A laboratory experimental device for rapidly preparing nano calcium carbonate

Abstract

The utility model discloses a kind of experimental apparatus for rapidly preparing nanometer calcium carbonate in laboratory, including carbonization jar, sealing cover, sliding assembly, microporous gas-permeable membrane and temperature control assembly;Carbonization jar is equipped with carbon dioxide ventilation pipe;Sealing cover is matched with carbonization jar;Sealing cover is equipped with telescopic link;Telescopic link top end is connected with sealing cover, bottom end is connected with carbonization jar;Sliding assembly is located at sealing cover bottom end;Microporous gas-permeable membrane is connected with sealing cover by sliding assembly;Temperature control assembly includes heating module, temperature sensor and controller;Heating module is located in carbonization jar;Temperature sensor is located in carbonization jar inside one side;Controller is located in carbonization jar outside one side;The utility model increases the contact area with carbon dioxide gas by spraying reaction liquid on microporous gas-permeable membrane, ensures that carbon dioxide gas and calcium hydroxide fully occur carbonization reaction, overall reaction efficiency is high, temperature control assembly can accurately regulate temperature, ensure that reaction condition is stable while facilitating drying operation.

Description

Technical Field

[0001] This utility model relates to the field of calcium carbonate preparation technology, specifically to an experimental apparatus for the rapid preparation of nano-calcium carbonate in the laboratory. Background Technology

[0002] Nano-calcium carbonate is an important new inorganic salt product synthesized from inorganic non-metallic mineral limestone. Due to its small particle size, large specific surface area, and high surface activity, it is widely used in plastics, rubber, papermaking, coatings, inks, and other fields. Preparation methods include physical and chemical methods, with the chemical method being the mainstream method in industrial production. The physical method involves mechanically crushing natural limestone and chalk with high calcium carbonate content to prepare nano-calcium carbonate, which is relatively expensive. The chemical method mainly includes carbonation and metathesis methods. Carbonation is the primary method for preparing nano-calcium carbonate. Carbonation utilizes the reaction of calcium hydroxide (lime milk) with carbon dioxide to generate calcium carbonate. The contact method between carbon dioxide and calcium hydroxide suspension during carbonation is crucial. Carbonation can be further divided into intermittent bubbling carbonation, continuous spray carbonation, hypergravity carbonation, and non-freezing methods. The metathesis method prepares nano-calcium carbonate by reacting water-soluble calcium salts (such as calcium chloride) with water-soluble carbonates (such as ammonium carbonate or sodium carbonate).

[0003] Traditional laboratory preparation of nano-calcium carbonate using carbonation requires the use of calcium hydroxide slurry in a carbonation tank, resulting in high raw material consumption and a lengthy carbonation process. This not only reduces experimental efficiency but also increases costs. Furthermore, the carbonized product requires processing steps such as filtration, washing, and drying, involving numerous pieces of equipment and cumbersome procedures, further increasing the complexity and workload of the experiment. In the development of multiple formulations, repeated operations are necessary, leading to a large overall workload and low efficiency. Utility Model Content

[0004] The purpose of this invention is to provide a laboratory apparatus for the rapid preparation of nano-calcium carbonate with high reaction efficiency, precise temperature control, and simple operation steps. This apparatus aims to solve the technical problems of low reaction efficiency, numerous and complex operating devices, and large repetitive workload in the development of experiments for preparing nano-calcium carbonate using traditional carbonation methods with multiple formulations, which result in long experimental cycles.

[0005] To solve the above technical problems, the solution adopted by this utility model is as follows: An experimental apparatus for the rapid preparation of nano-calcium carbonate in the laboratory includes a carbonization vessel. The carbonization vessel comprises a sealing lid, a sliding assembly, a microporous breathable membrane, and a temperature control assembly. A carbon dioxide vent pipe is provided at one end of the carbonization vessel. The sealing lid is fitted to the carbonization vessel. The sealing lid is equipped with a telescopic rod. The top end of the telescopic rod is connected to the sealing lid, and the bottom end is connected to the carbonization vessel. The sliding assembly is installed at the bottom end of the sealing lid. The microporous breathable membrane is connected to the sealing lid via the sliding assembly. The temperature control assembly includes a heating module, a temperature sensor, and a controller. The heating module is located on both the front and rear sides of the bottom end of the carbonization vessel. The temperature sensor is fixedly installed on one side of the carbonization vessel. The controller is fixedly installed on the outside of the carbonization vessel and electrically connected to the heating module, the temperature sensor, and the telescopic rod. The entire device is powered by an external power source, and the controller is a PLC. The temperature inside the carbonization tank is adjustable, ranging from 5 to 110°C. The microporous breathable membrane is a functional material with a unique microporous structure; its micropore diameter is typically between a few nanometers and a few micrometers, allowing gas and water vapor to pass through while effectively blocking liquid water and solid particles. The heating module is an electric heater, and the entire system is powered by an external power source.

