WO2008043313A1

WO2008043313A1 - Reaction system

Info

Publication number: WO2008043313A1
Application number: PCT/CN2007/070845
Authority: WO
Inventors: Guilin Wang; Ling Liu; Yonghua Xu; Sibiao Xu; Jun Zhang
Original assignee: Accelergy Shanghai R & D Center Co., Ltd.
Priority date: 2006-09-30
Filing date: 2007-09-30
Publication date: 2008-04-17
Also published as: CN101219363A

Abstract

A reaction system(100) includes a reaction chamber(103), a reactor(105) detachably disposed in the reaction chamber and a temperature control device(107) thermally coupled to the reaction chamber. A space(106) between the reaction chamber and the reactor is filled with a fluid medium(206) having a thermal conductivity substantially higher than that of stagnant air, so that heat can be rapidly and uniformly transferred from the reaction chamber to the respective reactor.

Description

Reaction system

FIELD OF INVENTION

[0001] The invention relates to a reaction system, particularly to a reaction system for parallel reactions.

BACKGROUND OF THE INVENTION

[0002] High throughput screening has become more and more widely used in materials research field. For example, high throughput parallel reaction methods and parallel reaction systems may be used to perform parallel reactions in order to synthesize and evaluate a large number of materials at about the same time, so as to increase the efficiency and reduce the time for material research projects.

[0003] In many cases, reaction conditions in multiple reactors of the parallel reaction system need to be substantially the same. For example, it is important to maintain temperature uniformity of the reaction system, including temperature uniformity across the multiple reactors and temperature uniformity along each reactor.

[0004] A typical parallel reaction system comprises multiple reaction chambers and multiple reactors detachably disposed in the multiple reaction chambers, respectively. A space filled with air may be formed between each reaction chamber and the respective reactor. Due to the poor thermal conductivity of the air in the space, a relatively long time is

needed to attain temperature uniformity of the system. Nonuniform heat

distribution across the multiple reactors or along each reactor may occur

as a result.

[0005] This problem could also exist for a reaction system having

only one reaction chamber and one reactor, such as a single pipe reactor,

which is mainly used for extensive research on some catalysts.

SUMMARY OF THE INVENTION

[0006] Embodiments of the present invention provides a reaction

system comprising a reaction chamber, a reactor detachably

accommodated in the reaction chamber, and a temperature control device

thermally coupled to the reaction chamber. The space between the

reaction chamber and the reactor is filled with a fluid medium having a

thermal conductivity higher than that of stagnant air under similar

ambient conditions.

[0007] In one embodiment, the reaction system comprises multiple

reaction chambers and multiple reactors disposed respectively in the

reaction chambers. A space formed between each reactor and the

respective reaction chamber is filled with the fluid medium.

[0008] In one embodiment, the fluid medium has a thermal

conductivity higher than that of stagnant air when the temperature of the fluid medium and the temperature of the stagnant air are the same and are above 200 ^°C . For example, the fluid medium may have a thermal conductivity higher than 0.5 W-(m-K)^"1, or higher than 5 W-(m-K)^"1, or higher than 30W-(Tn-K)^"1 when the temperature of the fluid medium is above 200 ^°C . In one embodiment, the fluid medium has a thermal conductivity ranged from 30 to 300 W-(m-K)^"1 when the temperature of the fluid medium is above 200 ^°C .

[0009] Embodiments of the present invention further provides a complex reaction system which includes multiple such reaction systems arranged in series such that an output of one reaction system feed into an input of another reaction system.

BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Fig. 1 is a partially cutaway perspective view showing a cross section of a reaction system according to one embodiment, wherein some components of the system are omitted for the sake of simplicity.

[0011] Fig. 2 is a longitudinal cross-sectional view of the reaction system of Fig. 1.

[0012] Fig. 3 is a longitudinal cross-sectional view of the reaction system of Fig. 1 illustrating a flowable fluid medium utilized by the reaction system. [0013] Fig. 4 is a cross-sectional view showing temperature sensors of the reaction system of Fig. 1.

[0014] Fig. 5 is a longitudinal cross- sectional view of a reaction system according to an alternative embodiment.

[0015] Fig. 6 is a partially cutaway perspective view showing a cross section of a reaction system according to another alternative embodiment, wherein some components of the system are omitted for the sake of simplicity.

