CN102527086A - Method simulating moving bed to separate three-component compound - Google Patents
Method simulating moving bed to separate three-component compound Download PDFInfo
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Abstract
A method simulating a moving bed to separate three-component compound comprises the steps of (a) providing a three-area simulating moving bed device which comprises an alpha area, a beta area and a gamma area which are sequentially communicated and respectively provided with a first flow speed ratio, a second flow speed ratio and a third flow speed ratio; (b) providing the three-component compound containing three components of a strong absorption component, a middle absorption component and a weak absorption component which respectively have a henry absorption constant Ka, Kb and Kc on an absorption agent; (c1) inputting the three-component compound into the three-area simulating moving bed so that the first flow speed ratio is larger than Ka, the second flow speed ratio and the third flow speed ratio are smaller than Kb and larger than Kc, and the weak absorption component of the three-component compound is separated; and (c2) when the first flow speed ratio is larger than Kb and smaller than Kc, and the second flow speed ratio and the third flow speed ratio are smaller than Kb and larger than Kc, the middle absorption component of the three-component compound is separated.
Description
Technical field
The invention relates to a kind of method of simulation moving-bed separation three composition mixtures, particularly a kind of the separation in this three compositions mixture to the middle absorption affinity of adsorbent or the method for weak absorption affinity composition.
Background technology
Composition in the existing simulation moving-bed separating mixture, the operator must select to be fit in order to separate the solid absorbent of desiring separator (fixedly phase, Stationary Phase) and towards washing agent (mobile phase, Mobile Phase).Please with reference to shown in Figure 1; Existing simulation moving-bed be that to have a four-range simulation moving-bed; This four zone is respectively α, β, γ and δ zone, and in this is simulation moving-bed, is flowed towards washing agent by this, and this solid absorbent then presents rightabout flowing with respect to this towards washing agent.When utilizing the strong absorption affinity composition A in this existing simulation moving-bed separating mixture; Should flow in this simulation moving-bed order in advance towards washing agent according to α, β, γ and δ zone; Because this composition A is to the strong absorption affinity of this solid absorbent; Then this composition A flows to the β zone with this solid absorbent, and all the other compositions (comprising weak adsorptivity composition B) reach towards washing agent and then flow to the γ zone, and by the regional weak absorption discharging place O of this γ
γFlow out, all the other dash and wash agent and then flowed out by the δ zone, and flow to the front end in α zone, and the tubing string that gets into series connection again uses to reclaim, and the composition A that will be stranded in α and β zone dashes and wash, and adsorb discharging O from the last one in this α zone
αFlow out, wherein, aforementioned simulation moving-bed dashing washs that to have the pattern that flows relatively between agent and the solid absorbent be to utilize the switching time of pipeline configuration and switching valve, simulates the reverse flow of this solid absorbent.
Please with reference to shown in Fig. 2 a and the 2b; This simulation moving-bed tubing string group that includes four section S91, S92, S93 and S94 connects in regular turn; Each section S is provided with at least one tubing string; The tubing string quantity of each section S is the demand setting according to the user, all is provided with the charging aperture I and the discharging opening O that can control Push And Release between each tubing string.
It is to have strong adsorptivity to desiring separator (composition A) that the tubing string of this four section S all is filled with a solid absorbent; Has weak adsorptivity to desiring separator (composition B); And be somebody's turn to do towards washing agent is this simulation moving-bed middle will not left by other adsorbed composition bands of solid absorbent of infusion port entering via charging aperture or setting in addition; And this solid absorbent was opposite with the flow direction of being somebody's turn to do towards washing agent, reached the effect of isolating composition A and composition B whereby.
Existing technology with the two compositions of simulation moving-bed separation is to get into existing simulation moving-bed feed entrance point by changing mixture; Make this solid absorbent simulation have the state that past relative direction moves; More in detail; When this simulation moving-bed change direction of mixture entering was forward, this solid absorbent just had moving relative to negative sense.
Discharging place or charging place and this simulation moving-bed regional relativeness shown in please showing, and the pipeline configuration and discharging opening or the charging aperture switch sketch map that cooperate corresponding 2a and 2b to scheme with reference to Fig. 1 and the 1st.Because this mixture is to change it with different time to get into this simulation moving-bed position; Have four zones in that existing four sections of this definition are simulation moving-bed; Be respectively α, β, γ and δ zone; When defining a very first time t1, the tubing string group of this first section S91 is the α zone, and the end in this α zone is provided with the last one absorption discharging place O
α, this second section S92 the tubing string group be that the tubing string group of β zone, the 3rd section S93 is the γ zone, and the front end in this γ zone is provided with a mixture charging place I
γAnd absorption discharging place O a little less than in the of
γAnd the tubing string group of the 4th section S94 is the δ zone; And after after a while, switch to the second time t2, then this α, β, γ and δ zone will move to next section, after switching to the 4th time t4; The pattern that very first time t1 is got back in recirculation, the discharging opening position of this desire collection thing are to need each the section discharging opening O shown in contrast the 1st table.
The 1st table: discharging place or charging place and this simulation moving-bed regional relativeness
For example; Please with reference to Fig. 2 a; Wash agent when getting into the tubing string group of this series connection when dashing by the charging aperture I91 of the first section S91; This mixture is then got into the tubing string group of this series connection by the charging aperture I93 of the 3rd section S93, the while then has the collection fluid of strong adsorptivity composition from the discharging opening O92 output of the second section S92, and the discharging opening O94 of the 4th section S94 output has the raffinate of weak adsorptivity composition.Please refer again to Fig. 2 b, when after after a while (switching to second time T 2), with this mixture charging place I
γ, this adsorbs discharging place O by force
αAnd should weak absorption discharging place O
γMove to next section S simultaneously, (switching to the 3rd time T 3) switches to next section S again after after a while, constantly switches this mixture charging place I so in regular turn
γ, this adsorbs discharging place O by force
αAnd should weak absorption discharging place O
γThe position, then can simulate the behavior that solid absorbent flows toward the opposite direction of gateway transfer sequence.Owing to dashes and to wash agent and continuously charging of separator, and solid absorbent is modeled into reverse flow, so solid absorbent is with similar mutual reverse and flow towards washing contacting of agent.
