GB2451900A - Flow apparatus - Google Patents
Flow apparatus Download PDFInfo
- Publication number
- GB2451900A GB2451900A GB0716113A GB0716113A GB2451900A GB 2451900 A GB2451900 A GB 2451900A GB 0716113 A GB0716113 A GB 0716113A GB 0716113 A GB0716113 A GB 0716113A GB 2451900 A GB2451900 A GB 2451900A
- Authority
- GB
- United Kingdom
- Prior art keywords
- support means
- heat
- transfer device
- reaction vessel
- tubular reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 238000006243 chemical reaction Methods 0.000 claims abstract description 192
- 238000012546 transfer Methods 0.000 claims abstract description 101
- 230000000694 effects Effects 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000012530 fluid Substances 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 40
- 238000001816 cooling Methods 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005111 flow chemistry technique Methods 0.000 claims description 7
- 239000012809 cooling fluid Substances 0.000 claims description 5
- 239000013529 heat transfer fluid Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- CNQCVBJFEGMYDW-UHFFFAOYSA-N lawrencium atom Chemical compound [Lr] CNQCVBJFEGMYDW-UHFFFAOYSA-N 0.000 abstract description 68
- 230000008602 contraction Effects 0.000 abstract description 4
- 239000011541 reaction mixture Substances 0.000 description 14
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 description 13
- 239000003153 chemical reaction reagent Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 238000004891 communication Methods 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000004696 Poly ether ether ketone Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 4
- 229920002530 polyetherether ketone Polymers 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 239000011810 insulating material Substances 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003570 air Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000004323 axial length Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920001470 polyketone Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D1/00—Heat-exchange apparatus having stationary conduit assemblies for one heat-exchange medium only, the media being in contact with different sides of the conduit wall, in which the other heat-exchange medium is a large body of fluid, e.g. domestic or motor car radiators
- F28D1/06—Heat-exchange apparatus having stationary conduit assemblies for one heat-exchange medium only, the media being in contact with different sides of the conduit wall, in which the other heat-exchange medium is a large body of fluid, e.g. domestic or motor car radiators with the heat-exchange conduits forming part of, or being attached to, the tank containing the body of fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/243—Tubular reactors spirally, concentrically or zigzag wound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L7/00—Heating or cooling apparatus; Heat insulating devices
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Clinical Laboratory Science (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
A heat-transfer device 101 comprises an element 103 to effect a change in temperature of at least one tubular reaction vessel 107, the device further comprising at least one support means 105 detachably disposed about a surface of the heat-transfer element, the at least one support means being configured to support the at least one tubular reaction vessel. The present invention is characterised in that the support means is adapted to detachably maintain the tubular reaction vessel in optimised thermal contact with the support means and at least one of the support means and the element substantially surrounds at least a portion of the other. Preferably the reaction vessel comprises capillary tubing which is wound around the support means in a coil for continuous flow reactions. The heat transfer element further may have a slot 109 and channel 113 to allow for contraction and expansion and may comprise adjustment means 111 to effect a change in diameter of the element. Preferably, the support means is comprised of a material having a coefficient of expansion that is equal to or lower than that of the reaction vessel.
Description
ID 2451900
IMPROVEMENTS TO FLOW APPARATUS
Field of the Invention
The present invention relates to a heat-transfer device comprising an element to effect a change in temperature of at least one tubular reaction vessel, the device further comprising at least one support means detachably disposed about a surface of the element, which is configured to support the at least one tubular reaction vessel. In particular although not exclusively, the heat-transfer device is suitable for use in flow chemistry.
Background to the Invention
Flow chemistry is a term used for a chemical reaction which is run in a * continuously flowing stream rather than by batch production. In flow chemistry, pumps transfer a reagent into a tube and where this tube joins a second tube containing a second reagent, the reagents contact and a chemical reaction takes place. The benefits of flow chemistry include: * Increased reaction yields; * Increased reaction selectivity; * Improved control of exothermic reactions; * Reproducible; * Improved scalability; * Faster reaction optimisation; and * Superheating of reactions with no limit on scale.
These reactions may be undertaken in a laboratory environment and often require either heating or cooling of the reaction mixture in order to effect completion of the reaction and form the required products.
A number of different methods for heating and/or cooling flow reactions have emerged which aim to impart a heat transfer effect on a reaction tube in 1809.spec
ID
which the reagents are flowing. One prior art method of effecting a temperature change in the reaction mixture is by submersion of the reaction tubing in an oil bath which is then heated as the reaction requires. However, there are many disadvantages in using this method as the oil bath will take a considerable amount of time to reach the required temperature. Furthermore, once at the required temperature it is difficult to maintain the exact temperature during the reaction. Submerging the reaction tube in an oil bath may also be extremely messy and poses a safety risk to the user when inserting and removing the reaction tubing from the oil bath.
A more recent method of heating a flow reaction system has emerged which provides an improved system for heating the reaction tubing than the oil bath. The FRXTM tube reactor by Syrris Limited comprises a polytetrafluoroethylene (PTFE) tube configured to receive a reaction mixture which is held within a support unit. The support unit is then fixed over a regular hotplate stirrer which effects a change in temperature of the reaction mixture contained within the PTFE tube by transfer of heat from the hotplate to the support device and hence to the PTFE tube contained therein. A disadvantage of this type of tube reactor is that there is slow heat transfer from the hotplate to the PTFE tube due to the mass of the support unit situated therebetween.
