A micro-reaction device for preparing nano manganese tetraoxide and its use method

Abstract

The present invention discloses a micro-reaction device for preparing nano-manganese tetraoxide and a method for using the device, which relates to the field of micro-reaction and comprises: an upper kettle body; a lower kettle body, which is placed below the upper kettle body and has a placement groove in the middle; a disperser, which is placed in the placement groove; a dispersed phase inlet, which is opened on the side wall of the upper kettle body and is connected to an adjustable air pump to transport the dispersed phase; a dispersed phase channel, which is opened inside the upper kettle body and connects the dispersed phase inlet and the disperser; and a continuous phase channel, which is opened in the lower kettle body, runs through the entire lower kettle body, and has an opening direction perpendicular to the direction of the dispersed phase channel.

Description

Technical Field

[0001] The present invention relates to the field of micro-reactions, and in particular to a micro-reaction device for preparing nano manganese tetraoxide and a use method thereof. Background Art

[0002] There are various methods for preparing Mn3O4. According to the source of raw materials, it can be divided into the following methods: oxidizing or reducing manganese oxide or hydroxide, or oxidizing or reducing manganese salt to produce Mn3O4. Among them, MnSO4 can react with ammonia water to produce Mn(OH)2 precipitate. When the Mn(OH)2 precipitate comes into contact with air, it will undergo an oxidation reaction with O2 in the air to produce Mn3O4.

[0003] However, on the one hand, when solid Mn(OH)2 is oxidized to Mn3O4, it is easy to adhere to and condense each other, causing Mn3O4 to exist in larger particles. The reactant Mn(OH)2 exists in solid form and the reactant O2 exists in liquid form. It is difficult for the two to fully contact each other in a liquid environment, resulting in incomplete reaction. On the other hand, traditional reactors are difficult to achieve continuous production, with high manufacturing costs and low production efficiency.

[0004] Therefore, it is necessary to provide a micro-reaction device for preparing nano-manganese tetraoxide and a method for using the same to solve the problems raised in the above background technology. Summary of the Invention

[0005] To achieve the above objectives, the present invention provides the following technical solutions: a micro-reaction device for preparing nano-manganese tetraoxide and a method for using the same, comprising:

[0006] Upper cauldron body;

[0007] The lower kettle body is placed below the upper kettle body and has a placement groove in the middle;

[0008] a disperser, placed in the placement tank;

[0009] A dispersed phase inlet is provided on the side wall of the upper kettle body and is connected to an adjustable air pump for conveying the dispersed phase;

[0010] a dispersed phase channel, which is provided inside the upper kettle body and communicates with the dispersed phase inlet and the disperser; and

[0011] The continuous phase channel is opened in the lower kettle body, passes through the entire lower kettle body, and the opening direction is perpendicular to the direction of the dispersed phase channel.

[0012] Furthermore, as a preference, a positioning groove is provided on the lower surface of the upper kettle body, and the overall opening trajectory of the positioning groove is parallel to the peripheral trajectory of the lower end surface of the upper kettle body. A rubber ring is also placed in the positioning groove, which, on the one hand, facilitates the positioning of the upper kettle body and the lower kettle body during installation, and on the other hand, can form a closed environment between the upper kettle body and the lower kettle body.

[0013] Furthermore, preferably, a continuous phase inlet and a continuous phase outlet are provided on the outer wall of the lower kettle body corresponding to the continuous phase channel, and the continuous phase inlet is connected to a liquid pump with adjustable flow rate to transport the continuous phase, and the continuous phase outlet is connected to a precipitation and filtration device.

[0014] Furthermore, preferably, a dispersion chamber and a microarray channel are provided inside the disperser, and the dispersion chamber is communicated with the dispersed phase channel, and the microarray channel is communicated with the dispersion chamber and the continuous phase channel.

[0015] Furthermore, as a preference, the disperser can be replaced according to different requirements for the diameter of the microarray channels, and the microarray channels are uniformly distributed at the bottom of the disperser.

[0016] Furthermore, preferably, the cross-sectional diameter of the continuous phase channel is 1 cm, an upper staggered groove is provided at the bottom of the disperser corresponding to the position of the continuous phase channel, the continuous phase channel is cut by the placement groove, and a lower staggered groove is formed correspondingly. The disperser and the lower kettle body are fitted together, and the upper staggered groove and the lower staggered groove form a cross-flow channel.

