CN113493429B - Industrialized gulonic acid three-component separation device and separation method thereof - Google Patents

Abstract

The invention relates to an industrialized gulonic acid three-component separation system and a separation method thereof, wherein the separation system comprises a separation unit consisting of six chromatographic column groups (1); the six chromatographic column groups (1) are sequentially numbered as 1# -6# according to the circulation direction of liquid in the system; the 1# -6# chromatographic column group (1) is sequentially connected end to end through a circulating pipe section to form a circulating loop; the top parts of the six chromatographic column groups (1) are respectively provided with a water distribution pipe (14) with a water inlet valve (19), the bottom parts of the six chromatographic column groups are respectively provided with a CD branch pipe (16) with a CD valve and an AD branch pipe (15) with an AD valve, and only the top part of the 1# chromatographic column group (1) is provided with a raw material branch pipe (13) with a feed valve (18); only the bottom of the 6# chromatographic column group (1) is provided with a BD tube (12) with a BD valve; in the separation method, only the 1# chromatographic column group is fed, and the middle component in the row at the 6# chromatographic column group is fed; and the fast and slow components are discharged from the bottoms of the plurality of chromatographic column groups through a plurality of closed-loop cycles, so that intermittent feeding and a plurality of impurity removal are realized.

Description

Industrialized gulonic acid three-component separation device and separation method thereof

Technical Field

The invention relates to the technical field of compound separation, in particular to an industrialized gulonic acid three-component separation device and a separation method thereof.

Background

Gulonic acid is an important intermediate for the production of vitamin C. At present, gulonic acid is mainly prepared by a biological fermentation method, and gulonic acid crystals are prepared by removing solid substances such as protein, hypha and the like from fermentation liquor through pretreatment and then evaporating and crystallizing. The gulonic acid mother liquor generated in the crystallization process usually contains 15-20% of heteropolyacid, 60-70% of gulonic acid and 5-15% of vitamin C and heterosugar. The prior separation method is difficult to completely separate the gulonic acid product and obtain the gulonic acid product with higher purity. The application range of the gulonic acid mother liquor is small, so that manufacturers generally carry out price pasting treatment on the gulonic acid mother liquor.

In the prior art, an attempt is made to separate a mixed solution of gulonic acid and vitamin C by using a chromatographic separation technology, but the current chromatographic separation means mainly comprises two-component separation, namely, a gulonic acid mother solution can be only separated into a gulonic acid-rich material flow and a VC-rich material flow, but not mixed acid and mixed sugar can be separated simultaneously, so that the purity of a separated product is low, and the application range is limited.

On the other hand, the diameter of the chromatographic column is limited by the packing effect of the chromatographic column and the feed liquid distribution technology, so that the large flow demand of industrial production is difficult to apply. Although the limitation of the upper limit of the diameter of the chromatographic columns on the treatment capacity can be overcome by a multi-column parallel connection mode, the multi-column parallel connection mode has the defects that uniform and controllable flow distribution among the columns is difficult to realize, and quick response to concentration change cannot be realized, so that the simulated moving bed chromatography is difficult to construct so as to realize continuous separation operation. In addition, the continuous withdrawal of the target component during the chromatographic separation results in a significant reduction in the amount of liquid passing through the subsequent column, which leads to insufficient driving force of the liquid flowing through the column downstream of the withdrawal point.

In view of this, the invention is particularly proposed.

Disclosure of Invention

In order to solve the defects in the prior art, the invention provides an industrial gulonic acid three-component separation device and a separation method thereof. The method comprises the following specific steps:

an industrialized gulonic acid three-component separation device comprises a separation unit formed by six chromatographic column groups, wherein the six chromatographic column groups are sequentially numbered from 1# to 6# according to the circulation direction of liquid in a system, the numbers correspond to columns and do not change along with the change of the execution functions of the chromatographic column groups in different time periods, namely the numbers are fixed and do not change along with a functional area; each chromatographic column group comprises a plurality of chromatographic columns which are connected in parallel, and the chromatographic columns in the same chromatographic column group have the same parameters (including but not limited to column size, adsorbent type, loading amount, loading density and the like), so that even if the chromatographic column group adopts a multi-column parallel combination mode, the chromatographic columns can show the same or at least acceptable error flow performance and separation performance under the same operation conditions, and can be regarded as a single-color packed column in the aspect of separation effect.

To meet such a requirement, it is preferable to constitute the column set using an industrially prepared column produced by a standardized production process.

The invention adopts a multi-column parallel connection chromatographic column group to meet the large flow requirement of industrial scale. It will be appreciated that in some cases, for example where the flow rate of the material to be treated is not large, it is also possible to use a single column to form the set, i.e. the set of columns of the present invention includes a plurality of combinations of columns including only one column and a plurality of columns connected in parallel. The present invention will be discussed below with a focus on multi-column parallel chromatography column sets for high flow rates.

Each chromatographic column group comprises a mixing distributor, and the mixing distributor can receive incoming flow (comprising raw material flow and/or water flow and/or circulating flow) and uniformly distribute the incoming flow to upper inlets of the chromatographic columns forming the corresponding chromatographic column group through distribution pipes after the incoming flow is fully mixed; the bottom outlets of a plurality of chromatographic columns forming the corresponding chromatographic column group are collected in the circulating pipe through a confluence branch pipe.

The mixing distributor is provided with a symmetrical columnar structure, the upper end and the lower end of the mixing distributor are respectively provided with a receiving port, and the two receiving ports are respectively connected with an incoming flow pipe through an incoming flow branch pipe so as to be used for receiving incoming flow.

The six chromatographic column groups are connected end to end through a circulating pipe to form a circulating loop; specifically, the bottom outlet (the outlet after the confluence branch pipes are converged) of the 1# chromatographic column group is connected with the inflow pipe of the mixing distributor corresponding to the 2# chromatographic column group through a circulating pipe; the bottom outlet of the No. 2 chromatographic column group is connected with the inflow pipe of the mixing distributor corresponding to the No. 3 chromatographic column group through a circulating pipe; …; the bottom outlet of the No. 6 chromatographic column group is connected with the inflow pipe of the mixing distributor corresponding to the No. 1 chromatographic column group through a circulating pipe; each section (the section of the circulating pipe connected between the outlet and the inlet of the adjacent or head-tail two chromatographic column groups) is provided with a circulating valve.

The six chromatographic column groups of the separation unit are divided into 6 functional regions in total by 2 adsorption regions (represented by Z31 and Z32), 1 isolation region (represented by Z4), 1 resolution region (represented by Z1) and 2 separation regions (represented by Z21 and Z22) according to separation procedures, and the 6 chromatographic column groups correspond to the functional regions according to different separation procedures.

The separation device also comprises a water tank for storing and supplying the resolving agent (namely water), wherein the bottom of the water tank is connected with a main water pipe with a delivery pump, and the main water pipe is connected to incoming flow pipes of the mixing distributors corresponding to the chromatographic column groups through a plurality of mutually independent water distribution pipes; each water dividing pipe is provided with a water inlet valve which is used for selectively connecting the water dividing pipe, so that the inlet position of the resolving agent is allowed to be adjusted; the downstream end of the main water pipe is connected to the upper inlet of the water tank, thereby forming a water supply loop.

