A micro-reaction device for preparing nano-ferric phosphate / ferromanganese phosphate and its use method

Abstract

The present invention discloses a micro-reaction device for preparing nano-ferrophosphate / ferromanganese phosphate / ferromanganese phosphate and a method for using the micro-reaction device, comprising: an air compressor, on the right side of which two groups of first brackets, a second bracket and a third bracket are sequentially placed; two groups of storage tanks are symmetrically arranged and respectively fixedly assembled on the two groups of the first brackets; a constant temperature water bath is horizontally fixed directly above the second bracket; a micro-reaction component is fixedly assembled directly above the third bracket, and a collection tank is fixedly connected to the bottom of the micro-reaction component; the air compressor is connected to the two groups of storage tanks through a ventilation pipe, the lower ends of the two groups of storage tanks are each provided with a connecting pipe, and the other ends of the two groups of connecting pipes are connected to the micro-reaction component; the collection tank is externally connected to a centrifugal drying device.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of nano-iron phosphate / ferromanganese phosphate, and in particular to a micro-reaction device for preparing nano-iron phosphate / ferromanganese phosphate and a method for using the micro-reaction device. Background Art

[0002] A microreactor is a three-dimensional structure fabricated from a solid matrix using specialized micromachining techniques for conducting chemical reactions. Microreactors typically have small channel sizes (less than 500 μm in equivalent diameter) and a high diversity of channels through which fluids flow and within which the desired reactions occur. This results in a very large surface area to volume ratio within the microstructured chemical device.

[0003] However, existing microreactors usually only contain microreaction channels of one size. Therefore, in actual preparation, it is usually necessary to shut down the equipment and replace it with a microreactor of a different model to change the microreaction channel, thereby effectively regulating the nucleation and growth of the reaction grains. This method is time-consuming and labor-intensive, and the repeated startup of the equipment greatly affects the preparation efficiency of iron phosphate.

[0004] Therefore, it is necessary to provide a micro-reaction device for preparing nano-ferric phosphate / ferromanganese phosphate to solve the above problems. Summary of the Invention

[0005] To achieve the above objectives, the present invention provides the following technical solution: a micro-reaction device for preparing nano-ferric phosphate / ferromanganese phosphate, comprising:

[0006] The air booster has two sets of first brackets, second brackets, and third brackets placed on the right side in sequence;

[0007] There are two symmetrical groups of storage tanks, which are fixedly assembled on the two groups of the first brackets respectively;

[0008] a constant temperature water bath, fixed horizontally just above the second bracket;

[0009] A micro-reaction assembly is fixedly assembled directly above the third bracket, and a collection tank is fixedly connected to the bottom of the micro-reaction assembly;

[0010] The air compressor is connected to the two groups of storage tanks through a vent pipe. The lower ends of the two groups of storage tanks are provided with a connecting pipe, and the other ends of the two groups of connecting pipes are connected to the micro-reactor assembly;

[0011] The collecting tank is externally connected with a centrifugal drying device.

[0012] Furthermore, preferably, the middle parts of the two groups of connecting pipes are placed in a constant temperature water bath, and a flow controller is coaxially fixed on the connecting pipe between the storage tank and the constant temperature water bath.

[0013] Furthermore, preferably, the micro-reactor assembly includes:

[0014] A micro-reactor housing is fixedly mounted directly above the third bracket;

[0015] A first drive motor is fixedly mounted on the inner portion of the bottom of the micro-reactor housing;

[0016] A limit housing is fixedly assembled on the first drive motor, and a rotating disk is coaxially rotated therein, and the rotating disk is coaxially fixedly assembled on the output shaft of the first drive motor;

[0017] The mechanical arm is coaxially rotatably assembled above the rotating disk, and a clamping claw is fixedly assembled on the upper end of the mechanical arm.

[0018] Furthermore, preferably, eight groups of rectangular grooves are provided on the circumference of the rotating disk, on which microchannel plates are slidably mounted, and a locking assembly is fixedly mounted above each group of microchannel plates.