[0006] In use, prepare a calcium hydroxide solution of the required concentration, add 1%~10% of a modifier to emulsify it into a reaction solution, turn on the heating module inside the carbonization tank, adjust the temperature inside the carbonization tank, and wait for the temperature to stabilize. Then, use the controller to extend the telescopic rod, opening the sealing cover. Remove the microporous breathable membrane from the sliding assembly, spray the reaction solution onto the top of the microporous breathable membrane, ensuring the surface of the membrane is completely covered by the reaction solution, and place it back into the sliding assembly. Close the sealing cover using the telescopic rod, and connect the carbon dioxide gas generator externally through the carbon dioxide vent pipe. Carbon dioxide gas is introduced into a sealed carbonization tank for carbonization reaction. After the carbonization reaction is completed, the reaction product calcium carbonate is dried at high temperature. The overall carbonization reaction and drying process takes 10-20 minutes. The carbon dioxide gas source is then turned off and the gas supply is stopped to ensure that the carbon dioxide gas fully reacts with the calcium hydroxide on the breathable membrane to generate calcium carbonate. After the gas in the equipment is completely discharged, the sealing cover is opened through the telescopic rod, the microporous breathable membrane is taken out, and the product on the breathable membrane is gently scraped off and collected in a drying container for subsequent processing or analysis.

[0007] Furthermore, the sliding assembly includes several crossbars and slide rails; the slide rails are located on both sides of the bottom end of the sealing cap; the two ends of the crossbars are slidably connected to the slide rails; the microporous breathable membrane is connected to the sealing cap via the crossbars and slide rails. The two ends of the crossbars are slidably connected to the slide rails, and the microporous breathable membrane is connected to the sealing cap via the crossbars and slide rails. The microporous breathable membrane is suspended on several crossbars, and by adjusting the crossbars, the microporous breathable membrane can be adjusted to a suitable position to ensure sufficient contact between carbon dioxide and the reaction liquid, thereby improving the overall reaction efficiency of the experiment.

[0008] Furthermore, the carbonization tank is equipped with a circulation system; the circulation system consists of two circulating fans, diagonally installed at the left and right ends of the bottom of the carbonization tank. The airflow generated by the rotating fans at the two corners of the bottom of the carbonization tank circulates the carbon dioxide gas and the heat generated by the heating module within the carbonization tank, ensuring uniform temperature and thorough mixing of carbon dioxide with the reaction liquid, thereby improving the efficiency of the carbonization reaction and reducing the drying time of the reaction products.

[0009] Furthermore, a drying layer is provided at the bottom of the carbonization tank; the inner side of the drying layer is filled with a desiccant. The desiccant's hygroscopic properties adsorb the moisture generated by the evaporation of calcium carbonate during the drying process, maintaining a dry environment inside the tank and ensuring the smooth progress of the carbonization reaction.

[0010] Furthermore, the temperature control component includes a refrigeration module and a connecting pipe. The connecting pipe is located within the interlayer on both the front and rear sides of the carbonization tank. The refrigeration module is located outside the carbonization tank and connected to it via the connecting pipe. The connecting pipe acts as an evaporator in the refrigeration system. The refrigeration module also includes a compressor, a condenser, and a throttling valve. After absorbing heat from the object being cooled within the connecting pipe in the interlayer of the carbonization tank, the refrigerant vaporizes into low-temperature, low-pressure steam. This steam is then drawn into the compressor and compressed into high-pressure, high-temperature steam before being discharged into the condenser. In the condenser, the refrigerant releases heat to the cooling medium and condenses into a high-pressure liquid. This liquid is then throttled by the throttling valve into low-pressure, low-temperature refrigerant before re-entering the connecting pipe to absorb heat and vaporize, achieving a cyclic refrigeration process. The refrigerant flows within the connecting pipe in the interlayer of the carbonization tank, exchanging heat with the material inside the tank. If cooling of the carbonization tank is required, the refrigeration module can be controlled by a controller to cool the tank. This allows for convenient temperature adjustment, accelerating carbonization efficiency and facilitating subsequent heating for drying.

