The present invention relates to a reactor device for reaction fluid.
Traditionally, large scale chemical reactions are carried out as batch processes, typically using stirred tank reactors as shown in
An alternative to a batch reaction process is to use a flow reactor. An example flow reactor is shown in
Typically the reactant streams are brought up (or down) to the reaction temperature before they are fed into the reactor. The static mixer provides rapid mixing which ensures that the reactant concentration is consistent in the reactor, resulting in a higher quality reaction product. For a flow reactor the area of heat transfer is typically large relative to the reactor volume which results in significantly improved temperature control for exothermic and endothermic reactions.
Examples of other existing flow reactors are described with reference to
Other prior art includes U.S. Pat. No. 3,976,129 which shows a heat exchanger defining a tank through which extends a spiral shaped tube; and FIG. 1 from EP 1,965,900 which shows a crystallisation apparatus having a temperature controlled tube.
According to a first aspect of the present invention, there is provided a reactor device for reaction fluid comprising:
In this way, excess heat/cold in the reaction vessel can be transmitted to the manifold via the end cap, such to bring the temperature of the reaction fluid inside the manifold towards the temperature of the reaction fluid inside the reaction vessel.
To further improve the thermal coupling between the control fluid and the manifold, the end cap may have a thermal conductivity of greater than 10 watts per square meter kelvin, preferably 25 watts per square meter kelvin, more preferably 50 watts per square meter kelvin, or even more preferably 100 watts per square meter kelvin.
Preferably the end cap, or a portion of the end cap, is detachable. In this way, the inside of the reaction vessel can be easily accessed, allowing easier maintenance of the reaction vessel.
To make the manifold easier to handle and maintain, preferably the manifold is a block.
To prevent damage to the manifold when it is in use, and to improve the thermal coupling between the manifold and the end cap, preferably the manifold sits on the end cap. In this case, the manifold may sit within a cavity located in the top cap.
Although control fluid inside the reaction vessel may be periodically refilled by detaching the end cap from the rest of the reaction vessel, preferably the reaction vessel comprises an entry port and an exit port for changing the control fluid inside the reaction vessel.
The at least one inlet of each channel may comprise a first inlet for receiving a first reaction fluid and a second inlet for receiving a second reaction fluid, wherein each channel comprises a region downstream of the first and second inlets for combining the first and second reaction fluids. In this way, two separate reaction fluids can be introduced into the device and then mixed inside the manifold.
If there is a plurality of channels inside the manifold, these channels may not necessarily be connected to each other, thus allowing two different reaction fluid flows to pass independently through the manifold.
The or each channel preferably comprises a region defining a tortuous path for reaction fluid flowing through the channel. Due to the direction changes in the tortuous path, mixing of the reaction fluid as it passes through the manifold is improved.
Mixing of the reaction fluid in each channel may also be improved by adding a region in the channel where it splits and then recombines.
If there is a plurality of tubes inside the reaction vessel, each of these may be connected to the same outlet from the manifold, or each connected to a different outlet in the manifold. In some cases, the plurality of tubes may not be connected to each other, thus allowing two different reaction fluid flows to pass separately through the reaction vessel.
To maximise the time that the reaction fluid can react inside the at least one tube, preferably each tube forms a spiral inside the reaction vessel. Other than a spiral, each tube may have any other shape that maximises the length of the tube inside the reaction vessel.
Preferably, the internal diameter of each tube is between 1 mm-10 mm. Within this range, the internal diameter of the tube is preferably less than 5 mm as above this amount, fluid flow within each tube tends to stratify, rather than form as a plug/slug, thus making the fluid flow more difficult to handle.
In some cases, a mixing device may be located in each tube for mixing the fluid passing through the tube.
Preferably, the device comprises a temperature sensor for measuring the temperature of fluid inside the device, or for measuring the temperature of the reaction fluid. The temperature sensor may be located in a channel(s) of the manifold, or in a tube(s). A temperature sensor may additionally/alternatively be located to measure the temperature of the control fluid inside the reaction vessel. As required, the temperature sensor may be supplemented or replaced with any other sensor(s) for measuring a property (for instance, but not limited to, the pressure/composition/absorption/optical properties/pH/turbidity) of the fluid inside the device.
The reactor device may comprise a sampling port for extracting a sample of fluid from the device.
Preferably at least one of the manifold and a portion of the reactor vessel, such as each tube is made of glass. The benefits of glass include excellent chemical resistance and that it allows good visibility inside the tube/manifold. Glass is also a material that chemists are very familiar with as it is commonly used for lab-scale reactions.
In some cases, at least one of the manifold and the tube may be made of a chemically resistive metal/metal alloy, such as stainless steel or Hastelloy® (a Nickel based alloy). Use of these materials would be beneficial if the device needs to withstand high thermal stresses or temperature differentials.
Preferably the manifold comprises a base layer and a top layer which are bonded together, wherein a channel from the manifold is formed at the interface between the two layers.