[0019] Furthermore, preferably, a sliding outlet is provided on the left side of the limiting shell.

[0020] Furthermore, as a preference, a switch valve is embedded in the upper end of the micro-reactor shell, and connecting pipes are fixedly connected to both sides of the switch valve;

[0021] The liquid collecting funnel is fixedly embedded on the inner wall of the bottom of the micro-reactor housing, is coaxial with the lower side of the switch valve, and its lower side is fixed to prevent it from being assembled on the collection tank.

[0022] Furthermore, preferably, the locking assembly includes:

[0023] The sliding sleeve is coaxially slidably assembled on the input pipe above the microchannel plate, and an internal thread is provided on the inner side of the sliding sleeve. An opening and closing column is fixedly provided below the internal thread, and a plurality of discharge holes are provided at the lower end of the opening and closing column.

[0024] The spiral blade is coaxially fixedly assembled on the outer wall of the sliding sleeve.

[0025] Further, preferably, a fourth bracket is fixedly mounted on the microchannel plate, a second drive motor is fixedly mounted on the fourth bracket, a drive roller is fixedly mounted on the output shaft of the second drive motor, and the drive roller is engaged with the spiral blade.

[0026] Furthermore, preferably, the switch valve includes:

[0027] The valve body shell is provided with branch pipes on the upper, lower, left and right sides. The branch pipes on the left and right sides are respectively fixedly equipped with two sets of connecting pipes. A baffle is provided on the upper branch, on which a return spring is fixedly installed. The other end of the return spring is coaxially fixed with a closing plug. The closing plug is placed at the intersection of the four roads of the valve body shell, and a threaded opening is provided on the lower branch.

[0028] A method for using a micro-reaction device for preparing nano-ferric phosphate / ferromanganese phosphate comprises the following steps:

[0029] S1. The raw materials for preparing nano-ferric phosphate / ferromanganese phosphate are injected into two groups of storage tanks;

[0030] S2. Select a suitable microchannel plate according to the preparation requirements, connect it to the switch valve and lock it;

[0031] S3. Adjust the values ​​of the two flow controllers to change the feed rate of the two storage tanks according to the actual situation, and set the appropriate water bath temperature for the constant temperature water bath;

[0032] S4. After the preparations are completed, open the air compressor and the valves of the two storage tanks, so that the two mixtures enter the micro-reactor assembly after being heated in a water bath;

[0033] S5. The two mixed solutions react in the micro-reactor assembly to generate a nanoscale iron phosphate solution, which falls into the collection tank;

[0034] S6. After the liquid in the collection tank is precipitated, it is sent to a centrifugal drying device to finally produce nano-scale iron phosphate powder.

[0035] Compared with the prior art, the present invention provides a micro-reaction device for preparing nano-ferric phosphate / ferromanganese phosphate and a method for using the same, which has the following beneficial effects:

[0036] In the present invention, a storage tank and a flow controller are provided, so that the raw materials for preparing nano-iron phosphate / ferromanganese phosphate are passed into the micro-reactor at a certain flow rate for liquid-liquid precipitation reaction to obtain nano-iron phosphate / ferromanganese phosphate products, and an air compressor is provided to directly press the two solutions into the micro-reactor using air pressure, thereby improving the preparation efficiency and preventing the problem of clogging of the micro-reactor. At the same time, multiple groups of microchannel plates are provided in the micro-reactor, and the micro-reaction units formed by the microchannels inside the microchannel plates effectively regulate the nucleation and growth of the grains, and by switching different microchannel plates To change the diameter of the microchannel, and then prepare iron phosphate / ferromanganese phosphate powders of different nanometer sizes, the device can achieve continuous production and reduce product manufacturing costs compared with traditional reactors. At the same time, the products produced also have the performance advantages of uniform particle size, high crystallinity and regular morphology due to the process intensification effect of the microchannel. In addition, due to the particularity of the locking component and the switch valve, the equipment does not need to shut down other components when replacing the microchannel. After the current microchannel plate is detached, the reset spring will push the closing plug to re-close the switch valve, thereby saving the startup time of the equipment to a certain extent and improving the preparation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 A schematic diagram of the structure of a micro-reaction device for preparing nano-iron phosphate / ferromanganese phosphate;