Furthermore, such a reactor may take a considerate amount of time to cool down and so may delay continuation of the reaction.
It is beneficial for the user to be able to change the reaction tubing within a tube reactor in order to suit the particular conditions of the reaction. The FRXTM tube reactor offers two types of PTFE reaction tubing, one having an internal volume of 4ml and the second having an internal volume of 16m1. Therefore, the user is limited to the type of reactions they can carry out as the material and volume of the tubes cannot be selected for optimum reaction conditions.
Furthermore, the reaction tube is permanently fixed in the support means and so it is not possible for the user to change the reaction tube themselves as and when they need to.
1809.spec A further disadvantage of the FRXTM tube reactor is that expansion and contraction of the hotplate and metallic portion of the support device during heating and cooling may lead to stress and damage of the reaction tube as these components apply pressure to the tube.
Furthermore, it is only possible to carry out one flow reaction on the hotplate at a time which may be disadvantageous if the user wishes to obtain comparative results for the same reaction as the user will have to perform sequential reactions on the same hotplate or set up a number of hotplates each with one tube reactor mounted thereon.
Therefore, what is required is a specific unit designed for the purpose of temperature stability and control of a flow reaction which negates the above described disadvantages.
Summary of the Invention
An object of the present invention is to provide an improved heat transfer device which facilitates interchangeability of the reaction tubing upon a heating element which is required as a consequence of the different types of reagents used and the necessary reaction conditions. The invention seeks to provide such a device whilst maintaining excellent thermal contact between the reaction tubing and the heating element. Furthermore, the invention seeks to provide a flexible heating element that will accommodate a wide range of reaction tubing and hence allow interchangeability of the thermal transfer path thereon.
The invention achieves the object for an improved heat-transfer device of the above type by providing a heat-transfer device comprising an element to effect a change in temperature of at least one tubular reaction vessel, said device further comprising: 1 809.spec at least one support means detachably disposed about a surface of said heat-transfer element, said at least one support means being configured to suDport said at least one tubular reaction vessel; wherein said support means is adapted to detachably maintain said tubular reaction vessel in optimised thermal contact with said support means; and at least one of said support means and said element substantially surrounds at least a portion of the other.
In the field of flow chemistry, the chemist needs to be able to change the reaction tubing for different materials, diameters and lengths so that the reaction tubes can be used with a wide array of chemicals at very low and at elevated temperatures, different resonance times and pressures. Therefore, interchangeability of the reaction tubing on the heating element of a device of the present invention enables the chemist to change the reaction tubing to optimise reaction conditions without the need to disrupt the electrical circuits or any heat * transfer fluids that may be attached to the heating element. Furthermore, the interchangeability of the reaction tubing upon a support means allows the user to wind on a desired reaction tubing of different lengths and materials depending upon the reaction conditions.
The heat transfer device of the present invention has many advantages over the prior art methods. A major advantage is that a reduced mass of the heating element and the support means enables rapid heat transfer there between ensuring better quality of products resulting from the flow reaction.
Preferably the support means is substantially comprised of a material having a coefficient of expansion which is equal to or lower than the coefficient of expansion of said at least one tubular reaction vessel.
1809.spec In a preferred embodiment the support means comprises at least one groove disposed at a surface thereof said at least one groove being helical. The tubular reaction vessel may then be disposed within the helical groove of the support means. The support means may further comprises at least one clamping means configured to secure the tubular reaction vessel upon the support means.
The clamping mechanism of the support means is provided to hold the reaction tubing in close contact with the support means and therefore effect excellent heat transfer there between.
The support means may be detachably disposed on an external surface of the heat-transfer element such that the support means substantially surrounds at least a portion of the external surface of the element. Preferably the element and the support means are substantially cylindrical, the diameter of the support means being greater than the diameter of the element.
The arrangement of a cylindrical heating element with a substantially cylindrical support means placed thereover and reaction tubing disposed between a helical groove in the surface of the support means enable excellent thermal contact and hence effective heat transfer from the heating element to the reaction tubing. Therefore the reaction mixture is effectively heated.
In order to to effect a change in the diameter of the element, the element may comprise an adjustment means in the form of an adjustable expansion slot, a channel and an adjustment mechanism; wherein said adjustable expansion slot and said channel are disposed equidistant to one another about said element; and said adjustment mechanism is configured to effect a change in the width of said adjustable expansion slot.
1809.spec Preferably the adjustment mechanism is in the form of a nut and bolt arrangement or a cam arrangement.
The incorporation of an adjustment means, comprising an adjustable expansion slot, a channel and an adjustment mechanism on the heating element allows the support means with reaction tubing attached thereon to be easily placed on and off the heating element whilst enabling good thermal transfer from the heating element to the support means. This adjustment means also allows materials of different coefficients of expansion to be used for the support means without causing stress to the heating element due to expansion of the support means due to heat. The adjustment means imparts flexibility on the heating element which may be further enhanced by the positioning of a resilient member within the adjustment mechanism. Furthermore, when the element is made a material with a high coefficient of expansion than the support means, expansion of the element upon heating is restricted by the support means. Therefore, the resilient member compensates for the expansion of the element and so prevents damage to the support means whilst maintaining optimised thermal contact there between.
