CN114588850A - Integrated micro-reactor for liquid-liquid heterogeneous exothermic reaction and use method - Google Patents
Integrated micro-reactor for liquid-liquid heterogeneous exothermic reaction and use method Download PDFInfo
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- CN114588850A CN114588850A CN202210207439.6A CN202210207439A CN114588850A CN 114588850 A CN114588850 A CN 114588850A CN 202210207439 A CN202210207439 A CN 202210207439A CN 114588850 A CN114588850 A CN 114588850A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- B01J19/0053—Details of the reactor
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
Abstract
The invention relates to an integrated microreactor for liquid-liquid heterogeneous exothermic reaction and a using method thereof. In the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction, the heat-conducting rotary drum is arranged in the reactor shell, and a reaction gap is formed between the reactor shell and the heat-conducting rotary drum. The separation of the light and heavy phases takes place in the cavity of the heat-conducting drum with the continuous addition of the reactants. In the process, the separation between two phases and the reaction of the reactant are respectively integrated in the inner side area and the outer side area of the heat conduction rotary drum, the heat emitted by the reaction can be timely and efficiently transmitted to the outer side of the heat conduction rotary drum from the inner side of the heat conduction rotary drum through the heat conduction rotary drum, and the utilization rate of the heat in the reaction process is effectively improved.
Description
Technical Field
The invention relates to the field of reactors, in particular to an integrated microreactor for liquid-liquid heterogeneous exothermic reaction and a using method thereof.
Background
In the chemical reaction process, the transfer and utilization of heat have important influences on the progress of the reaction, the yield of the product, and the like. For example, among the many types of chemical reactions, nitration is a widely used and significant reaction. In the nitration reaction, a multi-stage series kettle type process is usually adopted in the traditional mode, the process can better promote the nitration reaction to be carried out, the process has better maturity, but the problem of low heat utilization rate often exists, extra temperature rise and fall intervention is needed to enable the reaction to be carried out smoothly, extra equipment is needed to be used for the extra temperature rise and fall intervention, and accordingly the cost and the complexity of the reaction are correspondingly improved.
Disclosure of Invention
In view of the above, there is a need for an integrated microreactor for liquid-liquid heterogeneous exothermic reactions and a method of using the same, which can effectively improve the heat utilization rate during the reaction process.
In order to solve the technical problems, the technical scheme of the invention is as follows:
an integrated microreactor for liquid-liquid heterogeneous exothermic reactions comprises a reactor shell, a heat-conducting rotary drum and a driving mechanism;
the heat-conducting rotary drum is connected to the inside of the reactor shell, a reaction gap is formed between the outer wall of the heat-conducting rotary drum and the inner wall of the reactor shell, and the outer top of the heat-conducting rotary drum is abutted against the inner top of the reactor shell; the interior of the heat conduction rotary drum is provided with a cavity, the bottom of the heat conduction rotary drum is provided with an opening, and the opening, the cavity and the reaction gap are communicated;
the reactor shell is provided with a light phase feed inlet, a heavy phase feed inlet, a light phase discharge outlet and a heavy phase discharge outlet; the light phase feed port and the heavy phase feed port are communicated with the reaction gap; the light phase discharge port and the heavy phase discharge port are both arranged at the top of the reactor shell and are both communicated with the cavity, and the light phase discharge port is closer to the central axis of the heat-conducting rotary drum than the heavy phase discharge port;
the driving mechanism is connected with the heat conduction rotary drum and is used for driving the heat conduction rotary drum to rotate.
In one embodiment, the top of the reactor shell is further provided with a light phase flow guide weir and a heavy phase flow guide weir, the light phase flow guide weir is close to the light phase discharge hole for guiding the light phase, and the heavy phase flow guide weir is close to the heavy phase discharge hole for guiding the heavy phase.
In one embodiment, the inner diameter of the reactor shell is 0.6 cm-10 cm; and/or the presence of a gas in the gas,
the internal height of the reactor shell is 2-32 cm; and/or the presence of a gas in the gas,
the width of the reaction gap is 0.05 cm-1 cm.
In one embodiment, the outer diameter of the heat conducting rotary drum is 0.5 cm-10 cm; and/or the presence of a gas in the gas,
the height of the heat conducting rotary drum is 2 cm-30 cm; and/or the presence of a gas in the gas,
the wall thickness of the heat-conducting rotary drum is 0.1 cm-1 cm; and/or the presence of a gas in the gas,
the diameter of the opening is 0.05 cm-1.5 cm.
In one embodiment, the light phase feed inlet and the heavy phase feed inlet are both located in a side wall of the reactor shell; and/or the presence of a gas in the gas,
the diameter of the light phase feed inlet is 0.2 mm-6 mm; and/or the presence of a gas in the gas,
the diameter of the heavy phase feed inlet is 0.2 mm-6 mm.
In one embodiment, the included angle between the axis of the light phase feed inlet and the axis of the heavy phase feed inlet is 90-180 °.
