CN219308688U

CN219308688U - Efficient hydrothermal solvothermal parallel synthesis device

Info

Publication number: CN219308688U
Application number: CN202320183511.6U
Authority: CN
Inventors: 魏宇学; 孙松
Original assignee: Anhui University
Current assignee: Anhui University
Priority date: 2023-02-10
Filing date: 2023-02-10
Publication date: 2023-07-07
Anticipated expiration: 2033-02-10

Abstract

The utility model provides a high-efficiency hydrothermal solvothermal parallel synthesis device which comprises a tube furnace, a multichannel microreactor and a clamping device; the tubular furnace comprises a furnace top, a first pipe wall and a furnace bottom which are sequentially connected from top to bottom, and a semi-closed structure is formed; a first clamping groove is formed in one side of the first pipe wall; one side of the furnace bottom, which is far away from the first clamping groove, is provided with a first connecting bulge, and the top of the first connecting bulge is provided with a connecting column. The utility model can realize flexible disassembly of the multichannel microreactor, improves the research and development speed and is convenient for operators to clean; the utility model creates a stable environment with high temperature and high pressure through the design of the first pipe wall and the second pipe wall, so that the experiment can normally run; the utility model accelerates the synthesis of wet chemistry micro-nano powder materials from research to industrialization, reduces the research and development cost, and has important significance for accelerating the research and development of new materials.

Description

Efficient hydrothermal solvothermal parallel synthesis device

Technical Field

The utility model relates to the technical field of material preparation, in particular to a high-efficiency hydrothermal solvothermal parallel synthesis device.

Background

The low-dimensional combined material chip preparation is broadly classified into high-density membrane morphological sample preparation and multi-channel powder parallel synthesis, not only can meet the high-throughput preparation and screening requirements of most functional materials, but also can provide reference and guidance for high-throughput screening of part of structural materials, becomes a high-throughput experimental technology for supporting material genome research, has wide application prospect in the fields of accelerating new material discovery, existing material modification and high added value emerging equipment, and is an international research and development hot spot field. Aiming at the high-flux preparation technology of the micro-nano powder, the development of a multi-channel parallel synthesis technology has become the industry consensus.

The hydrothermal/solvothermal method is a main means for wet chemical synthesis of micro-nano powder materials at present, but the synthesis period is longer, generally more than one day, and even more than ten days, and because the hydrothermal/solvothermal reaction involves complex physicochemical processes occurring at the surface and interface, the reaction process of the product surface structure and the surface interface is in rapid dynamic change, resulting in high sensitivity of the micro-nano powder materials to the structure, the components and the element proportion. Therefore, a great deal of research effort is consumed in the long-term traditional synthesis process characterized by trial and error, and the innovation speed of the micro-nano powder material is severely restricted. The existing equipment and instruments developed based on the parallel synthesis of micro-nano powder materials have the problems of low flux, uneven product phases, small single micro-reactor volume and the like. In addition, the synthesis technology and experimental conditions applicable to related equipment are very limited, and the requirements of high-flux preparation of powder materials by a hydrothermal/solvothermal method are difficult to meet. Therefore, how to provide a high-flux parallel synthesis technology of a hydrothermal/solvothermal method, which can realize uniform mixing and heating of raw materials with different components, so as to improve the efficiency of the catalyst preparation process, reduce the research and development cost, save the labor force and reduce the waste is a technical problem to be solved by the technicians in the field.

Disclosure of Invention

Based on the technical problems in the background technology, the utility model provides a high-efficiency hydrothermal solvothermal parallel synthesis device, which can realize flexible disassembly of a multi-channel micro-reactor, improves the research and development speed and is convenient for operators to clean; the utility model creates a stable environment with high temperature and high pressure through the design of the first pipe wall and the second pipe wall, so that the experiment can normally run; the utility model accelerates the synthesis of wet chemistry micro-nano powder materials from research to industrialization, reduces the research and development cost, and has important significance for accelerating the research and development of new materials.

In order to achieve the above purpose, the present utility model adopts the following technical scheme:

an efficient hydrothermal solvothermal parallel synthesis device comprises a tube furnace, a multichannel microreactor and a clamping device;

the tubular furnace comprises a furnace top, a first pipe wall and a furnace bottom which are sequentially connected from top to bottom, and a semi-closed structure is formed; a first clamping groove is formed in one side of the first pipe wall; one side of the furnace bottom, which is far away from the first clamping groove, is provided with a first connecting bulge, and the top of the first connecting bulge is provided with a connecting column.