Preferably, the device comprises a first end at which the manifold is located, and a second end opposite the first end. In this case, the second end of each tube may be located in the second end of the device.
Alternatively, the second end of each tube may be located in the first end of the device. Here, the second end of each tube may be in fluid communication with a further fluid channel in the manifold.
In a second aspect of the invention, there is provided a reactor assembly comprising a first reactor device as described above, and a second reactor device for the reaction fluid comprising:
Preferably, the manifold from the first reactor device is locatable between the end cap of the first reactor device and the end cap of the second reactor device to fluidly connect the two reaction vessels, and so that the manifold is protected from accidental damage.
In its most basic form, the second aspect of the invention therefore provides a modular system where two (or more) reaction vessels can be connected in series as required to generate the necessary reaction conditions required for a given reaction.
As will be appreciated, the second reactor device may further comprise any/all of the other features described according to the first aspect of the invention.
The invention will now be described with reference to the accompany Figures in which:
With reference to
The reaction vessel 102 is preferably made of glass ora chemically resistant metal/metal alloy. Each of the top cap 104 and the bottom cap 106 is predominately made of a material(s) with good thermal conductivity, such as metal (for example stainless steel or aluminium). In this way, when the device is used, the end caps 104;106 are heated/cooled towards the temperature of the control fluid inside the space 107.
A respective flange 108:110 extends around the circumference of the top and bottom end cap 104;106. In use the flange 108 is connectable to the flange 110 of a neighbouring device 100 such that the two devices can be connected together end-to-end as will be described later and as is shown in
Extending through the top cap 104 is a channel 112 which defines a hole to allow reaction fluid to pass through the top cap 104. A corresponding channel 114 extends through the bottom cap 106 to allow reaction fluid to pass therethrough. The channel 112 in the top cap 104 is fluidly connected to the channel 114 in the bottom cap 106 by a tube 116, preferably made of glass, which is located in the space 107 and which preferably extends through the channels 112;114. Together, the channel 112, the tube 116 and the channel 114 allow reaction fluid to pass from outside the device 100 through the top cap 104, through the space 107 and out of the device 100 via the bottom cap 106.
A first retaining means is provided on the top cap 104 which engages with the tube 116 for holding the tube 116 in position within the channel 112. In one embodiment, the retaining means is a collar that grips the outer surface of the tube 116 and which is fastened to the top surface of the top cap 104. Preferably the collar is made of a plastic, such as polyether ether ketone (PEEK), or aluminium.
A second retaining means, similar to the first retaining means, is provided on the bottom cap 106 for holding the tube 116 in position within the channel 114.
The tube 116 is preferably coiled in the space 107 so that the tube is as long as possible inside the space 107.
To help seal the space 107, an O-ring seal 117 is located between the tube 116 and the channels 112;114.
Although not shown in the Figures, a mixing device may be located in the tube 116 to assist with the mixing of any reaction fluid flowing there through. Example mixing devices that may be present include protuberances/recesses located on the inside of the tube, a propeller, baffle, mesh screen, or any form of static mixer located inside of the tube.
An inlet port 118 is provided on the bottom cap 106 to allow the control fluid to be pumped into the space 107. The inlet port 118 extends from a lateral opening 120 located on the side of the bottom cap 106, and defines an L-shaped channel that terminates at an opening 122 in the top surface of the cap 106 that is in fluid communication with the space 107.
A corresponding outlet port 124 is located on the top cap 104 and defines an L-shaped channel which allows the control fluid to pass from the space 107 through the bottom surface of the top cap 104 and out from the device 100 via an opening 126 located on the side of the top cap 104.
A supplementary port 130 is provided in each of the top and bottoms caps 104;106. Each supplementary port 130 can act as supplementary inlet/outlet for the space, or can be connected to an aspirating mechanism (not shown in the Figures) to allow a portion of the working fluid in the space to be aspirated for analysis/sampling, or connected to any form of probe/sensor that measures a property (for instance, but not limited to, the temperature/pressure/composition/absorption/optical properties/pH/turbidity) of the working fluid.
The top surface of the top cap 104 defines a cavity 134 for receiving a manifold 200. The manifold of
It will be seen from
The manifold block 200 comprises a first inlet 202 for the receipt of a first reaction fluid, a second inlet 204 for the receipt of a second reaction fluid, a channel 206 where the two reaction fluids are mixed together, and an outlet 208 located at the end of the channel 206. The manifold 200 is releasably connected to the cavity 134 and is located in use such that the outlet 206 from the manifold 200 is in fluid communication with the tube 116 located in the channel 112 from the top cap 104 of the reactor device 100.
An example construction of the manifold 200 is shown in each of
To operate the device shown in
As the temperature in the space 107 is brought to the required temperature, the thermally conductive end caps 104 and 106 that are in contact with the control fluid in the space 107 are brought towards the required temperature. Since the manifold 200 is in good thermal contact with the top cap 104, the temperature of the manifold 200 is similarly brought towards the required temperature. Thus the top cap 104 acts as a temperature controlling component for controlling the temperature of the manifold.
