CN106267894B - Series connection simulation moving bed system - Google Patents

Series connection simulation moving bed system Download PDF

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Publication number
CN106267894B
CN106267894B CN201610729228.3A CN201610729228A CN106267894B CN 106267894 B CN106267894 B CN 106267894B CN 201610729228 A CN201610729228 A CN 201610729228A CN 106267894 B CN106267894 B CN 106267894B
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China
Prior art keywords
section
moving bed
effluent
simulated moving
series connection
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CN201610729228.3A
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CN106267894A (en
Inventor
梁茹茜
梁明在
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Jope Tech Co
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Jope Tech Co
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/18Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
    • B01D15/1814Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns recycling of the fraction to be distributed
    • B01D15/1821Simulated moving beds
    • B01D15/1842Simulated moving beds characterized by apparatus features
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/18Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
    • B01D15/1814Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns recycling of the fraction to be distributed
    • B01D15/1857Reactive simulated moving beds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/18Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
    • B01D15/1864Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using two or more columns
    • B01D15/1871Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using two or more columns placed in series

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The invention provides a series-connection simulation moving bed system which is suitable for separating intermediate components with intermediate retention constants in a mixture with three components. The series simulated moving bed system comprises a first-stage simulated moving bed, a second-stage simulated moving bed, a side flow pipeline and a liquid concentration homogenization module. The first and second simulated moving beds are respectively composed of a mobile phase and a stationary phase, the mobile phase is respectively arranged in the first and second simulated moving beds and flows along a first direction, and the stationary phase is in simulated movement relative to the mobile phase towards a second direction opposite to the first direction. And the side flow pipeline and the liquid concentration homogenizing module are used for connecting the first-stage simulated moving bed and the second-stage simulated moving bed. The series-connected simulated moving bed system provided by the invention can provide a side stream with stable concentration, continuously and stably separate out middle retention components, and can discharge strong retention components out of the system in time.

Description

Series connection simulated moving bed system
Technical field
This case relates to a kind of simulated moving bed system, and can isolate intermediate anelasticity in particular to one kind The series connection simulated moving bed system of ingredient.
Background technique
Four traditional sections or three section Simulation moving beds (Simulated Moving Bed, SMB) can only be by multicomponents Mixture be separated into two component groups.If being separately separated out intermediate anelasticity ingredient, then need to arrange in pairs or groups other separation skills Art or twice Simulation moving bed operation.Four traditional section Simulation moving beds cannot be detained what ingredient was separated for intermediate This limitation, so that the industry application of Simulation moving bed is concentrated mainly on the simple system of material composition, such as glucose/fructose point From, xylene isomer separation, optical isomeric compound separation etc..Natural goods intermediate raw material or the medical material of fermentation synthesis, because It is complicated and concentration is low for material composition, while it being frequently present of the very strong ingredient of anelasticity, therefore utilizing Simulation moving bed On be restricted.
Existing scholar proposes concatenated Simulation moving bed to separate ternary intermediate anelasticity ingredient at present, and also leads to Cross the feasibility that simulation calculates it.But the design of this series connection Simulation moving bed still has some problems: first, for connecting Fluctuation of concentration in the effluent of first, second grade of Simulation moving bed influences the separating effect of second level Simulation moving bed big.The Two, between concatenated first, second grade of Simulation moving bed, it is necessary to online concentration process is installed additional, so that processing procedure becomes complicated.The Three, when system is there are when superpower anelasticity ingredient, the system of will lead to can not operate steadily in the long term.Therefore in addition to needs will be intermediate stagnant Except the System and method for that the property stayed ingredient is separated, also to have can be in time by setting outside strong anelasticity ingredient discharge system Meter just can effectively solve simulated moving bed technology the problem of the application of these industries is met with.
Summary of the invention
This case provides a variety of series connection simulated moving bed systems and multicomponent chromatographic separating process, is capable of providing concentration and stablizes Effluent, it is continuous and stable isolate intermediate anelasticity ingredient, and can in time will be outside strong anelasticity ingredient discharge system.