[0016] Fig. 7 is a longitudinal cross-sectional view of the reaction system of Fig. 6.

[0017] Fig. 8 is a longitudinal cross- sectional view of a reaction system according to yet another alternative embodiment.

[0018] Fig. 9 is a schematic view showing a complex reaction system comprising three reaction systems of Fig. 8.

[0019] Fig. 10 is a schematic view showing a complex reaction system comprising three reaction systems each having two reaction chambers.

[0020] Fig. 11 is a schematic view showing a complex reaction system comprising three reaction systems each having three reaction chambers.

[0021] Fig. 12 is a schematic view showing a complex reaction system comprising three reaction systems each having eight reaction chambers.

DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0022] Figs. 1-4 show a reaction system 100 comprising multiple

reaction chambers provided in a block of thermally conductive material.

[0023] As shown in Fig. 1, the reaction system 100 comprises

multiple reaction chambers 103 formed in a block of thermally

conductive material 101 and multiple reactors 105 detachably disposed in

the multiple reaction chambers 103 respectively, wherein the reactors 105

may be vessels, tubes, pipes or the like and may be loaded with catalysts,

reactants, etc. A space 106 is formed between the reaction chamber 103

and the reactor 105 disposed in the reaction chamber 103.

[0024] The block of thermally conductive material 101 may have any

shape allows the formation of the reaction chambers 103. In one

embodiment, the block of thermally conductive material 101 is a ring

having a hollow cylindrical shape with concentric inner and outer

cylindrical surfaces, and the reaction chambers 103 are longitudinally

parallel to the axial direction of the inner and outer cylindrical surfaces.

As seen from a cross sectional view of the ring 101 in Fig. 1, the reaction

chambers 103 are circularly arrangement within the ring 101 such that

each reaction chamber 103 is substantially equidistant from adjacent

reaction chambers on both sides and substantially equidistant from the inner and/or outer cylindrical surfaces of the ring 101 when compared to the other reaction chambers of the system.

[0025] The reaction system 100 further comprises a temperature control device 107 which is thermally coupled to the reaction chambers 103. The temperature control device 107 used herein may include one or more heating elements, cooling elements, or other establishments capable of changing the temperatures of objects thermally coupled to it, and may be automatically or manual operated to control the temperature of the objects.

[0026] In one embodiment, the temperature control device 107 includes a first heating element 109 contacting the outer cylindrical surface of the block of thermally conductive material 101 (may be referred as ring 101 or block 101 hereafter for short) and a second heating element 111 contacting the inner cylindrical surface of the ring 101, and therefore is thermally coupled to the reaction chambers 103 via the ring 101. Alternatively, in other embodiments, the temperature control device 107 may be coupled to the reaction chambers 103 from either the inner surface or the outer surface of the ring 101.

[0027] The reaction system 100 may further comprise one or more hole, slot or the like to receive a temperature sensor which is adapted to detect a temperature in the reaction system. In one embodiment, there are sensor receiving holes 113 defined near the reaction chambers 103 in the block 101.

[0028] Fig. 2 is a longitudinal cross section view of the reaction system 100 of Fig. 1. As shown in Fig. 2, each reaction chamber 103 has an inlet 201 and an outlet 202, and each reactor 105 has an inlet 203 and an outlet 204. In one embodiment, the inlet 203 of the reactor 105 is connected to an inputting conduit 207 by a connecting device 205 such as a tie-in, so that gas or liquid reactants can be fed into the reactor 105 through the inputting conduit 207. In one embodiment, the outlets 204 of the reactors 105 are respectively connected to a corresponding liquid collecting container (referred as a liquid collector hereafter) 209, a temperature of which may be controlled at a relatively lower level in order to disengage gases and liquids of the resultants, keep the liquid resultants and let out gaseous resultants. In one embodiment, all the liquid collector 209 are formed in a same block of thermal conductive material 211 and there is a cover 215 for covering the liquid collectors 209. In order to let out the gaseous resultants, each liquid collector 209 has a gaseous resultant outlet 213 which may be defined in the block 211 or preferably in the cover 215.