In one embodiment, the heat conducting drum is made of stainless steel and/or hastelloy.
In one embodiment, the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction further comprises a light phase storage tank and a light phase feeding pipe, wherein two ends of the light phase feeding pipe are respectively connected to the light phase feeding port and the light phase storage tank, and a light phase feeding pump is arranged on the light phase feeding pipe; and/or the presence of a gas in the gas,
the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction further comprises a heavy phase storage tank and a heavy phase feeding pipe, wherein two ends of the heavy phase feeding pipe are respectively connected to the heavy phase feeding port and the heavy phase storage tank, and the heavy phase feeding pipe is provided with a heavy phase feeding pump; and/or the presence of a gas in the gas,
the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction further comprises a light phase material receiving tank and a light phase material receiving pipe, wherein two ends of the light phase material receiving pipe are respectively connected to the light phase material outlet and the light phase material receiving tank; and/or the presence of a gas in the gas,
the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction further comprises a heavy phase material receiving tank and a heavy phase material receiving pipe, wherein two ends of the heavy phase material receiving pipe are respectively connected with the heavy phase material outlet and the heavy phase material receiving tank.
A method of using an integrated microreactor for liquid-liquid heterogeneous exothermic reactions as described in any of the above embodiments, comprising the steps of:
the driving mechanism drives the heat conduction rotary drum to rotate;
and adding a light-phase reactant into the reaction gap through the light-phase feed opening, and adding a heavy-phase reactant into the reaction gap through the heavy-phase feed opening.
In one embodiment, the autorotation speed of the heat conducting rotary drum is 1000rpm to 8000 rpm; and/or the presence of a gas in the gas,
the feeding speed of the light phase reactant is 0.5mL/min to 15 mL/min; and/or the presence of a gas in the gas,
the feeding speed of the heavy phase reactant is 0.1 mL/min-15 mL/min.
In the above-mentioned integral type microreactor for heterogeneous exothermic reaction of liquid-liquid, reactor shell is inside to set up the heat conduction rotary drum to make reactor shell and heat conduction rotary drum between have reaction gap, when the reaction goes on, based on little space-time scale effect and the plug flow characteristic of little chemical technology, the reactant reacts in the rotatory microchannel that reaction gap formed, along with the continuous joining of reactant, the reaction mixed phase gets into the cavity of heat conduction rotary drum by the opening of the bottom of heat conduction rotary drum, provide centrifugal field through the rotation of heat conduction rotary drum simultaneously, carry out the separation of light phase and heavy phase in the cavity of heat conduction rotary drum. In the process, the separation between two phases and the reaction of the reactant are respectively integrated in the inner side area and the outer side area of the heat conduction rotary drum, the heat emitted by the reaction can be timely and efficiently transmitted to the outer side of the heat conduction rotary drum from the inner side of the heat conduction rotary drum through the heat conduction rotary drum, the initial temperature of the reaction can be effectively guaranteed, extra temperature rise and fall intervention is not needed, the internal coupling of the heat inside the reaction system is realized, and the utilization rate of the heat in the reaction process is effectively improved. Meanwhile, the reaction of reactants, the separation of different phases and the conduction and supply of heat are carried out in the integrated microreactor, additional equipment is not needed, and the cost and complexity of the reaction are effectively reduced. And with the continuous addition of reactants, the mixed phase in the cavity of the heat-conducting rotary drum is divided into a light phase and a heavy phase and is discharged through a light phase discharge port and a heavy phase discharge port respectively, so that the continuous reaction is effectively realized. In addition, when the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction is adopted, heat in the reaction system can be timely and efficiently transferred, the problem that the product quality is influenced due to the fact that local hot spots are too high in the reaction system is effectively avoided, and the quality of the product can be effectively maintained through the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction.
Furthermore, in the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction, a centrifugal field is provided by the rotation of the heat-conducting rotary drum, so that the transfer distance between reactants can be greatly reduced, the dispersion and mixing performance of liquid drops can be improved, the transfer speed of a reaction phase and the conversion rate of a product can be further improved, the liquid holding rate of a reaction system is obviously reduced, the danger of a chemical reaction is greatly reduced, and the safety of the reaction process is improved.
Furthermore, when the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction is used, reaction mixed phases are separated in a cavity of the heat-conducting rotary drum, heavy phases are thrown to the inner wall of the heat-conducting rotary drum under the action of the centrifugal field, light phases are extruded to the center of the heat-conducting rotary drum, the restriction of slow phase separation speed existing between reactants under the conventional gravity field is broken, the phase separation time is effectively shortened, the effect of rapid quenching reaction is achieved, the generation of byproducts is favorably reduced, the difficulty of subsequent treatment is reduced, and the reaction cost is further reduced.