Preferably the element is configured to receive an electrical current to effect a change in the temperature of the element, the at least one support means and the at least one tubular reaction vessel. This electrical current may effect conventional resistance heating of the device or alternatively the electrical current may used in combination with Peltier technology to effect heating and/or cooling of the reaction mixture contained within the tubular reaction vessel.
The tubular reaction vessel may be made from a material selected from the following group: * metal * metal alloy 1 809.spec * glass * silica * quartz * polymers * ceramics * composites The material, internal diameter and working volume of the tubular reaction vessel may be selected in order to provide optimum reaction conditions for the reaction mixture contained therein.
Preferably the element comprises a fluid passageway, said passageway having a fluid inlet and a fluid outlet. The fluid passageway may be formed by a fluid conduit connected to the element or the element may comprises at least one hollow region wherein the fluid passageway is formed within the element at the hollow region. In the latter case the fluid passageway may be a network of passageways.
In a preferred embodiment of the present invention a cooling fluid is capable of flowing through the fluid passageway to provide a cooling effect to the element, the at least one support means and the at least one tubular reaction vessel. In this embodiment the cooling fluid may be a liquid such as water or a gas such as compressed air, nitrogen or argon.
Alternatively, a heat-transfer fluid may be capable of flowing through the passageway to provide a heating and/or cooling effect to the element, the at least one support means and the at least one tubular reaction vessel.
In a further alternative embodiment of the present invention the central hollow region of the cylindrical heating element may allow positioning of a further 1809 spec heating and/or cooling element therein. This would enable heating and/or cooling the reaction mixture to extreme temperatures as the flow reaction dictates.
It is preferred that the heat-transfer device further comprises a cover portion configured to be placed over and substantially surround the element, the at least one support means and the at least one tubular reaction vessel. The positioning of a cover unit over the heat transfer device during the reaction prevents heat loss to the local environment as the reaction progresses by effectively insulating the heat transfer device. Furthermore, the provision of a cover portion of the heat- transfer device enables uniform homogeneous distribution of heat during the reaction, therefore enabling the reaction to proceed to successful completion whilst in the reaction tubing.
The element may further comprises a plurality of locating feet and a fixing means configured to allow the device to be fixed to a support structure.
The element of the heat-transfer device of the present invention may be configured to support one or a plurality of support means. This is because the interchangeability of the reaction tubing upon the heating element allows more than one arrangement of the reaction tubing and support means to be mounted on the heating element at one time. This enables the user to place several reaction tubing potentially of different materials and volumes to be used on the heating element at one time.
The heat-transfer device of the present invention is preferably configured for use in flow chemistry, however the inventors can foresee further uses for this apparatus in biological applications such as biological screening.
It is a further object of the present invention is to provide an improved heat transfer device which prevents the reaction tubing from experiencing stress which ultimately results in damage of the reaction tubing due to the expansion and contraction of the heating element and the means supporting the tubular reaction 1809.spec vessel during heating. The invention also seeks to overcome the prior art problem of poor heat transfer whilst maintaining the integrity of the flow path of the reaction.
The invention achieves this further object by providing a heat-transfer device comprising: at least one tubular reaction vessel; and at least one support means for supporting said at least one tubular reaction vessel; wherein said support means is substantially comprised of a material having a coefficient of expansion which is equal to or lower than the coefficient of expansion of said at least one tubular reaction vessel.
The use of specialist support means formed from materials having a co-efficient of expansion that is equal to or less than the material of the reaction tubing prevents damage or rupturing of the reaction tubing during heating as the support means will have the same resistance to expansion as a reaction tubing.
According to a third aspect of the present invention there is provided a kit of parts for a heat-transfer device comprising an element to effect a change in temperature of at least one tubular reaction vessel, said kit of parts comprising: at least one support means detachably disposed about a surface of said heat-transfer element, said at least one support means being configured to support said at least one tubular reaction vessel; wherein said support means is adapted to detachably maintain said tubular reaction vessel in optimised thermal contact with said support means; and 1809.spec at least one of said support means and said element substantially surrounds at least a portion of the other.
Brief Description of the Drawings
For a better understanding of the invention and to show how the same may be carried into effect, there will now be described by way of example only, specific embodiments, methods and processes according to the present invention with reference to the accompanying drawings in which: Figure 1 shows a perspective view of a heat-transfer device in accordance with one embodiment of the present invention; Figure 2 is a cut-away view of a portion the element of the heat-transfer device of figurel; Figure 3 is a partially exploded view of the heat-transfer device of figure 1; Figure 4 is a top perspective view of the element of the heat-transfer device offigurel; Figure 5 is a perspective view of the heat-transfer device of figure 1 wherein the heat-transfer device showing the cover portion of the device; and Figure 6 is a cross-sectional perspective view of the heat-transfer device of figure 5.
Detailed Description
There will now be described by way of example a specific mode contemplated by the inventors. In the following description numerous specific details are set forth in order to provide a thorough understanding. It will be apparent however, to one skilled in the art, that the present invention may be I 809.spec practiced without limitation to these specific details. In other instances, well known methods and structures have not been described in detail so as not to
S unnecessarily obscure the description.
Referring to figure 1, a heat-transfer device 101 according to one embodiment of the present invention comprises an element 103, a support means 105 and reaction tubing 107.
Element 103 has an adjustment means in the form of a slot 109, a nut and bolt arrangement 111 and a keyhole-shaped channel 113. Element 103 further comprises four locating feet 115 (three of which are shown) and a fluid exchange comprising a box portion 117, a fluid inlet pipe 119 and a fluid outlet pipe (not shown).