[0029] The spaces 106 between the reaction chambers 103 and the corresponding reactors 105 are filled with a fluid medium 206 which has a thermal conductivity substantially higher than that of stagnant air. [0030] The fluid medium is made of a material with fluidity and ability to fill cavity or space, and it includes but is not limited to one or more liquid materials, a mixture of solid and liquid materials, a substance between solid and liquid (such as gelatin), one or more gaseous materials, or combinations thereof.

[0031] Particularly, the fluid medium with a thermal conductivity higher than that of stagnant air is a fluid that, when heated to 200 "C or above, has a thermal conductivity higher than that of stagnant air under the same temperature, i.e., 200 "C or above. For example, the fluid medium may have a thermal conductivity higher than 0.5 W-(m-K)^"1, or higher than 5 W-(m-K)^"1, or higher than 30W-(In-K)^"1 when the temperature of the fluid medium is above 200 ^°C . In one embodiment, the fluid medium is made of one or more kinds of liquid metal (e.g., liquid stannum, etc) and has a thermal conductivity ranged from 30 to 300 W-(IIi-K)^"1.

[0032] An excellent thermal conductivity of the block 101 can cause the temperatures of the multiple reaction chambers 103 to be nearly the same, and an excellent thermal conductivity of the fluid medium 206 can result in the heat to be rapidly and uniformly transferred from each reaction chamber 103 to the corresponding reactor 105. Therefore, both the temperature uniformity across the multiple reactors 105 and throughout each of the reactors 105 can be achieved. [0033] The reaction system 100 may further comprise a sealing element 216 adapted to prevent the fluid medium 206 against leaking from the outlet 202 of the reaction chambers 103. In one embodiment, the sealing element 216 includes a step portion 217 protruding inwards from an inner surface of the reaction chamber 103, and a sealing material (not shown) adapted to seal a space between the step portion 217 and the reactor 105. The sealing material may be high temperature resistant silica gel or the like which can seal spaces.

[0034] The fluid medium 206 may be stagnant or flowing in the spaces 106 between the reaction chambers 103 and the reactors 105. For instance, in one embodiment as shown in Fig. 3, the fluid medium 206 is connected to a pump or the like 301 which may drive the fluid medium 206 to flow and cycle in the space. Only one pump is illustrated in the Fig. 3 for the sake of simplicity. Flowing fluid medium 206 may further increase temperature uniformity throughout each reactor 105. The pumps 301 and cyclically inputting and outputting conduits 302 and 303 can be controlled to be at a constant temperature.

[0035] Retuning to Fig. 2, the reaction chamber 103 is elongated along an axial direction, and the first and second heating elements 109 and 111 of the temperature control device 107 are respectively two single heating rings covering a whole length of the chamber 103 along the axial direction. Alternatively, the temperature control device 107 may include multiple heating elements placed in different locations along the axial direction of the reaction chamber 103, and the multiple heating elements may have independent temperature control means. For example, the first and second heating elements 109 and 111 may each include three heating rings which are separated from each other in the axial directions of the reaction chambers 103, and temperatures of the three heating rings can be independently controlled. In one embodiment, temperatures of the two heating rings respectively adjacent to the two ends of the reaction chamber 103 may be controlled to be higher than that of the heating ring located in the middle where a heat loss is relatively smaller than the ends. [0036] The reaction system 100 may further comprise a heat preservation arrangement to prevent or decrease heat exchange between the reaction chambers 103 and an outside environment. The heat preservation arrangement may include one or more elements adapted to prevent undesired heat exchange by conduction, convection, or radiation. [0037] In one embodiment, the heat preservation arrangement includes heat insulators 219 substantially surrounding the reaction chambers 103 in order to decrease heat exchange by conduction or convection. Examples of the heat insulator include a cavity, wherein the cavity is substantially a vacuum chamber, a cavity filled with air, or a cavity filled with some other insulating material. Examples of other insulating material include without limitation foam, polyurethane, perlite, fiberglass, and Teflon. The insulator may also be a series of cavities or insulators as described here, such as a series of separate cavities wherein each cavity is a vacuum chamber, a cavity filled with are or some other insulating material.