The separation device further comprises a raw material liquid tank, the raw material liquid tank is used for storing, stirring and supplying raw material liquid (namely the gulonic acid mother liquid) to be separated, the bottom of the raw material liquid tank is connected with a raw material main pipe with a conveying pump, and the raw material main pipe is connected with an incoming flow pipe of a mixing distributor corresponding to the 1# chromatographic column group through a raw material branch pipe. The inflow pipe of the mixing distributor corresponding to the 2# -6# chromatographic column group is only connected with a circulating pipe and a water dividing pipe, but not connected with a raw material branch pipe.

That is, only the # 1 column set is in communication with the feed solution tank.

The raw material branch pipe is provided with a feeding valve which is used for controlling the opening and closing of the raw material branch pipe so as to control the feeding time; the downstream end of the raw material main pipe is connected to the upper inlet of the raw material liquid tank, so that a raw material liquid supply loop is formed.

The separation device further comprises an extracting solution (hereinafter referred to as BD) tank, wherein an inlet of the BD tank is connected to a bottom outlet of the 6# chromatographic column group through a BD pipe, and particularly, the BD tank can be connected to any position on a circulating pipe section between the 6# chromatographic column group and the 1# chromatographic column group. That is, only the bottom of the 6# chromatographic column set is provided with a BD extraction port.

The separation device further comprises a raffinate (AD) tank, an AD main pipe is connected to an inlet of the AD tank, each section of the circulating pipe is located on the upstream of the circulating valve and is connected with the AD main pipe through an AD branch pipe, and each AD branch pipe is provided with an AD valve so as to selectively control the opening and closing of the corresponding AD branch pipe, so that the AD extraction position can be adjusted.

The separation device also comprises a residual liquid (hereinafter referred to as CD) tank, wherein a CD main pipe is connected to the inlet of the CD tank, a CD branch pipe is connected to the CD main pipe at the upstream of the circulating valve on each section of the circulating pipe, and a CD valve is arranged on each CD branch pipe to selectively control the opening and closing of the corresponding CD branch pipe, so that the CD extraction position is allowed to be adjusted.

Preferably, the mixing distributor further comprises a power cavity between the two receiving ports, and the two receiving ports are respectively communicated with the corresponding end parts of the power cavity through a connecting channel, namely the bottom parts of the receiving ports positioned on the upper part of the power cavity are communicated with the top surface of the power cavity through a connecting channel; the top of the receiving port positioned at the lower part of the power cavity is connected to the bottom surface of the power cavity through a connecting channel; at least one mixing device, such as a static mixer or the like known in the art, is disposed in each of the connecting channels so as to be substantially mixed as the incoming flow passes through the connecting channels under the driving force. The tail end (referring to one end connected with the power cavity) of each connecting channel is provided with a first one-way valve which can only be opened inwards, and the first one-way valve only allows the incoming flow to enter the power cavity through the connecting channel and does not allow the incoming flow to be reversely discharged from the power cavity through the connecting channel.

The top peripheral wall and the bottom peripheral wall of the power cavity are provided with a plurality of flow dividing pipes at equal intervals, the interior of the power cavity is provided with a piston which can seal and slide, and the piston divides the power cavity into an upper power chamber and a lower power chamber; the shunt pipes are respectively positioned at the top of the upper power chamber and the bottom of the lower power chamber, and the number and the size of the shunt pipes positioned in the upper power chamber and the lower power chamber are the same. Each shunt tube transversely penetrates through the side wall of the mixing distributor and is connected to a corresponding slot arranged on the side wall of the mixing distributor; the connection between the slots and the corresponding shunt tubes is provided with a second one-way valve which can only be opened outwards, and the second one-way valve allows the water to flow through the shunt tubes to the corresponding slots but does not allow the water to flow reversely at the connection.

Under the configuration, through the reciprocating action of the piston, incoming flows can be sucked into the corresponding power chambers through the upper connecting channel and the lower connecting channel respectively, and in the sucking process, the incoming flows are fully mixed, so that the concentration distribution caused by uneven material mixing is eliminated; when the upper power chamber absorbs liquid, the lower power chamber discharges liquid through the shunt pipe at the lower part, and conversely, when the lower power chamber absorbs liquid, the upper power chamber discharges liquid through the shunt pipe at the upper part.

Preferably, the piston can be closely attached to the end of the corresponding power chamber when the corresponding first check valve is closed, so that the liquid in the corresponding power chamber can be drained in each liquid drainage process, namely, the liquid does not remain in the power chamber in each liquid suction and liquid drainage operation, and therefore, the piston can quickly respond to the change of the incoming flow concentration.

Preferably, the piston comprises a magnetic inner core and a corrosion-resistant layer wrapping the magnetic inner core, and the corrosion-resistant layer is preferably made of PTFE (polytetrafluoroethylene), so that the method and the excellent lubricating and sealing performance can be provided; meanwhile, magnetic induction coils are respectively arranged at the upper side and the lower side of the power cavity, and a magnetic field for driving the piston to reciprocate is formed by supplying current to the magnetic induction coils, so that liquid suction and liquid discharge operations are completed.

The periphery of the mixing distributor is provided with a plurality of Y-shaped pipes, and each Y-shaped pipe comprises two Y-shaped branch pipes and a Y-shaped main pipe connected to one end of each Y-shaped branch pipe; the two Y-shaped branch pipes are respectively connected with an upper slot and a lower slot of the mixing distributor in a matching way, and then the flow dividing pipes corresponding to the corresponding slots are connected with the Y-shaped main pipe of the Y-shaped pipe; the Y-shaped main pipe is connected with each chromatographic column in the chromatographic column group through the distribution pipes which are independent mutually.

Preferably, the Y-shaped main pipe is provided with an adjusting valve and a flow sensor, and the adjusting valve allows to adjust the flow of incoming flow flowing through the corresponding Y-shaped main pipe or completely close the corresponding Y-shaped main pipe. The degree of adjustment and the closing effect can be determined from the readings of the corresponding flow sensors. The flow regulation in the Y-shaped main pipe here allows the mixing distributor and the corresponding Y-shaped pipe, distribution pipe conditions to be calibrated before the separation operation starts. It should be noted, however, that when the calibration is completed, i.e., the resistance of the flow path between each shunt tube of the mixing distributor and the top inlet of each column in the corresponding column set is balanced, during actual operation, uniform distribution of the incoming flow between each column is achieved without relying on the regulating valve and the flow sensor, which benefits from the uniform upstream pressure at each shunt tube when the piston recompresses the corresponding power cell.

On the other hand, the selection of the number of the chromatographic columns actually connected into the chromatographic column group can be realized by selectively closing the communication state of a certain Y-shaped pipe through the regulating valve, the function is important for eliminating the problem of insufficient driving force in the chromatographic column at the downstream side of the material extraction point, and after a certain Y-shaped pipe is closed, the number of the chromatographic columns actually connected into the corresponding chromatographic column group is reduced (it should be noted that materials can be uniformly distributed among the columns due to the fact that the materials are extruded and distributed by the piston), so that the effective column sectional area of the corresponding chromatographic column group is reduced, and the problems of reduction of driving liquid volume and reduction of power caused by the extraction of materials at the upstream side can be further compensated.

