CN1923330A - Stationary type moving bed imitation chromatogram separation facility - Google Patents
Stationary type moving bed imitation chromatogram separation facility Download PDFInfo
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- CN1923330A CN1923330A CN 200610053183 CN200610053183A CN1923330A CN 1923330 A CN1923330 A CN 1923330A CN 200610053183 CN200610053183 CN 200610053183 CN 200610053183 A CN200610053183 A CN 200610053183A CN 1923330 A CN1923330 A CN 1923330A
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Abstract
The invention relates to a fixed analogue movable bed spectrum separator, which comprises several adsorption posts with absorber, whose inlets and outlets are connected to at least one distributor formed by stable disc and movable disc; the movable disc via one motor that drives one cam step motor intermission rotates; the movable disc has through holes relative to the inlets and outlets of adsorption posts, and relative annular grooves; the groove hole of each annular groove is through to the entrance of stable disc; the stable disc also has through holes relative to the inlets and outlets; the side through hole are divided into two groups to connect the inlets and outlets of relative adsorption posts; the movable disc has one pushing disc to generate tension force to contact the friction surfaces of movable and stable discs; the adsorption posts are mounted on one annular platform at the middle of frame; the lower part of frame has motor and cam step motor. The invention has simple structure, low cost and simple control.
Description
Technical field
What the present invention relates to is a kind of stationary type moving bed imitation process-scale chromatography separator, and especially a kind of multicolumn combination can realize the stationary type moving bed imitation chromatogram separation facility of serialization, automated production requirement, belongs to the chromatographic separation technology field.
Background technology
The SMBC partition method is a kind of advanced chromatographic separation technology that grows up on ion-exchange moving bed basis.This isolation technics has been widely used in fields such as petrochemical industry, medicine, food and Biochemical Engineering at present, and has obtained good society and economic benefit.
The U.S. universal oil product sixties in 20th century (uop) company takes the lead in adopting the SMBC method successfully to finish the separation of multiple liquid hydrocarbon, as from C
8Separate P-dimethylbenzene in aromatic hydrocarbons and the non-aromatics mixture, from the wide boiling point mixture of alkane and alkene, separate linear alkene, from light naphthar, kerosene, gas oil, separate normal alkane etc.
The research that Advanced Separation Technologies, Inc.'s (Advanced SeparationTechnologic Inc. is called for short AST) specializes in continuous ionic exchange and chromatographic isolation has been founded by the U.S. in 1986 in the Lakeland of Florida State.Above-mentioned two kinds of chromatographic separation devices are used in the industry such as petrochemical industry, pharmacy, chemical industry, starch sugar and amino acid of states such as the U.S., France, Japan and Canada, and obtain user's favorable comment.China introduced the ISEP device of the U.S. since 97 years in food, amino acid industry, be applied to separation and Extraction lysine from zymotic fluid, and the purifies and separates of the refining and sugar alcohol of starch sugar etc. have also obtained techno-economic effect preferably.
Chromatogram portion of French Separex company in 1996 integrates and has set up a new Novasep, and the said firm adopts the simulation shifting principle to develop many valves of 4-8 post automatic control chromatographic separation device, just promotes in China's starch sugar industry at present.
China's starch sugar industry develop rapidly in recent years, product category is increasing, is maximum with fruit/glucose slurry output especially wherein.Yet at present homemade high fructose syrup is first generation product (fructose content 42%), and in beverage industry, all adopting the fructose content of external import as " Coca-Cola ", " Jilibao " used sweetener is 55% second generation high fructose syrup.Therefore, homemade 42% high fructose syrup product is badly in need of updating, and adopts chromatographic separation technology exactly and make the optimal technological means of 55% high fructose syrup.And the major technique means of realization process-scale chromatography isolation technics, simulation moving-bed process-scale chromatography separator is adopted in optimal lectotype selection exactly.
In recent years, along with the development of simulated moving bed system design, the continuous appearance of new separation material kind and non-linear chromatography separated the further perfect of Mathematical Modeling, had effectively promoted the fast development of SMBC isolation technics.