[0017] Furthermore, preferably, the microarray channel consists of a main channel, a diffusion groove and a delivery hole, the main channel, the diffusion groove and the delivery hole are connected in sequence, and the diffusion grooves are arranged in three groups coaxial with the upper staggered grooves, and the output end of the delivery hole is connected to the continuous phase channel, wherein the diameter of the main channel is 1 mm, and the diameter of the delivery hole ranges from 100 μm to 300 μm.

[0018] Furthermore, preferably, the conveying holes are all opened at an angle and are symmetrically divided into two groups in corresponding directions.

[0019] A method for using a micro-reaction device for preparing nano-manganese tetraoxide comprises the following steps:

[0020] Step 1: Component Installation: Select a suitable disperser 3 according to the specifications of the microarray channel 32, and place the disperser 3 in the placement tank 7. Place the upper kettle body 1 on top of the lower kettle body 2 to complete the fixation. At the same time, the dispersed phase inlet 5 is connected to the air pump, the continuous phase inlet is connected to the liquid pump, and the continuous phase outlet is connected to the precipitation device;

[0021] Step 2: Device adjustment; start the air pump to deliver the dispersed phase, detect the air tightness between the upper kettle body 1 and the lower kettle body 2, and turn off the air pump and readjust it if there is any leakage. Keep the air pump on to prevent the continuous phase from flowing back from the microarray channel 32, then start the liquid pump to deliver the continuous phase to start the reaction, and adjust the flow rate of the air pump and the liquid pump to control the reaction rate;

[0022] Step 3: Precipitation sampling; after the device is stably operated, the product in the precipitation device is dried to obtain the desired manganese tetraoxide.

[0023] Compared with the prior art, the present invention provides a micro-reaction device for preparing nano-manganese tetraoxide and a method for using the same, which has the following beneficial effects:

[0024] 1. The cross-flow channel formed by the upper and lower staggered grooves allows the continuous phase in the continuous phase channel to mix and react with the dispersed phase output from the microarray channel. At the same time, the dispersed phase and the continuous phase are in a circulating state. The cross-flow channel ensures that the entire process continues under normal conditions. Compared with traditional reactors, continuous production can be achieved to effectively reduce manufacturing costs. At the same time, the narrow cross-flow channel ensures sufficient contact between the dispersed phase and the continuous phase, effectively improving reaction efficiency.

[0025] 2. In the present invention, part of the Mn(OH)2 reactant will precipitate at the bottom and will not come into contact with O2, resulting in an incomplete reaction. The delivery holes are all inclined, and when the dispersed phase is delivered into the continuous phase, the continuous phase will be promoted to form a circulation, stirring the continuous phase so that the Mn(OH)2 inside is evenly dispersed. At the same time, multiple groups of delivery holes are distributed at intervals along the axial direction of the cross-flow channel. The whole process ensures that the reactants are fully mixed to ensure that the reaction is complete. At the same time, by replacing dispersers of different specifications, the output of the dispersed phase can be controlled, and the size of the bubbles formed by the dispersed phase in the continuous phase can be indirectly controlled, thereby controlling the length of the unit reaction time to affect the scale of the generated Mn3O4;

[0026] 3. In the present invention, during the reaction process, the dispersed phase is transported into the cross-flow channel through the delivery hole and mixed with the continuous phase. After the dispersed phase and the continuous phase are mixed, they initially exist in the form of bubbles. Spatially, the reaction occurs around a single dispersed phase bubble. In terms of time, from the beginning to the consumption of the limited O2 in the bubble, the entire process of generating Mn3O4 around a single dispersed phase bubble is regarded as a unit reaction. Macroscopically, the entire gas-liquid-solid oxidation reaction is composed of countless unit reactions. The unit reactions are discontinuous, and the continuous phase is stirred by the bubbles, thereby effectively controlling the scale of the generated Mn3O4. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Other features, objects and advantages of the present invention will become more apparent upon reading the detailed description of non-limiting embodiments with reference to the following drawings:

[0028] Figure 1 This is a schematic diagram of the overall structure of a micro-reaction device for preparing nano-manganese tetraoxide and its use method;