Once the device 100 has been sufficiently brought towards the required temperature, reaction fluids are then fed into the inlets of the manifold 200. As the reaction fluids pass through the tortuous path 216 of channel 206, they are thoroughly mixed together and preheated/precooled towards the required temperature due to the preheating/precooling of the manifold 200 by the top cap 104.
At the outlet 208 of the channel 206, the mixed reaction fluid passes into the channel 112 of the top cap 104 and then into the tube 116. As it passes through the tube 116, the surrounding control fluid brings the reaction fluid to the required temperature, thus allowing the reaction fluid to react inside the tube 116. The coil-shape of the tube 116 provides the reaction fluid with as much time to react inside the space 107 as possible.
Once the reaction fluid has reacted inside, and exited, the tube 116, the reaction fluid passes through the channel 114 in the bottom cap 106 and out of the device 100 for further processing.
With reference to
The manifold 200C only comprises one inlet 202 which is operable to connect to a supply of premixed reaction fluid. A sprung seal 226 surrounds the inlet 202 to accommodate for any movement that might occur between the inlet 202 and the supply of premixed reaction fluid (which might, for example, be caused by thermal expansion in the manifold 200C as it heats up in use).
As the manifold 200C receives premixed reaction fluid, the channel 206 in the manifold 206 does not necessarily define a tortuous path and instead may define a straight horizontal portion 220 between the inlet 202 and the outlet 208. A slot 222 is preferably located at one end of the horizontal channel for the receipt of a probe/sensor 224 that measures a property (for instance, but not limited to, the temperature/pressure/composition/absorption properties/optical properties/pH/turbidity) of the reaction fluid passing through the straight portion 220 of the manifold 200.
Rather than holding a probe/sensor 224, the slot 222 may connect to a valve (not shown in the Figures) which allows a portion of the fluid in the channel 206 to be aspirated;
With reference to
The first portion 240 of the manifold 200D is the same as the manifold 200C but has two fluid inlets 202;204, two channels 206A;206B extending therethrough, and two fluid outlets 208A;208B. The channels 206A;206B are separate to each other thus allowing two separate reaction fluids to extend through the first portion 240 of the manifold 200D without mixing.
The second portion 242 of the manifold 200D is connected underneath, and downstream of, the first portion 240. The second portion 242 comprises a first and second inlet 202′;204′ in respective fluid communication with the first and second outlet 208A;208B from the first portion 240. A seal 248 is positioned at the interface of the first inlet 202′ and the first outlet 208A, and at the interface of the second inlet 204′ and the second outlet 208B, to accommodate for any movement that might occur between the first and second portions 240;242 of the manifold 200D.
To allow for a property of the fluid flowing through the second portion 242 of the manifold 200D to be measured, a slot 244 and a corresponding probe/sensor 246 may be provided in the second portion 242, as shown in
The first reactor device 100A comprises a reaction vessel 102 with a modified top and bottom cap 104;106. In each of the ends caps 104;106, there is provided a plurality of channels 112;114, and the reaction vessel 102 comprises a plurality of tubes 116 in parallel with each other. In this way, the reaction vessel 100A is operable to allow different reaction fluids to pass through the reaction vessel 100A independently of each other.
The second reactor device 100B is identical to the reactor device shown in
In this connected state, each of the reaction fluids passing through the tubes 116 from the first reactor device 100A are fed into respective inlets 202;204 located in the manifold 200 of the second reactor device 100B. Flow of these fluids through the second reactor device 100B is then as described with reference to
From the above description, it will be appreciated that the temperature of the control fluid in the first reactor device 100A need not be the same as the temperature of the control fluid in the second reactor device 100B. In this way, a complex heating regime can be imposed on the reaction fluids as they pass through the different reactor devices 100A;100B of the reactor assembly 1000.
It also will be appreciated that any combination of different reactor devices and manifolds can be selected and stacked in series, as required, to achieve the necessary splitting/combining/mixing/passage of reaction fluids through the manifolds, and to achieve the necessary heating/cooling of the reaction fluids in the tube(s) of each reactor vessel.
Rather than having the reactor devices 100A;100B connected end-to-end, it will also be appreciated that a reactor device could be provided as shown in
It can also be seen from
It will also be appreciated that the reactor device 100 could be configured such that the manifold 200 is inserted from the side of the top cap 104, rather than positioned on the top surface of the top cap 104. An example of such a reactor device 100 is shown in
As required, a slot and a corresponding probe/sensor may be provided through the side of manifold 200 and its sleeve 232, to allow for a property of the reaction fluid flowing through the manifold 200 to be measured.
In the reactor device 100 shown in
An advantage of the reactor device 100 shown in
Number | Date | Country | Kind |
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1521670.8 | Dec 2015 | GB | national |