DE102007023690A1 - Process control module has medium chamber, where multiple process control modules are assembled on micro-reaction system and connected with one another by fluidic connections - Google Patents

Abstract

The process control module (1) has a medium chamber (5), where multiple process control modules are assembled on a micro-reaction system and connected with one another by fluidic connections. The medium chamber is provided for receiving a micro fluid operation unit or a combined micro fluidic operation unit, and the fluidic connections meet in a connecting flange (3). A fluid line is guided into a cavity between the connecting flange and the operation unit, which is provided with vacuum.

Description

The The invention relates to a device in which individual operating elements, so-called "unit operations" of chemical or pharmaceutical Process engineering, in particular miniaturized operational elements, especially at extreme temperatures, d. H. very deep or very high temperatures, can be operated without the Exterior surfaces harmful to health temperatures to reach. These operation elements may be z. B. heaters, Mixers, heat exchangers, reactors, separators, extractors or combined miniaturized operational elements, d. H. combinations from z. As heaters, mixers, heat exchangers, reactors, separators or extractors that work together with sensors for process monitoring and if necessary. with actuators or miniaturized actuators, such. B. Valves, can be accommodated in a confined space. These operation elements can be used individually or by inexpensive and secure connection of several of these devices to a complete process line for chemical or pharmaceutical reactions are built.

in view of the ever increasing cost pressure sets the chemical and pharmaceutical Industry reinforces components of micro process technology to develop new products or to improve existing ones Products, but especially for the production of these products. Especially in the so-called modular microreaction systems it has been found that the process control of these installations built in a confined space is very problematic. These modules are often one Well built up heat conductive material, so that adjacent Components influence each other. The desired local Temperature control of the process line, d. H. an insulated tempering a single operation element, especially at very deep or very high temperatures, can be - if at all - only accomplish with a great technological effort.

Further is the question of the lifetime of micro-procedural operational elements not yet resolved. While Ablations of fractions of millimeters in a macroscopic Component can hardly affect functionality of a micro-procedural operational element characterized strong be impaired or to complete failure to lead.

Modular microreaction systems are already known. A system will be in DE 10 2004 037 059 described. A film stack is inserted into a solid housing, which is usually made of metal. To isolate the film stack, in which the chemical reaction takes place substantially, the film stack can be placed on insulating spacers, which accomplish a certain thermal insulation. Nevertheless, the media must first be fed through holes in the massive housing to the film stack. In particular, in a prolonged operation of the functional element, there is a significant heating or cooling of the housing and thus to a thermal influence of adjacent components. This design is not suitable for process control at high temperatures, ie at temperatures above 150 ° C or at low temperatures, ie at temperatures below -10 ° C. In addition, the surfaces of the functional elements can reach harmful temperatures, so that a safe touch is not allowed.

DE 202 01 753 U1 describes a microreactor system consisting of a carrier system and microreactor modules interconnected by mass transfer channels. Also in this system, film stacks are inserted into a housing. There is no thermal insulation to neighboring components. In addition, this device has the disadvantage that it relies on a carrier plate, which also consists of metal. Also via this carrier plate is a heat transfer to adjacent systems. Thus, this design is not particularly suitable for carrying out chemical or pharmaceutical reactions at higher or lower temperatures.

moreover Aggressive chemical substances require the use of appropriate corrosion resistant materials. These materials are i. d. R. costly and difficult to work. Therefore, after Solutions sought, the necessary amount of this corrosion resistant Minimize materials.

in view of In the sketched state of the art, the invention has the task of a process control system for chemical or pharmaceutical process engineering, especially the micro process technology, to provide that is also used at temperatures above 150 ° C and below -10 ° C can be, without causing a special warm-up of the housing or icing of the housing comes.

According to the invention the object is achieved by a process control module according to claim 1. Advantageous further embodiments are in the subclaims described.

The invention also makes it possible for substantially only the parts that really touch the media to be heated or cooled by the stream of material flowing through. The mass of these media contacting parts is minimized. This will be a high Dynamic in the temperature control achieved. Temperature changes of the media through a material conversion can be reacted faster. The use of energy to heat or cool the material streams is minimized, thereby drastically improving the energy balance of the chemical or pharmaceutical process. At the same time, the use of very expensive materials with high corrosion resistance, z. As Hastelloy ^® or tantalum, be reduced to exactly these media contacting parts. As a result, the production of microprocedure components with excellent corrosion resistance can be carried out much more cost-effectively, and thus the use of these materials can be made in a large width.