[0038] Figure 2 This is a schematic diagram of the structure of a micro-reaction component of a micro-reaction device for preparing nano-iron phosphate / ferromanganese phosphate;

[0039] Figure 3 A schematic cross-sectional view of a locking assembly of a micro-reaction device for preparing nano-iron phosphate / ferromanganese phosphate;

[0040] In the figure: 1. air booster; 2. first bracket; 3. storage tank; 4. second bracket; 5. constant temperature water bath; 6. third bracket; 7. micro reaction component; 8. collecting tank; 9. connecting pipe; 10. flow controller; 11. vent pipe; 71. micro reaction housing; 72. first drive motor; 73. limit housing; 74. rotating disk; 75. micro channel plate; 76. robotic arm; 77. locking assembly; 78. switch valve; 79. liquid collecting funnel; 710. clamping claw; 771. sliding sleeve; 772. opening and closing column; 773. spiral blade; 774. fourth bracket; 775. second drive motor; 776. drive roller; 777. discharge hole; 781. valve body housing; 782. return spring; 783. closing plug; 784. threaded mouth. DETAILED DESCRIPTION

[0041] See also Figures 1 to 3 The present invention provides a micro-reaction device for preparing nano-ferric phosphate / ferromanganese phosphate, comprising:

[0042] The air booster 1 has two sets of first brackets 2, second brackets 4 and third brackets 6 placed on its right side in sequence;

[0043] The storage tanks 3 are symmetrically arranged in two groups and are respectively fixedly assembled on the two groups of the first brackets 2;

[0044] A constant temperature water bath 5 is fixed horizontally above the second bracket 4;

[0045] The micro-reactor assembly 7 is fixedly mounted directly above the third bracket 6, and a collecting tank 8 is fixedly connected to the bottom of the micro-reactor assembly 7;

[0046] The air compressor 1 is connected to the two groups of storage tanks 3 through a vent pipe 11. The lower ends of the two groups of storage tanks 3 are provided with a connecting pipe 9, and the other ends of the two groups of connecting pipes 9 are connected to the micro-reactor assembly 7;

[0047] The collecting tank 8 is externally connected to a centrifugal drying device;

[0048] As a preferred embodiment, the two groups of storage tanks 3 are respectively filled with raw materials for preparing nano-ferric phosphate / ferromanganese phosphate, and the air booster 1 uses air pressure to directly press the two solutions into the micro-reaction component, thereby improving the preparation efficiency while preventing the problem of clogging of the micro-reaction component 7. The constant temperature water bath 5 is provided with an adjustable constant temperature module, which can adjust the temperature therein according to actual conditions and maintain a constant temperature during the preparation process.

[0049] Furthermore, the middle parts of the two groups of connecting pipes 9 are placed in the constant temperature water bath 5, and a flow controller 10 is coaxially fixed on the connecting pipe 9 between the storage tank 3 and the constant temperature water bath 5;

[0050] As a preferred embodiment, the two groups of connecting tubes 9 are placed in a constant temperature water bath 5 so that the solution reaches a suitable reaction temperature before entering the micro-reaction component 7, thereby improving the preparation efficiency of iron phosphate / ferromanganese phosphate. The flow controller 10 can allow the two solutions to pass into the micro-reaction equipment at a certain flow rate for liquid-liquid precipitation reaction to obtain nano-iron phosphate / ferromanganese phosphate products, while controlling the reaction speed to prevent blockage and controlling the reaction concentration of the two solutions, thereby improving the reaction efficiency to a certain extent.