Providing a method for separating gulonic acid mother liquor by using the separation device, which comprises a plurality of separation periods which are continuously executed; each separation cycle comprises the following steps which are executed in sequence:

1. a feeding step; the feeding step comprises two substeps of feeding front and rear sections which are executed in sequence; wherein, in the front feeding stage, the raw material liquid is fed from the top of the No. 1 chromatographic column group, and part of the fast component CD is discharged from the bottom of the No. 2 chromatographic column group; simultaneously, feeding a water resolving agent from the top of the 4# chromatographic column group, and discharging an intermediate component BD from the bottom of the 6# chromatographic column; when feeding the rear section, continuously feeding the top of the 1# chromatographic column group; continuously extracting BD from the bottom of the No. 6 chromatographic column group; and the bottom of the 2# column set stopped discharging the fast component CD; and stopping water inflow from the top of the No. 4 chromatographic column group; when the BD component in the No. 6 chromatographic column is exhausted, the step is switched to the closed-loop circulation step.

The feeding front section can ensure that the total amount of liquid in the system is unchanged when partial fast component CD is discharged by supplementing the system with the solution agent water; the latter stage of feeding is to make up the liquid to the system by feeding to allow the intermediate fraction BD contained in the previous separation cycle to be completely removed from the bottom of the column set # 6 while keeping the total amount of liquid in the system constant.

2. A closed cycle step; the 1# -6# chromatographic column groups form a closed loop which is communicated end to end in sequence; meanwhile, all chromatographic column groups cannot enter or exit, and the material flow in the columns is driven by a circulating pump arranged between each chromatographic column group; and acquiring a liquid circulation volume of the closed circulation stage through a flowmeter arranged on the circulation pipe, and switching to a first impurity removal step after the circulation volume enables materials in each chromatographic column group 1 to move one column position downstream.

3. A first impurity removal step; the device comprises a first row C section and a first row A section which are executed in sequence; when the first row C section is formed, discharging the fast component CD from the bottom of the 3# chromatographic column group, and simultaneously inputting the analysis agent water from the top of the 5# chromatographic column group; when the section A is arranged in the first row, the analytic reagent water is input from the top of the No. 5 chromatographic column group, and the slow component AD is discharged from the bottom; and after the first row A section is finished, switching to a closed cycle step, moving the feed liquid in the column to a column position downstream again, and switching to a second impurity removing step.

4. A second impurity removal step; the device comprises a second row C section and a second row A section which are executed in sequence; during the second row of section C, fast component CD is discharged from the bottom of the No. 4 chromatographic column group, and meanwhile, the analytic agent water is input from the top of the No. 6 chromatographic column group; when the section A is arranged in the second row, the analytic agent water is input from the top of the 6# chromatographic column group, and the slow component AD is discharged from the bottom; and after the section A of the second row is finished, switching to a closed cycle step, moving the feed liquid in the column to a column position downstream again, and switching to a third impurity removing step.

5. A third impurity removing step; the device comprises a third row C of sections and a third row A which are executed in sequence; in the third row C section, fast component CD is discharged from the bottom of the No. 5 chromatographic column group, and meanwhile, the analysis agent water is input from the top of the No. 1 chromatographic column group; when the section A is arranged in the third row, the analytic reagent water is input from the top of the 1# chromatographic column group, and the slow component AD is discharged from the bottom; and after the section A in the third row is finished, switching to a closed cycle step, moving the feed liquid in the column to a column position downstream again, and then switching to a fourth impurity removing step.

6. A fourth impurity removing step; the device comprises a fourth row C section and a fourth row A section which are executed in sequence; during the fourth row of section C, fast component CD is discharged from the bottom of the No. 6 chromatographic column group, and meanwhile, the analytic agent water is input from the top of the No. 2 chromatographic column group; when the section A is arranged in the fourth row, the analytic agent water is input from the top of the 2# chromatographic column group, and the slow component AD is discharged from the bottom; and after the fourth row A section is finished, switching to a closed cycle step, moving the feed liquid in the column to a column position downstream again, and switching to a fifth impurity removal step.

7. A fifth impurity removing step; the device comprises a fifth row C section and a fifth row A section which are executed in sequence; in the fifth row of section C, fast component CD is discharged from the bottom of the 1# chromatographic column group, and meanwhile, the analytic reagent water is input from the top of the 3# chromatographic column group; when the section A is arranged in the fifth row, the analytic agent water is input from the top of the 3# chromatographic column group, and the slow component AD is discharged from the bottom; and after the section A in the fifth row is finished, switching to the closed cycle step, moving the feed liquid in the column to a column position again downstream, and then switching to the feeding step.

Feeding the raw material liquid to the top of the No. 1 chromatographic column group only in the stage of the feeding step in each separation period, and not feeding in the processes of other steps; discharging the intermediate component BD from the bottom of the # 6 column set 1 only during the feeding step; in a separation period, each step comprises a row C section sub-step, namely comprising 6 row C sections; the first through fifth impurity removing steps include row a segment sub-steps, i.e., including 5 row a segments.

Compared with the prior art, the invention can at least obtain the following beneficial effects: the adoption of the chromatographic column group with a plurality of columns connected in parallel increases the incoming flow treatment capacity on the premise of ensuring the filling effect and the liquid flow distribution effect in the columns, thereby allowing the application to separation operation in industrial scale; each chromatographic column group is provided with a mixing distributor, two ends of the mixing distributor are connected with an inflow pipe through inflow branch pipes, the mixing distributor can realize high-frequency pulse suction and transmission of inflow (each reciprocating action of the piston is a pulse) by means of an electromagnetically driven piston, and because the two sides of the piston are respectively provided with an upper power chamber and a lower power chamber, the adjacent two pulses for suction and transmission can be continuously connected into a continuous transmission process, specifically, the liquid suction process of the upper power chamber is the liquid discharge process of the lower power chamber, and vice versa, although the inflow alternately enters the upper power chamber and the lower power chamber in a pulse form and is mixed, the inflow is continuously connected into a continuously transmitted material flow again when being discharged, and meanwhile, the piston exhausts the liquid in the corresponding power chamber in each pulse process, and the process allows quick response to the concentration change of the inflow; by reducing the volume of the power chamber and correspondingly improving the reciprocating frequency of the piston, the incoming flow sucked into the power chamber in each pulse process can be further reduced under the condition of unchanged delivery volume, so that the incoming flow concentration which is continuously changed can be better adapted; the Y-shaped pipe with the regulating valve and the flow sensor is arranged outside the mixing distributor, so that the flow resistance between each chromatographic column and the flow dividing pipe is allowed to be calibrated and balanced, and the incoming flow is uniformly distributed among the chromatographic columns of the chromatographic column group; the regulating valve also allows selective closing of the communication between the section of the column and the mixing distributor, thereby compensating for the reduction in the amount of liquid driven on the downstream side caused by the withdrawal of material.

Drawings

FIG. 1 is a piping layout of the separation apparatus of the present invention;

FIG. 2 is a schematic top view of a chromatography column set;

FIG. 3 is a schematic diagram of the connection of a # 1 column set with a mixing distributor;

FIG. 4 is a schematic diagram of the connection of 2# -6# chromatographic column set with a mixing distributor;

fig. 5 is a longitudinal sectional view of the mixing distributor.