A kind of series connection simulated moving bed system of this case is suitable for separating mixture, and mixture includes first composition group, second Components group and third components group, the first delay constant, the second delay constant and the third being respectively provided with from small to large are detained constant, The first composition group includes at least first composition, and the second composition group includes at least second composition, the third components group Including at least third ingredient.Connect simulated moving bed system include first, second grade of Simulation moving bed, side-stream line, dashpot, Effluent pressure regulator, effluent pump and regeneration interval.First order Simulation moving bed includes arranged in the first direction first, Two, third section.Second level Simulation moving bed includes the four, the 5th section arranged in the first direction.First, second grade of simulation Moving bed is made of mobile phase and stationary phase, and mobile phase is respectively in first, second grade of Simulation moving bed along first direction Flowing, stationary phase mutually simulate movement towards the second direction in contrast to first direction relative to mobile.Side-stream line connection first, the It second level Simulation moving bed and is exported including effluent entrance and effluent.Effluent entrance is connected between the first section and the second section, Effluent outlet is connected between the 4th section and the 5th section.Dashpot configures in side-stream line.Effluent pressure regulator is matched It sets in side-stream line and is located between dashpot and effluent outlet.Effluent pump configuration is in side-stream line and is located at dashpot And between effluent pressure regulator.First order Simulation moving bed is used for the first composition group of separating mixture, and the of mixture Binary group, third components group are moved to along side-stream line through dashpot, effluent pump, effluent pressure regulator from the second section Between 4th section and the 5th section, and it is separated in the Simulation moving bed of the second level.Regeneration interval is the 6th section, edge First direction is arranged in by the 5th section and including wetted area and strong cleaning area.
In an embodiment of this case, above-mentioned series connection simulated moving bed system further includes central valve group, including first Point and second part, wherein first part along axis selectively relative to second part rotate, to switch the more of first part Alignment between a first passage and multiple second channels of second part, these second channels of part are respectively with One, second, third, fourth, fifth and the connection of the 6th section.
In an embodiment of this case, above-mentioned series connection simulated moving bed system further includes multiple liquid supply tanks, multiple Mainstream pump, multiple liquid recoveries and multiple mainstream pressure regulators.These liquid supply tanks respectively with part these first Channel connection, movement mutually respectively include at least one punching and wash liquid, and at least one punching is accommodated in each liquid supply tank and washs liquid.These mainstreams pump It is connected to respectively with these first passages of these liquid supply tanks and part.These liquid recoveries respectively with part these First passage connection, and liquid recovery is suitable for accommodating at least one punching and washs liquid.These mainstream pressure regulators, respectively with these liquid Body accumulator tank is connected to these first passages of part.
In an embodiment of this case, the quantity of these above-mentioned liquid supply tanks and these mainstreams pump is respectively five, Five liquid supply tanks and five mainstreams pump be separately positioned between source, the second section and the third section of the first section, the Source, wetted area and the strong cleaning area of four sections.
In an embodiment of this case, the quantity point of these above-mentioned liquid recoveries and these mainstream pressure regulators Wei not be two, two liquid recoveries and two mainstream pressure regulators are separately positioned on the end of third section, the 5th area The end of section.
In an embodiment of this case, the section of above-mentioned first, second, third, fourth, the 5th and the 6th distinctly include to Lack a root canal column, there is inside filler particles the stationary phase of hole in every root canal column.
In an embodiment of this case, above-mentioned mobile phase flows through the first, second, third, fourth, the 5th with first direction The strong cleaning area of section and the 6th section, and flow through with second direction the wetted area of the 6th section.
Based on above-mentioned, the series connection simulated moving bed system of this case passes through side-stream line first, second grade of simulation of connecting and moves Bed is detained the inter-level of constant between to isolate in mixture.Since Simulation moving bed is switched to by these tubing strings Fluctuation of concentration is had when different sections, separating effect of the fluctuation of concentration in the effluent of side-stream line to second level Simulation moving bed It influences greatly, in order to reduce the fluctuation of concentration in effluent, this case installs dashpot additional in side-stream line, and middle delay ingredient and height are stagnant Profit retention point can be introduced into dashpot in side-stream line, and concentration tends to after stablizing in dashpot, can just flow to second level mould Quasi- moving bed, so that second level Simulation moving bed has preferable separating effect.In addition, the series connection simulated moving bed system of this case It further include regeneration interval, the stationary phase of the first section of first order Simulation moving bed is recycled back into the by regeneration interval cleaning Second level Simulation moving bed can in time and effectively will be strong without taking strong anelasticity ingredient toward second level Simulation moving bed The discharge of anelasticity ingredient, and enable the use of simulated moving bed system for a long time of connecting.In addition, the design of regeneration interval The flow velocity of effluent can also be improved it is unnecessary to guarantee the function of second level Simulation moving bed, operating condition can be more convenient Setting.
To make the foregoing features and advantages of the present invention clearer and more comprehensible, special embodiment below, and it is detailed to cooperate attached drawing to make Carefully it is described as follows.
Detailed description of the invention
Fig. 1 is the schematic diagram according to a kind of series connection simulated moving bed system of an embodiment of this case;
Fig. 2 is schematic diagram of the series connection simulated moving bed system in next timing of Fig. 1;
Fig. 3 is the multicomponent chromatographic separating process according to a kind of series connection simulated moving bed system of an embodiment of this case Flow diagram;
Fig. 4 is the piping schematic diagram of Fig. 1;
Fig. 5 is the diagrammatic cross-section of the central valve group of the series connection simulated moving bed system of Fig. 1;
Fig. 6 is the diagrammatic cross-section of the line A-A section along Fig. 5;
Fig. 7 is the diagrammatic cross-section of the line B-B section along Fig. 5;
Fig. 8 to Figure 11 is the second of the series connection simulated moving bed system of Fig. 1 and the second of third section and third phase convection current The relational graph of 4th and the 5th relative velocity m4 and m5 of fast m2 and m3 and the 4th and the 5th section.