[0051] Furthermore, the micro-reaction component 7 includes:

[0052] The micro-reactor housing 71 is fixedly mounted directly above the third bracket 6;

[0053] A first drive motor 72 is fixedly mounted on the inner portion of the bottom of the micro-reactor housing 71;

[0054] The limiting housing 73 is fixedly assembled on the first driving motor 72, and a rotating disk 74 is coaxially rotated therein. The rotating disk 74 is coaxially fixedly assembled on the output shaft of the first driving motor 72;

[0055] The mechanical arm 76 is coaxially rotatably assembled above the rotating disk 74 , and a clamping claw 710 is fixedly assembled on the upper end of the mechanical arm 76 .

[0056] Furthermore, eight groups of rectangular grooves are provided on the circumference of the rotating disk 74, on which microchannel plates 75 are slidably mounted, and a locking assembly 77 is fixedly mounted above each group of microchannel plates 75;

[0057] As a preferred embodiment, the eight groups of microchannel plates 75 are respectively provided with microchannels of different sizes. The microreaction units formed by the microchannels inside the microchannel plates 75 effectively regulate the nucleation and growth of grains, and the diameter of the microchannels is changed by switching different microchannel plates 75, thereby preparing raw material powders of iron phosphate / manganese phosphate of different nanoscales. Compared with traditional reactors, the device can achieve continuous production and reduce product manufacturing costs. At the same time, the products obtained also have the performance advantages of uniform particle size, high crystallinity and regular morphology due to the process strengthening effect of the microchannels.

[0058] Furthermore, a sliding opening is provided on the left side of the limiting shell 73;

[0059] As a preferred embodiment, the limiting shell 73 is used to limit the movement of the microchannel plate 75 to prevent the microchannel plate 75 from sliding out of the rotating disk 74. During implementation, a microchannel plate 75 of appropriate size is selected according to the preparation requirements, and the first drive motor 72 is started to rotate the rotating disk 74 to an appropriate angle so that the required microchannel plate 75 is facing the sliding outlet on the left side of the limiting shell 73. However, after rotating to the specified position, the robotic arm 76 is started, and the clamping claw 710 at its front end clamps the microchannel plate 75. The robotic arm 76 slides it out of the rotating disk 74 and places it directly above the collection tank 8.

[0060] Furthermore, a switch valve 78 is embedded in the upper end of the micro-reactor housing 71, and connecting pipes 9 are fixedly connected to both sides of the switch valve 78;

[0061] The liquid collecting funnel 79 is fixedly embedded on the inner wall of the bottom of the micro-reactor housing 71. It is coaxial with the lower side of the switch valve 78, and its lower side is fixed to prevent it from being assembled on the collection tank 8. The liquid collecting funnel 79 is used to collect the product and send it into the collection tank 8 to prevent it from falling onto the micro-reactor housing 71, which will reduce the production efficiency and cause a certain degree of corrosion to it.

[0062] Furthermore, the locking assembly 77 includes:

[0063] The sliding sleeve 771 is coaxially slidably assembled on the input pipe above the microchannel plate 75, and an internal thread is provided on the inner side thereof, and an opening and closing column 772 is fixedly provided below the internal thread. The lower end of the opening and closing column 772 is provided with multiple discharge holes 777.

[0064] The spiral blade 773 is coaxially fixedly assembled on the outer wall of the sliding sleeve 771.

[0065] Furthermore, a fourth bracket 774 is fixedly mounted on the microchannel plate 75, a second drive motor 775 is fixedly mounted on the fourth bracket 774, a drive roller 776 is fixedly mounted on the output shaft of the second drive motor 775, and the drive roller 776 is kept in mesh with the spiral blade 773;

[0066] As a preferred embodiment, when the second driving motor 775 is started, the driving roller 776 rotates synchronously, and the spiral blade 773 engaged therewith drives the sliding sleeve 771 to spirally rise.

[0067] Furthermore, the switch valve 78 includes:

[0068] The valve housing 781 is provided with branch pipes on the top, bottom, left and right sides. Two sets of connecting pipes 9 are fixedly installed on the branch pipes on the left and right sides respectively. A baffle is provided on the upper branch, on which a return spring 782 is fixedly installed. The other end of the return spring 782 is coaxially fixedly installed with a closing plug 783. The closing plug 783 is placed at the intersection of the four roads of the valve housing 781. A threaded opening 784 is provided on the lower branch.