Yet; Shown in Figure 1 simulation moving-bedly only can separate to two constituents mixts; As when desiring three composition A, B and the C in the separating mixture; Then must utilize the two groups of simulation moving-bed separation that just can reach three composition A, B, C as shown in Figure 3, wherein, this three composition to the absorption affinity of this solid absorbent in regular turn by strong to weak be composition A (absorption affinity by force), composition B (middle absorption affinity) and composition C (weak absorption affinity).
Please with reference to shown in Figure 3; Be two groups of four above-mentioned regional simulation moving beds of combination; The 1st group of simulation moving-bed four zones that include are respectively 1 α, 1 β, 1 γ and 1 δ zone, and the 2nd group of simulation moving-bed four zones that also include; Be respectively 2 α, 2 β, 2 γ and 2 δ zone, and these two groups simulation moving-bed the last the one absorption discharging place O that are respectively equipped with
1 α, O
2 α, a mixture charging place I
1 γ, I
2 γAnd absorption discharging place O a little less than in the of
1 γ, O
2 γ
Should dash and washed after agent gets into arbitrary zone in the 1st group of 1 simulation moving-bed α, 1 β, 1 γ and 1 δ zone; In each zone, flow in regular turn; Simultaneously; Should dash and washed after agent gets into arbitrary zone in the 2nd group of 2 simulation moving-bed α, 2 β, 2 γ and 2 δ zone, in each zone, flow in regular turn, and in this four zone respectively, circulate and make these two groups of simulation moving-bed dashing wash conditional stability.
With this mixture that contains composition A, B, C via the 1st group of simulation moving-bed strong absorption discharging place O
1 αWhen getting into this 1 γ zone, this composition A flows to 1 β zone with this solid absorbent, this composition B, C and dash and wash agent and then flow to this 1 γ zone, and this composition B, C are by absorption discharging place O a little less than this
1 γFlow out, this moment this composition A be stranded in this 1 α and 1 β zone by clean dashing wash agent dash wash after, certainly should strong absorption discharging place O
1 αFlow out.
This composition B, C are by the 1st group weak absorption discharging place O
1 γWhen flowing out, get into the 2nd group of simulation moving-bed mixture charging place I
2 γ, greater than this composition C, this composition B flows to this 2 β zone with this solid absorbent to this composition B to the absorption affinity of this solid absorbent at this moment, and this composition C reaches towards washing agent and then flows to this 2 γ zone, and this composition C is by adsorbing discharging place O a little less than this
2 γ, this composition B was stranded in this 2 α and 2 β zones and was washed agent by clean dashing and dash and wash this moment, certainly should strong absorption discharging place O
2 αFlow out, so far just accomplish the separation of three compositions.
From the above, the existing method of utilizing simulation moving-bed separation three composition mixtures is must be earlier with after the composition A of absorption affinity separates by force among this three composition A, B, the C, the composition C of the composition B of absorption affinity or weak absorption affinity in could separating.More in detail, middle absorption affinity composition B or weak absorption affinity composition C that existing separation method can't only separate to institute's desire directly separate, must be strong and weak according to the absorption affinity of this three composition A, B, C, isolate composition A in regular turn, and just can isolate composition B; After perhaps isolating composition A, B in regular turn, just can isolate composition C, the program of therefore separating composition B or C is many and loaded down with trivial details, and its separable programming palpus is through the multi units tube post, so required time is also longer; In addition, owing to separate composition B or the necessary multi units tube post that uses in addition of C, the method that therefore should have now incurs a considerable or great expense, and middle absorption affinity composition B that desire is separated or low absorption affinity composition C person all can't avoid bearing expensive problems such as tubing string expense.
Summary of the invention
Main purpose of the present invention is the method that is to provide a kind of simulation moving-bed separation three composition mixtures; But in this three compositions mixture of this method direct separation to the middle absorption affinity of solid absorbent or the composition of weak absorption affinity, with the operating time of the composition of absorption affinity in shorten separating or weak absorption affinity.
An of the present invention purpose provides a kind of method of simulation moving-bed separation three composition mixtures; It is to the middle absorption affinity of solid absorbent or the composition of weak absorption affinity, to reduce the cost of its separation in separable this three compositions mixture that this method is only utilized three the simulation moving-bed of zone.
For reaching aforementioned goal of the invention, the technology contents that the present invention used includes:
A kind of method of simulation moving-bed separation three composition mixtures; This method is to comprise: the device that a kind of three regional simulation moving beds (a) are provided; Regional for the α, β and the γ that are connected in regular turn; The end in this α zone is provided with the last one absorption discharging place, and the front end in this γ zone is provided with mixture charging place, and the rear end in this γ zone is provided with weak absorption discharging place; (b) this three regional simulations moving bed contains an adsorbent, and one dashes and to wash agent and circulate in this α, β and the γ zone and contact with this adsorbent, and this α, β and γ zone have a first-class speed ratio value, one second flow velocity ratio and one the 3rd flow velocity ratio respectively; Reach (c) and three composition mixtures are injected this three regional simulations moving bed by this mixture charging place; This three compositions mixture is to include relatively that this adsorbent has an absorption affinity composition and a weak absorption affinity composition in the last the one absorption affinity composition, respectively, this is strong, in and a little less than the absorption affinity composition have a Henry absorption constant Ka, Kb and Kc respectively; (d) with the simulation moving-bed device of this three compositions mixture this three section of input; And this first-class speed ratio value is greater than this Henry absorption constant Ka; This second flow velocity ratio and the 3rd flow velocity ratio are less than this Henry absorption constant Kb and greater than this Henry absorption constant Kc, and then the weak absorption affinity composition in this three compositions mixture is concentrated by absorption discharging place a little less than this and separates.