Preferably, the top of the furnace bottom is also provided with a high-heat-conductivity electric heating plate.

Preferably, the multichannel microreactor comprises a reaction kettle and a second pipe wall arranged on the side surface of the reaction kettle, wherein a second connecting protrusion is arranged at the bottom of one side of the second pipe wall, a connecting groove is arranged at the bottom of the position, corresponding to the connecting column, of the second connecting protrusion, and the connecting groove is movably connected with the connecting column; the bottom of one side of the second pipe wall, which is far away from the second connecting protrusion, is provided with a second clamping groove; the first clamping groove is movably connected with the second clamping groove through a clamping device.

More preferably, the clamping device comprises a clamping button, one end of the clamping button is arranged outside the second clamping groove, the other end of the clamping button is connected with a spring, the spring is abutted against the inside of the second clamping groove, a limiting block is arranged in the middle of the clamping device and penetrates through the second clamping groove and stretches into the inside of the first clamping groove, and one side, away from the clamping button, of the limiting block is provided with a limiting protrusion.

More preferably, the reaction kettle is internally provided with a sample groove, the top of the sample groove is provided with a reaction channel, the top of the sample groove is provided with a groove cover, and the bottom of the position of the groove cover corresponding to the reaction channel is provided with a sealing plug.

More preferably, the capacity of the reaction channels is 1-20mL, and the number of the reaction channels is 10-1000 and distributed in an array.

More preferably, the top of the reaction kettle is provided with a kettle cover, the top of the kettle cover is provided with a handle, and the side surface of the handle is provided with a round hole in a penetrating way; the bottom of the kettle cover is provided with a mechanical extrusion male connector, and a mechanical extrusion female connector is arranged above the inner wall of the reaction kettle.

More preferably, the number of the tube furnaces is 2 or more, and the furnace tops and furnace bottoms of the adjacent tube furnaces are connected with each other.

Compared with the prior art, the utility model has the following beneficial effects:

(1) The utility model can realize flexible disassembly of the multichannel micro-reactor, can realize efficient regulation and control of the reaction temperature, is easier to control the reaction, improves the research and development speed, reduces the research and development cost and is convenient for operators to clean.

(2) The utility model can enable the whole synthesis device to be in seamless connection through the design of the first pipe wall and the second pipe wall, and enable the synthesis device to be rapidly and stably opened or closed under the ingenious design of the clamping device, so that the device is flexible and changeable without losing heat, and a stable environment with high temperature and high pressure is created, so that the experiment can normally run.

(3) The utility model has multiple reaction channels, can realize simultaneous reaction of multiple samples and multiple conditions under the setting of the multi-layer reaction furnace, can lead each furnace to have different reaction temperatures, can timely disassemble and exchange the multi-channel microreactors in the tubular furnace with different temperatures according to the needs, further regulate and control the reaction temperatures, is efficient and time-saving, accelerates the synthesis of wet chemistry micro-nano powder materials from research to industrialization, reduces the research and development cost, and has important significance for accelerating the research and development of new materials.

Drawings

FIG. 1 is a schematic structural diagram of a high-efficiency hydrothermal solvothermal parallel synthesis device according to the utility model;

FIG. 2 is a schematic structural view of a tube furnace according to the present utility model;

FIG. 3 is a schematic structural view of a multi-channel microreactor according to the present utility model;

FIG. 4 is a schematic view showing the internal structure of the multi-channel microreactor of the present utility model;

fig. 5 is a schematic structural view of the clamping device of the present utility model.

The reference numerals are as follows: 100. a tube furnace; 110. a furnace roof; 120. a furnace bottom; 121. a high thermal conductivity electric heating plate; 122. a first connection protrusion; 123. a connecting column; 130 a first tube wall; 131. a first clamping groove; 200. a multichannel microreactor; 210. a reaction kettle; 211. mechanically extruding the female joint; 212. a sample tank; 213. a reaction channel; 214. a slot cover; 215. a sealing plug; 216. a kettle cover; 217. mechanically extruding the male connector; 218. a handle; 219. a round hole; 220. a second tube wall; 221. a second clamping groove; 222. a second connection protrusion; 223. a connecting groove; 300. a clamping device; 310. a clamping button; 320. a spring; 330. a limiting block; 331. and a limit protrusion.