[0069] As a preferred embodiment, the pitches of the spiral blade 773, the threaded opening 784 and the sliding sleeve 771 are equal, and the return spring 782 provides a part of the elastic force to keep the closing plug 783 tangent to the intersection of the four branches, while preventing the liquid in the branches on both sides from flowing out, so that the switch valve 78 is in a closed state. When the robot arm 76 places the microchannel plate 75 at the specified position, it will drive the microchannel plate 75 to move upward while keeping it coaxial with the collection tank 8 until the upper end of the opening and closing column 772 is tangent to the closing plug 783. At this time, the robot arm 76 remains fixed, and the lower end plane of the threaded opening 784 coincides with the upper end plane of the sliding sleeve 771. The second drive motor 775 is started to drive the roller 776 to rotate synchronously and keep it engaged. The spiral blade 773 will drive the sliding sleeve 771 to spiral upward, and the threaded port 784 will engage with the sliding sleeve 771, locking the switch valve 78 and the microchannel plate 75 while ensuring the airtightness of the connection to prevent liquid leakage. At the same time, the opening and closing column 772 pushes the closing plug 783 upward to compress the reset spring 782 and move upward to open the switch valve 78. The two liquids can then enter the microchannel plate 75 to prepare phosphoric acid / ferromanganese phosphate. Due to the particularity of the locking component 77 and the switch valve 78, the equipment does not need to shut down other components when replacing the microchannel. After the current microchannel plate 75 is detached, the reset spring 782 will push the closing plug 783 to close the switch valve 78 again, thereby saving the startup time of the equipment to a certain extent and improving the preparation efficiency.

[0070] A method for using a micro-reaction device for preparing nano-ferric phosphate / ferromanganese phosphate comprises the following steps:

[0071] S1. The raw materials for preparing nano-ferric phosphate / ferromanganese phosphate are injected into two groups of storage tanks 3;

[0072] S2. Select a suitable microchannel plate 75 according to the preparation requirements, connect it to the switch valve 78 and lock it;

[0073] S3. According to the actual situation, adjust the values ​​of the two flow controllers 10 to change the feed rate of the two storage tanks 3, and set the appropriate water bath temperature to the constant temperature water bath 5;

[0074] S4. After the preparations are completed, open the air booster 1 and the valve ports of the two storage tanks 3, so that the two mixtures enter the micro-reaction assembly 7 after being heated in a water bath;

[0075] S5. The two mixed solutions react in the micro-reaction assembly 7 to generate a nanoscale iron phosphate solution, which falls into the collection tank 8;

[0076] S6. After the liquid in the collection tank 8 is precipitated, it is sent to a centrifugal drying device to finally produce nano-scale iron phosphate powder.