A kind of method of simulation moving-bed separation three composition mixtures; This method is to comprise: the device that a kind of three regional simulation moving beds (a) are provided; Regional for the α, β and the γ that are connected in regular turn; The end in this α zone is provided with the last one absorption discharging place, and the front end in this γ zone is provided with mixture charging place, and the rear end in this γ zone is provided with weak absorption discharging place; (b) this three regional simulations moving bed contains an adsorbent, and one dashes and to wash agent and circulate in this α, β and the γ zone and contact with this adsorbent, and this α, β and γ zone have a first-class speed ratio value, one second flow velocity ratio and one the 3rd flow velocity ratio respectively; (c) by this mixture charging place three composition mixtures are injected this three regional simulations moving bed; This three compositions mixture is to include relatively that this adsorbent has an absorption affinity composition and a weak absorption affinity composition in the last the one absorption affinity composition, respectively, this is strong, in and a little less than the absorption affinity composition have a Henry absorption constant Ka, Kb and Kc respectively; And (d) with the simulation moving-bed device of this three compositions mixture this three section of input; And this first-class speed ratio value is greater than this Henry absorption constant Kb and less than this Henry absorption constant Ka; This second flow velocity ratio and the 3rd flow velocity ratio are less than this Henry absorption constant Kb and greater than this Henry absorption constant Kc, and then the middle absorption affinity composition in this three compositions mixture is concentrated by this strong absorption discharging place and separates.
Description of drawings
Fig. 1: existing one group of four discharging place or charging place and this simulation moving-bed regional relativeness figure that section is simulation moving-bed.
Fig. 2 a: existing one group of four simulation moving-bed pipeline sketch map one of section (very first time t1).
Fig. 2 b: existing one group of four simulation moving-bed pipeline sketch map two of section (the second time t2).
Fig. 3: existing two group of four discharging place or charging place and this simulation moving-bed regional relativeness figure that section is simulation moving-bed.
Fig. 4: the pipeline configuration schematic diagram of three regional simulation moving beds of the present invention.
Fig. 5: discharging place of three regional simulation moving beds of the present invention or charging place and this simulation moving-bed regional relativeness figure.
Fig. 6: with the sketch map of the strong absorption affinity composition of the separation of three regional simulation moving beds A.
Fig. 7: with the sketch map of absorption affinity composition C a little less than the separation of three regional simulation moving beds.
Fig. 8: with the sketch map of absorption affinity composition B in the separation of three regional simulation moving beds.
Fig. 9: the HPLC chromatography collection of illustrative plates that present embodiment perfume (or spice) is eaten.
Figure 10: each composition HPLC chromatography collection of illustrative plates of first each discharging opening of embodiment.
Figure 11: each composition HPLC chromatography collection of illustrative plates of second each discharging opening of embodiment.
[main element symbol description]
A, B, C composition
γ γ zone, α α region beta β zone
O
αStrong absorption discharging place I
γMixture charging place O
γWeak absorption discharging place
The S1 first section S2 second section S3 the 3rd section
C11, c12, c21, c22, c31, c32 tubing string
The I1 first charging aperture I2 second charging aperture I3 the 3rd charging aperture
The O1 first discharging opening O2 second discharging opening O3 the 3rd discharging opening
P metering liquid pump A, B, C composition
α, 1 α, 2 α α region beta, 1 β, 2 β β zone
γ, 1 γ, 2 γ γ zone δ, 1 δ, 2 δ δ zone
O
α, O
1 α, O
2 αStrong absorption discharging place I
γ, I
1 γ, I
2 γMixture charging place
O
γ, O
1 γ, O
2 γWeak absorption discharging place
The S91 first section S92 second section
S93 the 3rd section S94 the 4th section
I91, I92, I93, I94 charging aperture
O91, O92, O93, O94 discharging opening
The specific embodiment
For letting above-mentioned and other purposes, characteristic and the advantage of the present invention can be more obviously understandable, hereinafter is special lifts preferred embodiment of the present invention, and conjunction with figs., elaborates as follows:
The present invention is in order to separate the method for the specific composition in the mixture; Particularly with a kind of method that includes three composition mixtures of a simulation moving-bed separation; Wherein this three composition is respectively composition A, composition B and composition C, this three composition to the absorption affinity of this absorption tubing string in regular turn by strong to weak be composition A (absorption affinity by force), composition B (middle absorption affinity) and composition C (weak absorption affinity).
Please with reference to shown in Figure 4; It is simulation moving-bed (Simulated MovingBed) used in the present invention pipeline configuration schematic diagram; This is simulation moving-bed to be the tubing string group that is provided with the one first section S1, one second section S2 and the 3rd section S3 that are connected in regular turn, and this tubing string group is to comprise an adsorbent (promptly fixing phase is called for short SP) and to dash that to wash agent (be mobile phase; Abbreviation MP) device; Wherein, this adsorbent be filling in a tubing string, and the adsorbent in this tubing string with dash the flow direction rightabout each other wash agent.Used in the present invention simulation moving-bed in each section S all be provided with at least one tubing string (tubing string of this of present embodiment first section S1 be c11 and c12; The tubing string of this second section S2 is c21 and c22; The tubing string of the 3rd section S3 is c31 and c32); Tubing string in each section S is to contact each other and make to dash to wash agent and can be circulated to next section S in regular turn, and when the tubing string number of each section S is many more, it is good more then desire to be separated the separating effect of composition (be called for short desire come together thing).Have hole in this three tubing string, this is dashed wash agent and can flow to the other end, and flow to this second section S2, flow to the 3rd section S3 again from the end of this first section S 1.The front and back ends of this first section S1 is respectively equipped with one first charging aperture I1 and one first discharging opening O1; The front and back ends of this second section S2 is respectively equipped with the one second charging aperture I2 and the second discharging opening O2, and the front and back ends of the 3rd section S3 is respectively equipped with one the 3rd charging aperture I3 and one the 3rd discharging opening O3.