Under Microstructures in this context are structures to be understood, which are smaller than 1 mm in at least one dimension. fluids, as they are called in this context are very far too understand and are not limited to liquids only but also include gases, emulsions, dispersions, mixtures of the most different kind etc .. Operation elements are functional units chemical or pharmaceutical or biochemical engineering such as z. As heaters, heat exchangers, mixers, separators, rectifiers, Filters or reactors. The function of these operation elements is in this context by integrated or external sensors (eg. Flow sensors, temperature sensors, pressure sensors, pH sensors, Conductivity sensors, turbidity sensors, particle sensors) and controlled by integrated or external actuators (eg valves). A microreaction system is an array of at least two Operation elements ggfls. with at least one actuator or sensor or at least one operation element and at least one actuator or sensor.

The process control module is expediently constructed of two separate chambers, a media chamber and an electronics chamber, as it already is DE 10 2004 037 059 is known. In the media chamber, an operation element in the form of any microfluidic structuring is introduced. This structuring can z. B. consist of a film stack of microstructured individual films, one or more specially shaped capillary tubes or structures produced by laser sintering. Regardless of the way in which the fluidic structures are manufactured, it is essential that the fluidic structures have direct contact with the surrounding housing only insofar as it is necessary to supply or discharge the media. This chamber can be connected via a corresponding connection z. B. be evacuated by means of a diaphragm pump. In this case, a negative pressure of a few millibars is already sufficient to achieve sufficient thermal insulation to the housing. As an alternative to vacuum insulation, the space between the media-carrying structures and the housing can also be filled by a thermally highly insulating material. For this purpose, the material should have a thermal conductivity of less than 0.1 W / K, preferably less than 0.001 W / K.

The wall, which separates the two chambers, is divided into two parts and has trenches in which z. B. capillary tubes are inserted, in which the streams are supplied to the operating element in the media chamber. At both ends of the capillary tubes devices can be attached, with which on the one hand allows a connection of adjacent Prozeßleitmodule and on the other hand, a connection to the operation module in the media chamber is achieved. These capillary tubes have no contact with the housing. Only the devices at the two ends of the capillary tubes have a slight contact with the housing. After the vacuum tight assembly of the two halves of the wall, the capillary tubes and the devices at the ends of the capillary tubes, the space between the halves of the wall can also be evacuated. As an alternative to vacuum insulation, the space between the capillary tubes and the two halves of the wall can be filled with a thermally highly insulating material. For this purpose, the material should have a thermal conductivity of less than 0.1 W / K, preferably less than 0.001 W / K. In this way, a cost-effective super insulation of all media-carrying parts of the environment is achieved. At the same time, almost complete super insulation can be maintained across the entire process line, which can consist of any number of process control modules. Thus, only the microfluidic structures and necessary for the supply of the material flow line elements, ie, for example, the capillaries and the fittings, made of a highly corrosion-resistant material such. B. Hastelloy ^® or tantalum exist.

The Housing, the wall between the two chambers and cover and press plates can be made from less corrosion resistant and thus cheaper material or easier to edit Material to be made. The assembly may be preferred by soldering, brazing, welding, diffusion soldering or diffusion welding. Moreover, it is conceivable that the Individual parts sealed with each other via elastic seals become. The partition between the media chamber and the electronics chamber can also be prepared by various other methods. Here offers z. B. the method of laser sintering. The production can also be done by assembling appropriately structured Sheets or foils.

The Temperature measurement of the material flows takes place through the Outside of the capillaries mounted temperature sensors. Because these sensors also have no contact with the housing have, is the thermal mass that is in contact with the sensors comes, extremely small. In this way, the temperature can be highly dynamic the sometimes small amounts of material flow are detected. Because the Temperature sensors in the immediate vicinity of the microfluidic Be attached structures in which the material conversion or the temperature control of the material flows takes place, it is possible the exact temperature z. B. during the chemical reaction too to capture.