Stationary type moving bed imitation is called for short FSMB, and it all is the chromatographic separation device that grows up on chromatographic isolation theoretical foundation with simulation moving-bed the same with the moving bed principle.Chromatographic separation process mainly is the operation of certain different component in a kind of material being carried out purifies and separates, it is to adopt a kind of each component to be had the adsorbent (also being fixedly phase) of different adsorption capacities as adsorbing medium, when containing different component (as the feed liquid of A, B two components, also be the phase that flows) cross when adsorbent bed with certain velocity flow, because of the difference of adsorbent to A, two kinds of component adsorption capacities of B in the feed liquid, and make strong absorbed component A, in adsorption bed the holdup time long slightly, slower to the Way out translational speed; And the weak absorbed component B by adsorbent bed, then the holdup time is short slightly in bed, and is very fast to the Way out translational speed, flows out from outlet prior to component A, and component A then is later than B component a period of time and just flows out from outlet.Meanwhile, by flowing out sequencing, collect respectively, can reach the chromatographic isolation purpose of A, two kinds of components of B in outlet.Development abroad has the simulation mobile system of single valve list tower (UOP), rotation adsorption column (CSEP) and the many valves of fixed leg (Novasep) now.But their complex structure, the cost height is unfavorable for domestic application and popularization.
Summary of the invention
The object of the present invention is to provide and a kind ofly on existing stationary type moving bed imitation separator basis, make improvement design, to adapt to the stationary type moving bed imitation chromatogram separation facility that domestic production enterprise produces needs.
The objective of the invention is to finish by following technical solution, it includes a plurality of adsorption columns that adsorbent is housed, the import of described a plurality of adsorption columns is communicated in the distributor that at least one is made up of Moving plate and quiet dish respectively with outlet, and the Moving plate of this distributor is done intermittently stepping by a motor by cam stepping mechanism drive and rotated.
Have on the described Moving plate with adsorption column import and the corresponding runner through hole of outlet number and reach the annular groove that adapts with the requirement of different process flow process, the slotted eye of every annular groove communicates with input and output material hole on the quiet dish respectively, be provided with equally on quiet dish and adsorption column import and the corresponding runner through hole of outlet, quiet dish side through hole is divided into two groups and is connected with exporting with corresponding adsorption column import respectively.
Described quiet dish side through hole is divided into by branches such as two rows arranges that every row is one group, and following exhausting hole is by the outer tube adsorption column import or export connection corresponding with it, and the through hole of the row of going up is equally with outer tube and corresponding adsorption column outlet or import connection; The side of Moving plate also is provided with and can changes the materials flow flow direction arbitrarily, realizes the through hole of multicolumn series, parallel or cross-over connection.
Be provided with one above the described Moving plate and can produce the thrust disc that rubbing surface that pretightning force makes dynamic and static dish fits tightly.
Described adsorption column is installed on the ring-shaped platform by uniform, and this ring-shaped platform is arranged on the middle part of a frame, and motor and cam stepping mechanism are equipped with in frame center line bottom.
The present invention compared with prior art has following technical characterstic: the one, and it can make ion-exchange and chromatographic separation process serialization, automation, not only can enhance productivity, and can stably control product quality; The 2nd, it adopts multicolumn circulated in countercurrent mode, can improve the utilization rate of adsorbent significantly, reduces the consumption of industrial chemicals and leaching requirement; The 3rd, be in operation, flow in each section with different speed continuous-flow, regulate to obtain high product concentration by flow velocity, thereby reduced the concentrated expense of downstream process, the saving energy; The 4th, the core component of this device is a stock distributor, it has adopted special structure design, neither utilizes the cylindricality rotation, does not adopt many valve controls again, can reach the effect that the adverse current simulation is moved equally, realize that the continuous ionic exchange separates the effective of material different component with continuous chromatography; The 5th, this Design of device has been considered the flexibility of system to the diversity that adapts to different material and separate and use, adjustment, as long as the link position of external hose import and export on the conversion distributor, can change the allocation flow of material, enlarge the application of device; The 6th, device has adopted constant charging flow velocity and the control of adsorbent translational speed, can realize stable discrete spectrum peak, the products export constant concentration; The 7th, this installs and is the multicolumn system, can adjust flow phase and fixing flow velocity mutually by changing the series-parallel system of adsorption column, can obtain best absorption and desorption time; The 8th, this device employing PLC controls the input and output material flow in the continuous separation process, auxiliary equipment capacity such as pump, groove can be reduced to minimum; Have simple in structurely, easy to use, cost is low, work efficiency height, characteristics such as control is simple, and convenient operation and management is applied widely, and is easy to utilize.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is a feed state distributor inner pipe passway schematic diagram of the present invention.
Fig. 3 is the desorbing agent state assignment device inner pipe passway schematic diagram that advances of the present invention.
Fig. 4 is a recurrent state distributor inner pipe passway schematic diagram of the present invention.