[0038] In one embodiment, the heat preservation arrangement may alternatively or additionally include a heat radiation shield which is able to reflect back the heat radiation from the reaction chambers 103 and reflect off the heat radiation from the outside environment of the reaction system 100, so as to prevent heat exchange between the reaction system 100 and the outside environment through radiation (details about the heat radiation shield are provided in another embodiment hereafter). [0039] The reaction system 100 may further comprise a shell 221 to accommodate all the aforementioned members. The shell 221 may be a hollow container of any shape. In one embodiment, the shell 221 comprises a top 223, a bottom 225 and a cylinder-like mid-portion 227 joining the top 223 and the bottom 225, wherein the top 223, the bottom 225, and the mid-portion 227 are independent from each other, yet the bottom 225 is integrally formed on the block 101.

[0040] Fig. 4 is a view showing temperature sensors 401 disposed in the holes 113 (as shown in Fig. 1) defined in the block of thermally conductive material 101. Although in the embodiment as illustrated, the sensors 401 are placed in the block 101, actually there is no limitation as to positions of the temperature sensors 401 and they may be placed anywhere a reaction temperature in the reactor 105 can be detected. [0041] Fig. 5 shows another reaction system 500, structure of which is similar to the reaction system 100 as shown in Figs. 1-4. The following description will focus on the main differences from the reaction system 100.

[0042] A temperature control device 521 of the reaction system 500 comprises two elements 523 and 525, both of which contact an outer cylindrical surface of a block of thermally conductive material 501 formed with reaction chambers 503. The two elements 523 and 525 are separated from each other in an axial direction, along which the reaction chambers 503 are elongated, and respectively adjacent to two ends of the reaction chambers 503 along the axial direction.

[0043] A sealing element 516 adapted to prevent leakage of the fluid medium 506 comprises an inner-screw-threaded structure 517 which is formed at a bottom portion of the block 501, a screw plug 519 engaging with the inner-screw-threaded structure 517, and a sealing tool (not shown) sealing a space between the screw plug 519 and a periphery surface of the reactor 505. In one embodiment, the sealing tool is an asbestos cord winding around the periphery surface of the reactor 505. [0044] Multiple liquid collectors 509 of the reaction system 500 are respectively formed in multiple blocks of thermally conductive material. Each of the liquid collectors 509 is an independent container 511 with an independent cover 513. The reactors 505 are connected to the covers 513 of the liquid collectors 511, respectively. Therefore, any one of the reactors 505 can be detached together with the respective cover 513 without involving covers of other liquid collector 509. In one embodiment, the multiple independent liquid collectors 511 are accommodated in a shell 512.

[0045] A gas resultant outlet 515 is defined in an upper portion of each liquid collector 509. The reactor 507 is inserted into the liquid collector 509 such that an outlet 507 of the reactor 505 is located near a bottom of the liquid collector 509. It would benefit a separation of the gas and liquid resultants to increase a distance between the gas resultant outlet 515 and the outlet 507 (serving as a total resultant outlet). [0046] Figs. 6 and 7 show another kind of reaction system 600 in which a plurality of reaction chambers 603 are respectively provided in a plurality of blocks of thermally conductive material 601. [0047] As shown in Fig. 6, the reaction system 600 comprises a plurality of reaction chambers 603 respectively provided in a plurality of blocks of thermally conductive material 601. The reaction system 600 further comprises a plurality of reactors (not shown) detachably disposed in the plurality of reaction chambers 603 respectively, and fluid medium (not shown), which is similar to the fluid medium in the reaction system 100, filled in spaces between the reaction chambers 603 and corresponding reactors. In one embodiment, the plurality of reaction chambers 603 are arranged in a circle, and preferably, the circle of reaction chambers 603 are enclosed in a shell 605.

[0048] As shown in Fig. 7, the reaction system 600 may further comprise a top portion 701 and a bottom portion 703. In one embodiment, the top portion 701 and the bottom portion 703 are respectively a plate made of a thermally conductive material. Top ends 702 and bottom ends 704 of the plurality of reaction chambers 603 are respectively fixed to the top portion 701 and bottom portion 703.

[0049] The reaction system 600 may further comprise a temperature control device. In one embodiment, the temperature control device includes a first pair of heating rings 705 and 707 disposed at the top portion 701 and a second pair of heating rings 709 and 711 disposed at the bottom portion 703. The heating rings 705 and 709 are respectively placed at an inner side of the circle of the reaction chambers 603 and the heating rings 707 and 711 are placed at an outer side of the circle of the reaction chambers 603.