Description of symbols:
A: first composition (group);
B: second composition (group);
C: third ingredient (group);
D1: first direction;
D2: second direction;
L1, L2: liquid is washed in punching;
100: series connection simulated moving bed system;
110: first order Simulation moving bed;
Z1: the first section;
Z2: the second section;
Z3: third section;
120: second level Simulation moving bed;
Z4: the four section;
Z5: the five section;
130: regeneration interval;
Z6: the six section;
132: wetted area;
134: strong cleaning area;
140: side-stream line;
142: effluent entrance;
144: effluent outlet;
150: strength of fluid homogenizes module;
152: dashpot;
155: effluent pressure regulator;
157: effluent pump;
160: central valve group;
162: first part;
164: first passage;
166: second part;
168: second channel;
170: liquid supply tank;
172: mainstream pump;
174: liquid recovery;
176: mainstream pressure regulator;
180: tubing string;
200: the multicomponent chromatographic separating process for simulated moving bed system of connecting;
210~240: step.
Specific embodiment
The series connection simulated moving bed system 100 of the present embodiment, which is suitable for isolating, at least to be had in ternary mixture, stagnant Stay the inter-level of constant between.More particularly, mixture includes at least first composition group A, second composition group B and the Three components group C, the first delay constant, the second delay constant and the third being respectively provided with from small to large are detained constant.First composition Group includes at least first composition, and second composition group includes at least second composition, and third components group includes at least third ingredient.When So, the series connection simulated moving bed system 100 of the present embodiment can also be applied to more than it is more than three components groups (such as with four ingredients Group) mixture, be not limited in be used in separation three components groups mixture.
Fig. 1 is the schematic diagram according to a kind of series connection simulated moving bed system 100 of an embodiment of this case.Please referring initially to figure 1, the series connection simulated moving bed system 100 of the present embodiment is by taking six section Simulation moving beds as an example.Series connection simulated moving bed system 100 Module 150 is homogenized including first order Simulation moving bed 110, second level Simulation moving bed 120, side-stream line 140, strength of fluid And regeneration interval 130.
Specifically, first order Simulation moving bed 110 includes the first, second, third section along first direction D1 arrangement Z1,Z2,Z3.Second level Simulation moving bed 120 includes the four, the 5th section Z4, Z5 along first direction D1 arrangement.In this implementation In example, respectively there are two tubing strings 180 respectively by first, second, third section Z1, Z2, Z3, the four, the 5th section Z4, Z5.Renewing zone Section 130 is the 6th section Z6, is arranged in by the 5th section along first direction D1 and equally includes two tubing strings 180, one of them Tubing string 180 is wetted area 132, another tubing string 180 is strong cleaning area 134.Certainly, 180 quantity of tubing string in each section can also To be one or three or more, it is not limited thereto system.
First, second grade of Simulation moving bed 110,120 and regeneration interval 130 are made of mobile phase and stationary phase respectively. More particularly, there is the stationary phase of hole, mixture is admitted to specific in every root canal column 180 of each section inside filler particles It can be adsorbed in stationary phase after in tubing string 180.Mobile mutually includes that liquid L1, L2 are washed at least one punching, mobile mutually to flow into and outflow tubing string 180 rinse the mixture being adsorbed in stationary phase, to separate the components into.As shown in Figure 1, mobile mutually respectively first, second It is flowed in strong cleaning area 134 in grade Simulation moving bed 110,120 and regeneration interval 130 along first direction D1, stationary phase is opposite Movement mutually is simulated towards the second direction D2 in contrast to first direction D1 in mobile.By mobile phase and the mutual counter current contacting of stationary phase It is detained the lower ingredient of constant to rinse to isolate.
It to be explained further herein, it is to pass through that relative to mobile phase, D2 simulates mobile mode to stationary phase in a second direction Switch the inlet and outlet of mobile phase and the import of mixture, constantly to produce stationary phase with opposite direction (being counterclockwise in Fig. 1) The phenomenon that flowing.Such as in current Fig. 1, tubing string 180 from left to right is sequentially first, second, third, fourth, the 5th, Six section Z1, Z2, Z3, Z4, Z5, Z6, if allow mobile phase inlet and outlet and mixture import after a period of time clockwise Direction switches to next tubing string 180, will be as shown in Figure 2.