Detailed Description

The following description of the embodiments of the present utility model will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are some, but not all embodiments of the utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.

Example 1

As shown in fig. 1, a high-efficiency hydrothermal solvothermal parallel synthesis device comprises a tube furnace 100, a multi-channel microreactor 200 and a clamping device 300;

as shown in fig. 2, the tube furnace 100 comprises a furnace top 110, a first tube wall 130 and a furnace bottom 120 which are sequentially connected from top to bottom, and forms a semi-closed structure; a first clamping groove 131 is formed in one side of the first pipe wall 130; a first connecting protrusion 122 is arranged on one side of the furnace bottom 120 far away from the first clamping groove 131, and a connecting column 123 is arranged on the top of the first connecting protrusion 122.

In this embodiment, a high thermal conductivity electric plate 121 is further disposed on the top of the furnace bottom 120 to heat the reaction kettle.

As shown in fig. 3, in this embodiment, the multi-channel micro-reactor 200 includes a reaction kettle 210 and a second pipe wall 220 disposed on a side surface of the reaction kettle 210, a second connection protrusion 222 is disposed at a bottom of one side of the second pipe wall 220, a connection groove 223 is disposed at a bottom of a position of the second connection protrusion 222 corresponding to the connection column 123, and the connection groove 223 is movably connected with the connection column 123, so that the disassembly and cleaning of the multi-channel micro-reactor 200 can be flexibly implemented. A second clamping groove 221 is formed at the bottom of one side of the second pipe wall 220 away from the second connecting protrusion 222; the first clamping groove 131 and the second clamping groove 221 are movably connected by the clamping device 300. The first pipe wall 130 and the second pipe wall 220 are in seamless connection under the action of the clamping device, so that the synthesizing device does not lose heat, and a stable environment with high temperature and high pressure is created.

As shown in fig. 5, in this embodiment, the clamping device 300 includes a clamping button 310, one end of the clamping button 310 is disposed at the outside of the second clamping groove 221, the other end of the clamping button 310 is connected with a spring 320, the spring 320 abuts against the inside of the second clamping groove 221, a limiting block 330 is disposed in the middle of the clamping device 300, the limiting block 330 penetrates through the second clamping groove 221 and extends into the inside of the first clamping groove 131, and a limiting protrusion 331 is disposed on one side, away from the clamping button 310, of the limiting block 330. When the synthesis device needs to be opened, the clamping button 310 is pressed tightly, the spring 320 is extruded, the limiting block 330 moves inwards, the limiting boss 331 is separated from the first clamping groove 131, then the multi-channel microreactor 200 is rotated, the synthesis device is opened, when the synthesis device needs to be closed, the clamping button 310 is pressed tightly, then the first pipe wall 130 and the second pipe wall 220 are closed, the clamping button 310 is loosened, under the rebound action of the spring 320, the limiting boss 331 is clamped into the first clamping groove 131, the synthesis device is closed, and the synthesis device is efficient and simple.

As shown in fig. 4, in this embodiment, a sample tank 212 is disposed inside the reaction kettle 210, a reaction channel 213 is disposed at the top of the sample tank, a tank cover 214 is disposed at the top of the sample tank, and a sealing plug 215 is disposed at the bottom of a position of the tank cover 214 corresponding to the reaction channel 213. The sealing plugs 215 may be inserted into the corresponding reaction channels 213, respectively, to achieve sealing.

In this embodiment, the capacity of the reaction channels 213 is 10mL, and the number of the reaction channels 213 is 69 and distributed in an array. Can better meet the synthesis requirement of high-flux micro-nano powder materials.

In this embodiment, a kettle cover 216 is disposed on the top of the reaction kettle 210, a handle 218 is disposed on the top of the kettle cover 216, and a round hole 219 is formed on a side surface of the handle 218 in a penetrating manner; the bottom of the kettle cover 216 is provided with a mechanical extrusion male connector 217, and a mechanical extrusion female connector 211 is arranged above the inner wall of the reaction kettle 210. The reaction kettle 210 and the kettle cover 216 are sealed through a mechanical extrusion type male-female joint, so that high-pressure sealing of the micro-volume reaction liquid is realized.