The simulation moving-bed charging aperture of at least one each section S of switching valve control and the switch of discharging opening of being provided with used in the present invention; And respectively be provided with a metering liquid pump P between each section S; To cooperate different time T to control the adsorbent volume flow velocity Qsp of each section S and to dash and wash agent volume flow rate Qmp; Particularly control moving of charging aperture with switching valve, and then regulate and control this adsorbent volume flow velocity Qsp, this metering liquid pump P of each section S then can control this towards washing agent volume flow rate Qmp.
As the 1st described discharging place of table or charging place and this simulation moving-bed regional relativeness notion; Please with reference to shown in Figure 5; Simulation moving-bed three zones that also have used in the present invention; Wash the agent circulation for α, β and the γ zone that is connected dashes this in regular turn, the end in this α zone is provided with the last one absorption discharging place O
α, be the outlet that supplies adsorbent is had the composition outflow of strong absorption affinity; The front end in this γ zone is provided with a mixture charging place I
γ, be to supply this mixture to get into this simulation moving-bed inlet; The rear end in this γ zone is provided with a weak absorption discharging place O
γ, be the outlet that supplies adsorbent is had the composition outflow of more weak absorption affinity.By simulation moving-bed pipeline configuration shown in Figure 4 and this mixture charging place of switching valve control I
γMove, and then this dashes and washs the mobile relatively of agent and adsorbent to reach simulation.
The present invention is that the flow direction of this adsorbent of definition (SP) is negative sense (by the direction stream of this γ zone towards this α zone); Should dash the flow direction wash agent (MP) be forward (by the direction stream of this α zone towards this γ zone), and this volume flow rate Q is meant in the unit interval, to dash and washs agent or volume that adsorbent passed through; This α zone has an adsorbent volume flow velocity Qsp1 and towards washing agent volume flow rate Qmp1; This β zone has an adsorbent volume flow velocity Qsp2 and towards washing agent volume flow rate Qmp2, and this γ zone has an adsorbent volume flow velocity Qsp3 and towards washing agent volume flow rate Qmp3.
This adsorbent is meant the material that this three composition is had characterization of adsorption; Have an absorption affinity between this adsorbent and the desire collection thing and make this desire collection thing of this adsorbents adsorb; This absorption affinity can be anion and cation, polarity and suction-operated such as nonpolar; This adsorbent may be selected to be activated carbon, activated carbon fiber, carbon molecular sieve, CNT, silica gel, silica, aluminium oxide, zeolite, resin, pillared clay ... Deng; Each desire collection thing all has a specific Henry adsorption coefficient K for a kind of adsorbent, determines the adsorption strength between this desire collection thing and this adsorbent, for same adsorbent; The high more person of Henry adsorption coefficient K of each composition, then its adsorption strength to this adsorbent is strong more.
Should dash and wash agent be the material that can in this tubing string, flow, and wash in this mixture can't be by these adsorbent other compositions (general designation extract remainder) in order to dash, and with this extract remainder band from this tubing string, reach and separate the come together effect of thing of this desire.
Separating the characteristic of composition according to desire selects adsorbent of different nature to reach towards washing agent; Can improve effect from many compositions mixture separation desire collection thing; " separation " of the present invention is meant with suitable adsorbent and dashes and wash a composition is carried out in agent to many compositions mixture separation; Be meant especially this composition is concentrated, the concentration of this composition improved, so that the follow-up operation of analyzing or utilizing; The present invention provides a separation method, makes the operator can separate the composition in (or concentrating) three composition mixtures according to this method.
The present invention be directed to a kind of mixture that contains composition A, B or C and carry out the separation of a specific composition A, B or C; Wherein this composition A, B or C are respectively Ka＞Kb＞Kc for the Henry absorption constant K of this adsorbent; Therefore, this composition A, B or C are respectively A＞B＞C for the adsorption strength of this adsorbent.
According to the theoretical (Yu of triangle; H.W.; C.B.Ching; " Optimization of a simulatedmoving bed based on an approximated Langmuir Model " AIChE is (2002) 2240-2246 J.48) this simulation moving-bed each regional adsorbent that defines be respectively Qsp and Qmp with dashing the volume flow rate wash agent, and the clean mass flux F (Net flux) of this desire collection thing must satisfy formula I in each zone, this clean mass flux F is meant that desire collection thing passes through the clean mass flux in this zone; When this clean mass flux F greater than zero; Represent that this composition A, B or C move with dashing the flow direction wash agent, when this clean mass flux F less than zero, represent that this composition A, B or C are that the flow direction with this adsorbent moves.
F=Qsp (1-ε) (n C-q) (formula I)
Wherein, ε is a porosity, is meant the shared ratio of this zone tubing string inner pore, promptly dash and wash the position that agent can be flowed through, and 1-ε is meant the ratio of deduction hole in the tubing string, the i.e. shared position of adsorbent; N is the interior adsorbent of the same area and dashes and wash the flow velocity ratio n of agent; C is that desire collection thing dashes the concentration of washing agent in this zone; Q is that desire collection thing is in the concentration of this zone adsorbent.The delay intensity of composition A, B and the C of present embodiment is A＞B＞C, then represents the clean mass flux F of each composition A, B, C to should be Fa＜Fb＜Fc.
The definition of this flow velocity ratio n is please with reference to formula II; Be should dash in the unit interval T to wash the agent positive flow through the volume of tubing string and this adsorbent negative flow ratio through the volume of tubing string, wherein, V represents the tubing string volume; Then V ε multiply by porosity ε (pore volume) for this tubing string volume V; Promptly dash and wash the volume of agent, and V (1-ε) multiply by the ratio of deducting porosity (1-ε) in the tubing string for this tubing string volume V, promptly represent the shared volume of adsorbent; V
DBe the dead angle volume of representing in the tubing string (Deadvolume), for example, V
DBe that connecting pipeline between two tubing strings does not contain adsorbent, so dashing in this connecting pipeline volume wash agent and do not have separating effect, should give deduction.When multiply by unit interval T towards washing agent volume flow rate Qmp; Be to dash and wash the volume of agent in this unit interval T; This volume is deducted two definite value V ε (because the switching of charging aperture and discharging opening; Except making the solid absorbent negative sense flows, also simultaneously the intrapore liquid of solid absorbent is taken toward negative sense and is flowed) and V
D, then obtain dashing in this unit interval T and wash the actual volume of agent.