Fig. 5 is a fructose discharging state assignment device inner pipe passway schematic diagram of the present invention.
Fig. 6 is a glucose discharging state assignment device inner pipe passway schematic diagram of the present invention.
Fig. 7 is a FSMB operating principle schematic diagram of the present invention.
Fig. 8 is the another schematic diagram of FSMB operating principle of the present invention.
The specific embodiment
The present invention will be described in detail below in conjunction with accompanying drawing: shown in the accompanying drawing 1, the present invention includes a plurality of adsorption columns 4 that adsorbent 3 is housed, the import of described a plurality of adsorption column 4 is communicated at least one respectively by the distributor 8 that Moving plate 7 and quiet dish 9 are formed with outlet, is provided with one above the described Moving plate 7 and can produces the thrust disc 10 that rubbing surface that pretightning force makes dynamic and static dish fits tightly.The Moving plate 7 of distributor 8 is driven by a cam stepping mechanism 5 by a motor and does intermittently stepping rotation.Have on the described Moving plate 7 and adsorption column 4 imports and outlet number corresponding runner through hole and require the annular groove that adapts with the different process flow process, the slotted eye of every annular groove communicates with input and output material hole on the quiet dish 9 respectively; Be provided with equally on quiet dish 9 and adsorption column 4 imports and the corresponding runner through hole of outlet, quiet dish 9 side through holes are divided into two groups and are connected with exporting with corresponding adsorption column 4 imports respectively.Described quiet dish 9 side through holes are divided into by branches such as two rows arranges that every row is one group, and following exhausting hole is by the outer tube 13 adsorption column 4 import or exports connection corresponding with it, and the through hole of the row of going up is equally with outer tube 14 and corresponding adsorption column 4 outlets or import connection; The side of Moving plate 7 also is provided with and can changes the materials flow flow direction arbitrarily, realizes that the multicolumn series, parallel closes the through hole 12 of cross-over connection.
Figure 1 shows that at ring-shaped platform upper edge Zhou Junbu 20 adsorption columns 4 that adsorbent 3 is housed are installed.The kind of adsorbent can be separated the requirement of purpose according to difference, screens by small test, can use as ion exchange resin, gel, macroporous type polymeric adsorbent, silica gel or active carbon etc.Described cam stepping mechanism 5 is as the drive system of this device, and by the torque of main shaft 6, the Moving plate 7 that drives distributor is finished the material of each circulation, the allocating task of product turnover along intermittently stepping of counter-clockwise direction.The distributor 8 that is arranged on frame 1 top is significant components that this device is finished the chromatographic isolation task, also is one of core technology of the present invention.The quiet dish 9 usefulness alloy steel materials of distributor are made, and Moving plate 7 is by highly dense, high-strength graphite manufacturing and form friction pair, and the pretightning force that adopts thrust disc 10 to be produced fits tightly the rubbing surface of dynamic and static dish, prevent that materials flow from leaking from sealing surface.Quiet dish 9 is to float to be installed on the frame 1, can freely adjust self-position under the situation of Moving plate 7 bias voltages, keeps constant face pressure with Moving plate all the time.Go back organic block 11, feed pipe 15 and drainpipe 16 among Fig. 1.
Have 40 runner through holes and annular groove on Moving plate 7, the slotted eye of every annular groove communicates respectively at the enterprising discharge opening of quiet dish.Moving plate 7 side through holes can be by outer tube 12 interfaces free conversion, change materials flow arbitrarily and flow to, can realize modes such as the connection in series-parallel of multicolumn and cross-over connection, to adapt to the requirement of multiple different process flow process, so can enlarge the range of application of FSMB.
Be provided with 40 runner through holes on quiet dish 9 equally, quiet dish side through hole is pressed branch layouts such as two rows, and 20 holes of following row connect by the outer tube 13 adsorption column import corresponding with it respectively; 20 through holes of last row with outer tube 14 and corresponding adsorption column outlet connection, make materials flow form clocklike pre-adsorbent counter current contacting in system equally, realize continuous circulating.Annular groove and passage on Moving plate and the quiet dish, main effect is to make the various materials flows in the chromatographic fractionation system realize organized circulation, finish material simultaneously to the timing of each adsorption column, rationed task, the composition of channel track requires to decide with different process, but, adopt the dispensing arrangement of four grooves, 80 passages can satisfy the requirement of general chromatographic isolation fully with regard to the chromatographic isolation of bi-component or three component materials.