The use method of the integrated microreactor for the liquid-liquid heterogeneous exothermic reaction comprises the following steps: the driving mechanism drives the heat-conducting rotary drum to rotate; and adding the light-phase reactant into the reaction gap through the light-phase feed inlet, and adding the heavy-phase reactant into the reaction gap through the heavy-phase feed inlet. The light phase reactant and the heavy phase reactant are introduced under the condition that the driving mechanism drives the heat conduction rotary drum to rotate, the continuous proceeding of reaction and phase separation can be realized along with the addition of the reactants, and the using method is simple and easy to implement and convenient to popularize.
Drawings
FIG. 1 is a schematic structural diagram of an integrated microreactor for liquid-liquid heterogeneous exothermic reactions in an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an integrated microreactor for liquid-liquid heterogeneous exothermic reactions in another embodiment of the present invention.
The notation in the figure is:
100. an integrated microreactor for liquid-liquid heterogeneous exothermic reactions; 101. a reactor shell; 102. a heat conducting drum; 103. a drive mechanism; 104. a reaction gap; 105. a cavity; 106. an opening; 107. a light phase feed inlet; 108. a heavy phase feed inlet; 109. a light phase discharge port; 1010. a heavy phase discharge port; 1011. a light phase drainage weir; 1012. a heavy phase drainage weir; 1013. a drive shaft; 1014. a base; 1015. a light phase storage tank; 1016. a light phase feeding pipe; 1017. a light phase feed pump; 1018. a heavy phase storage tank; 1019. a heavy phase feed pipe; 1020. a heavy phase feed pump; 1021. a light phase collecting tank; 1022. a light phase material receiving pipe; 1023. a heavy phase material receiving tank; 1024. heavy phase collecting pipe.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, as those skilled in the art will recognize without departing from the spirit and scope of the present invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, but are not intended to indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and are not to be construed as limiting the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an embodiment of the present invention provides an integrated microreactor 100 for liquid-liquid heterogeneous exothermic reactions. The integrated microreactor 100 for liquid-liquid heterogeneous exothermic reactions comprises a reactor housing 101, a thermally conductive rotating bowl 102, and a drive mechanism 103. The heat conducting rotating cylinder 102 is connected to the inside of the reactor shell 101, a reaction gap 104 is formed between the outer wall of the heat conducting rotating cylinder 102 and the inner wall of the reactor shell 101, and the outer top of the heat conducting rotating cylinder 102 is abutted to the inner top of the reactor shell 101; the interior of the heat conducting drum 102 has a cavity 105, the bottom of the heat conducting drum 102 has an opening 106, and the opening 106, the cavity 105 and the reaction gap 104 are communicated. A light phase feed inlet 107, a heavy phase feed inlet 108, a light phase discharge outlet 109 and a heavy phase discharge outlet 1010 are arranged on the reactor shell 101; the light phase feed port 107 and the heavy phase feed port 108 are both communicated with the reaction gap 104; the light phase discharge port 109 and the heavy phase discharge port 1010 are both arranged at the top of the reactor shell 101, the light phase discharge port 109 and the heavy phase discharge port 1010 are both communicated with the cavity 105, and the light phase discharge port 109 and the heavy phase discharge port 1010 are closer to the central axis of the heat conducting rotary drum 102. The driving mechanism 103 is connected to the heat conducting drum 102 for driving the heat conducting drum 102 to rotate.
In the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction of the present embodiment, a heat-conducting rotating cylinder 102 is disposed inside a reactor housing 101, and a reaction gap 104 is provided between the reactor housing 101 and the heat-conducting rotating cylinder 102, when the reaction proceeds, reactants react in a rotating microchannel formed by the reaction gap 104 based on the micro-space-time scale effect and the plug flow characteristic of the microchemical technology, and as the reactants are added continuously, a reaction mixed phase enters a cavity 105 of the heat-conducting rotating cylinder 102 from an opening 106 at the bottom of the heat-conducting rotating cylinder 102, and a centrifugal field is provided by the self-rotation of the heat-conducting rotating cylinder 102, so that the separation of a light phase and a heavy phase is performed in the cavity 105 of the heat-conducting rotating cylinder 102. In the process, the separation between two phases and the reaction of the reactant are respectively integrated in the inner side area and the outer side area of the heat conduction rotary drum 102, the heat emitted by the reaction can be timely and efficiently transmitted to the outer side of the heat conduction rotary drum 102 from the inner side of the heat conduction rotary drum 102 through the heat conduction rotary drum 102, the initial temperature of the reaction can be effectively guaranteed, additional temperature increase and decrease intervention is not needed, the internal coupling of the heat inside the reaction system is realized, and the utilization rate of the heat in the reaction process is effectively improved. Meanwhile, the reaction of the reactants, the separation of different phases and the conduction supply of heat are carried out in the integrated microreactor 100, no additional equipment is required, and the cost and complexity of the reaction are effectively reduced. And with the continuous addition of the reactants, the mixed phase in the cavity 105 of the heat-conducting drum 102 is divided into a light phase and a heavy phase and is discharged through the corresponding light phase discharge port 109 and the heavy phase discharge port 1010, so that the continuous reaction is effectively realized. In addition, when the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction is adopted, heat inside a reaction system can be timely and efficiently transferred, and the problem that the product quality is affected due to the fact that local hot spots are too high in the reaction system is effectively avoided, namely, the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction can effectively keep the product quality.