Fig. 2 is schematic diagram of the series connection simulated moving bed system 100 in next timing of Fig. 1.As shown in Fig. 2, from a left side to Right tubing string 180 be sequentially the 6th section Z6 the 134, first, second, third, fourth, the 5th section Z1, Z2 of strong cleaning area, The wetted area 132 of Z3, Z4, Z5 and the 6th section Z6.It is further continued for edge after a period of time and switches to next tubing string clockwise 180, by just will form the similar emulation mode for allowing stationary phase to flow along counterclockwise after continuously switching.And This simultaneously, mobile phase then always continuously clockwise flow, and reach simulation stationary phase and flowing the continuous reverse flow of item The process of contact.
Therefore, it is detained the different two-component group of constant and enters Simulation moving bed when having, and is adsorbed on stationary phase and is flowed When Xiang Suochong is washed, wherein the components group of low hold-up constant can be gone out stationary phase by mobile phase, and with mobile phase toward clockwise Direction is moved to next tubing string 180 on first direction D1;The components group that height is detained constant is gone out due to being not easy by mobile phase, After inlet and outlet switching, can mutually it drive and as being fixed toward being counterclockwise moved to next pipe on second direction D2 Column 180.
Fig. 1 is gone back to, side-stream line 140 connects first, second grade of Simulation moving bed 110,120 and makes first, second grade Simulation moving bed 110,120 is cascaded.Side-stream line 140 includes effluent entrance 142 and effluent outlet 144.Effluent entrance 142 are arranged between the first section Z1 of first order Simulation moving bed 110 and the second section Z2, and 144 setting of effluent outlet is the Between 4th section of second level Simulation moving bed 120 and the 5th section.
It is noted that the mixture due to part can be moved to second level Simulation moving bed from side-stream line 140 120, the fluctuation of concentration of the mixture in side-stream line 140 separating effect of second level Simulation moving bed 120 is influenced it is big, in order to It can reduce the fluctuation of concentration of the mixture in side-stream line 140, the present embodiment is dense by configuring liquid in side-stream line 140 Degree homogenization module 150.More particularly, strength of fluid homogenization module 150 includes dashpot 152, in side-stream line 140 In mixture can be introduced into dashpot 152, in dashpot 152 concentration tend to stablize after, can just flow to the second level simulation Moving bed 120, so that second level Simulation moving bed 120 has preferable separating effect.In the unshowned embodiment of an embodiment In, strength of fluid homogenization module 150 further includes the agitator in dashpot 152, to accelerate to flow into dashpot 152 The homogenization of strength of fluid.
In addition, effluent pressure regulator 155 is arranged in side-stream line 140 and is located at dashpot 152 and effluent exports Between 144.Effluent pump 157 is arranged in side-stream line 140 and between dashpot 152 and effluent pressure regulator 155. In the present embodiment, effluent pump 157 also has metering other than having and improving effluent in the pressure in side-stream line 140 Function.In addition, in the present embodiment, effluent pressure regulator 155 can be counterbalance valve, the effect of pressure stabilizing is provided, effluent exists Pressure in side-stream line 140 needs that second level Simulation moving bed could be flowed to from side-stream line 140 within the scope of certain 120.That is, effluent pressure regulator 155 can make the flow control for the fluid for flowing into second level Simulation moving bed 120 exist Within a certain range.In the present embodiment, mistake of the part mixes from first order Simulation moving bed 110 Jing Guo side-stream line 140 Cheng Zhonghui enters back into second level simulation movement after sequentially passing through dashpot 152, effluent pump 157 and effluent pressure regulator 155 Bed 120, and the mixture with stable concentration and flow velocity is capable of providing to second level Simulation moving bed 120.
According to above-mentioned actuation mode, Fig. 3 is a kind of series connection simulated moving bed system 100 according to an embodiment of this case Multicomponent chromatographic separating process flow diagram.Referring to Fig. 3, the series connection simulated moving bed system 100 of the present embodiment can It is isolated by following multicomponent chromatographic separating process and is detained the second composition group B of constant between, series connection simulation moves The multicomponent chromatographic separating process 200 of bed system 100 includes the following steps.
Firstly, series connection simulated moving bed system 100 is provided such as step 210, wherein series connection simulated moving bed system 100 is wrapped First order Simulation moving bed 110, second level Simulation moving bed 120, side-stream line 140 and strength of fluid homogenization module 150 are included, First, second grade of Simulation moving bed 110,120 is made of mobile phase and stationary phase respectively, and mobile mutually includes that liquid is washed at least one punching L1, L2, system has a hole inside stationary-phase particle size, mobile mutually respectively in first, second grade of Simulation moving bed 110,120 along the One direction D1 flowing, stationary phase mutually simulate movement, the first order towards the second direction D2 in contrast to first direction D1 relative to mobile Simulation moving bed 110 includes first, second, third section Z1, Z2, Z3 along first direction D1 arrangement, second level simulation movement Bed 120 includes the four, the 5th section Z4, Z5 along first direction D1 arrangement, and side-stream line 140 is connected to the first section Z1 and the Between two section Z2 and between the 4th section and the 5th section, strength of fluid homogenization module 150 is configured at side-stream line 140 On.