Each support means 105 comprises two clamping means 121 configured to secure the reaction tubing 107 about the support means 105.
Element 103 is cylindrical having an open central portion and is made from aluminum. Slot 109 and keyhole-shaped channel 113 of the adjustment means are spaced equidistant from one another about the uppermost surface 129 of element 103 and extend in axial direction from the uppermost surface 129 of the element 103 to the lowermost surface thereof. Slot 109 extends in a radial direction from the outer surface 131 to the inner surface of the element 103, whereas the keyhole-shaped channel 113 extends substantially through the radial width of element 103 but is not open at the inner surface thereof.
The edges of element 103 which define the slot 109, are attached to two guide members 123 and 124 at the lowermost surface of element 103. These guide members 123 and 124 comprise a ledge portion having corresponding apertures through which the nut and bolt arrangement 111 is located. The nut and bolt arrangement 111 comprises an alien screw and four hexagonal nuts.
1809.spec Locating feet 115 extend radially and axially outwards from the lowermost surface of the element 103. Each locating feet 115 has an aperture 125 extending axially there-through which is configured to receive a fixing means to secure the heat-transfer device 101 to a support structure. Locating feet 115 are disposed equidistant from one another about the lowermost surface of element 103 to ensure stability of the heat-transfer device 101 when positioned on a support structure (not shown).
Locating feet 115 further comprise electrical wires (not shown) extending io there-through to provide the element 103 with an electrical current from an electrical supply in order to heat and/or cool the heat-transfer device 101. If heating of the heat-transfer device 101 is required then normal resistance heating by an electrical current is be employed. However, if it is necessary to heat and/or cool the heat transfer device 101, Peltier technology can be employed to achieve this effect by use an electrical current.
Locating feet 115 are made from an insulating plastics material, for example, polytetrafluoroethylene (PTFE) or a polyketone such as PEEK. In this way, heating of the heat transfer device 101 will not lead to heating of the support structure to which the heat transfer device 101 is attached via the locating feet which would create a safety hazard to the user and also could lead to heat loss of the heat transfer device 101 thereby reducing its effectiveness.
With reference to figures 1 and 2 herein, the box portion 117 of fluid exchange is rectangular in shape and fixed to the lowermost surface of element 103. A fluid inlet pipe 119 and a fluid outlet pipe (not shown) are provided which enter the box portion 117 at opposite sides thereof and are in fluid communication with a cooling channel 201 which extends through the box portion 117 of the fluid exchange and into a hollow interior region 203 of element 103 in an axial direction. A seal plate 113 is disposed on the uppermost surface 129 of the element 103 overlying cooling channel 201 in order to prevent leakage of a cooling fluid therefrom.
1809.spec In an alternative embodiment of the present invention; fluid inlet pipe 119 and fluid outlet pipe (not shown) are provided in fluid communication with box portion 117 and hollow interior region 203 of the element 103 so as to allow flow of a heat transfer fluid into and from hollow interior region 203 of the element 103. The heat transfer fluid may be heated or cooled by an electrical current * applied to element 103 or it may pass through a heat exchanger (not shown) prior to entering the fluid inlet pipe 119 to effect a change in temperature.
In this embodiment of the present invention, three support means 105 are cylindrical in shape and are located about the outer surface 131 of element 105 extending along a portion of its axial length. Support means 105 has a greater diameter than the diameter of the element 103 such that support means 105 can be placed on and removed from element 103 with ease.
Support means 105 comprises a helical groove (not shown) through which reaction tubing 107 is wound in order to maintain excellent thermal contact between support means 105 and reaction tubing 107 thereby effecting successful heat-transfer therebetween.
Clamping means 121 are located at both edges of support means 105, one at the uppermost edge (as illustrated) and the second at the lowermost edge (not shown) of support means 105. Clamping means 121 serve to secure both ends of reaction tubing 107 in place on the support means 105 such that once they are wound in place, they cannot unwind or become loose, thereby disrupting thermal contact and hence heat-transfer between support means 105 and reaction tubing 107.
In this embodiment of the present invention, three sets of reaction tubing 107 are provided upon each support means 105. Reaction tubing 107 has an internal diameter of 1 mm and a working volume of 25ml. It is advantageous to 1809.spec use reaction tubing having an internal diameter of 1 mm as this allows excellent heat transfer to the reaction mixture and superior mixing of the reagents.
A first end 127 of the reaction tubing 107 is connected to pumps located on the support structure (not shown) which pumps the reagents into reaction tubing 107 via a 1-piece (not shown) which allows the reagents to be mixed prior to entering reaction tubing 107. The second end of the reaction tubing 107 (not shown) allows the product of the flow reaction to drain out of the reaction tubing 107 and into a collection means (not shown) such as a test tube, conical flask or beaker.
Depending upon the reaction taking place in the reaction tubing 107, the first end 127 of the reaction tubing 107 may be fed with reagents which have undergone a first reaction in a column type reactor located on the support is structure (not shown) in order to provide a continuous, multi-stage flow reaction.
Alternatively, the second end of the reaction tubing 107 may be linked to a column type reactor located on the support structure such that the product formed by flow reaction through the heat-transfer device of the present invention may then undergo further reaction in a column type reactor.
