CN2557201Y - Multi-filling column series connected reaction separation coupler - Google Patents
Multi-filling column series connected reaction separation coupler Download PDFInfo
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- CN2557201Y CN2557201Y CN 02216135 CN02216135U CN2557201Y CN 2557201 Y CN2557201 Y CN 2557201Y CN 02216135 CN02216135 CN 02216135 CN 02216135 U CN02216135 U CN 02216135U CN 2557201 Y CN2557201 Y CN 2557201Y
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Abstract
The utility model discloses a reaction separation coupling device with a plurality of filling columns connected in series, comprising three or more filling columns, with the outlet end of the previous filling column is sequentially connected with the inlet end of the subsequent filling column; the inlet end of each filling column is connected with a raw material liquid inlet pipeline where the reactant is input and an inlet pipe for inputting the eluent by respective switch-typed valve; the outlet end of each filling column is connected with a residual liquid outlet pipeline which outputs the weak adsorption compositions in the reaction products, and an extraction liquid outlet pipeline which outputs the strong adsorption compositions in the reaction products by respective switch-typed valve. By controlling the on/off state of the valve, chromatogram separation process and reaction process can be carried out at the same time. The utility model can automatically and continuously run, and not only improves the conversion ratio of the reaction, but also improves the separation efficiency of products. The utility model is particularly suitable for the reaction separation coupling process where the filling column chromatogram technology required be adopted to separate the different compositions of products and to separate reaction products and reactants.
Description
Technical field
The utility model relates to and includes the Reaction Separation coupling device that comes treat liquid with catalyst and adsorbent, relates in particular to a kind of Reaction Separation coupling device of many packed columns series connection.
Background technology
In chemical industry, medicine, biology and fine chemistry industry industrial application, the downstream of chemical reactor or biochemical reactor generally has a series of separators and matches to constitute whole flow process, and these separators mainly are separating with physical method realization response product and reactant, and the purification of realization response product, thereby obtain meeting the product of quality index.But, can make the situation of catalyst poisoning for reversible reaction or byproduct of reaction, just there are shortcomings such as reaction conversion ratio is low, the product yield is low, separative efficiency is low, production capacity is low in this type of technological process.To react with separating the Reaction Separation coupling device that is coupled as a chemical industry operation unit be the effective way that addresses the above problem and adopt.
In recent years, chemical reaction and two processes of separated are incorporated into the reaction distillation process of carrying out in the equipment successfully realize industrialization, relatively successful application is the catalysis synthesizing technology of methyl tertiary butyl ether(MTBE) (MTBE).
Yet the physico-chemical property of each part of mixture that constitutes when reactant, product and accessory substance is very approaching, uses conventional isolation technics to wait when being difficult to separate as distillation, just needs to use chromatographic separation technology usually.United States Patent (USP) (US 2976132) and Canadian Patent (CAN 631882) disclose a class in succession with chemical reaction and two PROCESS COUPLING of chromatographic isolation chromatographic reactor technology together, and the characteristics of above-mentioned patented technology are intermittently operated.Because intermittently chromatogram has mutually fixing and mobile consumption mutually is big, the adsorbent utilization rate is low, separated product concentration is low, separation costs is crossed high shortcoming, makes the chromatographic reactor technology with chromatogram feature at intermittence be difficult to apply at industrial circle.
Summary of the invention
A kind of chemical reactor is connected with the multicolumn with continuous chromatography feature of the utility model design washed the Reaction Separation coupling device that colour atlas becomes many packed columns series connection of a chemical industry operation unit.
The technical solution adopted in the utility model is: it comprises the packed column more than three or three, be connected successively by the port of export of last packed column and the entrance point of a back packed column, the port of export of last root packed column is connected with the entrance point of connecting line with first packed column with connecting line or open-close type valve through circulating pump; The open-close type valve that the entrance point of every packed column passes through respectively separately is connected with material liquid entrance pipe, the input eluent entrance pipe of input reactant; Open-close type valve by separately is enriched with the residual solution export pipeline of weak adsorptivity composition in the product with output to the port of export of every packed column respectively, the extract export pipeline that output is enriched with strong adsorptivity composition in the product is connected.