FIG. 6A is a schematic view of the front section of the feed;

FIG. 6B is a schematic illustration of a later stage of the feed;

FIG. 7 is a schematic diagram of a closed cycle step;

FIG. 8A is a schematic view of a first row C of segments;

FIG. 8B is a schematic view of the first row A of segments;

FIG. 9A is a schematic view of section C of the second row;

FIG. 9B is a schematic view of section A of the second row;

FIG. 10A is a schematic view of section C of the third row;

FIG. 10B is a schematic view of section A of the third row;

FIG. 11A is a schematic view of section C of the fourth row;

FIG. 11B is a schematic view of section A of the fourth row;

FIG. 12A is a schematic view of section C of the fifth row;

fig. 12B is a schematic view of the fifth row a of segments.

In the figure: the device comprises a chromatographic column group 1, a water tank 2, a raw material liquid tank 3, a lifting Yu Yeguan, a residual liquid tank 5, a lifting liquid tank 6, a main water pipe 7, a raw material main pipe 8, a circulating pipe 9, an AD main pipe 10, a CD main pipe 11, a BD pipe 12, a raw material branch pipe 13, a water diversion pipe 14, an AD branch pipe 15, a CD branch pipe 16, a circulating valve 17, a feed valve 18, a feed valve 19, a control valve 20, a confluence branch pipe 21, a chromatographic column 22, a distribution pipe 23, a mixing distributor 24, an incoming flow pipe 25, an incoming flow branch pipe 26, a Y-shaped branch pipe 27, a receiving port 28, a power cavity 29, a connecting channel 30, a mixing device 31, a shunt pipe 32, a piston 33, a first one-way valve 34, a magnetic induction coil 35, an insertion slot 36, a second one-way valve 37, a Y-shaped main pipe 38, a regulating valve 39 and a flow sensor 40.

ABC in fig. 6A-12B refers to a gulonic acid mother liquor feedstock containing a fast component CD, an intermediate component BD and a slow component AD; a refers to slow component AD; b refers to the intermediate component BD; c means fast component CD; d is the resolving agent water.

Detailed Description

Example 1

An industrialized gulonic acid three-component separation device is shown in a figure 1-2 and comprises a separation unit consisting of six chromatographic column groups 1; the six chromatographic column groups 1 are sequentially numbered as 1# -6# according to the arrangement sequence; each chromatographic column group 1 comprises at least two chromatographic columns 22 which are connected in parallel, wherein the chromatographic columns 22 are filled with homogeneous type strong acid cation resin, the particle size of the resin is 200-350 μm, the homogeneity of the resin is kept above 80%, each chromatographic column 22 has the same parameters, and the top of each chromatographic column 22 is provided with a material distribution pore plate or other flow equalizing devices in columns known in the art.

Preferably, the chromatographic column 22 is a preparative column.

Referring to fig. 2-3, each of the chromatography column sets 1 includes a mixing distributor 24, and the mixing distributor 24 is capable of receiving an incoming flow, sufficiently mixing the incoming flow, and uniformly distributing the mixed incoming flow to upper inlets of the chromatography columns 22 forming the corresponding chromatography column set 1 through a distribution pipe 23; the bottom outlets of the plurality of columns 22 constituting the corresponding column group 1 are collected in the circulation pipe 9 through the confluence branch pipe 21.

The mixing distributor 24 has a symmetrical cylindrical structure, a receiving opening 28 is respectively provided at the upper and lower ends thereof, and the two receiving openings 28 are respectively connected to the inflow pipe 25 through an inflow branch pipe 26 for receiving the inflow.

The six chromatographic column groups 1 are connected end to end through a circulating pipe 9 to form a circulating loop; specifically, the bottom outlet (the outlet after the confluence branch pipes 21 are converged) of the 1# chromatographic column set 1 is connected with the inflow pipe 25 of the mixing distributor 24 corresponding to the 2# chromatographic column set 1 through the circulating pipe 9; the bottom outlet of the 2# chromatographic column group 1 is connected with an incoming flow pipe 25 of the mixing distributor 24 corresponding to the 3# chromatographic column group 1 through a circulating pipe 9; …; the bottom outlet of the No. 6 chromatographic column group 1 is connected with an incoming flow pipe 25 of the mixing distributor 24 corresponding to the No. 1 chromatographic column group 1 through a circulating pipe 9; each section (the section of the circulating pipe connected between the outlet and the inlet of the adjacent or head-tail two chromatographic column groups 1) is provided with a circulating valve 17 on the circulating pipe 9.

The six chromatographic column groups 1 of the separation unit are divided into 6 functional regions in total by 2 adsorption regions (represented by Z31 and Z32), 1 isolation region (represented by Z4), 1 resolution region (represented by Z1), and 2 separation regions (represented by Z21 and Z22) according to the separation procedure, and the 6 chromatographic column groups 1 correspond to the functional regions according to different separation procedures.

It should be noted that the correspondence relationship between the functional regions and the six chromatographic column sets 1 is changed along with the progress of the separation process, and the correspondence relationship in a certain separation state is only shown in fig. 1; specific correspondence and switching logic can be seen in the separate process schematic at different states or times shown in fig. 6A-12B.

The separation device also comprises a water tank 2 for storing and supplying the resolving agent (namely water), the bottom of the water tank 2 is connected with a main water pipe 7 with a delivery pump, and the main water pipe 7 is connected to an inflow pipe 25 of a mixing distributor 24 corresponding to each chromatographic column group 1 through a plurality of mutually independent water distribution pipes 14; each of the water distribution pipes 14 is provided with a water inlet valve 19 for selectively connecting the water distribution pipe 14, thereby allowing the inlet position of the resolving agent to be adjusted; the downstream end of the main water pipe 7 is connected to the upper inlet of the water tank 2, thereby forming a water supply circuit.

The separation device further comprises a raw material liquid tank 3 for storing, stirring and supplying raw material liquid (i.e. gulonic acid mother liquid) to be separated, the bottom of the raw material liquid tank 3 is connected with a raw material main pipe 8 with a delivery pump, and the raw material main pipe 8 is connected to an incoming flow pipe 25 of a mixing distributor 24 corresponding to the # 1 chromatographic column group 1 through a raw material branch pipe 13. Shown in fig. 3 is a mixing distributor 24 corresponding to # 1 column set 1, with feed manifold 13 connected to inflow tube 25.

FIG. 4 shows a mixing distributor 24 corresponding to the 2# -6# chromatographic column set 1, and as shown, the inflow pipe 25 is connected with only the circulation pipe 9 and the water separation pipe 14, but not with the raw material branch pipe 13.

That is, only the # 1 column 1 communicates with the raw material liquid tank 3.

The raw material branch pipe 13 is provided with a feeding valve 18 for controlling the opening and closing of the raw material branch pipe 13 so as to control the feeding time; the downstream end of the raw material main pipe 8 is connected to the upper inlet of the raw material liquid tank 3, thereby forming a raw material liquid supply circuit for returning the raw material liquid to the raw material liquid tank 3 when the feed valve 18 is closed, so that the raw material liquid pump can be kept in a normally open state during operation; this allows the feed valve 18 to be opened suddenly, and to respond quickly and supply the raw material to the # 1 column group 1, avoiding the problems of feed lag and difficulty in accurately controlling the feed amount due to the restart of the raw material liquid pump.