[0077] 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-ferric phosphate / ferromanganese phosphate, characterized by: include: An air booster (1), on the right side of which two groups of first brackets (2), second brackets (4) and third brackets (6) are sequentially placed; The material storage tanks (3) are symmetrically arranged in two groups and are respectively fixedly assembled on the two groups of the first brackets (2); A constant temperature water bath (5) is fixed horizontally just above the second bracket (4); A micro-reaction component (7) is fixedly mounted directly above the third bracket (6), and a collection tank (8) is fixedly connected to the bottom of the micro-reaction component (7); The air compressor (1) is connected to the two groups of storage tanks (3) via a vent pipe (11); the lower ends of the two groups of storage tanks (3) are both provided with a connecting pipe (9), and the other ends of the two groups of connecting pipes (9) are connected to the micro-reaction component (7); The collecting tank (8) is externally connected to a centrifugal drying device; The micro-reaction component (7) comprises: A micro-reactor housing (71) is fixedly mounted directly above the third bracket (6); A first driving motor (72) is fixedly mounted on the inside of the bottom of the micro-reactor housing (71); A limiting shell (73) is fixedly assembled on the first driving motor (72), and a rotating disk (74) is coaxially rotated therein, and the rotating disk (74) is coaxially fixedly assembled on the output shaft of the first driving motor (72); A mechanical arm (76) is coaxially rotatably mounted above the rotating disk (74), and a clamping claw (710) is fixedly mounted on the upper end of the mechanical arm (76); The rotating disk (74) is provided with eight groups of rectangular grooves on its circumference, each of which is slidably mounted with a microchannel plate (75), and a locking assembly (77) is fixedly mounted above each group of the microchannel plates (75); The locking assembly (77) comprises: A sliding sleeve (771) is coaxially slidably assembled on the input pipe above the microchannel plate (75), and an internal thread is provided on the inner side of the sliding sleeve. An opening and closing column (772) is fixedly provided below the internal thread, and a plurality of discharge holes (777) are provided at the lower end of the opening and closing column (772); The spiral blade (773) is coaxially fixedly assembled on the outer wall of the sliding sleeve (771); A fourth bracket (774) is fixedly mounted on the microchannel plate (75), a second drive motor (775) is fixedly mounted on the fourth bracket (774), a drive roller (776) is fixedly mounted on the output shaft of the second drive motor (775), and the drive roller (776) is kept in mesh with the spiral blade (773).

2. The micro-reactor for preparing nano-ferric phosphate / ferromanganese phosphate according to claim 1, characterized in that: The middle parts of the two groups of connecting pipes (9) are placed in a constant temperature water bath (5), and a flow controller (10) is coaxially fixed on the connecting pipe (9) between the storage tank (3) and the constant temperature water bath (5).

3. The micro-reactor for preparing nano-ferric phosphate / ferromanganese phosphate according to claim 1, characterized in that: The left side of the limiting shell (73) is provided with a sliding outlet.

4. The micro-reactor for preparing nano-ferric phosphate / ferromanganese phosphate according to claim 1, characterized in that: A switch valve (78) is embedded in the upper end of the micro-reactor housing (71), and connecting pipes (9) are fixedly connected to both sides of the switch valve (78); The liquid collecting funnel (79) is fixedly embedded on the inner wall of the bottom of the micro-reactor housing (71), is coaxial with the lower side of the switch valve (78), and its lower side is fixed to prevent it from being assembled on the collection tank (8).

5. The micro-reactor for preparing nano-ferric phosphate / ferromanganese phosphate according to claim 4, characterized in that: The switch valve (78) comprises: The valve body shell (781) is provided with branch pipes on the upper, lower, left and right sides. The branch pipes on the left and right sides are respectively fixedly equipped with two sets of connecting pipes (9). A baffle is provided on the upper branch, on which a return spring (782) is fixedly installed. The other end of the return spring (782) is coaxially fixedly equipped with a closing plug (783). The closing plug (783) is placed at the intersection of the four roads of the valve body shell (781). A threaded opening (784) is provided on the lower branch.

6. A method for using a micro-reactor for preparing nano-ferric phosphate / ferromanganese phosphate, comprising: The following steps are involved: S1. The raw materials for preparing nano-ferric phosphate / ferromanganese phosphate are injected into two groups of storage tanks (3); S2. Select a suitable microchannel plate (75) according to the preparation requirements, connect it to the switch valve (78) and lock it; S3. According to the actual situation, adjust the values ​​of the two flow controllers (10) to change the feed rate of the two storage tanks (3), and set the appropriate water bath temperature to the constant temperature water bath (5); S4. After the preparations are completed, open the air compressor (1) and the valves of the two storage tanks (3), so that the two mixed solutions enter the micro-reaction assembly (7) after being heated in a water bath; S5. The two mixed solutions react in the micro-reactor assembly (7) to generate a nanoscale iron phosphate solution, which falls into the collection tank (8); S6. After the liquid in the collection tank (8) is precipitated, it is sent to a centrifugal drying device to finally produce nano-scale iron phosphate powder.

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