In general, the Reaction Separation coupling device of many packed column series connection is formed by connecting from beginning to end by the packed column more than four or four, flow to a direction at the inner fluid of forcing of device, set gradually the eluent entrance according to the on off state of fluid flow direction by by-pass valve control, the extract exit point, the material liquid entrance, the residual solution exit point, thereby all packed columns four subregions have been divided into, each subregion comprises a packed column at least, after having passed through a given time interval, by changing the on off state of valve, make each entrance, exit point is passed along the packed column that is directed downwards that fluid flows respectively, same four subregions are also passed to next root packed column thereupon, move in circles like this and just formed solid filler virtual flow round about, thus the effect that relatively moves between realization solid filler and fluid.The characteristic of this counter-current operation both can improve the transformation efficiency of catalyst, can improve the separative efficiency of adsorbent again.
Four subregions of the Reaction Separation coupling device of many packed column series connection are finished different functions respectively.Be mainly used to adsorb as yet in the product of wash-out not adsorptivity composition by force at eluent inlet and subregion I between the extract outlet; Adsorptivity composition a little less than in extract outlet is used for the elution of reactive product with subregion II between the material liquid inlet; Strong adsorptivity composition in the main adsorption reaction product of subregion III between material liquid inlet and residual solution outlet; Adsorptivity composition a little less than residual solution outlet and subregion IV between the eluent inlet are mainly used to adsorb as yet in the product of wash-out not.Subregion II and subregion III also are reactors simultaneously, and wherein subregion III is main conversion zone.
Whether directly be communicated with subregion I according to subregion IV, the Reaction Separation coupling device of many packed column series connection can be divided into closed-loop structure and open loop structure.The Reaction Separation coupling device structure that subregion IV connects with many packed columns of the direct closed-loop structure that is communicated with of subregion I is comparatively compact, but must be equipped with fluid circulation pump.Though the Reaction Separation coupling device that subregion IV connects with many packed columns of the disconnected open loop structure of subregion I needs to increase valve member, but need not to be equipped with fluid circulation pump, simple to operate, can prevent the accessory substance or other contaminating impurity target product that flow out in the subregion IV simultaneously.For the Reaction Separation coupling device that many packed columns of open loop structure are connected, if weak adsorptivity composition absorption hardly on adsorbent in the product is certain polymer or big molecule such as this composition, then subregion IV can omit.
The utility model has the advantages that:
1. the difference of adsorption capacity on solid absorbent according to product and reactant, the realization response product separates continuously with reactant, destroys chemical balance, quickens chemical reaction velocity, increases conversion ratio, improves production capacity;
2. according to the difference of the adsorption capacity on solid absorbent of different components in the product, weak adsorptivity composition and strong adsorptivity composition separates continuously in the realization response product;
3. this device can move automatically and continuously, can improve the conversion ratio of reaction, can improve the separative efficiency of product again, has flexibility with the commercial production scale of compact package formation efficiently, be specially adapted to have only employing packed column chromatographic technique, the Reaction Separation coupling process of ability reaction product isolated different components, reaction product isolated and reactant.
Description of drawings
Fig. 1 is the structural representation of Reaction Separation coupling device of many packed columns series connection of closed-loop structure;
Fig. 2 is the structural representation of Reaction Separation coupling device of many packed columns series connection of four subregion open loop structures;
Fig. 3 is the structural representation of Reaction Separation coupling device of many packed columns series connection of three subregion open loop structures;
Fig. 4 is packed column structure and inner stuffing schematic diagram.