Further, in the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction of the embodiment, a centrifugal field is provided by the rotation of the heat conducting rotating drum 102, so that the transfer distance between reactants can be greatly reduced, the dispersion and mixing performance of liquid drops can be improved, the transfer speed of a reaction phase and the conversion rate of a product can be further improved, the liquid holding rate of a reaction system is obviously reduced, the risk of a chemical reaction is greatly reduced, and the safety of the reaction process is improved.
Still further, when the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction of the present embodiment is used, a reaction mixed phase is separated in the cavity 105 of the heat-conducting rotating cylinder 102, a heavy phase is thrown to the inner wall of the heat-conducting rotating cylinder 102 under the action of the centrifugal field, and a light phase is extruded to the center of the heat-conducting rotating cylinder 102, so that the restriction of slow phase separation speed existing between reactants under a conventional gravity field is broken, the phase separation time is effectively shortened, the effect of rapid quenching reaction is achieved, the generation of byproducts is favorably reduced, the difficulty of subsequent processing is reduced, and further the reaction cost is reduced.
It will be appreciated that there is a reaction gap 104 between the outer wall of the thermally conductive drum 102 and the inner wall of the reactor housing 101, and the outer top of the thermally conductive drum 102 abuts the inner top of the reactor housing 101. At this time, when the light phase and the heavy phase are fed through the light phase feed port 107 and the heavy phase feed port 108, respectively, the light phase and the heavy phase are first brought into contact with each other in the reaction gap 104. With the continuous addition of the light phase and the heavy phase, the reaction mixed phase enters the cavity 105 of the heat-conducting drum 102 from the opening 106 at the bottom of the heat-conducting drum 102, and then the mixed phase continuously rises in the cavity 105 of the heat-conducting drum 102, so that the light phase and the heavy phase are discharged from the light phase discharge port 109 and the heavy phase discharge port 1010, respectively. The outer top of the conductive bowl 102 abuts the inner top of the reactor housing 101, and the light and heavy phases do not enter the reaction gap 104 from the cavity 105 of the conductive bowl 102.
In one particular example, an integrated microreactor 100 for liquid-liquid heterogeneous exothermic reactions is suitable for nitration reactions. At this time, the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction is the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction for the nitration reaction, and the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction for the nitration reaction includes all the features of the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction described above.
When the integrated micro-reactor 100 is used for nitration reaction, the initial temperature of the nitration reaction can be effectively ensured without additional temperature increase and decrease intervention, the internal coupling of heat inside a nitration reaction system is realized, and the utilization rate of heat in the nitration reaction process is effectively improved. Meanwhile, the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction can effectively realize the continuous implementation of the nitration reaction, avoid the problem that the product quality is influenced by the overhigh local hot spot in a nitration reaction system, and improve the product quality of the nitration reaction. Further, when the integrated microreactor 100 is used for nitration reaction, the integrated microreactor can effectively reduce the liquid holding rate of a nitration reaction system, greatly reduce the risk of nitration reaction and improve the safety of the nitration reaction process. Furthermore, when the integrated microreactor 100 is used for nitration reaction, the integrated microreactor is beneficial to reducing the generation of byproducts such as polynitrophenol and the like, the difficulty of subsequent process treatment such as alkali washing and the like is reduced, and the reaction cost is further reduced.
It will be appreciated that when used in the nitration reaction, the light phase is the oil phase and the heavy phase is the mixed acid phase. Specifically, the light phase is a benzene/nitrobenzene mixed solution, wherein the volume ratio of benzene to nitrobenzene is 1: 4. The heavy phase is mixed nitric acid and sulfuric acid, wherein the volume ratio of nitric acid to sulfuric acid is 1: 7.
It is to be understood that in some specific examples, the integrated microreactor 100 for liquid-liquid heterogeneous exothermic reactions is also suitable for sulfonation reactions, polymerization reactions, rearrangement reactions, diazotization reactions, and the like.
It is understood that the driving mechanism 103 has a driving shaft 1013, and the driving shaft 1013 is connected to the heat-conducting drum 102 to rotate the heat-conducting drum 102. Further, the heat conductive drum 102 rotates on its axis.
In one specific example, the top of the reactor shell 101 is further provided with a light phase diversion weir 1011 and a heavy phase diversion weir 1012, the light phase diversion weir 1011 is near the light phase outlet 109 for diverting the light phase, and the heavy phase diversion weir 1012 is near the heavy phase outlet 1010 for diverting the heavy phase.