In the present embodiment, the cleaning solution L1 of the mobile phase of first order Simulation moving bed 110 is from the source of the first section Z1 It is sent into and is moved in first order Simulation moving bed 110 along first direction D1.
Then, it such as step 220, injects the mixture between second and third section Z2, Z3, wherein mixture includes first Components group A, second composition group B and third components group C are respectively provided with the first delay constant, the second delay constant from small to large And third is detained constant.More particularly, second section Z2 and third section Z3 of the mixture from first order Simulation moving bed 110 Between be sent into first order Simulation moving bed 110.
Come again, such as step 230, controls second and third relative velocity m2 and m3 of second and third section Z3 between first It is detained between constant and the second delay constant, so that first composition group A is moved to third section Z3, second composition group B and third Components group C is moved to the second section Z2 and is moved to second level mould along side-stream line 140, strength of fluid homogenization module 150 Quasi- moving bed 120.
In detail, since the delay constant of first composition group A is minimum, first composition group A can mutually be flow to movement Third section Z3 and flow out, and first composition group A is located away from second, third components group B, C.Be detained constant it is higher second, Third components group B, C can be mobile toward the second section Z2, and partial second, third components group B, C can be flowed along side-stream line 140 To between the four, the 5th section Z4, Z5 of second level Simulation moving bed 120.
Then, such as step 240, control the 4th and the 5th relative velocity m4 and m5 of the 4th and the 5th section Z4, Z5 between Second is detained between constant and third delay constant, so that third components group C is moved to the 4th section Z4, second composition group B is moved It moves to the 5th section Z5, and isolates second composition group B.
The cleaning solution L2 of the mobile phase 2 of second level Simulation moving bed 120 is sent into from the source of the 4th section Z4 and second It is moved in grade Simulation moving bed 120 along first direction D1.Similarly, since the delay constant of second composition group B is than third ingredient The delay constant of group C comes low, and second composition group B can mutually flow to the 5th section Z5 with movement and flow out, and by the second one-tenth Group B is divided to be located away from third components group C.In this way, which being detained the second composition group B of constant between just can successfully be separated Out.It should be noted that since the mobile phase of first, second grade of Simulation moving bed 110,120 respectively operates, so first, The rushing of second level Simulation moving bed 110,120 washs liquid L1, L2 can be identical or different.
In addition it is worth mentioning, in the first order Simulation moving bed 110 of Fig. 1, height is detained the third components group C meeting of constant Simulation is movably mobile toward second direction D2 and is stranded in the stationary phase of the first section Z1 (namely positioned at Fig. 1 leftmost Tubing string 180).In order to avoid the high third components group C for being detained constant pollutes tubing string 180, and make series connection simulation movement Bed system 100 can not act on continuously for a long time, and in the present embodiment, the 6th relative velocity m6 for controlling strong cleaning area 134 is big It is detained constant in third, the high third components group C for being detained constant can be removed by regeneration interval 130 (or even has delay constant Higher 4th components group etc.) to regenerate stationary phase.Please arrange in pairs or groups Fig. 2, due to after next switching, the pipe of Fig. 1 leftmost Column 180 is converted to the strong cleaning area 134 of regeneration interval 130 (the 6th section Z6), the high delay being attracted in stationary phase originally The third components group C of constant can leave stationary phase by the effect inversely cleaned by force.Therefore, the series connection simulation of the present embodiment Mobile bed system 100 passes through the design of regeneration interval 130, it can be ensured that after each switching, is attached with high delay constant originally The stationary phase of third components group C can be clearly regenerated.That is, if mixture also has stronger the four one-tenth of anelasticity Divide group's (not shown), the 6th section can effectively remove the 4th components group more stronger than third components group C anelasticity, to ensure to fix The complete regeneration of phase, and then guarantee the stability of long period of operation.
Thereafter, the stationary phase originally positioned at strong cleaning area 134 can be converted to wetting after next switching (not shown) Area 132, in wetted area 132, the moving direction of mobile phase is identical as the simulation moving direction of stationary phase (with second direction D2 shifting It is dynamic), it is used primarily as wetting stationary phase.Next one switching, the stationary phase positioned at wetted area 132 is converted to second originally Grade Simulation moving bed 120 the 5th section Z5, can effectively avoid bring in any strong anelasticity third components group C enter the 5th area Section Z5 and polluted the second composition group B of intermediate anelasticity.