[0029] Figure 2 A schematic diagram of a disperser for a micro-reaction device for preparing nano-manganese tetraoxide and a method for using the same;

[0030] Figure 3 A schematic diagram of the working principle of a micro-reaction device for preparing nano-manganese tetraoxide and its use method;

[0031] In the figure: 1. Upper kettle body; 2. Lower kettle body; 3. Disperser; 31. Dispersion chamber; 32. Microarray channel; 321. Main channel; 322. Diffusion groove; 323. Delivery hole; 33. Upper staggered groove; 34. Lower staggered groove; 35. Cross-flow channel; 4. Positioning groove; 5. Dispersed phase inlet; 6. Dispersed phase channel; 7. Placement groove; 8. Continuous phase channel. DETAILED DESCRIPTION

[0032] See also Figure 1-3 In an embodiment of the present invention, a micro-reaction device for preparing nano manganese tetraoxide and a method for using the same include:

[0033] Upper cauldron body 1;

[0034] The lower kettle body 2 is placed below the upper kettle body 1 and has a placement slot 7 in the middle;

[0035] The disperser 3 is placed in the placement tank 7;

[0036] The dispersed phase inlet 5 is provided on the side wall of the upper kettle body 1 and is connected to an adjustable air pump (not shown in the figure) to deliver the dispersed phase;

[0037] a dispersed phase channel 6, which is opened inside the upper kettle body 1 and communicates with the dispersed phase inlet 5 and the disperser 3; and

[0038] The continuous phase channel 8 is opened in the lower kettle body 2 , passes through the entire lower kettle body 2 , and has an opening direction perpendicular to the dispersed phase channel 6 .

[0039] As a preferred embodiment, a positioning groove 4 is provided on the lower surface of the upper kettle body 1, and the overall opening trajectory of the positioning groove 4 is parallel to the peripheral trajectory of the lower end surface of the upper kettle body 1. A rubber ring is also placed in the positioning groove 4. On the one hand, it is convenient for positioning the upper kettle body 1 and the lower kettle body 2 during installation, and on the other hand, a closed environment can be formed between the upper kettle body 1 and the lower kettle body 2.

[0040] As a preferred embodiment, a continuous phase inlet and a continuous phase outlet are provided on the outer wall of the lower kettle body 2 corresponding to the continuous phase channel 8, and the continuous phase inlet is connected to a liquid pump with adjustable flow rate (not shown in the figure) to transport the continuous phase, and the continuous phase outlet is connected to a precipitation and filtration device (not shown in the figure).

[0041] It should be explained that the dispersed phase is air, and the continuous phase is a mixture of MnSO4 and ammonia water. Mn(OH)2 will react in the mixture, and the Mn(OH)2 is insoluble in water and exists in the continuous phase in solid form. After the continuous phase comes into contact with the dispersed phase, the Mn(OH)2 in the continuous phase reacts with the O2 in the air to generate the required Mn3O4. The overall reaction rate can be controlled by controlling the flow rate of the dispersed phase output by the air pump and the flow rate of the continuous phase output by the liquid pump.

[0042] In this embodiment, Figure 2 The disperser 3 has a dispersion chamber 31 and a microarray channel 32 inside, and the dispersion chamber 31 is connected to the dispersed phase channel 6, and the microarray channel 32 is connected to the dispersion chamber 31 and the continuous phase channel 8.

[0043] As a preferred embodiment, the disperser 3 can be replaced according to different requirements for the diameter of the microarray channel 32 , and the microarray channels 32 are evenly distributed at the bottom of the disperser 3 .

[0044] As a preferred embodiment, the cross-sectional diameter of the continuous phase channel 8 is 1 cm, and an upper staggered groove 33 is provided at the bottom of the disperser 3 corresponding to the position of the continuous phase channel 8. The continuous phase channel 8 is cut by the placement groove 7 to form a corresponding lower staggered groove 34. The disperser 3 and the lower kettle body 2 are fitted together, and the upper staggered groove 33 and the lower staggered groove 34 form a cross-flow channel 35.