This formula II can be obtained formula III divided by unit interval T together, wherein, V ε/T and V
D/ T is a certain value, therefore, can be pushed away by this formula III, and the adsorbent volume flow velocity Qsp that flow velocity ratio n representative dashing in the same area washed in agent volume flow rate Qmp and this zone (is the ratio of V (1-ε)/T).
Can know by inference by triangle theory and formula I, II, III, each regional flow velocity ratio n size be this regional adsorbent of decision with each composition between the regulation and control key of whether adsorbing.More in detail, when desiring to make desire collection thing to the forward to move, then the clean mass flux F of this desire collection thing should be greater than zero:
F＝Qsp(1-ε)(n?C-q)＞0(I.1)
Wherein, when this clean mass flux F greater than zero, Qsp＞0, and (1-ε)＞0 o'clock then obtains formula (I.2):
→nC-q＞0(I.2)
Obtain
According to the definition of Henry absorption constant K, then obtain formula I.4 again:
When the phenomenon of this adsorbents adsorb desire collection thing is linear, formula I.5
I.3, I.5 combinatorial formula reaches, and obtain formula and I.6 reach I.7, and then the condition that the clean mass flux F of each composition A, B and C in each zone can be met separate or concentrate with this flow velocity ratio n and the relation of Henry absorption constant K.
When desiring to make desire collection thing to move toward negative sense, then I.7 the clean mass flux F of this desire collection thing should with above-mentioned derivation mode, can obtain formula less than zero:
The come together relation of Henry absorption constant K of thing of the flow velocity ratio n that obtains each region alpha, β and γ zone shown in the 2nd table whereby and desire.For example, when separating composition A, please with reference to shown in Figure 5, for making the strong absorption discharging place O of this composition A in this α zone like desire
αFlow out; Then this composition A should be less than zero in the clean mass flux Fa in this α zone; Represent the Henry absorption constant Ka of the first-class speed ratio value n1 in this α zone less than this composition A, then this composition A is adsorbed by the adsorbent in this α zone, and not can by this dash wash the agent band from and flow out this α zone; As the first-class speed ratio value n1 in this α zone Henry absorption constant Ka greater than this composition A; Then this composition A should be dashed and washed the agent band from this α zone; And this first discharging opening O1 flows out certainly, and then this composition B and C should be greater than zero in the clean mass flux Fb and the Fc in this β and γ zone, and promptly the flow velocity ratio n2 and the n3 in this β and γ zone should be greater than Henry absorption constant Kb; And, to the forward move in this β and γ zone to avoid this composition A less than Henry absorption constant Ka.
The 2nd table: the present invention separates the condition of composition A, B or C
The simulation moving-bed pipeline sketch map that please refer to the 2nd condition enactment of showing and Fig. 5 promptly can one group of three regional simulation moving-bed separation this desire collection thing such as composition A, B or C.
Please with reference to shown in Figure 6; The first embodiment of the present invention is method separation this composition A (its Henry absorption constant Ka is the maximum among three composition A, B or the C) that contains three composition A, B and C mixture with the simulation moving-bed separation in one or three zones; This is simulation moving-bed to be to comprise an adsorbent to move towards its negative sense; And one dash and to wash agent and move towards its forward, and should dash and wash agent be to get into this simulation moving-bed α zone, and this mixture is by this mixture charging place I
γGet into that this is simulation moving-bed, wherein the first-class speed ratio value n1 in this α zone is greater than this Henry absorption constant Ka, and the flow velocity ratio n2 and the n3 in this β zone and this γ zone, is less than this Henry absorption constant Ka, and greater than this Henry absorption constant Kb.
More in detail, this mixture is from this mixture charging place I
γGet into this simulation moving-bed after, the flow velocity ratio n in these three zones is all greater than this Henry absorption constant Kb or Kc, therefore, should dash and wash agent this composition B and C or other impurity bands are moved towards this simulation moving-bed forward from this adsorbent, and a little less than this absorption discharging place O
γFlow out; And the flow velocity ratio n2 in this β and γ zone and n3 are all less than this Henry absorption constant Ka; Therefore; The adsorbent in this β and γ zone is this composition A absorption, and this adsorbent moves towards this simulation moving-bed negative sense, when this composition A moves to this α zone; The first-class speed ratio value n1 in this α zone is greater than this Henry absorption constant Ka, and then this composition A should be dashed and wash the agent band from this adsorbent and from this strong absorption discharging O
αFlow out.
By on can know; The simulation moving-bed composition A that isolates strong absorption affinity in the present invention three zones capable of using; Particularly by the flow velocity ratio n1 in regulation and control α zone greater than Ka, with the flow velocity ratio n2 in this β zone less than Ka, this composition A is moved to negative sense; All the other absorption affinities move than this composition A weak person Ze Chao forward, and then in this strong absorption discharging place O
αIsolate this composition A.
Please with reference to shown in Figure 7; The second embodiment of the present invention is the method that contains three composition A, B and C mixture equally with the simulation moving-bed separation in one or three zones; Directly this composition C (its Henry absorption constant Kc is the third-largest person among three composition A, B or the C) is concentrated and separate, do not need to isolate earlier this composition A and B.This mixture is by this mixture charging place I
γGet into that this is simulation moving-bed, wherein the first-class speed ratio value n1 in this α zone is greater than this Henry absorption constant Ka; The flow velocity ratio n2 and the n3 in this β and γ zone are less than this Henry absorption constant Kb, and greater than this Henry absorption constant Kc.