In addition, be explained below between each time section (e.g. under the situation of Fig. 1), control it is mobile mutually with The mechanism part of the flowing of mixture.Fig. 4 is the piping schematic diagram of Fig. 1.Please refer to Fig. 1 and Fig. 4, Simulation moving bed of connecting System 100 further includes multiple liquid supply tanks 170, multiple mainstreams pump 172, multiple liquid recoveries 174 and multiple mainstream pressure Adjuster 176.Liquid supply tank 170 mainly store it is mobile mutually or mixture, these mainstreams pump 172 respectively with these liquid Supply tank 170 is connected to, and provide it is mobile mutually or the enough pressure of mixture enter first, second grade of Simulation moving bed 110, 120 and regeneration interval 130.The mobile phase or mixture of the storage recycling of liquid recovery 174, these mainstream pressure regulators 176 are respectively communicated in these liquid recoveries 174, to reduce pressure so that mobile phase or mixture can be moved to liquid Accumulator tank 174.
More particularly, in the present embodiment, the quantity of these liquid supply tanks 170 and these mainstreams pump 172 is respectively Five, five liquid supply tanks 170 and five mainstreams pump 172 pass through the source of first passage 164 and the first section Z1, the respectively Between two section Z2 and third section Z3, the source of the 4th section Z4, wetted area 132 and strong cleaning area 134 be connected to.These liquid The quantity of accumulator tank 174 and these mainstream pressure regulators 176 is respectively two, two liquid recoveries 174 and two Mainstream pressure regulator 176 is connected to by first passage 164 with the end of the end of third section Z3, the 5th section Z5 respectively.
In addition, simply introduce the inlet and outlet of mobile phase and the import of mixture be how be switched.Fig. 5 is Fig. 1 Series connection simulated moving bed system central valve group diagrammatic cross-section.Please refer to Fig. 4 and Fig. 5, Simulation moving bed of connecting System 100 further includes central valve group 160, and central valve group 160 includes first part 162 and second part 166, first part 162 It is the valve group of the upper half, second part 166 is the valve group of lower half.First part 162 include multiple first passages 164 ( In the present embodiment for 24), second part 166 includes that multiple second channels 168 (are in the present embodiment with 24 Example).It should be noted that Fig. 4 is only the first passage 164 for schematically representing first part 162 in a manner of being arranged in a row And the second channel 168 of second part 166, the arrangement mode of actually the first channel 164 and second channel 168 please refer to Fig. 6 With Fig. 7.
Fig. 6 is the diagrammatic cross-section of the line A-A section along Fig. 5.Fig. 7 is the diagrammatic cross-section of the line B-B section along Fig. 5.It needs It is bright, although Fig. 6 and Fig. 7, only for the channel cross-section of first part 162, the channel cross-section of second part 166 also can be with Fig. 6 is close with Fig. 7, therefore is no longer painted the channel cross-section of second part 166.
It will be appreciated from fig. 6 that in the present embodiment, the first part 162 of central valve group 160 is cylindrical, the isogonism on cylinder These first passages 164 are arranged out to degree, road first passage 164 can be that arrangement circularizes as shown in Figure 6.The center of the present embodiment Valve group 160 is to be respectively provided with 24 first in the section of Fig. 6 and Fig. 7 for being applicable to the valve group of 24 root canal columns 180 and lead to Road 164, that is, it is respectively provided with 24 first passages 164.In the present embodiment due to sharing 12 root canal columns 180, operator can With selected in this 24 first passages 164 wherein it is several angularly or non-equal angular first passage 164 and liquid are supplied Slot 170 is connected to liquid recovery 174, and similarly, operator can select wherein 12 etc. in this 24 second channels 168 Angle or the non-root canal of equal angular second channel 168 and 12 column 180 are connected to.In the section of Fig. 6 and Fig. 7 it can be seen that in difference The extension angle of first passage 164 in plane (A-A section, B-B section) is different, to avoid each other.
As shown in figure 4, wherein 12 first passages 164 of first part 162 respectively with these liquid supply tanks 170, this A little liquid recoveries 174 are connected to, that is, move the inlet and outlet of phase and the import of mixture.Wherein 12 of second part 166 These second channels 168 are connected to this 12 root canal column 180 of the first, second, third, fourth, the 5th and the 6th section Z6 respectively, Namely first, second grade of Simulation moving bed 110,120 and regeneration interval 130.
In the present embodiment, the first part 162 of central valve group 160 does not rotate, and second part 166 can along an axis Selectively rotated relative to first part 162.Spy is rotated in different timing relative to first part 162 by second part 166 Determine angle, and switches between multiple first passages 164 of first part 162 and multiple second channels 168 of second part 166 Alignment, to reach the emulation mode above-mentioned for flowing stationary phase along counterclockwise.