As some parameter examples of the reactor shell 101, the reactor shell 101 has an inner diameter of 0.6cm to 10 cm. For example, the reactor shell 101 can have an internal diameter of, but is not limited to, 0.6cm, 1cm, 1.5cm, 2cm, 2.5cm, 3cm, 3.5cm, 4cm, 4.5cm, 5cm, 5.5cm, 6cm, 6.5cm, 7cm, 7.5cm, 8cm, 8.5cm, 9cm, 9.5cm, or 10cm, etc.
The reactor shell 101 has an internal height of 2cm to 32 cm. For example, the internal height of the reactor shell 101 can be, but is not limited to, 2cm, 3cm, 4cm, 5cm, 8cm, 10cm, 15cm, 18cm, 20cm, 25cm, 30cm, or 32cm, and the like.
The width of the reaction gap 104 is 0.05cm to 1 cm. For example, the width of the reaction gap 104 can be, but is not limited to, 0.05cm, 0.08cm, 0.1cm, 0.2cm, 0.3cm, 0.4cm, 0.5cm, 0.6cm, 0.7cm, 0.8cm, 0.9cm, or 1cm, etc. It is understood that the width of the reaction gap 104 represents the distance between the outer wall of the thermally conductive drum 102 and the inner wall of the reactor housing 101.
In one particular example, the interior of the reactor shell 101 is cylindrical.
As some examples of parameters of the thermally conductive drum 102, the thermally conductive drum 102 has an outer diameter of 0.5cm to 10cm, alternatively, the thermally conductive drum 102 has an outer diameter of 0.5cm, 1cm, 1.5cm, 2cm, 2.5cm, 3cm, 3.5cm, 4cm, 4.5cm, 5cm, 5.5cm, 6cm, 6.5cm, 7cm, 7.5cm, 8cm, 8.5cm, 9cm, 9.5cm, or 10cm, and so forth. It is understood that the outer diameter of the thermally conductive bowl 102 is less than the inner diameter of the reactor shell 101. Further, the difference between the inner diameter of the reactor shell 101 and the outer diameter of the heat conductive drum 102 is the width of the reaction gap 104.
The height of the heat conducting drum 102 is 2cm to 30 cm. Alternatively, the height of the thermally conductive drum 102 is 2cm, 3cm, 4cm, 5cm, 8cm, 10cm, 15cm, 18cm, 20cm, 25cm, or 30cm, etc. It is understood that the height of the thermally conductive bowl 102 is less than the interior height of the reactor housing 101. Further, the difference between the inner height of the reactor housing 101 and the height of the heat conducting drum 102 is the width of the reaction gap 104. It is also understood that the height of the thermally conductive bowl 102 is the exterior height of the thermally conductive bowl 102.
The wall thickness of the heat-conducting rotary drum 102 is 0.1 cm-1 cm; alternatively, the wall thickness of the thermally conductive drum 102 is 0.1cm, 0.2cm, 0.3cm, 0.4cm, 0.5cm, 0.6cm, 0.7cm, 0.8cm, 0.9cm, 1cm, or the like.
The diameter of the opening 106 is 0.05cm to 1.5 cm. Alternatively, the opening 106 has a diameter of 0.05cm, 0.08cm, 0.1cm, 0.2cm, 0.3cm, 0.4cm, 0.5cm, 0.6cm, 0.7cm, 0.8cm, 0.9cm, 1cm, 1.1cm, 1.2cm, 1.3cm, 1.4cm, 1.5cm, or the like.
In one particular example, the exterior and/or interior of the thermally conductive drum 102 is cylindrical.
Referring again to fig. 1, in one specific example, the light phase feed 107 and the heavy phase feed 108 are located in the side wall of the reactor shell 101. Further, the diameter of the light phase feed port 107 is 0.2mm to 6mm, for example, the diameter of the light phase feed port 107 is 0.2cm, 0.3cm, 0.4cm, 0.5cm, 0.8cm, 1cm, 1.5cm, 2cm, 2.5cm, 3cm, 3.5cm, 4cm, 4.5cm, 5cm, 5.5cm, or 6cm, etc. Still further, the diameter of the heavy phase feed port 108 is 0.2mm to 6mm, for example, the diameter of the heavy phase feed port 108 is 0.2cm, 0.3cm, 0.4cm, 0.5cm, 0.8cm, 1cm, 1.5cm, 2cm, 2.5cm, 3cm, 3.5cm, 4cm, 4.5cm, 5cm, 5.5cm, or 6cm, etc. Still further, the light phase feed inlet 107 and/or the heavy phase feed inlet 108 are circular in cross-section.
In one particular example, the angle between the axis of the light phase feed 107 and the axis of the heavy phase feed 108 is between 90 and 180. At this time, the angle between the feeding direction of the light phase and the feeding direction of the heavy phase is 90 to 180 degrees. Further, the included angle between the axis of the light phase feed inlet 107 and the axis of the heavy phase feed inlet 108 may be, but is not limited to, 90 °, 100 °, 105 °, 110 °, 115 °, 120 °, 125 °, 130 °, 135 °, 140 °, 145 °, 150 °, 155 °, 160 °, 165 °, 170 °, 175 °, 180 °, or the like.