More in detail, this mixture is from this mixture charging place I
γGet into this simulation moving-bed after, the flow velocity ratio n in these three zones is all greater than this Henry absorption constant Kc, therefore, should dash and wash agent this composition C band was moved towards this simulation moving-bed forward from this adsorbent, and a little less than this absorption discharging place O
γFlow out; And the second flow velocity ratio n2 in this β zone is less than this Henry absorption constant Ka and Kb (but greater than this Henry absorption constant Kc); Therefore; The adsorbent in this β zone is this composition A and B absorption, and this adsorbent moves towards this simulation moving-bed negative sense, when this composition A and B move to this α zone; The first-class speed ratio value n1 in this α zone is greater than this Henry absorption constant Ka and Kb, and then this composition A and B are all dashed by this and wash the agent band from this adsorbent and from this strong absorption discharging O
αFlow out.
By on can know; The present invention be by the flow velocity ratio n2 of regulation and control this β and γ zone, S3, n3 greater than Kc and less than Kb, and the flow velocity ratio n1 in this α zone makes this composition C move towards forward greater than Ka; All the other absorption affinities move than this composition C powerhouse Ze Chao negative sense, can a little less than this, adsorb discharging place O
γObtain this composition C, and reach the effect of saving adsorbent (tubing string quantity); In addition, when the present invention separates this composition C, must not remove the composition A or the B that adsorbent are had strong absorption affinity in advance, the time-histories of therefore separating is short, can reach the timesaving effect.
Please with reference to shown in Figure 8; The third embodiment of the present invention is the method that contains three composition A, B and C mixture with the simulation moving-bed separation in one or three zones equally; This composition B (its Henry absorption constant Kb is second largest person among three composition A, B or the C) is concentrated and separates, do not need to isolate earlier this composition A.This mixture is by this mixture charging place I
γIt is simulation moving-bed to get into this; Wherein the first-class speed ratio value n1 in this α zone is greater than this Henry absorption constant Kb and less than this Henry's constant Ka; And the flow velocity ratio n2 and the n3 in this β and γ zone are greater than this Henry absorption constant Kc and less than this Henry absorption constant Kb.
More in detail, this mixture is from this mixture charging place I
γGet into this simulation moving-bed after, the flow velocity ratio n2 in this β and γ zone and n3 be all greater than this Henry absorption constant Kc, and less than this Henry absorption constant Kb; Therefore, this adsorbent adsorbs this composition A and B, and moves towards this simulation moving-bed negative sense; When this composition A and B move to this α zone; The first-class speed ratio value n1 in this α zone is greater than this Henry absorption constant Kb, but less than this Henry absorption constant Ka, then this composition B should be dashed and wash the agent band from this adsorbent and from this strong absorption discharging O
αFlow out; This adsorbent will continue to adsorb this composition A and move and can't go out towards this simulation moving-bed negative sense, therefore, when warp separation after a while, need to be dashed by the adsorbed composition A of this adsorbent and will wash out, avoid polluting absorption discharging place O by force
αThe concentrated effect of composition B; And flow velocity ratio n1, n2 and the n3 in these three zones be all greater than this Henry absorption constant Kc, therefore, should dash and wash agent this composition C band is moved towards this simulation moving-bed forward from this adsorbent, and a little less than this absorption discharging O
γFlow out.
By on can know; The present invention is by regulating and control the regional flow velocity ratio n1 of α greater than Kb and less than Ka, reach the regional flow velocity ratio n2 of this β and γ, n3 greater than Kc and less than Kb, this composition B being moved towards negative sense; Absorption affinity then moves towards forward less than the composition C of composition B; And the flow velocity ratio n in three zones makes this composition A can in any zone, do not concentrated the back and flows out from arbitrary discharging O all less than the Henry absorption constant Ka of this composition A, and in this strong absorption discharging place O
αObtain this composition B, this weak absorption discharging place O
γObtain this composition C; In addition, when the present invention separates this composition B, must not remove the composition A that adsorbent is had strong absorption affinity in advance, the time-histories of therefore separating is short, can reach the timesaving effect.
Can understand by aforementioned second and third embodiment; The present invention sees through the flow velocity ratio n in each zone is adjusted into the condition that meets aforementioned the 1st table; The forward or the negative sense of this condition control desire collection thing just capable of using flow; And direct separation goes out middle absorption affinity or weak absorption affinity composition, and then reaches the effect of saving tubing string number (cost) and shortening disengaging time.
Really can separate or concentrated absorption affinity is time strong or the composition of three strongest ones for the method that confirms the simulation moving-bed separation three composition mixtures of the present invention, the organic solvent extraction thing of eating to perfume (or spice) carries out the separation of one or three composition mixtures.
" perfume (or spice) is eaten the preparation of acetic acid ethyl ester extract "
Perfume (or spice) eats that to contain multiple minute compounds in (claiming smallflower beggarticks herb again) be to have functions such as anti-inflammatory, anti-hepatitis B virus and immunological regulation; For example oleanolic acid (Oleanolic acid), cyanidenon (Luteolin), cyanidenon-7-glucoside (Luteolin-7-glucoside) and other are not analyzed composition qualitatively as yet; Wherein, Cyanidenon is through confirming it is to have anti-oxidant, anti-inflammatory, anticancer and immunoregulatory important flavonoids; Oleanolic acid and cyanidenon-7-glucoside is to have the iNOS and the performance of COX-2 gene that inhibition is induced by the endotoxin LPS of bacterium secretion, and suppresses the effect that inspires inflammatory cell hormone (like TNF-α, IL-1 β, IL-6 and IL-12) that discharged through NF-κ B.