In addition, since first, second grade of Simulation moving bed 110,120 is connected, second and the second of third section Z3 and the Three relative velocity m2 and m3 will affect the 4th and the 5th relative velocity m4 and m5 of the 4th and the 5th section.It will simply visit below Beg for the flow velocity relation of these sections in first, second grade of Simulation moving bed 110,120, with improve second composition group B purity, The rate of recovery and the efficiency for increasing stationary phase.Fig. 8 to Figure 11 is second and third of the series connection simulated moving bed system 100 of Fig. 1 The the 4th and the 5th the relative velocity m4 and m5 of the second of section Z3 and third relative velocity m2 and m3 and the 4th and the 5th section Relational graph.
Firstly, under conditions of low concentration, adsorption isothermal curve of the solute component in stationary phase be it is linear, slope is Henry's constant, and its linear speed in chromatography tubing string 180, uiAnd the linear speed of the mobile phase of jth section, vj, between Relationship can use following formula and be illustrated:
Wherein KiFor the Henry's constant of i ingredient, and F is the solid-liquid phase volume ratio for chromatographing tubing string 180.
It, can be each to adjust by setting mobile phase and the stationary phase relative volumetric flow rates of different sections according to this formula The direction that components group moves in each section, wherein relative volumetric flow rates are defined as follows:
Wherein QjFor the mobile phase volume flow velocity in the area j, tswFor the switching time of valve, VCFor the blank pipe volume of chromatographic column, ε For filling batch voidage.
For being detained the mixture of three components group of behavior, when the progress of series connection simulated moving bed system 100 using Fig. 1 When separation, operating condition should meet the restrictive condition that triangle balanced is defined:
KB<m1 (3a)
KA<m2,m3<KB (3b)
KB<m2',m3'<KC (3c)
The another foundation conservation of mass:
m3'=m2'+m1-m2 (4)
So the conservation of mass can be rewritten into:
m3'-m2'=m1-m2∨m3'-m1=m2'-m2 (5)
If the third relative velocity m3 of third section Z3 is vertical using the second relative velocity m2 of the second section Z2 as horizontal axis Axis, the then operating condition that can be kept completely separate just are located in triangle, that is to say, that separable opereating specification is sat thus Triangle in marking on a map.Then there is optimal separating effect and separative efficiency in vertex of a triangle.
Accordingly, the step for setting the operating condition of the series connection simulated moving bed system 100 of Fig. 1 is as shown in Figure 8:
(a) m2 and m3 is set, so that a (m2, m3) point coordinate meets (3b) formula;
(b) m1 is set, so that b (m2, m1) point coordinate meets (3a) formula;
(c) m4 is set, so that c (m4, m5) point coordinate meets (3c) formula.
According to the conservation of mass of (5) formula, b point is online centainly parallel with the diagonal line of Fig. 8 with c point.It is grasped when changing single After making condition, the a-b-c step of setting operation condition, the coordinate in (m2, m3) phase plane will also change simultaneously.When representing After (m2, the m3) of 110 operating condition of level-one Simulation moving bed is fixed, the change of following operating condition can all cause to represent second (m4, the m5) of grade 120 operating condition of Simulation moving bed generates displacement:
(1) increase m1 (moving to b ' on b point), then the charging for representing second level Simulation moving bed 120 will increase, therefore m5 It will increase, so c point pan-up, such as Fig. 9.
(2) increase m4 (c point moves to right), then because m5 can also increase therewith, c point moves right along bc line, such as schemes 10。
(3) after flow velocity is fixed, if increasing switching time, the a-b-c step of setting operation condition, (m4, M5) coordinate in phase plane is then to right translation, such as Figure 11.
Using above-mentioned three kinds of features, can use the operating condition that following steps establish optimization: firstly, fixed m4 with Under the difference of m2, change the switching time tsw of valve, so that the coordinate of (m2, m3) and (m4, m5) two o'clock, with diagonal line It moves left and right in parallel.The calculating that purity and the rate of recovery are carried out for the separated outlet R ' come out of different switching times, then determines Make preferable switching time.According to step (1) as a result, reduce the difference of m4 and m2 to increase purity, or increase m4 with The difference of m2 is to increase the rate of recovery.Using m1 is increased, the rate of recovery can be improved and increase the efficiency of stationary phase.