In one specific example, the thermally conductive bowl 102 is made of stainless steel and/or hastelloy. The heat conducting rotary drum 102 made of a proper material is selected, so that the heat conductivity coefficient of the heat conducting rotary drum 102 is matched with that of the reaction system, and the utilization rate of heat of the reaction system is improved. It is understood that hastelloy includes nichrome and/or nichrome. Further, the heat conducting drum 102 is a stainless steel heat conducting drum or hastelloy heat conducting drum. Further, the heat conductive drum 102 is a nichrome heat conductive drum or a nichrome heat conductive drum.
Referring again to fig. 1, integrated microreactor 100 for liquid-liquid heterogeneous exothermic reactions further comprises a base 1014, base 1014 being located at the bottom of reactor housing 101 for supporting reactor housing 101.
Referring to fig. 2, the integrated microreactor 100 for liquid-liquid heterogeneous exothermic reaction further includes a light phase storage tank 1015 and a light phase feeding pipe 1016, wherein two ends of the light phase feeding pipe 1016 are respectively connected to the light phase feeding port 107 and the light phase storage tank 1015, and the light phase feeding pipe 1016 is provided with a light phase feeding pump 1017. The light phase in the light phase storage tank 1015 may be transferred to the light phase feed port 107 via the light phase feed pipe 1016 by a light phase feed pump 1017, and then fed into the interior of the reactor shell 101.
Further, the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction further comprises a heavy phase storage tank 1018 and a heavy phase feeding pipe 1019, two ends of the heavy phase feeding pipe 1019 are connected to the heavy phase feeding port 108 and the heavy phase storage tank 1018 respectively, and a heavy phase feeding pump 1020 is disposed on the heavy phase feeding pipe 1019. The heavy phase in the heavy phase storage tank 1018 may be fed by a heavy phase feed pump 1020 through the heavy phase feed pipe 1019 to the heavy phase feed port 108 for feeding the heavy phase into the interior of the reactor shell 101.
Still further, the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction further comprises a light phase receiving tank 1021 and a light phase receiving pipe 1022, wherein two ends of the light phase receiving pipe 1022 are respectively connected to the light phase discharge port 109 and the light phase receiving tank 1021. The light phase discharged from the light phase discharge port 109 is introduced into the light phase receiving tank 1021 through the light phase receiving pipe 1022.
Still further, the integrated microreactor 100 for the liquid-liquid heterogeneous exothermic reaction further comprises a heavy phase material receiving tank 1023 and a heavy phase material receiving pipe 1024, wherein two ends of the heavy phase material receiving pipe 1024 are respectively connected to the heavy phase material outlet 1010 and the heavy phase material receiving tank 1023. The heavy phase discharged from the heavy phase discharge port 1010 is introduced into the heavy phase collection tank 1023 through the heavy phase collection pipe 1024.
Yet another embodiment of the present invention provides a method of using an integrated microreactor 100 for liquid-liquid heterogeneous exothermic reactions. The using method comprises the following steps: the heat conducting rotary drum 102 is driven to rotate by the driving mechanism 103; the light phase reactant is introduced into the reaction gap 104 through the light phase feed inlet 107 and the heavy phase reactant is introduced into the reaction gap 104 through the heavy phase feed inlet 108. In the using method, the light-phase reactant and the heavy-phase reactant are introduced under the condition that the driving mechanism 103 drives the heat-conducting rotary drum 102 to rotate, and the continuous proceeding of reaction and phase separation can be realized along with the addition of the reactants.
In a specific example, the rotation speed of the heat conductive drum 102 is controlled to be 1000rpm to 8000 rpm. The rotation speed of the heat conducting drum 102 is controlled, which is more beneficial to forming a good and stable heat conducting environment, and further improves the utilization rate of heat. Alternatively, the rotation speed of the heat conductive rotary drum 102 is controlled to 1000rpm, 1500rpm, 2000rpm, 2500rpm, 3000rpm, 3500rpm, 4000rpm, 4500rpm, 5000rpm, 5500rpm, 6000rpm, 6500rpm, 7000rpm, 7500rpm, or 8000 rpm.
Further, the feeding speed of the light phase reactant is 0.5mL/min to 15 mL/min. For example, the light phase reactant feed rate is 0.5mL/min, 0.8mL/min, 1mL/min, 2mL/min, 3mL/min, 4mL/min, 5mL/min, 6mL/min, 7mL/min, 8mL/min, 9mL/min, 10mL/min, 11mL/min, 12mL/min, 13mL/min, 14mL/min, or 15 mL/min.
Further, the feeding speed of the heavy phase reactant is 0.1mL/min to 15 mL/min. For example, the feed rate of the heavy phase reactant is 0.1mL/min, 0.3mL/min, 0.5mL/min, 0.8mL/min, 1mL/min, 2mL/min, 3mL/min, 4mL/min, 5mL/min, 6mL/min, 7mL/min, 8mL/min, 9mL/min, 10mL/min, 11mL/min, 12mL/min, 13mL/min, 14mL/min, or 15 mL/min.