Perfume (or spice) eaten grind to form a perfume (or spice) and eat powder, it is to be 200# through a screen cloth specification that this perfume (or spice) is eaten powder, with alcohol this perfume (or spice) is eaten powder and extracts; This perfume (or spice) is eaten powder: alcohol is about 1: 4; And after 24 ± 2 hours extraction time, again residue is filtered, concentrates, obtain an alcoholic extract powder.This alcoholic extract powder is returned melt into one sticky thing (this alcoholic extract powder: 95% alcohol is about 4: 1) with 95% alcohol; And carry out ultrasonic concussion extraction 24 ± 2 hours with ethyl acetate (Ethyl acetate); And the concentrate drying of inciting somebody to action; Get an acetic acid ethyl ester extract, this acetic acid ethyl ester extract includes cyanidenon and cyanidenon-7-glucoside.With this acetic acid ethyl ester extract with high-effect LC appearance to cyanidenon and cyanidenon-when the 7-glucoside separated, its HPLC chromatography collection of illustrative plates was please with reference to Fig. 9, the composition C of drawing indication is an impurity; Composition A is cyanidenon-7-glucoside, and still contains composition B (cyanidenon) between this composition C and the A, wherein; The chromatography time of this composition C falls within 2～5 minutes; The chromatography time of composition B is about 10 minutes, and the chromatography time of composition A is about 12 minutes, by separation method of the present invention; Must in advance composition A and B not separated, can obtain this composition C.
" simulation moving-bed configuration used in the present invention and condition enactment "
Present embodiment is the separation of selecting to carry out with one or three sections simulation moving-bed composition A (cyanidenon-7-glucoside), composition B (cyanidenon) and composition C that perfume (or spice) eats; Wherein, The tubing string number of each section S is two, and this tubing string is as adsorbent (Merck Lichrospher 100RP-18,250 * 4.6mm with silica gel; Aperture 5 μ m); Dash and to wash agent that then to be 0.1% acetum formulated with volume ratio 7: 13 with methyl alcohol, should dash and wash agent and should before using, prepare again, and shake 30 minutes to remove the bubble in the solution with ultrasonic.Porosity ε=0.412 of this silica gel tubing string wherein, and employed simulation moving-bed dead angle volume V
D=0.117cm
3
Please with reference to the condition 1 shown in the 3rd table; It is the Henry absorption constant K of the first embodiment of the present invention composition A, composition B and the composition C that eat according to this perfume (or spice); Be respectively 5.304,4.179 and 0.222 to 2.196; The first-class speed ratio value n1 that sets this α zone with this condition 1 is 11.81, and the second flow velocity ratio n2 in this β zone is 3.05, and the 3rd flow velocity ratio n3 in this γ zone is 3.65.Present embodiment is to make n1, n2 and n3 all greater than Kc (0.222 to 2.196), and wherein, this n2 and n3 are less than Kb (4.179), and then this composition C adsorbs discharging place O a little less than this
γFlow out, and this composition A and B are all dashed by this and wash agent and take to negative sense, when this composition A and B flow to this α zone, this n1 was greater than this Ka, made this composition A and B all from should strong absorption discharging place O
αFlow out, and obtain the composition C of higher degree.
The 3rd table: present embodiment separates the condition of composition C
*Ka=5.304, Kb=4.179 and Kc=0.222～2.196
, be please respectively at this strong absorption discharging place O with simulation moving-bed composition A, B and the C that is separated used in the present invention with reference to the 4th table and shown in Figure 10
αAnd should weak absorption discharging place O
γConcentration and chromatography signal, and should weak absorption discharging place O
γCan access highly purified composition C, and not have the signal of composition A or B, the confirmation first embodiment of the present invention can be adsorbed discharging place O really a little less than this
γIn improve the concentration of the low absorption affinity composition C in this three compositions mixture, particularly in this extract, have highly purified composition C, and this composition A and B are in this strong absorption discharging place O
αBe separated, and unlikely pollution should weak absorption discharging place O
γComposition C.
The 4th table: present embodiment separates the result of composition C
Please with reference to shown in the 5th table, the first embodiment of the present invention is adsorbed discharging place O a little less than this
γThe product of gained is to contain highly purified composition C, and should weak absorption discharging place O
γThe product of gained contains in the initial charge 58.83% composition C, and therefore, the separation condition of present embodiment can concentrate and separate composition C really.
The 5th table: first embodiment separates the concentration and the purity of each composition
Please with reference to the condition 2 shown in the 6th table, its first-class speed ratio value n1 that to be the second embodiment of the present invention set this α zone with this condition 2 is 5.29, and the second flow velocity ratio n2 in this β zone is 3.05, and the 3rd flow velocity ratio n3 in this γ zone is 3.65.Present embodiment is to make n1, n2 and n3 all greater than Kc (0.222 to 2.196), and wherein, this n2 and n3 are less than Kb (4.179), and then this composition C adsorbs discharging place O a little less than this
γFlow out, and this composition A and B are all dashed by this and wash agent and take to negative sense, when this composition A and B flow to this first section S1, this n1 was greater than this Kb (4.179) but less than Ka (5.304), made this composition B from should strong absorption discharging place O
αFlow out, this composition A continues to move to this simulation moving-bed negative sense then by this adsorbents adsorb.
The 6th table: present embodiment separates the condition of composition B
*Ka=5.304, Kb=4.179 and Kc=0.222～2.196
, be please respectively at this strong absorption discharging place O with simulation moving-bed composition A, B and the C that is separated used in the present invention with reference to shown in the 7th table
αAnd should weak absorption discharging place O
γConcentration; Wherein, testing group is five groups, and the composition A concentration of the initial charge of each group is that 156.3ppm, composition B concentration are that 200.9ppm, composition C concentration are 73.8ppm; And each forms the concentration average out to 114.12ppm of part B, confirms that the second embodiment of the present invention can be in this strong absorption discharging place O
αExtract in improve the concentration of the middle absorption affinity composition B in this three compositions mixture.
The 7th table: present embodiment separates the result of composition B
Please with reference to shown in the 8th table, the second embodiment of the present invention is in this strong absorption discharging place O
αThe product of gained is the composition B that contains higher concentration, and should strong absorption discharging place O
αThe product of gained contains in the initial charge 56.80% composition B, and please with reference to shown in Figure 11, this composition B is in this strong absorption discharging place O
αThe chromatography signal greater than composition A in this strong absorption discharging place O
αThe chromatography signal, and should strong absorption discharging place O
αThe signal that does not contain composition C, and should weak absorption discharging place O
γBut this composition of chromatography A further improves composition B in this strong absorption discharging place O
αConcentration, the separation condition that confirms present embodiment can concentrate lifting really should strong absorption discharging place O
αThe concentration of composition B.