Preferably, a control valve 20 is respectively arranged at the upstream and downstream of the main water pipe 7 and the main raw material pipe 8, wherein the upstream control valve 20 is positioned at the upstream of the corresponding water diversion pipe 14 or the raw material branch pipe 13 and is positioned at the downstream of the corresponding delivery pump; the downstream control valve 20 is located downstream of the corresponding knock out pipe 14 or feed branch 13.

The separation device further comprises an extracting solution (hereinafter referred to as BD) tank 6, wherein an inlet of the BD tank 6 is connected to a bottom outlet of the No. 6 chromatographic column set 1 through a BD pipe 12, and particularly, can be connected to any position on the circulating pipe section between the No. 6 chromatographic column set 1 and the No. 1 chromatographic column set 1, which is upstream of a circulating valve 17. That is, only the bottom of the 6# column set 1 is provided with a BD extraction port.

The separation device further comprises a raffinate (hereinafter referred to as AD) tank 4, an AD main pipe 10 is connected to an inlet of the AD tank 4, each section of the circulation pipe 9 is connected to the AD main pipe 10 through an AD branch pipe 15 located at the upstream of the circulation valve 17, and each AD branch pipe 15 is provided with an AD valve so as to selectively control the opening and closing of the corresponding AD branch pipe 15, so that the AD extraction position can be adjusted.

The separation device further comprises a residual liquid (hereinafter referred to as CD) tank 5, a CD main pipe 11 is connected to an inlet of the CD tank 5, a CD branch pipe 16 is connected to the CD main pipe 11 at the upstream of the circulating valve 17 on each section of the circulating pipe 9, and a CD valve is arranged on each CD branch pipe 16 to selectively control the opening and closing of the corresponding CD branch pipe 16, so that the CD extraction position is allowed to be adjusted.

Preferably, referring to fig. 5, the mixing distributor 24 further comprises a power chamber 29 located between the two receiving ports 28, and the two receiving ports 28 are respectively communicated with the corresponding ends of the power chamber 29 through a connecting channel 30, i.e. the bottom of the receiving port 28 located at the upper part of the power chamber 29 is communicated with the top surface of the power chamber 29 through a connecting channel 30; the top of the receiving opening 28, which is located at the lower portion of the power chamber 29, is connected to the bottom surface of the power chamber 29 by a connecting channel 30; at least one mixing device 31, such as a static mixer or the like known in the art, is provided in each of the connecting channels 30 so that the incoming flow is mixed well when it passes through the connecting channels 30 under the driving force. The end of each of the connecting channels 30 (referred to as the end connected to the power chamber 29) is provided with a first one-way valve 34 that can only open inwardly, the first one-way valve 34 only allowing incoming flow through the connecting channel 30 into the power chamber 29, but not allowing reverse discharge from the power chamber 29 through the connecting channel 30.

A plurality of shunt tubes 32 are arranged on the top peripheral wall and the bottom peripheral wall of the power cavity 29 at equal intervals, a piston 33 is arranged in the power cavity 29 in a sealing and sliding manner, and the piston 33 divides the power cavity 29 into an upper power chamber and a lower power chamber; the plurality of the shunt tubes are respectively positioned at the top of the upper power chamber and the bottom of the lower power chamber, and the number and the size of the shunt tubes positioned in the upper power chamber and the lower power chamber are the same. Each of the shunt tubes 32 extends transversely through the side wall of the mixing distributor 24 and is connected to a corresponding socket 36 provided in the side wall of the mixing distributor 24; the connection between the socket 36 and the corresponding shunt tube 32 is provided with a second one-way valve 37 which can only be opened outwards, and the second one-way valve 37 only allows the incoming flow to flow through the shunt tube 32 to the corresponding socket 36, but not the reverse flow at the position.

Under the configuration, through the reciprocating action of the piston 33, incoming flows can be sucked into the corresponding power chambers through the upper connecting channel 30 and the lower connecting channel 30 respectively, and in the suction process, the incoming flows are fully mixed, so that the concentration distribution caused by uneven mixing of materials is eliminated; wherein, when the upper power chamber absorbs liquid, the lower power chamber discharges liquid through the shunt pipe 32 at the lower part, conversely, when the lower power chamber absorbs liquid, the upper power chamber discharges liquid through the shunt pipe 32 at the upper part.

Preferably, the piston 33 is adapted to engage closely with the end of the respective power chamber when the respective first one-way valve 34 is closed, so that the liquid in the respective power chamber is drained during each discharge, i.e. no liquid remains in the power chamber during each suction and discharge operation, thereby providing a quick response to changes in the incoming concentration.

Preferably, the piston 33 includes a magnetic inner core and a corrosion-resistant layer wrapping the magnetic inner core, and the corrosion-resistant layer is preferably made of PTFE, so that corrosion resistance and excellent lubricating and sealing performances can be provided; meanwhile, a magnetic induction coil 35 is respectively arranged at the upper side and the lower side of the power cavity 29, and a magnetic field for driving the piston 33 to reciprocate is formed by supplying current to the magnetic induction coil 35, so that the liquid suction and discharge operations are completed.

A plurality of Y-shaped pipes are arranged at the periphery of the mixing distributor 24, and each Y-shaped pipe comprises two Y-shaped branch pipes 27 and a Y-shaped main pipe 38 connected to one end of each Y-shaped branch pipe 27; the two Y-branch pipes 27 are respectively connected to an upper slot 36 and a lower slot 36 of the mixing distributor 24 in a matching manner, and the shunt pipes 32 corresponding to the respective slots 36 are connected to a Y-main pipe 38 of the Y-branch pipe; the Y-shaped main pipe 38 is connected to each column 22 in the column group 1 via the mutually independent distribution pipe 23.

Preferably, the Y-shaped main pipes 38 are provided with regulating valves 39 and flow sensors 40, and the regulating valves 39 allow the flow of the incoming flow through the respective Y-shaped main pipes 38 to be regulated or completely close the respective Y-shaped main pipes 38. The degree of adjustment and the effectiveness of the shut-down can be determined based on readings from the corresponding flow sensor 40. It should be noted here that the regulation of the flow in the Y-shaped main pipe 38 allows the calibration of the state of the mixing distributor 24 and of the corresponding Y-shaped pipe, the distributor pipe 23, before the separation operation starts. It should be noted, however, that when the calibration is completed, i.e. the resistance of the flow path between each shunt tube 32 of the mixing distributor 24 to the top inlet of each column 22 in the corresponding column set 1 is balanced, during actual operation, uniform distribution of the incoming flow between each column 22 is achieved without relying on the regulating valve 39 and flow sensor 40, which is due to the uniform upstream pressure developed at each shunt tube 32 by the piston 33 when compressing the corresponding power cell.

On the other hand, the selection of the number of columns 22 actually connected to the column group 1 can be realized by selectively closing the communication state of a certain Y-shaped tube by the regulating valve 39, which is important for eliminating the problem of insufficient driving force in the downstream side column at the material withdrawal point, because the number of columns 22 actually connected to the column group 1 is reduced after closing a certain Y-shaped tube (it should be noted that the material is uniformly distributed among the columns due to the extrusion distribution of the material by the piston), therefore, the effective column cross-sectional area of the corresponding column group 1 is reduced, and the problems of reduced driving fluid volume and reduced power caused by the withdrawal of the material at the upstream side can be compensated.