[0045] It should be explained that the cross-flow channel 35 formed by the upper staggered groove 33 and the lower staggered groove 34 allows the continuous phase to mix and react with the dispersed phase output from the microarray channel 32 in the continuous phase channel 8. At the same time, the dispersed phase and the continuous phase are in a circulation state. The cross-flow channel 35 ensures that the entire process continues under the condition that the reaction proceeds normally. Compared with the traditional reactor, continuous production can be achieved to effectively reduce manufacturing costs. At the same time, the narrow and long cross-flow channel 35 ensures sufficient contact between the dispersed phase and the continuous phase, effectively improving the reaction efficiency.

[0046] As a preferred embodiment, the microarray channel 32 is composed of a main channel 321, a diffusion groove 322 and a delivery hole 323. The main channel 321, the diffusion groove 322 and the delivery hole 323 are connected in sequence, and the diffusion groove 322 is arranged in three groups coaxial with the upper staggered groove 33. The output end of the delivery hole 323 is connected to the continuous phase channel 8, wherein the diameter of the main channel 321 is 1 mm, and the diameter of the delivery hole 323 ranges from 100 μm to 300 μm.

[0047] As a preferred embodiment, the delivery holes 323 are all opened at an angle and are symmetrically divided into two groups in corresponding directions.

[0048] It should be explained that part of the Mn(OH)2 reactant will precipitate at the bottom and will not come into contact with O2, resulting in incomplete reaction. The delivery holes 323 are all opened at an angle. When the dispersed phase is delivered into the continuous phase, the continuous phase will be promoted to form a circulation, stirring the continuous phase so that the Mn(OH)2 inside it is evenly dispersed. At the same time, multiple groups of delivery holes 323 are distributed axially at intervals along the cross-flow channel 35. The whole process ensures that the reactants are fully mixed to ensure that the reaction is complete. At the same time, by replacing dispersers 3 of different specifications, the output of the dispersed phase can be controlled, and the size of the bubbles formed by the dispersed phase in the continuous phase can be indirectly controlled, thereby controlling the length of the unit reaction time to affect the scale of the generated Mn3O4.

[0049] It should be explained that the dispersed phase and the continuous phase contact in the cross-flow channel 35, and the MnSO4 in the continuous phase reacts with ammonia water to form a Mn(OH)2 precipitate. After the dispersed phase contacts the continuous phase, the Mn(OH)2 precipitate contacts O2 to undergo an oxidation reaction to form Mn3O4. When O2 is fully supplied, the solid Mn(OH)2 in the entire reaction is easily attached to and condensed when oxidized to Mn3O4, so that the final required Mn3O4 exists in the form of larger particles. During the reaction, the dispersed phase is transported into the cross-flow channel 35 through the delivery hole 323 and mixed with the continuous phase. After the dispersed phase and the continuous phase are mixed, they initially exist in the form of bubbles. Spatially, the reaction occurs around a single dispersed phase bubble. In terms of time, from the beginning to the consumption of the limited O2 in the bubble, the entire process of generating Mn3O4 around a single dispersed phase bubble is regarded as a unit reaction. Macroscopically, the entire gas-liquid-solid oxidation reaction is composed of countless unit reactions. The unit reactions are discontinuous, and the continuous phase is stirred by the bubbles, thereby effectively controlling the scale of the generated M3O4.

[0050] In this embodiment, Figure 1-3 A method for using a micro-reaction device for preparing nano-manganese tetraoxide comprises the following steps:

[0051] Step 1: Component Installation: Select a suitable disperser 3 according to the specifications of the microarray channel 32, and place the disperser 3 in the placement tank 7. Place the upper kettle body 1 on top of the lower kettle body 2 to complete the fixation. At the same time, the dispersed phase inlet 5 is connected to the air pump, the continuous phase inlet is connected to the liquid pump, and the continuous phase outlet is connected to the precipitation device;

[0052] Step 2: Device adjustment; start the air pump to deliver the dispersed phase, detect the air tightness between the upper kettle body 1 and the lower kettle body 2, and turn off the air pump and readjust it if there is any leakage. Keep the air pump on to prevent the continuous phase from flowing back from the microarray channel 32, then start the liquid pump to deliver the continuous phase to start the reaction, and adjust the flow rate of the air pump and the liquid pump to control the reaction rate;

[0053] Step 3: Precipitation sampling; after the device is stably operated, the product in the precipitation device is dried to obtain the desired manganese tetraoxide.