The specific embodiment
The Reaction Separation coupling device of many packed column series connection of closed-loop structure as shown in Figure 1, it comprises four packed columns 1,2,3,4, be connected by the port of export of first packed column 1 and the entrance point of second packed column 2, the port of export of second packed column 2 is connected with the entrance point of the 3rd packed column 3, the port of export of the 3rd packed column 3 is connected with the entrance point of the 4th packed column 4, and the port of export of the 4th packed column 4 is connected with the entrance point of connecting line 7 with first packed column 1 through circulating pump 10; The entrance point of every packed column 1,2,3, the 4 material liquid entrance pipe 5, the eluent entrance pipe 6 of importing eluent of open-close type valve VA1, the VA2 by separately, VA3, VA4 and open-close type valve VB1, the VB2 by separately respectively, VB3, VB4 and input reactant respectively is connected; The port of export of every packed column 1,2,3,4 respectively open-close type valve VD1, the VD2 by separately, VD3, VD4 with respectively by open-close type valve VC1, VC2, VC3, VC4 and output separately be enriched with the residual solution export pipeline 8 of weak adsorptivity composition in the product, the extract export pipeline 9 that output is enriched with strong adsorptivity composition in the product is connected.In the above-mentioned device that is made of 4 packed columns, the on off state of all open-close type valves has 4 kinds of combinations, by suitable switching time, switches and moves in circles according to following order:
1. open valve VA3, VB1, VC1, VD3; Closing valve VA1, VA2, VA4, VB2, VB3, VB4, VC2, VC3, VC4, VD1, VD2, VD4.
2. open valve VA4, VB2, VC2, VD4; Closing valve VA1, VA2, VA3, VB1, VB3, VB4, VC1, VC3, VC4, VD1, VD2, VD3.
3. open valve VA1, VB3, VC3, VD1; Closing valve VA2, VA3, VA4, VB1, VB2, VB4, VC1, VC2, VC4, VD2, VD3, VD4.
4. open valve VA2, VB4, VC4, VD2; Closing valve VA1, VA3, VA4, VB1, VB2, VB3, VC1, VC2, VC3, VD1, VD3, VD4.
The Reaction Separation coupling device of many packed column series connection of four subregion open loop structures as shown in Figure 2, it comprises four packed columns 1,2,3,4, the port of export by first packed column 1 is connected with the entrance point of second packed column 2 through open-close type valve VF1, the port of export of second packed column 2 is connected with the entrance point of the 3rd packed column 3 through open-close type valve VF2, the port of export of the 3rd packed column 3 is connected with the entrance point of the 4th packed column 4 through open-close type valve VF3, and the port of export of the 4th packed column 4 is connected with the entrance point of connecting line 7 with first packed column 1 through open-close type valve VF4; The entrance point of every packed column 1,2,3, the 4 material liquid entrance pipe 5, the eluent entrance pipe 6 of importing eluent of open-close type valve VA1, the VA2 by separately, VA3, VA4 and open-close type valve VB1, the VB2 by separately respectively, VB3, VB4 and input reactant respectively is connected; The port of export of every packed column 1,2,3,4 respectively open-close type valve VD1, the VD2 by separately, VD3, VD4 with respectively by open-close type valve VC1, VC2, VC3, VC4 and output separately be enriched with the residual solution export pipeline 8 of weak adsorptivity composition in the product, the extract export pipeline 9 that output is enriched with strong adsorptivity composition in the product is connected; Open-close type valve VE1, VE2, VE3, VE4 that the port of export of every packed column 1,2,3,4 also passes through separately respectively are connected with the eluent export pipeline 11 of output eluent.In the above-mentioned device that is made of 4 packed columns, the on off state of all open-close type valves has 4 kinds of combinations, by suitable switching time, switches and moves in circles according to following order:
1. open valve VA3, VB1, VC1, VD3, VE4, VF1, VF2, VF3; Closing valve VA1, VA2, VA4, VB2, VB3, VB4, VC2, VC3, VC4, VD1, VD2, VD4, VE1, VE2, VE3, VF4.
2. open valve VA4, VB2, VC2, VD4, VE1, VF2, VF3, VF4; Closing valve VA1, VA2, VA3, VB1, VB3, VB4, VC1, VC3, VC4, VD1, VD2, VD3, VE2, VE3, VE4, VF1.