Example 2

The invention also provides a method for separating the gulonic acid mother liquor based on the separation device in the embodiment 1, which comprises a plurality of separation cycles which are continuously executed; each separation period consists of a feeding step, a closed cycle step, a first impurity removing step, a second impurity removing step, a third impurity removing step, a fourth impurity removing step and a fifth impurity removing step; and after the fifth impurity removing step of the previous period is finished, entering the feeding step of the next period.

Fig. 6A and 6B show the line-on state of the system at the feed step. The feeding step comprises two sub-steps, which are respectively referred to as a front feeding stage and a rear feeding stage for the convenience of description.

FIG. 6A shows the feed front section, the separation device is in a state of pipeline connection; at this time, the feed valve 18 is opened to supply the raw material liquid to the # 1 column group 1, the CD valve at the bottom of the # 2 column group 1 is opened, and the fast component CD (the fast component CD in this example is a heteropolyacid) is discharged from the bottom of the # 2 column group 1; simultaneously opening a water inlet valve 19 corresponding to the No. 4 chromatographic column group 1 and a BD valve at the bottom of the No. 6 chromatographic column group 1 to supply water analysis agent to the top of the No. 4 chromatographic column group 1 and discharging an intermediate component BD (in the embodiment, the intermediate component BD is gulonic acid) from the bottom of the No. 6 chromatographic column. In the stage, the 1# -6# chromatographic column group 1 is communicated end to end in sequence; wherein the top of column set 1# 1 is fed and the bottom of column set 1# 2 is lined with fast impurities (i.e. fast component CD), column set 1# and 2# are configured as two adsorption zones Z31 and Z32; feeding water into the top of the 4# chromatographic column group 1, and discharging the gulonic acid product (namely the intermediate component BD) from the bottom of the 6# chromatographic column group 1, wherein the 4# chromatographic column 1 forms a resolving area Z1, and the 5# and 6# chromatographic column groups 1 form two separation areas Z21 and Z22; in this stage, no stream is sent to the # 3 column set 1, since the fast component CD in the feed stream is discharged at the bottom of the # 2 column set 1; the inlet water is arranged at the top of the 4# chromatographic column group 1; in this stage, no material flows through the 3# column, thus forming an isolation zone Z4 separating the adsorption zone from the desorption zone.

It should be understood that the adsorption zone, the isolation zone, the resolution zone and the separation zone described in the present application are only descriptions of functions performed by each column set 1 at a certain stage or at a certain moment, and are not fixed at specific corresponding positions (i.e. corresponding column set numbers), but are continuously switched along with the separation process.

FIG. 6B shows the feeding back stage, in which the 1# -6# chromatographic column sets 1 are connected end to end in sequence, and the feeding is continued on the top of the 1# chromatographic column set 1; continuously extracting BD from the bottom of the No. 6 chromatographic column group 1; and the bottom of the 2# chromatographic column group 1 stops discharging the fast impurities; and the water feeding is stopped at the top of the 4# chromatographic column group 1.

The process described above refers to the inlet and outlet of each line after the separation process has run smoothly for several cycles. It is to be noted that when the separation apparatus is just in operation on and there is no liquid filling in each column set, at this particular time, the intermediate fraction BD is not discharged from the BD outlet at the bottom of the column set # 6 1 (because the feed has not yet moved to the column set # 6), but water. Therefore, to ensure the purity of the collected BD, the BD discharged from the bottom of the 6# column set 1 at that particular time period needs to be separately collected or discarded.

And when the BD in the No. 6 chromatographic column group 1 is detected to be exhausted in the process of the later feeding stage (the BD contained in the material flow fed through the No. 1 chromatographic column group in the last separation period moves into the No. 6 chromatographic column group after being subjected to impurity removal and elution for a plurality of times, and the BD contained in the material flow newly added into the No. 1 chromatographic column group in the current separation period does not move into the No. 6 chromatographic column group), switching to the closed cycle step.

FIG. 7 shows a closed cycle step, at this stage, the # 1 to # 6 column sets 1 are sequentially communicated end to end, and the bottom of the # 6 column set 1 is communicated with the top of the # 1 column set 1 to form a circulation loop; meanwhile, all the chromatographic column groups 1 are not fed or discharged (no feeding, no water feeding or no extraction), and the material flow in the columns is driven by a circulating pump arranged between the chromatographic column groups 1. The liquid circulation volume of the closed circulation stage is obtained by a flow meter arranged on the circulation pipeline (in the figure, at the outlet circulation pipe of the No. 4 chromatographic column group), when the circulation volume enables the material in each chromatographic column group 1 to move downstream, the corresponding amount of components are separated, when the circulation is carried out until the fast component CD just reaches the fast component outlet of the second Z3 (hereinafter, the material in the column is moved downstream by one column position), at the moment, the circulation is switched to the first impurity removing step.

It should be noted that although the drawings of the present invention show that the circulation pipe section connected between the # 6 column set 1 and the # 1 column set 1 is longer than the other circulation pipe sections, this is only for convenience of showing the connection relationship of each column set 1 in a plan view, and is not used for reflecting the real size of the circulation pipe section. The circulation pipe sections connected between the heads and the tails of the chromatographic column sets 1 in the present invention have the same length and inner diameter, and thus the volumes of the circulation pipe sections are the same.

The first impurity removal step includes two sub-steps, namely a first impurity removal step C, which is a step of removing the fast component CD in the first impurity removal step (in this embodiment, the fast component CD is specifically a heterosugar and other fast component impurities). As shown in figure 8A of the drawings,

in the first row C, in the process, the desorption agent water is input from the top of the 5# chromatographic column group 1 (corresponding to the functional zone Z1 at this time), the CD is discharged from the outlet at the bottom of the 3# chromatographic column group 1 (corresponding to the functional zone Z32 at this time), and due to the continuous addition of the fresh desorption agent water, the components in the system are still in the moving process during the CD discharge process, and the adsorption separation process of the resin on the material flow is continuously carried out.

When the first row C section is finished (the CD part clearly divided after flowing through the column group is completely discharged), the AD at this time is just at the outlet position of the 5# column group 1 (Z1 at this moment), and enters the first row a section, which is the process of resolving the AD, and the resolving water inlet is still injected at the top of the 5# column group 1 (Z1 inlet). At this time, the volume of the liquid circulation just passes through one column, and enters the next chromatographic column group after AD extraction is finished (the AD part clearly divided at the position is completely discharged). That is, after passing through closed cycle, the first row C section and the first row A section, the liquid in each chromatographic column group 1 in the system moves to the next chromatographic column group 1; for example, after one closed cycle, the liquid originally contained in column set # 1 moves into column set # 2, with the input and input rates of the desorbent water being the same as the production and production rates of CD and AD, respectively.

Here, the determination of the timing of ending the first row C section and the first row a section is described; after one closed cycle separation, the gulonic acid raw material solution containing ABC three components moves to the downstream side by a column position in a cycle separation device consisting of six chromatographic column groups; although in the last step (i.e., the feeding step), the fast component CD first separated through the # 1 and # 2 column set 1 has been discharged from the bottom of the # 2 column set; but after a closed cycle, the material again moves forward by the distance of the adsorbent layer with the length of the column; thus, new fast component CD is separated from the bulk feed stream to form a new clearly segmented CD fraction and reaches the bottom of the # 3 column set 1 earlier than the bulk feed; at this time, the bottom of the 3# column set 1 may start the first row C section until the first row C section is judged to be finished after all the newly generated clearly divided CD portions are discharged from the bottom of the 3# column set 1.