Based the drawings, the invention, for example, closer explained.

1 shows in a perspective view a assembled process control module with integrated super insulation.

2 shows in a sectional view the wall between the media chamber and the electronics chamber consisting of a top and a bottom.

3 shows in an exemplary embodiment, a flange for connecting adjacent process control modules.

4 shows an exemplary embodiment of a nozzle for connection to the microfluidic operation element in the interior of the media chamber.

5 shows in section the process control module 1 ,

1 shows a three-dimensional structure of a process control module 1 with integrated super insulation. In this embodiment, there is a process control module 1 on a housing foot 6 , In the lower part of the process control module 1 is the housing of an electronics chamber 4 to recognize. A media chamber 5 and the electronics chamber 4 are separated in this embodiment by a two-part wall 2 made of a lower part 2a and a top 2 B is constructed. On the wall 2 at least one flange is attached 3 for the fluidic connection to an adjacent process control module. The media chamber 5 is closed at the top by a clamping lid 15 , On the clamping lid 15 attached are a supply line 8th and a derivative 9 for the service medium. The inlet and outlet can be connected by commercially available connections z. B. Swagelok ^®. Likewise, on the clamping lid 15 a vacuum nozzle 16 with a vacuum valve 7 available. Here also a commercial vacuum valve from Swagelok ^® can be used. The vacuum may also be via one of the flanges in an alternative embodiment 3 be created. In this case, the corresponding flange 3 not with a fluid line 18 connected. The flange 3 to which a vacuum pump can be connected, in this case has the holes 32 and 33 an opening to the large recesses 19 and the media chamber 5 so that the cavities can be evacuated (see. 2 ).

2 shows the wall 2 between the electronics chamber 4 and the media chamber 5 , The wall consists in this embodiment of a lower part 2a and a top 2 B , In the lower part 2a is at least one hole 17 let in for introducing at least one temperature sensor 23 , These holes are sealed tightly after mounting the sensor vacuum. For this purpose, the bore z. B. be filled with a vacuum-resistant glass solder. The lower part 2a and the top 2 B have large recesses 19 , which serve the vacuum insulation after assembly. As an alternative to vacuum insulation, this room can 19 also be filled by a material with a low thermal conductivity. In addition, in these recesses 19 the flanges 3 , Support 11 and fluidic connections in the form of conduits 18 inserted so that only the flanges 3 and the neck 11 a firm connection to the wall 2 to have.

3 shows in an exemplary embodiment a flange 3 for connecting adjacent process control modules. This flange may be designed for a direct metal-to-metal seal with an adjacent flange. But it can also identify sealing surfaces or sealing grooves for elastic seals on its front page.

In the 4 In an exemplary embodiment, it is a nozzle 11 represented the connection between the line 18 and a fluidic operating element 10 in the media room 5 ( 5 ). In the illustrated embodiment are in the neck 11 seal grooves 21 for an elastic sealing ring attached. The seal to the fluidic operating element 10 but can also be done by other methods, for. As welding, soldering, diffusion soldering or diffusion welding. In these cases, appropriately adapted sealing structures in the nozzle 11 incorporated. The administration 18 gets through a hole 22 in the neck 11 introduced and vacuum tight with the neck 11 connected. The fluidic operation element 10 has only over the neck 11 a heat-conducting contact to the wall 2 or the housing of the process control module 1 ,

As 3 shows that are provided for the connection between adjacent process control modules seen flanges 3 with an approach 31 provided that a bore 32 has, whose diameter may be greater than the outer diameter of a flange 3 connected fluid line 18 in the middle hole 33 of the flange 3 is used. As 2 shows, so can the line 18 also on one through the connecting flange 3 leading portion to be surrounded by a vacuum-loadable cavity, so that the fluid line 18 only on the short end section in the hole 33 of the flange 3 with this in thermally conductive contact.