In one particular example, the light phase is controlled to enter the reaction gap 104 in a vertical direction, and/or the light phase is controlled to enter the reaction gap 104 in a tangential direction, and/or the heavy phase is controlled to enter the reaction gap 104 in a vertical direction, and/or the heavy phase is controlled to enter the reaction gap 104 in a tangential direction.
The following are specific examples.
Example 1
In the integrated microreactor 100 used in the liquid-liquid heterogeneous exothermic reaction in the present embodiment, the inner diameter of the reactor casing 101 is 0.6 cm. The internal height of the reactor shell 101 was 2 cm. The width of the reaction gap 104 was 0.05 cm. The heat conducting drum 102 is made of nichrome. The outer diameter of the heat conductive drum 102 is 0.5 cm. The height of the heat conductive drum 102 is 2 cm. The wall thickness of the heat conducting drum 102 is 0.1 cm. The opening 106 at the bottom of the heat conducting drum 102 is 0.05 cm. The angle between the axis of the light phase feed port 107 and the axis of the heavy phase feed port 108 was 180 °, the diameter of the light phase feed port 107 was 0.2mm, and the diameter of the heavy phase feed port 108 was 0.2 mm. The light phase is controlled to enter the reaction gap 104 tangentially, and the heavy phase is controlled to enter the reaction gap 104 tangentially.
Example 2
In the integrated microreactor 100 used in the liquid-liquid heterogeneous exothermic reaction in this example, the inner diameter of the reactor casing 101 was 3.5 cm. The internal height of the reactor shell 101 was 6 cm. The width of the reaction gap 104 was 0.5 cm. The material of the heat conducting drum 102 is stainless steel. The outer diameter of the heat conducting drum 102 is 2.5 cm. The height of the heat conducting drum 102 is 6.5 cm. The wall thickness of the heat conducting drum 102 is 0.5 cm. The opening 106 at the bottom of the heat conducting drum 102 is 0.5 cm. The included angle between the axis of the light phase feed port 107 and the axis of the heavy phase feed port 108 was 180 °, the diameter of the light phase feed port 107 was 3mm, and the diameter of the heavy phase feed port 108 was 3 mm. The light phase is controlled to enter the reaction gap 104 in a vertical direction, and the heavy phase is controlled to enter the reaction gap 104 in a vertical direction.
Example 3
A one-piece microreactor 100 for a liquid-liquid heterogeneous exothermic reaction was constructed as shown in fig. 2, wherein the parameters in example 1 were used for the respective parameters. The heat conducting rotary cylinder 102 is driven by the driving mechanism 103 to rotate, the light phase reactant is added into the reaction gap 104 through the light phase feed inlet 107, and the heavy phase reactant is added into the reaction gap 104 through the heavy phase feed inlet 108. The light phase is benzene/nitrobenzene mixed solution, wherein the volume ratio of benzene to nitrobenzene is 1: 4. The heavy phase is mixed nitric acid and sulfuric acid, wherein the volume ratio of nitric acid to sulfuric acid is 1: 7. The feed rate for the light phase was 0.5mL/min and the feed rate for the heavy phase was 0.1 mL/min. After the rotation speed of the heat-conducting rotary drum is 3000rpm and the reaction is stably operated, the benzene content in the reacted light phase is measured by using a gas chromatography, the conversion rate of benzene is more than 99.5 percent through calculation, and the pH value of the light phase is measured to be 6 by using an acid-base titrator.
Example 4
An integrated microreactor 100 for liquid-liquid heterogeneous exothermic reactions as shown in fig. 2 was constructed, wherein the parameters in example 1 were used for the corresponding parameters. The heat conducting rotary cylinder 102 is driven by the driving mechanism 103 to rotate, the light phase reactant is added into the reaction gap 104 through the light phase feed inlet 107, and the heavy phase reactant is added into the reaction gap 104 through the heavy phase feed inlet 108. The light phase is benzene/nitrobenzene mixed solution, wherein the volume ratio of benzene to nitrobenzene is 1: 4. The heavy phase is mixed nitric acid and sulfuric acid, wherein the volume ratio of nitric acid to sulfuric acid is 1: 7. The feed rate for the light phase was 15mL/min and for the heavy phase 15 mL/min. After the rotation speed of the heat-conducting rotary drum is 6000rpm and the reaction is stable, the benzene content in the reacted light phase is measured by using a gas chromatography, the conversion rate of benzene is more than 99.5 percent by calculation, and the pH value of the light phase is 6 by using an acid-base titrator.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the patent of the invention is subject to the appended claims, and the description and the drawings can be used for explaining the contents of the claims.