In this embodiment, the number of the tube furnaces 100 is 3, and the furnace roof 110 and the furnace bottom 120 of adjacent tube furnaces 100 are connected to each other. Each tube furnace is set with different temperature, heating is independently controlled, an operator can control the working time of the heating device according to different synthesis conditions, and the multi-channel micro-reactor 200 can be exchanged at any time according to the requirement.

The foregoing is only a preferred embodiment of the present utility model, but the scope of the present utility model is not limited thereto, and any person skilled in the art, who is within the scope of the present utility model, should make equivalent substitutions or modifications according to the technical scheme of the present utility model and the inventive concept thereof, and should be covered by the scope of the present utility model.

Claims

1. The efficient hydrothermal solvothermal parallel synthesis device is characterized by comprising a tube furnace (100), a multi-channel microreactor (200) and a clamping device (300);

the tubular furnace (100) comprises a furnace top (110), a first pipe wall (130) and a furnace bottom (120) which are sequentially connected from top to bottom, and a semi-closed structure is formed; a first clamping groove (131) is formed in one side of the first pipe wall (130); one side of the furnace bottom (120) far away from the first clamping groove (131) is provided with a first connecting bulge (122), and the top of the first connecting bulge (122) is provided with a connecting column (123).

2. The efficient hydrothermal solvothermal parallel synthesis device according to claim 1, wherein a high-thermal-conductivity electric plate (121) is further arranged on the top of the furnace bottom (120).

3. The efficient hydrothermal solvothermal parallel synthesis device according to claim 1, wherein the multichannel microreactor (200) comprises a reaction kettle (210) and a second pipe wall (220) arranged on the side surface of the reaction kettle (210), a second connecting protrusion (222) is arranged at the bottom of one side of the second pipe wall (220), a connecting groove (223) is arranged at the bottom of a position, corresponding to the connecting column (123), of the second connecting protrusion (222), and the connecting groove (223) is movably connected with the connecting column (123); a second clamping groove (221) is formed in the bottom of one side, far away from the second connecting protrusion (222), of the second pipe wall (220); the first clamping groove (131) and the second clamping groove (221) are movably connected through a clamping device (300).

4. A high-efficient hydrothermal solvothermal parallel synthesis device according to claim 3, characterized in that, chucking device (300) includes chucking button (310), the outside of second chucking groove (221) is located to the one end of chucking button (310), and the other end of chucking button (310) is connected with spring (320), spring (320) contradict in the inside of second chucking groove (221), the middle part of chucking device (300) is provided with stopper (330), stopper (330) pass second chucking groove (221) and stretch into the inside of first chucking groove (131), one side that stopper (330) kept away from chucking button (310) is equipped with spacing arch (331).

5. A high-efficiency hydrothermal solvothermal parallel synthesis device according to claim 3, wherein a sample groove (212) is formed in the reaction kettle (210), a reaction channel (213) is formed in the top of the sample groove, a groove cover (214) is arranged on the top of the sample groove, and a sealing plug (215) is arranged at the bottom of a position, corresponding to the reaction channel (213), of the groove cover (214).

6. The efficient hydrothermal solvothermal parallel synthesis device of claim 5, wherein the capacity of the reaction channels (213) is 1-20mL, and the number of the reaction channels (213) is 10-1000 and distributed in an array.

7. The efficient hydrothermal solvothermal parallel synthesis device according to claim 3, wherein a kettle cover (216) is arranged at the top of the reaction kettle (210), a handle (218) is arranged at the top of the kettle cover (216), and round holes (219) are formed in the side surfaces of the handle (218) in a penetrating manner; the bottom of the kettle cover (216) is provided with a mechanical extrusion male connector (217), and a mechanical extrusion female connector (211) is arranged above the inner wall of the reaction kettle (210).

8. A high efficiency hydrothermal solvothermal parallel synthesis apparatus according to any one of claims 1-7, wherein the number of tube furnaces (100) is 2 or more, and the tops (110) and bottoms (120) of adjacent tube furnaces (100) are connected to each other.