In conclusion the series connection simulated moving bed system of this case is moved by side-stream line first, second grade of simulation of series connection Bed is detained the inter-level of constant between to isolate in mixture.Since Simulation moving bed is switched to by these tubing strings Fluctuation of concentration is had when different sections, separating effect of the fluctuation of concentration in the effluent of side-stream line to second level Simulation moving bed It influences greatly, in order to reduce the fluctuation of concentration in effluent, this case installs dashpot additional in side-stream line, and middle delay ingredient and height are stagnant Profit retention point can be introduced into dashpot in side-stream line, and concentration tends to after stablizing in dashpot, can just flow to second level mould Quasi- moving bed, so that second level Simulation moving bed has preferable separating effect.In addition, the series connection simulated moving bed system of this case It further include regeneration interval, the stationary phase of the first section of first order Simulation moving bed is recycled back into the by regeneration interval cleaning Second level Simulation moving bed can in time and effectively will be strong without taking strong anelasticity ingredient toward second level Simulation moving bed The discharge of anelasticity ingredient, and enable the use of simulated moving bed system for a long time of connecting.In addition, the design of regeneration interval The flow velocity of effluent can also be improved it is unnecessary to guarantee the function of second level Simulation moving bed, operating condition can be more convenient Setting.This case more provides a kind of multicomponent chromatographic separating process applied to above-mentioned series connection simulated moving bed system.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into Row equivalent replacement;And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (7)

1. a kind of series connection simulated moving bed system is suitable for separating mixture, the mixture includes first composition group, second composition Group and third components group, the first delay constant, the second delay constant and the third being respectively provided with from small to large are detained constant, described First composition group includes at least first composition, and the second composition group includes at least second composition, and the third components group is at least Including third ingredient, which is characterized in that the series connection simulated moving bed system includes:
First order Simulation moving bed, including the first, second, third section arranged in the first direction;
Second level Simulation moving bed, including the four, the 5th sections arranged along the first direction, described first, described second Grade Simulation moving bed is made of mobile phase and stationary phase, and the mobile phase is simulated in the described first, second level respectively It is flowed in moving bed along first direction, the stationary phase is relative to described mobile mutually towards the second party in contrast to the first direction It is moved to simulation;
Side-stream line connects the described first, second level Simulation moving bed and exports including effluent entrance and effluent, wherein institute It states effluent entrance to be connected between first section and second section, the effluent outlet is connected to the 4th section Between the 5th section;
Dashpot configures in the side-stream line;
Effluent pressure regulator, configuration is in the side-stream line and is located between the dashpot and effluent outlet;
Effluent pump, configures in the side-stream line and between the dashpot and the effluent pressure regulator;With And
Regeneration interval is the 6th section, is arranged in by the 5th section and including wetted area and Qiang Qing along the first direction Area is washed, the mobile phase flows through the strong cleaning area of the 6th section along the first direction, and along described second Direction flows through the wetted area of the 6th section, wherein
The first order Simulation moving bed is used to separate the first composition group of the mixture, and described the of the mixture Binary group, the third components group from second section along the side-stream line through the dashpot, the effluent pump, The effluent pressure regulator is moved between the 4th section and the 5th section, and is simulated and moved in the second level It is separated in bed.
2. series connection simulated moving bed system according to claim 1, which is characterized in that further include:
Central valve group, including first part and second part, wherein the first part is along axis relative to the second part Rotation, to switch the contraposition shape between multiple first passages of the first part and multiple second channels of the second part State, the multiple second channel of part respectively with described first, the described second, third, the described 4th, the described 5th and The 6th section connection.
3. series connection simulated moving bed system according to claim 2, which is characterized in that further include:
Multiple liquid supply tanks are connected to the multiple first passage of part respectively, and the movement mutually respectively includes at least one Liquid is washed in punching, and at least one punching is accommodated in each liquid supply tank and washs liquid;
Multiple mainstream pumps, are connected to the multiple first passage of the multiple liquid supply tank and part respectively;
Multiple liquid recoveries are connected to the multiple first passage of part respectively, liquid recovery for accommodate it is described extremely Liquid is washed in a few punching;And
Multiple mainstream pressure regulators are connected to the multiple liquid recovery with the multiple first passage of part respectively.
4. series connection simulated moving bed system according to claim 3, which is characterized in that the multiple liquid supply tank and institute The quantity for stating multiple mainstream pumps is respectively five, and five liquid supply tanks are separately positioned on described with five mainstreams pump Between the source of first section, second section and the third section, the source of the 4th section, the wetted area and The strong cleaning area.
5. series connection simulated moving bed system according to claim 3, which is characterized in that the multiple liquid recovery and The quantity of the multiple mainstream pressure regulator is respectively two, described two liquid recoveries and described two mainstream pressure Adjuster is separately positioned on the end of the end of the third section, the 5th section.
6. series connection simulated moving bed system according to claim 1, which is characterized in that described first, described second, described Third, the described 4th, the described 5th and each of the 6th section include at least one tubing string, are filled out in the every tubing string The stationary phase with hole is filled inside particle.
7. series connection simulated moving bed system according to claim 1, which is characterized in that described mobile mutually with the first party To flow through described first, the described second, third, the described 4th and the 5th section.
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