Claims (10)
1. An integrated microreactor for liquid-liquid heterogeneous exothermic reactions is characterized by comprising a reactor shell, a heat-conducting rotary drum and a driving mechanism;
the heat-conducting rotary drum is connected to the inside of the reactor shell, a reaction gap is formed between the outer wall of the heat-conducting rotary drum and the inner wall of the reactor shell, and the outer top of the heat-conducting rotary drum is abutted against the inner top of the reactor shell; the interior of the heat conduction rotary drum is provided with a cavity, the bottom of the heat conduction rotary drum is provided with an opening, and the opening, the cavity and the reaction gap are communicated;
the reactor shell is provided with a light phase feed inlet, a heavy phase feed inlet, a light phase discharge outlet and a heavy phase discharge outlet; the light phase feed port and the heavy phase feed port are communicated with the reaction gap; the light phase discharge port and the heavy phase discharge port are both arranged at the top of the reactor shell and are both communicated with the cavity, and the light phase discharge port is closer to the central axis of the heat-conducting rotary drum than the heavy phase discharge port;
the driving mechanism is connected with the heat conduction rotary drum and is used for driving the heat conduction rotary drum to rotate.
2. The integrated microreactor for a liquid-liquid heterogeneous exothermic reaction according to claim 1, wherein the top of the reactor housing is further provided with a light phase flow-directing weir adjacent to the light phase outlet for directing the light phase and a heavy phase flow-directing weir adjacent to the heavy phase outlet for directing the heavy phase.
3. The integrated microreactor for a liquid-liquid heterogeneous exothermic reaction according to claim 1, wherein the reactor shell has an inner diameter of 0.6cm to 10 cm; and/or the presence of a gas in the gas,
the internal height of the reactor shell is 2-32 cm; and/or the presence of a gas in the gas,
the width of the reaction gap is 0.05 cm-1 cm.
4. The integrated microreactor for a liquid-liquid heterogeneous exothermic reaction according to claim 1, wherein the thermally conductive rotating drum has an outer diameter of 0.5cm to 10 cm; and/or the presence of a gas in the gas,
the height of the heat conducting rotary drum is 2 cm-30 cm; and/or the presence of a gas in the gas,
the wall thickness of the heat-conducting rotary drum is 0.1 cm-1 cm; and/or the presence of a gas in the atmosphere,
the diameter of the opening is 0.05 cm-1.5 cm.
5. The integrated microreactor for a liquid-liquid heterogeneous exothermic reaction according to claim 1, wherein the light phase feed inlet and the heavy phase feed inlet are both located at a side wall of the reactor shell; and/or the presence of a gas in the gas,
the diameter of the light phase feed inlet is 0.2 mm-6 mm; and/or the presence of a gas in the gas,
the diameter of the heavy phase feed inlet is 0.2 mm-6 mm.
6. An integrated microreactor for a liquid-liquid heterogeneous exothermic reaction according to claim 5, wherein the angle between the axis of the light phase feed inlet and the axis of the heavy phase feed inlet is 90 ° to 180 °.
7. The integrated microreactor for liquid-liquid heterogeneous exothermic reactions according to claim 1, wherein the thermally conductive drum is made of stainless steel and/or hastelloy.
8. The integrated microreactor for the liquid-liquid heterogeneous exothermic reaction according to any one of claims 1 to 7, further comprising a light phase storage tank and a light phase feeding pipe, wherein two ends of the light phase feeding pipe are respectively connected to the light phase feeding port and the light phase storage tank, and a light phase feeding pump is arranged on the light phase feeding pipe; and/or the presence of a gas in the gas,
the device also comprises a heavy phase storage tank and a heavy phase feeding pipe, wherein two ends of the heavy phase feeding pipe are respectively connected with the heavy phase feeding hole and the heavy phase storage tank, and a heavy phase feeding pump is arranged on the heavy phase feeding pipe; and/or the presence of a gas in the gas,
the device also comprises a light phase material receiving tank and a light phase material receiving pipe, wherein two ends of the light phase material receiving pipe are respectively connected with the light phase material outlet and the light phase material receiving tank; and/or the presence of a gas in the gas,
the heavy-phase material receiving tank is connected with the heavy-phase material receiving tank through a heavy-phase material receiving pipe.
9. Use of an integrated microreactor for a liquid-liquid heterogeneous exothermic reaction according to any one of claims 1 to 8, comprising the steps of:
the driving mechanism drives the heat conduction rotary drum to rotate;
and adding a light-phase reactant into the reaction gap through the light-phase feed opening, and adding a heavy-phase reactant into the reaction gap through the heavy-phase feed opening.
10. The method of using an integrated microreactor for a liquid-liquid heterogeneous exothermic reaction according to claim 9, wherein the spinning speed of the thermally conductive rotating drum is 1000rpm to 8000 rpm; and/or the presence of a gas in the gas,
the feeding speed of the light phase reactant is 0.5mL/min to 15 mL/min; and/or the presence of a gas in the gas,
the feeding speed of the heavy phase reactant is 0.1 mL/min-15 mL/min.
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