The material of the support means 105 depends upon the material of the reaction tubing 107 which is selected to provide optimum reaction conditions for the reaction mixture contained therein. For example, if reaction tubing 107 is formed from polytetrafluoroethylene (PTFE), which provides good chemical resistance, or stainless steel, which allows the reaction mixture to be heated to a high temperature and high pressure, support means 105 may also be formed from stainless steel.
Alternatively, if reaction tubing 107 is formed from a glass material such as silica, which provides excellent chemical resistance and allows the reaction * mixture to undergo high pressures, then support means 105 may be formed from * titanium which has a low co-efficient of expansion. Therefore, upon heating 1809.spec and/or cooling of the heat-transfer device 101, support means 105 does not undergo a greater level of expansion for contraction than reaction tubing 107 and so will not put reaction tubing 107 under stress which may lead to breakage.
In use, heat-transfer device 101 is fixed to a support structure via the apertures 125 in locating feet 115 of element 103. Initially, slot 109 of the adjustment means is in a closed arrangement such that the corresponding edges of element 103 are adjacent to one another.
Support means 105 may be pre-wound with reaction tubing 107, the ends of the reaction tubing 107 being clamped by the clamping means 121 of support means 105. Alternatively, the user may wind on their own reaction tubing 107 clamping the first end thereof to support means 105 via clamping means 121, using the helical groove (not shown) on the surface of the support means 105 to ensure excellent contact between reaction tubing 107 and support means 105 and clamping the second end of reaction tubing 107 to support means 105 via clamping means 121.
The support means 105 and reaction tubing 107 arrangement is then placed over the uppermost surface 129 of element 103 and slid downwards in an axial direction until it meets the lowermost surface of element 103. In this embodiment, two further support means 105 and reaction tubing 107 arrangements are disposed about the outer surface of the element 103 by the same operation.
Initially, the support means 105 and reaction tubing 107 arrangements are loosely disposed on element 103 and so are capable of circumferential and axial movement thereabout. However, in order to effect excellent thermal contact and therefore highly effective heat-transfer from the element 103 to the support means 105 and hence to the reaction tubing 107, the support means 105 and reaction tubing 107 arrangement is clamped securely on element 103. Clamping is effected by the adjustment means of element 103. The user of heat-transfer 1809.spec device 101 inserts an allen key into the head of the alien screw of the nut and bolt arrangement 111 and turns the alien screw in an anti-clockwise direction. The * anti-clockwise motion of nut and bolt arrangement 111 effects opening of slot 109 such that element 103 is brought into direct contact with support means 105. As the corresponding edges of slot 109 move apart, the outermost edges of the keyhole-shaped channel 113 moves closer together until they eventually meet.
The function of the keyhole-shaped channel 113 of the adjustment means is that it acts as a hinge allowing flexibility of element 103 and so preventing the * movement of slot 109 from resulting in damage to element 103.
Once the support means 105 and reaction tubing 107 arrangements are clamped in place on the element 103, an electrical current is supplied to element 103 from an electrical supply located on the support structure (not shown), via the electrical wires disposed in the locating fe et 115 to effect heating of the device 101.
When the reaction mixture contained within the reaction tubing 107 has reached completion and the reaction tubing 107 is empty, the user switches on the supply of cooling fluid such as water, compressed air, nitrogen or argon which enters the fluid inlet pipe 119 and circulates through the cooling channel 201 disposed within the hollow interior region 203 of element 103 and is removed via the fluid outlet pipe (not shown). In this way, the element 103 and the support means 105 and reaction tubing 107 arrangement may be rapidly cooled to an * ambient temperature such that the user can quickly re-use the device 101 or * 25 change the support means 105 and reaction tubing 107 arrangement for a different support means and reaction tubing arrangement suitable for a different set of reaction conditions.
As the support means 105 and reaction tubing 107 arrangements are detachably positioned about the element 103 which is independently coupled, in fluid communication with a fluid supply and electrical circuitry, the support means and reaction tubing 107 arrangements may be readily interchanged with 1 809.spec different size and material support means 105 and reaction tubing 107 without the user being required to de-couple or break the fluid supply or electrical circuit.
For example, to proceed with a subsequent reaction involving the use of a greater reaction flow time and/or different materials due to the required reaction conditions, a user simply releases support means 105 by use of the adjustment means of the element 103 which allows them to remove the support means 105 from the element 103 and insert a different support means and reaction tubing arrangement thereon. The support means and reaction tubing arrangement is then held in excellent thermal contact with the element by adjustment of the nut and bolt arrangement.
Referring to figure 3 one of the support means 105 has been removed from the element 103 of heat-transfer device 101. Furthermore, reaction tubing 107 has been removed from the support means 105 to reveal a helical groove 301 disposed on the outer surface of support means 105. Helical groove 301 is configured for positioning of the reaction tubing 107 there between as it is wound onto support means 105 and maintains excellent thermal contact between support means 105 and reaction tubing 107, enabling effective heat transfer.
Support means 105 further comprises a first and second clamping means 121 and 303 which are located on the uppermost and lowermost surface of the support means 105 respectively.
Reaction tubing 107 is wound in a coil shape having a first end 127 on the upper region of the coil and a second end 305 on the lower region of the coil of * the reaction tubing 107.
When the reaction tubing 107 is wound around the support means 105, the first end 127 of reaction tubing 107 is brought into communication with the first clamping means 121 located at the uppermost surface of support means 105 and the second end 305 is brought into communication with the second clamping means 3Ô3 of support means 105 and clamped therein. In this way, reaction 1809.spec tubing 107 is secured within the helical groove 301 located on the outer surface of support means 105 and so cannot un-wind or become loose during use.