Embodiment: existing composing with fruit/glucose paste colors is separated into example, the running status and timing, rationed function of four grooves, 80 channel distributors are described: 1, feed state, see shown in the accompanying drawing 2, concerning fruit/glucose chromatographic isolation, the materials flow that enters system is the solution that fructose and glucose mix, i.e. 42% fruit/glucose slurry.Really/glucose slurry converged with phegma from No. 10 posts 17 before feeding engine PS is delivered to quiet dish charging aperture, enter quiet biscuit liquid passage, and be full of Moving plate annular groove S, materials flow is drawn through quiet dish inlet along the Moving plate feeder channel again then, enter adsorption column 18 No. 11 by outer connecting leg, material and adsorbent whole process is contacted, carry out adsorbing separation.When reaching or during near poised state, Moving plate begins 18 ° of angles of stepping rotation, at this moment, the Moving plate feeder channel aligns with the quiet dish inlet of next station, begins to No. 12 post feedings.So, Moving plate stepping rotation successively, the stepping rotation is 20 times weekly, can make that 20 adsorption columns are realized regularly, quantitative accurate feeding.
Really/the used desorbing agent of glucose chromatographic isolation is a deionized water, see shown in the accompanying drawing 3, deionized water supply mode and sound dish channel design and above-mentioned feed situation are basic identical, after just entering quiet dish inlet from the eluant, eluent of PD, flow into the desorbing agent feed path of Moving plate through Moving plate annular groove D, enter adsorption column, difference is arranged slightly with the feed state.
2, recurrent state, see shown in the accompanying drawing 4, FSMB continuous chromatography lock out operation requires to flow and must form reverse advection continuous-flow with adsorption bed in system mutually, prevent axial back mixing, therefore, in the sound dish channel design design of distributor, consider that it is very necessary rationally arranging the circulation canal structure.For making the circulation continuously of flowing mutually of FSMB chromatographic separation device, be to realize by the circulation canal that is arranged on the distributor sound dish, shown in the figure, to reflux from No. 1 post 19 and introduce quiet dish import, must have a Moving plate circulation canal to align with it this moment, liquid stream (phase flows) promptly flows into No. 2 posts 20 adjacent with No. 1 post 19 by the outer connecting leg of Moving plate through quiet dish outlet, and the rest may be inferred, the continuous circulation of the phase that flows in the formation system.
3, discharging state sees shown in the accompanying drawing 5 that described distributor is provided with two exit passageways, and wherein A channel is a product fructose flow pass, and the B passage is a byproduct glucose flow pass.Shown in the figure, draw by circulation canal, enter the Moving plate inlet,, deliver to the finished product storage tank along quiet dish outlet with fructose pump PA again through Moving plate annular groove A by outer connecting leg from the fructose that No. 3 posts 21 are separated.Because No. 3 posts 21 reflux and occupied the position of No. 5 quiet dish inlets of posts 22 backflows by outer tube cross-over connection and fructose outlet, so adopt two post parallel waies No. 5, No. 6, it is refluxed merges, and introduces quiet dish inlet, makes it form continuous closed circuit.
The flow pass of byproduct glucose and above-mentioned fructose outflow state are similar, see shown in the accompanying drawing 6, it is that the phegma from No. 17 posts 23 is entered the Moving plate inlet by the outer tube cross-over connection, uses glucose pump PB through Moving plate annular groove B along quiet dish outlet, and glucose is delivered to the byproduct storage tank.Identical with fructose discharging state, the glucose discharge nozzle has occupied the return duct position of No. 15 posts 24, therefore must come the normal recurrent state of maintenance system with 15, No. 16 two posts by the outer tube parallel connection.
Among Fig. 2-Fig. 6, solid line represents to have material to pass through, and dotted line is represented not have material and passed through, and the code name of each notch is: D-eluant, eluent, A-fructose, S-42% syrup, B-glucose.