3. open valve VA1, VB3, VC3, VD1, VE2, VF1, VF3, VF4; Closing valve VA2, VA3, VA4, VB1, VB2, VB4, VC1, VC2, VC4, VD2, VD3, VD4, VE1, VE3, VE4, VF2.
4. open valve VA2, VB4, VC4, VD2, VE3, VF1, VF2, VF4; Closing valve VA1, VA3, VA4, VB1, VB2, VB3, VC1, VC2, VC3, VD1, VD3, VD4, VE1, VE2, VE4, VF3.
The Reaction Separation coupling device of many packed column series connection of three subregion open loop structures as shown in Figure 3, it comprises three packed columns 1,2,3, the port of export by first packed column 1 is connected with the entrance point of second packed column 2 through open-close type valve VF1, the port of export of second packed column 2 is connected with the entrance point of the 3rd packed column 3 through open-close type valve VF2, and the port of export of the 3rd packed column 3 is connected with the entrance point of connecting line 7 with first packed column 1 through open-close type valve VF3; The entrance point of every packed column 1,2, the 3 material liquid entrance pipe 5, the eluent entrance pipe 6 of importing eluent of open-close type valve VA1, the VA2 by separately, VA3 and open-close type valve VB1, the VB2 by separately, VB3 respectively and input reactant respectively is connected; The port of export of every packed column 1,2,3 respectively open-close type valve VD1, the VD2 by separately, VD3 with respectively by open-close type valve VC1, VC2, VC3 and output separately be enriched with the residual solution export pipeline 8 of weak adsorptivity composition in the product, the extract export pipeline 9 that output is enriched with strong adsorptivity composition in the product is connected.In the above-mentioned device that is made of 3 packed columns, the on off state of all open-close type valves has 3 kinds of combinations, by suitable switching time, switches and moves in circles according to following order:
1. open valve VA3, VB1, VC1, VD3, VF1, VF2; Closing valve VA1, VA2, VB2, VB3, VC2, VC3, VD1, VD2, VF3.
2. open valve VA1, VB2, VC2, VD1, VF2, VF3; Closing valve VA2, VA3, VB1, VB3, VC1, VC3, VD2, VD3, VF1.
3. open valve VA2, VB3, VC3, VD2, VF1, VF3; Closing valve VA1, VA3, VB1, VB2, VC1, VC2, VD1, VD3, VF2.
Open-close type valve is the combination of two general formula valves or triple valve or multiple-way valve or rotary valve or various open-close type valves.
Filler in the whole packed column is the homogeneous mixture (shown in Fig. 4 A) of solid porous pellet type catalyst and solid porous granular adsorption agent; Or packed column is made of the short column more than two sections or two sections and at least one section short column in filler be that filler in solid porous pellet type catalyst and at least one section short column is solid porous granular adsorption agent (shown in Fig. 4 B, C); Or the filler in the packed column is the solid porous particle (shown in Fig. 4 D) that contains catalyst composition and adsorbent composition simultaneously; Or the filler in the packed column is solid porous granular adsorption agent (shown in Fig. 4 E), and catalyst dissolution is from the eluent of eluent entrance pipe input or be dissolved in from the material liquid of material liquid entrance pipe input.
Catalyst is chemical catalyst or biocatalyst; Adsorbent is various separation solid fillers, as chiral stationary phase or resin or molecular sieve.
The Reaction Separation coupling device of many packed column series connection is not limited in the form of implementation that above-mentioned all subregions have all only disposed a packed column, in fact the packed column number that each subregion is all configurable more than, number is not necessarily identical, the annexation of device can be expanded, and the on off state of valve switches also can have more kinds of combinations.For instance, all dispose two packed columns at subregion I, subregion II, subregion IV and be beneficial to abundant separation, then dispose three packed columns as the subregion III that reacts main region and be beneficial to abundant reaction.In the above-mentioned device that constitutes by 9 packed columns, the on off state of all open-close type valves also just has 9 kinds of combinations, switch in regular turn by suitable switching time, make each entrance, exit point pass and move in circles along the packed column that is directed downwards that fluid flows respectively.