With reference to figure 4 herein there is shown a top perspective view of the element 103 of the heat-transfer device 101 of the present invention.
Element 103 comprises an adjustment means having a slot 109, a nut and bolt arrangement 111 and a keyhole-shaped channel 113. Element 103 further comprises four locating feet 115, a temperature sensor (not shown) and a fluid exchanger having a box portion 117, a fluid inlet pipe 119 and a fluid outlet pipe 401.
Slot 109 extends through the outer surface 131 of element 103 in an axial and radial direction. The width of slot 109 is controlled by an arrangement of two guide members 123 and 124 and the nut and bolt arrangement 111. Guide members 123 and 124 are attached to the lowermost surface of element 103, disposed one at either side of slot 109. Guide members 123 and 124 have a ledge portion 403 and 405 which extends in a radial direction from the guide members 123 and 124. Ledge portion 403 and 405 each have a corresponding aperture through which the nut and bolt arrangement 111 is located.
Nut and bolt arrangement 111 comprises an allen screw 407 and two pairs of hexagonal nuts 409 and 411. Both pairs of hexagonal nuts 409 and 411 are located about the left hand ledge portion 403 of guide members 124 such that the first pair of hexagonal nuts 409 are fitted against the left hand side of the ledge portion 403 and the second pair of hexagonal nuts 411 are located adjacent to the right hand side of the ledge portion 403. Allen screw 407 comprises a threaded section which extends through the apertures of ledge portions 403 and 405 and through the central portion of each pair of hexagonal nuts 409 and 411. Allen screw 407 further comprises a head portion having a cut out section at the end thereof, configured to receive an alien key in order to effect rotation of the allen screw 407. The head portion of the allen screw 407 has a 1809.spec larger diameter than the thread portion so as to prevent the head portion from entering the aperture of the ledge portion 405.
When the support means (not shown) supporting the reaction tubing (not shown) is placed over element 103, the alien screw 407 is turned in an anti-clockwise direction using an alien key to effect opening of slot 109 to secure the support means in direct thermal contact with the element 103. After use, in order to release the support means the allen screw 421 is turned in a clockwise direction thereby effecting closure of the slot 403.
Keyhole-shaped channel 113 extends axially along the length of element 103 and into element 103 in a radial direction. Keyhole-shaped channel 113 is open at the outer surface 131 of element 103 but does not extend throughout the width of element 103 thereby leaving a thin portion of the element 103 material.
is Keyhole-shaped channel 113 imparts a degree of flexibility on the element 103 during opening and closing of slot 109. For example when slot 109 is opened to secure a support means on the element 103, the outermost edges of keyhole-shaped channel 113 are brought into contact with one another. The advantage of this flexibility is that element 103 will not experience stress within the region of element 103 radially opposite to slot 109.
Element 103 of the heat-transfer device of the present invention comprises four locating feet 115 extending from the lowermost surface of element 103, spaced equidistant about the circumference of the lowermost surface of element 103. Locating feet 115 are provided with apertures 125 which allow element 103 to be fixed to a support structure by means of a screw or any similar fixing means. Locating feet 115 may further comprise electrical wires which supply an electrical current to the element 103. Locating feet 115 are formed from an insulating material such as PTFE or PEEK to prevent the transfer of heat from the heat-transfer device of the present invention to the support structure.
1 809.spec Element 103 further comprises a temperature sensor (not shown) which is positioned within a further hollow interior region of element 103. The temperature sensor feeds back to a remotely positioned control system, for example within the support structure upon which the heat transfer device 101 is mounted, to ensure that the temperature of the element 103 is maintained at the optimum temperature for the reaction mixture. Alternatively, the temperature sensor may be mounted directly upon the surface of the reaction tubing 107 such that it contacts this surface and hence regulates the temperature of the reaction tubing 107.
With reference to figure 5 and figure 6 herein there is shown a heat transfer device 101 according to an embodiment of the present invention wherein the heat-transfer device 101, illustrated in figure 1, further comprises a cover 503.
is Cover 503 comprises an outer body portion 505 and a handle portion 507.
Outer body portion 505 of cover 503 is of a cylindrical shape and is closed at its uppermost surface 511. Handle portion 507 extends from uppermost surface 511 and is secured to outer body portion 505 by a screw means 509 at either end of the handle portion 507. An aperture 512 is also provided at the uppermost surface 511 of the outer body portion 505 which allows tubing, connecting the reaction tubing 107 to remotely positioned pumps, to pass there between.
Outer body portion 505 of the cover 503 further comprises an open section 513 in the lower portion of outer body portion 505 which corresponds to the fluid inlet pipe 119 of the heat-transfer device 101 thereby allowing the pipe 119 to pass through the cover 503 in order for it to be connected to a fluid source. Outer body portion 505 comprises a further open section corresponding to the fluid outlet pipe (not shown) to allow drainage of the fluid from the element 103 of the heat-transfer device 101.
Cover 503 further comprises a cylindrically-shaped inner body portion 601 which is closed at the uppermost surface 602 thereof having a smaller diameter 1809 spec and length than the outer body portion 505. Inner body portion 601 is located between the outer body portion 505 and the element 103, support means 105 and reaction tubing 107 arrangement. An insulating material is sandwiched between the outer body portion 505 and the inner body portion 601 of the cover 503 so as to prevent loss of heat from the heat-transfer device 101 during use.