The ending time of the first row A section and the row C section and the row A section in the subsequent steps can be judged according to the same method.

It should be noted that the first row C of the section in the present invention does not mean that the fast component CD is discharged for the first time in one separation cycle, and as described above, the discharge of the fast component CD for the first time in the cycle is already performed in the feeding step.

The first impurity removal step further includes a first impurity removal section a, that is, a stage of removing the slow component AD (in this embodiment, the specific slow component AD is vitamin C and slow component impurities) in the first impurity removal step. As shown in fig. 8B, the analysis agent water was fed from the top of the 5# column set 1, and the slow component AD was drained from the bottom. The first row a section is executed after the first row C section, and at this stage, the input amount and input rate of the resolver water are the same as the production rate of the production magnitude of AD.

The relation between the input quantity and the input rate of the analysis agent water and the extraction quantity and the extraction rate of the CD and the AD is to ensure that the total quantity of liquid in the system is constant in the water inlet and extraction processes; it should be understood that the feeding, feeding and withdrawal processes of all separation stages, except the first start-up stage, follow the principle of keeping the total amount of liquid in the system constant, and will not be described in detail below.

As can be seen from fig. 8A-8B, after one closed cycle, the corresponding functional zone also moves a chromatographic column set to the downstream side as the material moves a column position to the downstream side.

And after the first row A section is finished, switching to a closed cycle step, and moving the material to a column position again.

And after the closed loop step is finished, switching to a second impurity removing step. Similar to the first purging step, the second purging step also includes two sub-steps, a second row C of sections and a second row a of sections.

Fig. 9A shows the second row C of sections, draining the fast component CD from the bottom of column set 4# 1 while feeding the resolver water from the top of column set 6# 1.

Fig. 9B shows the second row a section, with the input of the resolving agent water from the top and the bottom of column set # 6 1 to remove the slow component AD.

And after the second row A, switching to a closed cycle step, moving the material to a column position again, and then switching to a third impurity removal step.

The third impurity removing step comprises two sub-steps of a third row C section and a third row A section.

Figure 10A shows the third row C of sections, draining the fast component CD from the bottom of column set # 5 1 while feeding the resolver water from the top of column set # 1.

Fig. 10B shows the third row a section, with the input of the resolving agent water from the top and the bottom of column set 1# 1 to remove the slow component AD.

And after the section A of the third row is finished, switching to a closed cycle step, moving the material to a column position again, and then switching to a fourth impurity removing step.

The fourth impurity removing step comprises two sub-steps of a fourth row C section and a fourth row A section.

Fig. 11A shows the fourth row C of sections, draining the fast component CD from the bottom of column set # 6 1 while feeding the resolver water from the top of column set # 2 1.

Fig. 11B shows section a in the fourth row, feeding the resolving agent water from the top of column set # 21 and discharging the slow component AD from the bottom.

And after the section A of the fourth row is finished, switching to a closed cycle step, moving the material to a column position again, and then switching to a fifth impurity removing step.

The fifth impurity removing step comprises two sub-steps of a fifth row C section and a fifth row A section.

Figure 12A shows the fifth row C section, draining the fast component CD from the bottom of column set 1# 1 while feeding the resolver water from the top of column set 1# 3.

Fig. 12B shows the fourth row a section, with the input of the resolving agent water from the top of column set # 31 and the bottom with the slow component AD.

And after the section A in the fifth row is finished, switching to the step of closed cycle, moving the material by one column position again, and then switching to the feeding step of the next separation period.

As can be seen from the above description, the feed liquid is supplied to the top of the # 1 column set only during the feeding step stage during each separation cycle, and no feed is supplied during the other steps; discharging the intermediate fraction BD from the bottom of the # 6 column set 1 only during the feeding step; in a separation period, each step comprises a row C section sub-step, namely comprising 6 row C sections; the first through fifth impurity removing steps include row a segment sub-steps, i.e., including 5 row a segments.

The above is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. An industrialized gulonic acid three-component separation device comprises a separation unit consisting of six chromatographic column groups (1); the six chromatographic column groups (1) are sequentially numbered as 1# -6# according to the circulation direction of liquid in the system; the 1# -6# chromatographic column group (1) is sequentially connected end to end through a circulating pipe section to form a circulating loop; the top parts of the six chromatographic column groups (1) are respectively provided with a water distribution pipe (14) with a water inlet valve (19), and the bottom parts of the six chromatographic column groups are respectively provided with a CD branch pipe (16) with a CD valve and an AD branch pipe (15) with an AD valve; the method is characterized in that: only the top of the 1# chromatographic column group (1) is provided with a raw material branch pipe (13) with a feed valve (18); only the bottom of the 6# chromatographic column group (1) is provided with a BD tube (12) with a BD valve; each of said chromatography column sets (1) comprising a mixing distributor (24); the mixing distributor (24) is of a symmetrical cylindrical structure, a receiving opening (28) is respectively arranged at the upper end and the lower end of the mixing distributor, and the two receiving openings (28) are respectively connected to an incoming flow pipe (25) through an incoming flow branch pipe (26) to be used for receiving incoming flow; the mixing distributor (24) comprises a power cavity (29) positioned between the two receiving openings (28), and the two receiving openings (28) are respectively communicated with the corresponding ends of the power cavity (29) through a connecting channel (30); at least one mixing device (31) is arranged in each connecting channel (30), the tail end of each connecting channel (30) is provided with a first one-way valve (34) which can only be opened inwards, and the first one-way valve (34) only allows the incoming flow to enter the power cavity (29) through the connecting channel (30); a plurality of shunt tubes (32) are arranged on the circumferential wall of the top part and the circumferential wall of the bottom part of the power cavity (29) at equal intervals, a piston (33) is arranged in the power cavity (29) in a sealing and sliding manner, and the piston (33) divides the power cavity (29) into an upper power chamber and a lower power chamber; the plurality of the shunt tubes (32) are respectively positioned at the top of the upper power chamber and the bottom of the lower power chamber, and the number and the size of the shunt tubes (32) positioned in the upper power chamber and the lower power chamber are the same; wherein AD is a slow component, BD is an intermediate component, and CD is a fast component; each chromatographic column group (1) comprises a plurality of chromatographic columns (22) which are connected in parallel, and each chromatographic column (22) has the same parameter; the mixing distributor (24) can receive incoming flow, fully mix the incoming flow and uniformly distribute the mixed incoming flow to upper inlets of the chromatographic columns (22) forming the corresponding chromatographic column group (1) through a distribution pipe (23); the bottom outlets of a plurality of chromatographic columns (22) forming the corresponding chromatographic column group (1) are collected in the circulating pipe (9) through a confluence branch pipe (21); wherein, the incoming flow pipe (25) of the mixing distributor (24) corresponding to the 1# chromatographic column group (1) is connected with a circulating pipe (9), a water dividing pipe (14) and a raw material branch pipe (13); the inflow pipe (25) of the mixing distributor (24) corresponding to the 2# -6# chromatographic column group (1) is only connected with the circulating pipe (9) and the water dividing pipe (14); each of the shunt tubes (32) transversely penetrates through the side wall of the mixing distributor (24) and is connected to a corresponding slot (36) arranged on the side wall of the mixing distributor (24); the connection part of the slot (36) and the corresponding shunt tube (32) is provided with a second one-way valve (37) which can only be opened outwards, and the second one-way valve (37) only allows the shunt tube (32) to flow to the corresponding slot (36); the piston (33) can be tightly attached to the end part of the corresponding power chamber when the corresponding first one-way valve (34) is closed, so that the liquid in the corresponding power chamber can be drained during each liquid drainage process; the piston (33) comprises a magnetic inner core and a corrosion-resistant layer wrapping the magnetic inner core; meanwhile, a magnetic induction coil (35) is respectively arranged at the upper side and the lower side of the power cavity (29), and a magnetic field for driving the piston (33) to reciprocate is formed by supplying current to the magnetic induction coil (35), so that liquid suction and liquid discharge operations are completed; a plurality of Y-shaped pipes are arranged at the periphery of the mixing distributor (24), and each Y-shaped pipe comprises two Y-shaped branch pipes (27) and a Y-shaped main pipe (38) connected to one end of each of the two Y-shaped branch pipes (27); the two Y-shaped branch pipes (27) are respectively matched and connected with an upper slot (36) and a lower slot (36) of the mixing distributor (24); the Y-shaped main pipe (38) is connected with each chromatographic column (22) in the chromatographic column group (1) through the distributing pipe (23); the Y-shaped main pipe (38) is provided with an adjusting valve (39) and a flow sensor (40), and the adjusting valve (39) allows the incoming flow flowing through the corresponding Y-shaped main pipe (38) to be adjusted or completely closes the corresponding Y-shaped main pipe (38).