In theory, the packed column sum that the Reaction Separation coupling device of many packed column series connection is disposed is many more to be helped reacting and fully carrying out of separating more, but the increase of packed column number also causes the increase of equipment and complicated operation degree, so the packed column sum that the Reaction Separation coupling device of many packed column series connection is disposed generally is no more than 48.
In fields such as chiral drug, optical material, senior essence and flavoring agent, agricultural chemical insecticides, the production of chipal compounds single enantiomer is a great problem.Generally all be at first to adopt various reactors to produce racemic modification, adopt direct crystallization mechanical phonograph recorder separation, formation then and separate complex process such as diastereoisomer method, microorganism Split Method and the low method resolution of racemates of separative efficiency obtains single enantiomer.There are shortcomings such as reaction conversion ratio is low, separative efficiency is low in above-mentioned technological process, has seriously hindered the development of CHIRAL INDUSTRY.Adopt the Reaction Separation coupling device of many packed column series connection, select appropriate catalyst and chiral stationary phase adsorbent for use, carry out when just can realize racemic modification production and fractionation, can improve the conversion ratio of reaction, can improve the fractionation efficient of racemic modification again.The Reaction Separation coupling device of many packed column series connection can be applicable to the production of chiral drug single enantiomers such as salbutamol, Prozac, Ofloxacin, naproxen, brufen, Ketoprofen, phosphonomycin, Thiamphenicol, also be expected to be used for the production of the optical pure compound in fields such as optical material, senior essence and flavoring agent, agricultural chemical insecticide, have wide prospect in industrial application.
Claims (7)
1. the Reaction Separation coupling devices of many packed columns series connection, it is characterized in that: it comprises the packed column more than three or three, be connected successively by the port of export of last packed column and the entrance point of a back packed column, the port of export of last root packed column is connected with the entrance point of connecting line with first packed column with connecting line or open-close type valve through circulating pump; The open-close type valve that the entrance point of every packed column passes through respectively separately is connected with material liquid entrance pipe, the input eluent entrance pipe of input reactant; Open-close type valve by separately is enriched with the residual solution export pipeline of weak adsorptivity composition in the product with output to the port of export of every packed column respectively, the extract export pipeline that output is enriched with strong adsorptivity composition in the product is connected.
2. the Reaction Separation coupling device of many packed columns series connection according to claim 1, it is characterized in that: it comprises four packed columns [1], [2], [3], [4], be connected by the port of export of first packed column [1] and the entrance point of second packed column [2], the port of export of second packed column [2] is connected with the entrance point of the 3rd packed column [3], the port of export of the 3rd packed column [3] is connected with the entrance point of the 4th packed column [4], and the port of export of the 4th packed column [4] is connected with the entrance point of connecting line [7] with first packed column [1] through circulating pump [10]; The entrance point of every packed column [1], [2], [3], [4] is the open-close type valve [VA1] by separately, [VA2], [VA3], [VA4] and the open-close type valve [VB1] by separately, [VB2], [VB3], [VB4] and the material liquid entrance pipe [5] of importing reactant, the eluent entrance pipe [6] of importing eluent are connected respectively respectively; The port of export of every packed column [1], [2], [3], [4] respectively the open-close type valve [VD1] by separately, [VD2], [VD3], [VD4] with respectively by open-close type valve [VC1], [VC2], [VC3], [VC4] and output separately be enriched with the residual solution export pipeline [8] of weak adsorptivity composition in the product, the extract export pipeline [9] that output is enriched with strong adsorptivity composition in the product is connected.