[0050] Heat provided by the heating rings 705 and 707 is uniformly transferred to the top ends 702 of the reaction chambers 603 through the top portion 701, and similarly heat provided by the heating rings 709 and 711 is uniformly transferred to the bottom ends 704 of the reaction chambers 603 through the bottom portion 703. Then heat from the top end 702 and bottom end 704 of each reaction chamber 603 is uniformly transferred through the block of thermal conductive material 601 in which the reaction chamber 603 is formed, and is further uniformly transferred throughout each reactor (not illustrated) via the fluid medium (not illustrated) between the reaction chamber 603 and the reactor in the reaction chamber 603. Therefore, when the reaction system 600 is in a thermally stable state, both temperature uniformity across the reactors and throughout each reactor can be ensured.

[0051] The temperature control device may further comprise heating channels 713 and 715. In one embodiment, the channels 713 and 715 are respectively formed in the top and bottom portions 701 and 703 and respectively communicate with openings 717 and 719, though which fluids may be inputted to or withdrawn from the channels 713 and 715. Thus, temperatures of the top portion 701 and the bottom portion 703 can be further controlled through adjusting and controlling the temperatures of the fluids in the channels 713 and 715. Preferably, the fluids are flowing in the channels 713 and 715 in order to further improve temperature uniformity throughout the top and bottom portions 701 and 703.

[0052] The reaction system 600 may further comprise a temperature sensor 721 which may be disposed in sidewalls of the reaction chamber 603 or in the fluid medium (not illustrated) within the reaction chamber 603.

[0053] The reaction system 600 may further comprise a heat preservation arrangement. In one embodiment, the heat preservation arrangement includes heat insulators 723 and heat radiation shields 725. The insulators 723 may be formed with an opening 727 adapted to add or remove insulating materials. For example, the opening 727 may be adapted to vacummize or to add other insulating materials. [0054] In one embodiment, the heat radiation shields 725 surround the reaction chambers 603 in a parallel relation to the reaction chambers 603, and reflect back heat radiation both from the reaction chambers 603 and from an outside environment of the reaction system 600, such that heat exchange between the reaction system and the outside environment can be prevented.

[0055] The surface of the heat radiation shield may be coated with a material or may be constructed of a material that prevents or reduces radiation such as a reflective material. Reflective materials include radiant barriers and reflective insulations. A radiant barrier is a single sheet of reflective materials. Reflective insulation is a system of reflective sheets and insulator designed together act as insulation. Thus, reflective insulation would consist of a number of layers insulator and reflective sheets. Examples of reflective materials include without limitation, reflective foils, stainless steel, high-temperature metal alloy, and other metal or non-metal materials known in the art that can be made to have a smooth surface and are reflective to infra-red or visible light. [0056] Moreover, spirits of the present invention also extends to systems containing only one reaction chamber. Fig. 8 shows a reaction system 800 which comprises only one reaction chamber 803 formed in a block of thermally conductive material 801, one reactor 805 accommodated in the chamber 803, and a temperature control device 809 thermally coupled to the reaction chamber 803. In one embodiment, the temperature control device 809 contacts a periphery surface of the block of thermally conductive material 801 and surrounds the reaction chamber 803. A space between the reaction chamber 803 and the reactor 805 is filled with fluid medium 807 which improves temperature uniformity throughout the reactor 805. The reaction system 800 may also comprise a heat preservation arrangement 811 and a shell 813. [0057] Otherwise, multiple the reaction systems as described above may be combined into a complex reaction system in which the reaction systems may be arranged in series or in parallel. For instance, Fig. 9 depicts a complex reaction system, in which three reaction systems 800 of Fig. 8 combined in series. Figs. 10-12 respectively show a complex reaction system, in which three reaction systems each containing two reaction chambers combined in series, a complex reaction system, in which three reaction systems each containing three reaction chambers combined in series, and a complex reaction system, in which three reaction systems each containing eight reaction chambers combined in series.