In the same way is the nozzle 11 in 4 with a hole 25 provided whose diameter can be greater than the outer diameter of the line 18 into the hole 22 is inserted in an intermediate wall 22a of the approximately tubular neck 11 is introduced centrally. As 2 shows that way in the neck 11 used fluid line 18 be largely surrounded with a vacuum-loadable cavity to the isolation of the fluid line 18 to improve, with the fluid line 18 only on the short distance of the thickness dimension of the partition 22a with the neck 11 communicates. Furthermore, the nozzle has 11 at one end a radially projecting flange 26 on, through which the neck 11 at a heel in the bore of the shell 2 B the Wall 2 abuts the contact surface between nozzles 11 and wall 2 keep as small as possible. As 2 shows is also the outer circumference of the neck 11 on a section of a cavity of the hole in the shell 2 B surrounded, so that this area can be applied to vacuum.

If in a process control module no electronic chamber 4 is provided, instead of in 2 reproduced two-part wall 2 also a one-piece connection element with connecting flanges 3 be provided, wherein the connecting flanges 3 as shown in holes of this connection element according to the wall 2 are used.

5 provides the process control module 1 with integrated superinsulation in section. The fluidic operating element 10 has only over the neck 11 a heat-conducting contact with the housing 5a , The thermal insulation is achieved by the application of vacuum in the media chamber 5 and at the same time in the cavity of the wall 2 , As an alternative to vacuum insulation, the space between the operating element becomes 10 and the housing 5a the media chamber 5 filled with a material with a low thermal conductivity. The media chamber 5 comes with a sealing lid 24 Vacuum sealed. The sealing cover 24 has two holes for the feeder 8th and the exhaustion 9 of the service medium. These holes are also sealed tight vacuum. Furthermore, the sealing lid has 24 a hole for the vacuum nozzle 16 , which is also sealed tight vacuum. The fluidic operation element 10 is in the illustrated embodiment via a compression screw 17 and the sealing lid 24 on the neck 11 pressed, creating a fluid-tight seal between the fluidic operating element 10 and the neck 11 will be produced.

In a particular embodiment, only the nozzles exist 11 , the flanges 3 , the fluidic connections or lines 18 and the operation element 10 made of a particularly corrosion-resistant material (eg. as titanium, tantalum, Hastelloy ^®, glass, ceramic). Frequently, such materials are particularly expensive and also difficult to work. With this embodiment, only the media-contacting parts must be made of this material, while the other parts of the Prozeßleitmoduls can consist of a cheaper and / or easier-to-work material. So these parts z. B. also be made of plastic.

QUOTES INCLUDE IN THE DESCRIPTION

This list The documents listed by the applicant have been automated generated and is solely for better information recorded by the reader. The list is not part of the German Patent or utility model application. The DPMA takes over no liability for any errors or omissions.

Cited patent literature

• - DE 102004037059 [0004, 0011]
• - DE 20201753 U1 [0005]

Claims (5)

Process control module with a media chamber ( 5 ) for receiving a microfluidic operating element ( 10 ) or a combined microfluidic operation element, wherein a number of Prozessleitmodulen is assembled into a microreaction system and the Prozeßleitmodule communicate by fluidic connections with each other in a connecting flange ( 3 ), characterized in that fluid lines ( 18 ) in a cavity between connecting flange ( 3 ) and operation element ( 10 ) are guided, which is acted upon by vacuum. Process control module with a media chamber ( 5 ) for receiving a microfluidic operating element ( 10 ) or a combined microfluidic operation element, wherein a number of Prozessleitmodulen is assembled into a microreaction system and the Prozeßleitmodule communicate by fluidic connections with each other in a connecting flange ( 3 ), characterized in that fluid lines ( 18 ) in a cavity between connecting flange ( 3 ) and operation element ( 10 ), which is filled with a material with low thermal conductivity of less than 0.1 W / K, preferably less than 0.001 W / K. Process control module according to claim 1 or 2, wherein at the process control module ( 1 ) a hollow connection element ( 2 ), the bores for receiving the connecting flanges ( 3 ) and bores for receiving nozzles ( 11 ), wherein the fluid lines ( 18 ) between the nozzles ( 11 ) and the connection flanges ( 3 ). Process control module according to claim 3, wherein only the media Contacting parts of a particularly corrosion resistant Material are made. Process control module according to claim 3, wherein the connection element ( 2 ) is formed in two parts and the dividing line between the two parts ( 2a . 2 B ) centrally through the bores for the connecting flanges ( 3 ) runs.