The present invention adopts " fixed multicolumn absorption " and " distribution of single valve multichannel " mode, and you think that the stepping rotation closes feed liquid (phase flows) and just reached the chromatographic isolation effect that the counter current contacting simulation is moved with the homodromous result of stepping in system to fixing adsorption column by the distributor Moving plate.Shown in Figure 7, FSMB of the present invention in running, material S and eluent W by constant flow pump continuously from the inlet feed between No. 10 posts and No. 11 posts; Enter eluent W from the import between No. 20 posts and No. 1 post.Feed liquid S enters after the system under the suction-operated of adsorbent R, strong adsorbent F moves left simultaneously lentamente with adsorbent, when moving near No. 3 posts, then by eluant, eluent W from entering between No. 20 posts and No. 1 post, begin from left to right wash-out successively by No. 1 post, make strong adsorbate F desorb, and the direction that flows along eluant, eluent, by the product F outlet discharge that is located between No. 3 posts and No. 4 posts.In conjunction with shown in Figure 8, the S that enters system separates between post 11-17, weak adsorbate G enrichment between post 18-20.Be adsorbed agent simultaneously and carry from right to left, the eluent desorb of between post 11-17, being flowed to the right, byproduct G then discharges from the outlet between post 17-18, so F, G two components obtain separating.Among Fig. 7-8, Q-flow, U-flow velocity, W-eluant, eluent, F-fructose, S-fruit/glucose (material), G-glucose.
Claims (5)
1, a kind of stationary type moving bed imitation chromatogram separation facility, it includes a plurality of adsorption columns that adsorbent is housed, the import that it is characterized in that described a plurality of adsorption column (4) is communicated in the distributor (8) that at least one is made up of Moving plate (7) and quiet dish (9) respectively with outlet, and the Moving plate of this distributor (7) is done intermittently stepping by a motor by a cam stepping mechanism (5) drive and rotated.
2, stationary type moving bed imitation chromatogram separation facility according to claim 1, it is characterized in that having on the described Moving plate (7) and adsorption column (4) import and the annular groove that exports the corresponding runner through hole of number and adapt with the requirement of different process flow process, the slotted eye of every annular groove communicates with input and output material hole on the quiet dish (9) respectively, be provided with equally on quiet dish (9) and adsorption column (4) import and the corresponding runner through hole of outlet, quiet dish (9) side through hole is divided into two groups and be connected with exporting with corresponding adsorption column (4) import respectively.
3, stationary type moving bed imitation chromatogram separation facility according to claim 1 and 2, it is characterized in that described quiet dish (9) side through hole is divided into by branches such as two rows arranges, every row is one group, following exhausting hole connects by outer tube (13) adsorption column (4) import or export corresponding with it, and the through hole of the row of going up is used outer tube (14) and corresponding adsorption column equally
(4) outlet or import connect; The side of Moving plate (7) also is provided with and can changes the through hole that materials flow flows to, realizes multicolumn series, parallel or cross-over connection arbitrarily.
4, stationary type moving bed imitation chromatogram separation facility according to claim 3 is characterized in that being provided with above the described Moving plate (7) one and can produce the thrust disc (10) that rubbing surface that pretightning force makes dynamic and static dish fits tightly.
5, stationary type moving bed imitation chromatogram separation facility according to claim 1, it is characterized in that described adsorption column (4) is installed on the ring-shaped platform (2) by uniform, this ring-shaped platform (2) is arranged on the middle part of a frame (1), and motor and cam stepping mechanism (5) are equipped with in frame (1) center line bottom.
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| CN 200610053183 CN1923330A (en) | 2006-08-28 | 2006-08-28 | Stationary type moving bed imitation chromatogram separation facility |
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| CN 200610053183 CN1923330A (en) | 2006-08-28 | 2006-08-28 | Stationary type moving bed imitation chromatogram separation facility |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102338784A (en) * | 2010-07-21 | 2012-02-01 | 江苏天瑞仪器股份有限公司 | Control system and control method for high efficiency liquid chromatograph |
| CN104815460A (en) * | 2015-05-26 | 2015-08-05 | 陕西工信环保科技发展有限公司 | Continuous type adsorption equipment |
| CN106896178A (en) * | 2017-04-28 | 2017-06-27 | 新疆维吾尔自治区分析测试研究院 | A kind of intelligent glass packed column |
-
2006
- 2006-08-28 CN CN 200610053183 patent/CN1923330A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102338784A (en) * | 2010-07-21 | 2012-02-01 | 江苏天瑞仪器股份有限公司 | Control system and control method for high efficiency liquid chromatograph |
| CN104815460A (en) * | 2015-05-26 | 2015-08-05 | 陕西工信环保科技发展有限公司 | Continuous type adsorption equipment |
| CN106896178A (en) * | 2017-04-28 | 2017-06-27 | 新疆维吾尔自治区分析测试研究院 | A kind of intelligent glass packed column |
| CN106896178B (en) * | 2017-04-28 | 2018-08-17 | 新疆维吾尔自治区分析测试研究院 | A kind of intelligent glass packed column |
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