[0011] Furthermore, a vent hole is provided in the middle of the bottom of the carbonization tank; an exhaust hole is provided in the sealing cover. The exhaust hole on the sealing cover and the vent hole in the middle of the bottom of the carbonization tank can be used to discharge excess carbon dioxide gas in the carbonization tank, maintain the pressure balance inside the tank, and prevent the pressure inside the carbonization tank from becoming too high.

[0012] The working principle of this utility model is as follows: In use, place this experimental apparatus in a laboratory fume hood. Prepare a calcium hydroxide solution of the required concentration, add 1%~10% of a modifier to emulsify it into a reaction solution, turn on the internal circulating fan and electric heater of the carbonization tank, and adjust the internal temperature of the carbonization tank. Once the temperature stabilizes, use the controller to extend the telescopic rod, opening the sealing cover. Remove the microporous breathable membrane from the sliding component's crossbar, spray the reaction solution onto the microporous breathable membrane, ensuring the surface of the membrane is completely covered by the reaction solution, and place it back into the sliding component's crossbar. Adjust the position of the crossbar on the slide rail to position the microporous breathable membrane appropriately. Then, use the telescopic rod to close the sealing cover and allow carbon dioxide to ventilate. The carbon dioxide gas generator is connected to the outside of the pipe. Carbon dioxide gas is introduced into the sealed carbonization tank for carbonization reaction. After the carbonization reaction is completed, the reaction product calcium carbonate is dried at high temperature. The carbon dioxide gas source is then turned off, allowing the carbon dioxide gas and the heat generated by the heating module to circulate in the carbonization tank. This ensures that the carbon dioxide gas fully reacts with the calcium hydroxide on the breathable membrane to produce calcium carbonate. After the gas in the equipment is completely discharged, the sealing cover is opened by the telescopic rod, the microporous breathable membrane is removed, and the product on the breathable membrane is gently scraped off and collected in a drying container. When it is necessary to cool down the carbonization tank, the evaporator can be controlled by the controller to cool down the carbonization tank.

[0013] The beneficial effects of this utility model are as follows: 1. This utility model sprays the reaction liquid onto a microporous breathable membrane, ensuring that carbon dioxide gas fully reacts with calcium hydroxide on the breathable membrane curtain to form a carbonization reaction, which significantly improves the overall reaction efficiency. The temperature control component can precisely regulate the temperature, ensuring stable reaction conditions while facilitating drying operations. Overall, it realizes rapid carbonization and modification control in the preparation process of nano-calcium carbonate.

[0014] 2. This utility model uses a circulating fan to circulate the carbon dioxide introduced into the carbonization tank and the heat generated by the heating module, which can further improve the reaction uniformity and drying speed, accelerate the carbonization efficiency and drying speed. The vent and exhaust port can effectively maintain the pressure balance inside the tank and ensure the safe operation of the equipment. The position of the microporous vent membrane can be adjusted by the sliding component to ensure that the reaction liquid and carbon dioxide are in full contact, thereby improving the carbonization reaction speed. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the main structure of this utility model; Figure 2 This is a front view cross-sectional structural diagram of the present invention; Figure 3 This is a side view sectional structural diagram of the present invention; Figure 4This is a schematic diagram of the connection structure between the carbonization tank and the sealing cap of this utility model.

[0016] In the diagram: 1. Carbonization tank; 11. Carbon dioxide vent pipe; 12. Drying layer; 13. Connecting pipe; 2. Sealing cover; 21. Telescopic rod; 3. Sliding assembly; 31. Crossbar; 32. Slide rail; 4. Microporous breathable membrane; 5. Circulation system; 6. Temperature control assembly; 61. Refrigeration module; 62. Heating module; 63. Temperature sensor; 64. Controller. Detailed Implementation

[0017] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0018] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings and are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model; the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. In addition, unless otherwise explicitly specified and limited, the terms "installed," "connected," and "linked" should be interpreted broadly. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be a connection within two components. For those skilled in the art, the specific meaning of the above terms in this utility model can be understood according to the specific circumstances.