The inner and outer body portion, 601 and 505 of the cover 503 are formed of a metal material such as aluminum. Handle portion 507 is formed of an insulating plastics material such as PTFE or PEEK.
Handle portion 507 comprises two screws 509 at either end thereof which are passed through a corresponding aperture in the outer body portion 505 and a corresponding aperture in the inner body portion 601 A bolt 603 is screwed onto the innermost end of the screw 509 to secure both the handle portion 507 and the inner body portion 601 in place relative to the outer body portion 505. A -. spacer element 605 is placed between the inner and outer body portion 601 and 505 and screw 509 is threaded through the centre of the spacer element 605 to enable uniform separation of the inner and outer body portion 601 and 505.
Spacer element 605 is also formed of an insulating plastics material such as PTFE or PEEK.
The uppermost surface 602 of the inner body portion 601 comprises an aperture 607 positioned so as to be in communication with the aperture 512 of the uppermost surface 511 of the outer body portion 505, to allow positioning of tubing supplying the reaction mixture to reaction tubing 107 there between.
Alternatively, cover 503 may comprise a single body portion which is coated on its internal surface by an insulating material.
1809.spec Cover 503 is placed over the heat transfer device 101 whilst the reaction is in progress to insulate the device 101 thereby preventing heat loss which results in incomplete reaction within the reaction tubing 107. Such a cover 503 as illustrated in figure 5, also allows uniform homogeneous distribution of heat over the reaction tubing 107, therefore enabling complete and successful reactions within the reaction tubing 107.
The embodiments illustrated in figures 1 to 6 show the use of three support means and therefore three reaction tubings. However, the interchangeability of the support means and reaction tubing allows one or a plurality of reaction tubings to be supported thereon and so provides simultaneous heating and/or cooling to a plurality of reaction vessels.
1 809.spec
Claims (33)
- Claims: 1. A heat-transfer device comprising an element to effect a change in temperature of at least one tubular reaction vessel, said device further comprising: at least one support means detachably disposed about a surface of said heat-transfer element, said at least one support means being configured to support said at least one tubular reaction vessel; wherein said support means is adapted to detachably maintain said i''. tubular reaction vessel in optimised thermal contact with said support means; and is at least one of said support means and said element substantially * * surrounds at least a portion of the other.
- 2. A heat-transfer device according to claim 1 wherein said support means is substantially comprised of a material having a coefficient of expansion which is equal to or lower than the coefficient of expansion of said at least one tubular reaction vessel.
- 3. A heat-transfer device according to any one of claims 1 and 2 -, * wherein said support means comprises at least one groove disposed at a surface thereof.
- 4. A heat-transfer device according to claim 3 wherein said at least one groove is helical.
- 5. A heat-transfer device according to any one of claims 3 and 4 wherein * said tubular reaction vessel is disposed within said at least one groove of said support means.1 809.spec
- 6. A heat-transfer device according to any preceding claim wherein said support means further comprises at least one clamping means configured to secure said tubular reaction vessel upon said support means.
- 7. A heat-transfer device according to any preceding claim wherein said support means is detachably disposed on an external surface of said element such that said support means substantially surrounds at least a portion of said external surface of said element.
- 8. A heat-transfer device according to any preceding claim wherein said element is substantially cylindrical.
- 9. A heat-transfer device according to any preceding claim wherein said support means is substantially cylindrical.
- 10. A heat-transfer device according to claim 9 wherein the diameter of said support means is greater than the diameter of said element.
- 11. A heat-transfer device according to any preceding claim wherein said element comprises an adjustment means configured to effect a change in the diameter of said element.
- 12. A heat-transfer device according to claim 11 wherein said adjustment means is in the form of an adjustable expansion slot, a channel and an adjustment mechanism: wherein said adjustable expansion slot and said channel are disposed equidistant to one another about said element; and said adjustment mechanism is configured to effect a change in the width of said adjustable expansion slot.1809.spec
- 13. A heat-transfer device according to any one of claims 11 and 12 wherein said adjustment means further comprises a resilient member configured to impart flexibility to said element upon heating and/or cooling.
- 14. A heat-transfer device according to any preceding claim wherein said element is configured to receive an electrical current to effect a change in the temperature of said element, said at least one support means and said at least one tubular reaction vessel.
- 15. A heat-transfer device according to any preceding claim wherein said tubular reaction vessel is made from a material selected from the following group: * metal * metal alloy * glass * silica * quartz * polymers * ceramics * composites
- 16. A heat-transfer device according to any preceding claim wherein said element comprises a fluid passageway, said passageway having a fluid inlet and a fluid outlet.
- 17. A heat-transfer device according to claim 16 wherein said fluid passageway is formed by a fluid conduit connected to said element.
- 18. A heat-transfer device according to claim 16 wherein said element comprises at least one hollow region wherein said fluid passageway is formed within said element at said hollow region.1 809.spec
- 19. A heat-transfer device according to claim 18 wherein said fluid passageway is a network of passageways.
- 20. A heat-transfer device according to any one of claims 16 to 19 wherein a cooling fluid is capable of flowing through said fluid passageway to provide a cooling effect to said element, said at least one support means and said at least one tubular reaction vessel.