[0054] The above is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with this technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solutions and inventive concepts of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A micro-reactor for preparing nano-manganese tetraoxide, characterized by: include: Upper cauldron body (1); The lower kettle body (2) is placed below the upper kettle body (1) and has a placement groove (7) in the middle; A disperser (3) is placed in the placement tank (7); A dispersed phase inlet (5) is provided on the side wall of the upper kettle body (1) and is connected to an adjustable air pump for conveying the dispersed phase; A dispersed phase channel (6) is provided inside the upper kettle body (1) and is connected to the dispersed phase inlet (5) and the disperser (3); A continuous phase channel (8) is provided in the lower kettle body (2), penetrates the entire lower kettle body (2), and is provided in a direction perpendicular to the direction of the dispersed phase channel (6); The disperser (3) is provided with a dispersion chamber (31) and a microarray channel (32), wherein the dispersion chamber (31) is connected to the dispersed phase channel (6), and the microarray channel (32) is connected to the dispersion chamber (31) and the continuous phase channel (8); The disperser (3) is replaced according to different requirements for the diameter of the microarray channel (32), and the microarray channel (32) is evenly distributed at the bottom of the disperser (3); The cross-sectional diameter of the continuous phase channel (8) is 1 cm. An upper staggered groove (33) is provided at the bottom of the disperser (3) at a position corresponding to the continuous phase channel (8). The continuous phase channel (8) is cut by the placement groove (7) to form a corresponding lower staggered groove (34). The disperser (3) and the lower kettle body (2) are fitted together, and the upper staggered groove (33) and the lower staggered groove (34) form a cross-flow channel (35). The microarray channel (32) is composed of a main channel (321), a diffusion groove (322) and a delivery hole (323), wherein the main channel (321), the diffusion groove (322) and the delivery hole (323) are sequentially connected, and the diffusion groove (322) is arranged in three groups coaxial with the upper staggered groove (33), and the output end of the delivery hole (323) is connected to the continuous phase channel (8), wherein the diameter of the main channel (321) is 1 mm, and the diameter of the delivery hole (323) ranges from 100 μm to 300 μm; The delivery holes (323) are all opened at an angle and are symmetrically divided into two groups in corresponding directions.

2. The micro-reaction device for preparing nano-manganese tetraoxide according to claim 1, characterized in that: A positioning groove (4) is provided on the lower surface of the upper kettle body (1), and the overall opening trajectory of the positioning groove (4) is parallel to the peripheral trajectory of the lower end surface of the upper kettle body (1). A rubber ring is also arranged in the positioning groove (4), which, on the one hand, facilitates positioning of the upper kettle body (1) and the lower kettle body (2) during installation, and on the other hand, can form a closed environment between the upper kettle body (1) and the lower kettle body (2).

3. The micro-reaction device for preparing nano-manganese tetraoxide according to claim 2, characterized in that: The outer wall of the lower kettle body (2) corresponding to the continuous phase channel (8) is provided with a continuous phase inlet and a continuous phase outlet, and the continuous phase inlet is connected to a liquid pump with adjustable flow rate to transport the continuous phase, and the continuous phase outlet is connected to a precipitation filtering device.

4. A method for using a micro-reactor for preparing nano-manganic manganese tetroxide, comprising: The steps include: Step 1: Component installation; select a suitable disperser (3) according to the specifications of the microarray channel (32), and place the disperser (3) in the placement tank (7), and place the upper kettle body (1) on top of the lower kettle body (2) to complete the fixation. At the same time, the dispersed phase inlet (5) is connected to the air pump, the continuous phase inlet is connected to the liquid pump, and the continuous phase outlet is connected to the precipitation device; Step 2: Device adjustment; start the air pump to deliver the dispersed phase, detect the air tightness between the upper kettle body (1) and the lower kettle body (2), and if there is air leakage, turn off the air pump and readjust and fix it. If there is no air leakage, keep the air pump on to prevent the continuous phase from flowing back from the microarray channel (32), then start the liquid pump to deliver the continuous phase to start the reaction, and adjust the flow rate of the air pump and the liquid pump to control the reaction rate; Step 3: Precipitation sampling; after the device is stably operated, the product in the precipitation device is dried to obtain the desired manganese tetraoxide.

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