2. The industrial gulonic acid three-component separation device according to claim 1, wherein: the separation device also comprises an AD tank (4), a CD tank (5) and a BD tank (6); an AD main pipe (10) is connected to the inlet of the AD tank (4), and the AD main pipe (10) is connected to the upstream of each section of circulating pipe (9) located at the corresponding circulating valve (17) through an AD branch pipe (15) with an AD valve; a CD main pipe (11) is connected to the inlet of the CD tank (5), and a CD branch pipe (16) with a CD valve is connected to the CD main pipe (11) on the upstream of the corresponding circulating valve (17) on each section of circulating pipe (9); the inlet of the BD tank (6) is connected with the bottom of the 6# chromatographic column group (1) through a BD pipe (12).

3. A method for separating a gulonic acid mother liquor based on the separation device of any one of claims 1-2, characterized in that: comprises a plurality of separation periods which are continuously executed; each of the separation cycles comprises the following steps performed in sequence:

1. a feeding step; inputting a gulonic acid mother liquor raw material solution at the top of a 1# chromatographic column group (1), and discharging partial fast component CD from the bottom of the 2# chromatographic column group (1); discharging the intermediate component BD contained in the raw material liquid entering the system in the last separation period from the bottom of the No. 6 chromatographic column group (1);

2. a closed cycle step; all the chromatographic column groups are not fed and not extracted, and the material flow in the columns is driven by a circulating pump arranged between each chromatographic column group; acquiring the liquid circulation amount of the step through a flowmeter arranged on the circulation pipe, wherein the circulation amount enables the material in each chromatographic column group (1) to move one column position downstream;

3. a first impurity removal step; the device comprises a first row C section and a first row A section which are executed in sequence; when the first row C section is formed, discharging the fast component CD from the bottom of the 3# chromatographic column group, and simultaneously inputting the analysis agent water from the top of the 5# chromatographic column group; when the section A is arranged in the first row, the analytic agent water is input from the top of the No. 5 chromatographic column group, and the slow component AD is discharged from the bottom; after the first row A section is finished, switching to a closed cycle step, and enabling the feed liquid in the column to move downstream one column position again;

4. a second impurity removal step; the device comprises a second row C section and a second row A section which are executed in sequence; during the second row of section C, fast component CD is discharged from the bottom of the No. 4 chromatographic column group, and meanwhile, the analytic agent water is input from the top of the No. 6 chromatographic column group; when the section A is arranged in the second row, the analytic reagent water is input from the top of the 6# chromatographic column group, and the slow component AD is discharged from the bottom; after the section A of the second row is finished, switching to the closed cycle step, moving the feed liquid in the column to a column position downstream again, and then switching to the third impurity removing step;

5. a third impurity removing step; the device comprises a third row C of sections and a third row A which are executed in sequence; in the third row of section C, fast component CD is discharged from the bottom of the No. 5 chromatographic column group, and meanwhile, the analytic reagent water is input from the top of the No. 1 chromatographic column group; when the section A is arranged in the third row, the analytic agent water is input from the top of the 1# chromatographic column group, and the slow component AD is discharged from the bottom; after the third row of section A is finished, switching to a closed cycle step, moving the feed liquid in the column to a column position downstream again, and switching to a fourth impurity removal step;

6. a fourth impurity removal step; comprises a fourth row C section and a fourth row A section which are executed in sequence; during the fourth row of section C, fast component CD is discharged from the bottom of the No. 6 chromatographic column group, and meanwhile, the analytic agent water is input from the top of the No. 2 chromatographic column group; when the section A is arranged in the fourth row, the analytic agent water is input from the top of the 2# chromatographic column group, and the slow component AD is discharged from the bottom; after the section A in the fourth row is finished, switching to the closed cycle step, moving the feed liquid in the column to a column position downstream again, and then switching to the fifth impurity removing step;

7. a fifth impurity removing step; the first row C section and the second row A section are executed in sequence; during the section C of the fifth row, fast component CD is discharged from the bottom of the No. 1 chromatographic column group, and meanwhile, the analytic agent water is input from the top of the No. 3 chromatographic column group; when the section A is arranged in the fifth row, the analytic agent water is input from the top of the 3# chromatographic column group, and the slow component AD is discharged from the bottom; after the section A in the fifth row is finished, switching to a closed cycle step, moving the feed liquid in the column to a column position downstream again, and switching to a feeding step;

wherein A is a slow component, B is an intermediate component, and C is a fast component.

4. The method of claim 3, wherein: the feeding step comprises two substeps of feeding front section and feeding rear section which are executed in sequence; in the feeding of the former stage, the raw material liquid is fed from the top of the No. 1 column group (1), and part of the fast component CD is discharged from the bottom of the No. 2 column group (1); meanwhile, the water analysis agent is supplied from the top of the 4# chromatographic column group (1), and the intermediate component BD is discharged from the bottom of the 6# chromatographic column group (1); when feeding the rear section, feeding continuously from the top of the No. 1 chromatographic column group (1); continuously extracting BD from the bottom of the 6# chromatographic column group (1); and the bottom of the 2# column set (1) stopped discharging the fast component CD; and the water inlet is stopped at the top of the 4# chromatographic column group (1); when the BD component in the No. 6 chromatographic column was exhausted, the column was switched to the closed cycle step.

5. The method of claim 4, wherein: in each separation period, each step comprises a row C section sub-step, namely comprising 6 row C sections; the first to fifth impurity removing steps comprise a segment A removing sub-step, namely, comprising 5 segments A; each separation cycle is depleted of the fast component CD, the intermediate component BD and the slow component AD contained in the feed of the previous separation cycle.

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