- 21. A heat-transfer device according to any one of claims 16 to 19 wherein a heat-transfer fluid is capable of flowing through said passageway to provide a heating and/or cooling effect to said element, said at least one support means and said at least one tubular reaction vessel.
- 22. A heat-transfer device according to any preceding claim wherein said device further comprises a cover portion configured to be placed over and substantially surround said element, said at least one support means and said at least one tubular reaction vessel.*
- 23. A heat-transfer device according to any preceding claim wherein said * element further comprises a plurality of locating feet.
- 24. A heat-transfer device according to any preceding claim wherein said element further comprises a fixing means configured to allow said device to be fixed to a support structure.
- 25. A heat-transfer device according to any preceding claim wherein said element is configured to support a plurality of support means.
- 26. A heat-transfer device according to any preceding claim wherein said device is configured for use in flow chemistry.1809.spec
- 27. A heat-transfer device comprising: at least one tubular reaction vessel; and at east one support means for supporting said at least one tubular reaction vessel; wherein said support means is substantially comprised of a material having a coefficient of expansion which is equal to or lower than the coefficient of expansion of said at least one tubular reaction vessel.
- 28. A heat-transfer device according to claim 27 wherein said device further comprises an element configured to effect a change in temperature of said at least one tubular reaction vessel; said at least one support means being detachably disposed about a surface of said element.
- 29. A heat-transfer device according to any one of claims 27 and 28 wherein said support means is adapted to detachably maintain said tubular reaction vessel in optimised thermal contact with said support means.
- 30. A kit of parts for a heat-transfer device comprising an element to effect a change in temperature of at least one tubular reaction vessel, said kit of parts comprising: at least one support means detachably disposed about a surface of said heat-transfer element, said at least one support means being configured to support said at least one tubular reaction vessel; 1809.spec * -28-wherein said support means is adapted to detachably maintain said tubular reaction vessel in optimised thermal contact with said supporting means; and s at least one of said support means and said element substantially surrounds at least a portion of the other.
- 31. The kit of parts as claimed in claim 30 further comprising a cover portion configured to be placed over and substantially surround said element, said at least one support means and said at least one tubular reaction vessel.
- 32. The kit of parts as claimed in claims 30 and 31 wherein said support means is substantially comprised of a material having a coefficient of expansion which is equal to or lower than the coefficient of expansion of said at least one tubular reaction vessel.
- 33. The kits of parts as claimed in claims 30 to 32 wherein said element is configured to support a plurality of support means.1 809.spec
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB0716113A GB2451900A (en) | 2007-08-17 | 2007-08-17 | Flow apparatus |
GB0815063A GB2454294B (en) | 2007-08-17 | 2008-08-18 | Improvements to flow apparatus |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB0716113A GB2451900A (en) | 2007-08-17 | 2007-08-17 | Flow apparatus |
Publications (2)
Publication Number | Publication Date |
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GB0716113D0 GB0716113D0 (en) | 2007-09-26 |
GB2451900A true GB2451900A (en) | 2009-02-18 |
Family
ID=38566592
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB0716113A Withdrawn GB2451900A (en) | 2007-08-17 | 2007-08-17 | Flow apparatus |
GB0815063A Active GB2454294B (en) | 2007-08-17 | 2008-08-18 | Improvements to flow apparatus |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB0815063A Active GB2454294B (en) | 2007-08-17 | 2008-08-18 | Improvements to flow apparatus |
Country Status (1)
Country | Link |
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GB (2) | GB2451900A (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4256697A (en) * | 1978-12-21 | 1981-03-17 | Fred Baldwin | Blood incubator device |
GB2238005A (en) * | 1989-08-05 | 1991-05-22 | Scras | Apparatus for repeated automatic execution of a thermal cycle for treatment of samples |
WO1998016313A1 (en) * | 1996-10-12 | 1998-04-23 | Central Research Laboratories Limited | Heating apparatus |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6410801B1 (en) * | 1999-11-18 | 2002-06-25 | Basf Corporation | Continuous process for the production of polyether polyols |
JPWO2006051663A1 (en) * | 2004-11-09 | 2008-05-29 | 住友ベークライト株式会社 | Decomposition reaction apparatus, recycled resin composition raw material manufacturing system, recycled resin composition raw material manufacturing method, recycled resin composition raw material, and molded article |
GB0617877D0 (en) * | 2006-09-12 | 2006-12-13 | Vapourtec Ltd | Chamber Heater Module |
-
2007
- 2007-08-17 GB GB0716113A patent/GB2451900A/en not_active Withdrawn
-
2008
- 2008-08-18 GB GB0815063A patent/GB2454294B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4256697A (en) * | 1978-12-21 | 1981-03-17 | Fred Baldwin | Blood incubator device |
GB2238005A (en) * | 1989-08-05 | 1991-05-22 | Scras | Apparatus for repeated automatic execution of a thermal cycle for treatment of samples |
WO1998016313A1 (en) * | 1996-10-12 | 1998-04-23 | Central Research Laboratories Limited | Heating apparatus |
Non-Patent Citations (1)
Title |
---|
Syrris, "FRX modules - tube reactor" [online] * |
Also Published As
Publication number | Publication date |
---|---|
GB2454294A (en) | 2009-05-06 |
GB2454294B (en) | 2011-04-20 |
GB0815063D0 (en) | 2008-09-24 |
GB0716113D0 (en) | 2007-09-26 |
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