The 8th table: second embodiment separates the concentration and the purity of each composition
By on can know; The method of simulation moving-bed separation three composition mixtures of the present invention is by in each zone of regulation and control; This adsorbent is washed the flow velocity ratio n of agent with should dashing, and concentrating the desire collection thing of this three compositions mixture, and improves the concentration of this desire collection thing in each discharging opening products therefrom.
Whereby; After the method for simulation moving-bed separation three composition mixtures of the present invention must be not earlier be separated the composition A of strong absorption affinity; Composition B or the composition C of weak absorption affinity of absorption affinity in can obtaining have the effect that reaches the operating time that shortens the middle absorption affinity of separating this three compositions mixture or weak absorption affinity composition.
The method of simulation moving-bed separation three composition mixtures of the present invention is only can the middle absorption affinity or the weak absorption affinity composition of this three compositions mixture to be separated with the simulation moving-bed of a kind of three sections, has the required effect of quantity to reduce cost with tubing string of minimizing.
Claims (8)
1. the method for three kinds of composition mixtures of a simulation moving-bed separation is characterized in that this method is to comprise:
(a) a kind of device of three regional simulation moving beds is provided; Regional for the α, β and the γ that are connected in regular turn; The end in this α zone is provided with strong absorption discharging place, and the front end in this γ zone is provided with mixture charging place, absorption discharging place a little less than the rear end in this γ zone is provided with;
(b) this three regional simulations moving bed contains a kind of adsorbent; A kind of dash washed agent and circulates in this α, β and the γ zone and contact with this adsorbent, and this α, β and γ zone have a first-class speed ratio value, second a flow velocity ratio and one the 3rd flow velocity ratio respectively; And
(c) by this mixture charging place three kinds of composition mixtures are injected these three regional simulation moving beds; These three kinds of composition mixtures are to include relative this adsorbent to have a strong absorption affinity composition, a middle absorption affinity composition and a weak absorption affinity composition respectively, and the composition of this strong absorption affinity, middle absorption affinity and weak absorption affinity has Henry absorption constant Ka, Kb and a Kc respectively;
(d) with these three kinds of these three devices that section is simulation moving-bed of composition mixture input; And this first-class speed ratio value is greater than this Henry absorption constant Ka; This second flow velocity ratio and the 3rd flow velocity ratio are less than this Henry absorption constant Kb and greater than this Henry absorption constant Kc, then the weak absorption affinity composition in these three kinds of composition mixtures concentrated by this γ zone and a little less than this absorption discharging place separated.
2. the method for three kinds of composition mixtures of simulation moving-bed separation according to claim 1 is characterized in that, this adsorbent in each zone is washed agent and has an adsorbent volume flow velocity and one respectively and dash and wash the agent volume flow rate with should dashing.
3. the method for three kinds of composition mixtures of simulation moving-bed separation according to claim 2 is characterized in that, each regional flow velocity ratio is the ratio of washing agent volume flow rate and adsorbent volume flow velocity that dashes in this each zone.
4. based on the method for three kinds of composition mixtures of the described simulation moving-bed separation of claim 1, it is characterized in that this strong or middle absorption affinity composition is concentrated by this α zone and separates in this strong absorption discharging place.
5. the method for three kinds of composition mixtures of a simulation moving-bed separation is characterized in that this method is to comprise:
(a) a kind of device of three regional simulation moving beds is provided; Regional for the α, β and the γ that are connected in regular turn; The end in this α zone is provided with strong absorption discharging place, and the front end in this γ zone is provided with mixture charging place, absorption discharging place a little less than the rear end in this γ zone is provided with;
(b) these three regional simulation moving beds contain an adsorbent; One is dashed and to wash agent and circulate in this α, β and the γ zone and contact with this adsorbent, and this α, β and γ zone have a first-class speed ratio value, second a flow velocity ratio and one the 3rd flow velocity ratio respectively;
(c) by this mixture charging place three kinds of composition mixtures are injected these three regional simulation moving beds; These three composition mixtures are to include relative this adsorbent to have a strong absorption affinity composition, a middle absorption affinity composition and a weak absorption affinity composition respectively, and this strong absorption affinity, middle absorption affinity and weak absorption affinity composition have Henry absorption constant Ka, Kb and a Kc respectively; And
(d) with these three kinds of these three devices that section is simulation moving-bed of composition mixture input; And this first-class speed ratio value is greater than this Henry absorption constant Kb and less than this Henry absorption constant Ka; This second flow velocity ratio and the 3rd flow velocity ratio are less than this Henry absorption constant Kb and greater than this Henry absorption constant Kc, and then the middle absorption affinity composition in these three kinds of composition mixtures is concentrated by force by this α zone and be separated in this strong absorption discharging place.
6. the method for three kinds of composition mixtures of simulation moving-bed separation according to claim 4 is characterized in that, this adsorbent in each zone is washed agent and has an adsorbent volume flow velocity and one respectively and dash and wash the agent volume flow rate with should dashing.
7. the method for three kinds of composition mixtures of simulation moving-bed separation according to claim 6 is characterized in that, dashes the ratio of washing agent volume flow rate and adsorbent volume flow velocity in this each section of the flow velocity ratio of each section.
8. based on the method for three kinds of composition mixtures of the described simulation moving-bed separation of claim 4, it is characterized in that this weak absorption affinity composition is concentrated and a little less than this, adsorbed discharging place by this γ zone to be separated.
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| CN109761752A (en) * | 2017-11-10 | 2019-05-17 | 义守大学 | The method of purifying nonyl alcohol |
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| JPH05215736A (en) * | 1992-02-04 | 1993-08-24 | Daicel Chem Ind Ltd | Chromato separation method |
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