T5 are opened, components A and B are eluted with D2, and the stationary phase is regenerated. Part of the effluent of the mixture of A and B flows into Z4 through the bypass pipeline, and part of it is recycled to Z7;
Z7：T7开，组分A、B混合物和组分C精细分离；Z7: T7 open, component A, B mixture and component C are finely separated;
Z8和Z6：V811、T8和V622开，原料液中混合物A、B、C被吸附并分离，组分C流出液流入储液罐C。Z8 and Z6: V811, T8 and V622 open, the mixtures A, B and C in the raw material liquid are adsorbed and separated, and the effluent of component C flows into the liquid storage tank C.
断开2套模拟移动床之间的连接管路，可以构成3～7套模拟移动床控制体系，配备泵、管线、三通和储液罐，进行4-14组分分离。Disconnect the connecting pipelines between 2 sets of simulated moving beds to form 3 to 7 sets of simulated moving bed control systems, equipped with pumps, pipelines, tees and liquid storage tanks, for 4-14 component separations.
| Application Number | Priority Date | Filing Date | Title |
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| CN201610832972.6ACN106166402B (en) | 2016-09-19 | 2016-09-19 | A kind of moving bed imitation chromatogram separation facility |
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| CA2139033C (en)* | 1993-12-27 | 2004-04-20 | Masatake Tanimura | Method of separation into three components using a simulated moving bed |
| CN101732890A (en)* | 2009-12-08 | 2010-06-16 | 辽宁科技大学 | Three-section simulated moving bed chromatography device |
| CN105617714A (en)* | 2015-12-31 | 2016-06-01 | 厦门大学 | Asynchronous switching three-zone-belt simulation moving bed |
| CN206334397U (en)* | 2016-09-19 | 2017-07-18 | 辽宁科技大学 | A kind of moving bed imitation chromatogram separation facility |
| Publication number | Priority date | Publication date | Assignee | Title |
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| CA2139033C (en)* | 1993-12-27 | 2004-04-20 | Masatake Tanimura | Method of separation into three components using a simulated moving bed |
| CN101732890A (en)* | 2009-12-08 | 2010-06-16 | 辽宁科技大学 | Three-section simulated moving bed chromatography device |
| CN105617714A (en)* | 2015-12-31 | 2016-06-01 | 厦门大学 | Asynchronous switching three-zone-belt simulation moving bed |
| CN206334397U (en)* | 2016-09-19 | 2017-07-18 | 辽宁科技大学 | A kind of moving bed imitation chromatogram separation facility |
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| CN106166402A (en) | 2016-11-30 |
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