[0058] In the aforementioned reaction systems, the thermal conductive materials suitable for providing the reaction chambers or the liquid collectors can be any materials that are heat conductive and can withstand the temperature, pressure and chemicals, such as acids, bases, or other reactive compounds. The materials include, but are not limited to metals and alloys. For example, the thermally conductive material may be various grades of steel and stainless steel, which have a strong high-temperature and high-pressure resistance, a strong corrosion resistance as well as a good thermal conductivity, or may be aluminium and its alloys, which have an excellent thermal conductivity, proper high-temperature and high-pressure resistance, corrosion resistance, and light weight (which benefits to decrease the total weight of the reaction system). In one embodiment, the thermally conductive material is aluminium.

[0059] Compared to the prior art, in the aforementioned reaction systems, as the spaces between the reaction chambers and the corresponding reactors are filled with a fluid medium with a thermal conductivity higher than that of stagnant air under same temperature conditions, therefore temperature uniformity of the reaction system can be ensured and temperature equilibrium of the reaction system can be achieved within a relatively shorter time.

[0060] While the present invention has been illustrated and described with reference to some embodiments, the present invention is not limited to these embodiments. Those skilled in the art should recognize that various variations and modifications can be made without departing from the spirit and scope of the present invention as defined by the accompanying claims.

Claims

1. A reaction system, comprising: a reaction chamber, a reactor detachably disposed in the reaction chamber, and a temperature control device thermally coupled to the reaction chamber, wherein a space between the reaction chamber and the reactor is filled with a fluid medium having a thermal conductivity substantially higher than that of stagnant air.

2. The reaction system according to claim 1, wherein the fluid medium has a thermal conductivity higher than that of stagnant air when the temperature of the fluid medium and the temperature of the stagnant air are the same and are above 200 ^°C .

3. The reaction system according to claim 1 or 2, wherein the fluid medium has a thermal conductivity higher than 0.5 W-(m-K)^"1 when the temperature of the fluid medium is above 200 "C .

4. The reaction system according to claim 3, wherein the fluid medium has a thermal conductivity higher than 5 W-(m-K)^"1 when the temperature of the fluid medium is 200 "C .

5. The reaction system according to claim 4, wherein the fluid medium has a thermal conductivity higher than 30W-(In-K)^"1 when the temperature of the fluid medium is above 200 ^°C .

6. The reaction system according to claim 5, wherein the fluid medium has a thermal conductivity ranged from 30 to 300 W-(m-K)^"1 when the temperature of the fluid medium is above 200 ^°C .

7. The reaction system according to claim 1, wherein the reaction system comprises multiple reaction chambers and multiple reactors disposed respectively in the reaction chambers, and wherein a space formed between each reactor and the respective reaction chamber is filled with the fluid medium.

8. The reaction system according to claim 7, wherein the multiple reaction chambers are formed in a block of a thermally conductive material.

9. The reaction system according to claim 7, wherein the multiple reaction chambers are respectively formed in multiple blocks of a thermally conductive material.

10. The reaction system according to claim 9, wherein the multiple thermally conductive blocks are fixed to a common plate made of a thermally conductive material.

11. The reaction system according to claim 7, further comprising multiple liquid collecting containers fluidly connected to respective ones of the multiple reactors.

12. The reaction system according to claim 11, wherein the multiple liquid collecting containers are formed in a same block of thermally conductive material.

13. The reaction system according to claim 11, wherein the multiple liquid collecting containers are respectively formed in multiple blocks of a thermally conductive material.

14. The reaction system according to claim 1 or 7, wherein the reaction chamber has an inlet and an outlet.

15. The reaction system according to claim 14, further comprising a sealing element adapted to prevent the fluid medium from leaking from the outlet of the reaction chamber.

16. The reaction system according to claim 1, wherein the reaction chamber is elongated along an axial direction, and the temperature control device includes multiple elements placed in different locations along the axial direction of the reaction chamber, and wherein the multiple elements have independent temperature control means.

17. A complex reaction system comprising multiple reaction systems of claim 1 , wherein the multiple reaction systems are arranged in series such that an output of one reaction system feed into an input of another reaction system.

18. The complex reaction system according to claim 17, wherein each of the multiple reaction systems comprises multiple reaction chambers and multiple reactors disposed respectively in the reaction chambers, and wherein a space formed between each reactor and the respective reaction chamber is filled with the fluid medium.