3. the Reaction Separation coupling device of many packed columns series connection according to claim 1, it is characterized in that: it comprises four packed columns [1], [2], [3], [4], the port of export by first packed column [1] is connected through the entrance point of open-close type valve [VF1] with second packed column [2], the port of export of second packed column [2] is connected through the entrance point of open-close type valve [VF2] with the 3rd packed column [3], the port of export of the 3rd packed column [3] is connected through the entrance point of open-close type valve [VF3] with the 4th packed column [4], and the port of export of the 4th packed column [4] is connected with the entrance point of connecting line [7] with first packed column [1] through open-close type valve [VF4]; The entrance point of every packed column [1], [2], [3], [4] is the open-close type valve [VA1] by separately, [VA2], [VA3], [VA4] and the open-close type valve [VB1] by separately, [VB2], [VB3], [VB4] and the material liquid entrance pipe [5] of importing reactant, the eluent entrance pipe [6] of importing eluent are connected respectively respectively; The port of export of every packed column [1], [2], [3], [4] respectively the open-close type valve [VD1] by separately, [VD2], [VD3], [VD4] with respectively by open-close type valve [VC1], [VC2], [VC3], [VC4] and output separately be enriched with the residual solution export pipeline [8] of weak adsorptivity composition in the product, the extract export pipeline [9] that output is enriched with strong adsorptivity composition in the product is connected; Open-close type valve [VE1], [VE2], [VE3], [VE4] that the port of export of every packed column [1], [2], [3], [4] also passes through respectively separately are connected with the eluent export pipeline [11] of output eluent.
4. the Reaction Separation coupling device of many packed columns series connection according to claim 1, it is characterized in that: it comprises three packed columns [1], [2], [3], the port of export by first packed column [1] is connected through the entrance point of open-close type valve [VF1] with second packed column [2], the port of export of second packed column [2] is connected through the entrance point of open-close type valve [VF2] with the 3rd packed column [3], and the port of export of the 3rd packed column [3] is connected with the entrance point of connecting line [7] with first packed column [1] through open-close type valve [VF3]; The entrance point of every packed column [1], [2], [3] is the open-close type valve [VA1] by separately, [VA2], [VA3] and the open-close type valve [VB1] by separately, [VB2], [VB3] and the material liquid entrance pipe [5] of importing reactant, the eluent entrance pipe [6] of importing eluent are connected respectively respectively; The port of export of every packed column [1], [2], [3] respectively the open-close type valve [VD1] by separately, [VD2], [VD3] with respectively by open-close type valve [VC1], [VC2], [VC3] and output separately be enriched with the residual solution export pipeline [8] of weak adsorptivity composition in the product, the extract export pipeline [9] that output is enriched with strong adsorptivity composition in the product is connected.
5. according to the Reaction Separation coupling device of claim 1 or 2 or 3 or 4 described many packed columns series connection, it is characterized in that: open-close type valve is the combination of two general formula valves or triple valve or multiple-way valve or rotary valve or various open-close type valves.
6. according to the Reaction Separation coupling device of claim 1 or 2 or 3 or 4 described many packed columns series connection, it is characterized in that: the filler in the whole packed column is the homogeneous mixture of solid porous pellet type catalyst and solid porous granular adsorption agent, or packed column is made of the short column more than two sections or two sections and at least one section short column in filler be that filler in solid porous pellet type catalyst and at least one section short column is solid porous granular adsorption agent, or the filler in the packed column is the solid porous particle that contains catalyst composition and adsorbent composition simultaneously, or the interior filler of packed column is solid porous granular adsorption agent.
7. the Reaction Separation coupling device of many packed columns series connection according to claim 6, it is characterized in that: described catalyst is chemical catalyst or biocatalyst; Described adsorbent is various separation solid fillers, as chiral stationary phase or resin or molecular sieve.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376420A (en) * | 2016-04-20 | 2017-11-24 | 薛红 | Disperse mobile phase countercurrent chromatography separation method |
| CN110732159A (en) * | 2019-11-05 | 2020-01-31 | 大连大学 | continuous grading type high-efficiency extraction device |
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2002
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376420A (en) * | 2016-04-20 | 2017-11-24 | 薛红 | Disperse mobile phase countercurrent chromatography separation method |
| CN110732159A (en) * | 2019-11-05 | 2020-01-31 | 大连大学 | continuous grading type high-efficiency extraction device |
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