[0019] The following is a detailed description of the laboratory apparatus for the rapid preparation of nano-calcium carbonate according to the present invention, with reference to the accompanying drawings: Example 1: An experimental apparatus for the rapid preparation of nano-calcium carbonate in the laboratory, comprising a carbonization vessel 1, wherein the carbonization vessel 1 includes a sealing lid 2, a sliding assembly 3, a microporous breathable membrane 4, and a temperature control assembly 6; one end of the carbonization vessel 1 is provided with a carbon dioxide vent pipe 11; the sealing lid 2 is matched with the carbonization vessel 1; the sealing lid 2 is provided with a telescopic rod 21; the top end of the telescopic rod 21 is connected to the sealing lid 2, and the bottom end is connected to the carbonization vessel 1; the sliding assembly 3 is installed at the bottom end of the sealing lid 2; the microporous breathable membrane 4 is connected to the sealing lid 2 through the sliding assembly 3; The temperature control component 6 includes a heating module 62, a temperature sensor 63, and a controller 64; the heating module 62 is located on the front and rear sides of the bottom of the carbonization tank 1; the temperature sensor 63 is fixedly installed on one side of the carbonization tank 1; the controller 64 is fixedly installed on the outside of the carbonization tank 1 and is electrically connected to the heating module 62, the temperature sensor 63, and the telescopic rod 21.

[0020] The working principle of this embodiment is as follows: In use, prepare a calcium hydroxide solution of the required concentration, add 2% modifier to emulsify into a reaction solution, turn on the internal circulation system 5 and heating module 62 of carbonization tank 1, adjust the temperature inside carbonization tank 1, and wait for the temperature to stabilize. Control the extension rod 21 to extend via controller 64, which will open the sealing cover 2. Remove the microporous breathable membrane 4 from the sliding assembly 3, spray the reaction solution onto the microporous breathable membrane 4, ensuring that the surface of the microporous breathable membrane 4 is completely covered by the reaction solution, and put it back into the sliding assembly 3. Control the sealing cover 2 to close via extension rod 21, and allow the carbon dioxide to pass through. Carbon dioxide gas is generated by connecting the carbonation vent pipe 11 to a carbon dioxide gas generator. Carbon dioxide gas is introduced into the sealed carbonation tank 1 for carbonation reaction. After the carbonation reaction is completed, the reaction product calcium carbonate is dried at high temperature. The overall carbonation reaction and drying process takes 15 minutes. The carbon dioxide gas source is then turned off to ensure that the carbon dioxide gas fully reacts with the calcium hydroxide on the microporous breathable membrane 4 to generate calcium carbonate. After the gas in the equipment is completely discharged, the sealing cover 2 is opened by the telescopic rod 21, the microporous breathable membrane 4 is taken out, and the product on the breathable membrane is gently scraped off and collected in a drying container.

[0021] Example 2: The difference from Example 1 is that the sliding assembly 3 includes several crossbars 31 and slide rails 32; the slide rails 32 are opened on both sides of the bottom end of the sealing cover 2; the two ends of the crossbars 31 are slidably connected to the slide rails 32; the microporous breathable membrane 4 is connected to the sealing cover 2 through the crossbars 31 and slide rails 32; the carbonization tank 1 is provided with a circulation system 5; the circulation system 5 consists of two circulating fans, diagonally installed on the left and right ends of the bottom inside the carbonization tank 1; the bottom of the carbonization tank 1 is provided with a drying layer 12; the inner side of the drying layer 12 is filled with desiccant; the temperature control assembly 6 is provided with a cooling module 61 and a connecting pipe 13; the connecting pipe 13 is located in the interlayer on the front and rear sides of the carbonization tank 1; the cooling module 61 is located outside the carbonization tank 1 and is connected to the carbonization tank 1 through the connecting pipe 13; a vent is opened in the middle of the bottom end of the carbonization tank 1; and an exhaust hole is opened in the sealing cover 2.

[0022] The two ends of the crossbar 31 are slidably connected to the slide rail 32. The microporous breathable membrane 4 is connected to the sealing cover 2 through the crossbar 31 and the slide rail 32. The microporous breathable membrane 4 is suspended on several crossbars 31. By adjusting the crossbars 31, the microporous breathable membrane 4 can be adjusted to a suitable position. The rotating fan generates airflow, which makes the carbon dioxide gas in the carbonization tank 1 and the heat generated by the heating module 62 circulate in the carbonization tank 1, ensuring uniform temperature and full mixing of carbon dioxide with the reaction liquid. The hygroscopic properties of the desiccant in the drying layer 12 can adsorb the moisture generated by the evaporation of calcium carbonate during the drying process. The refrigeration module and the connecting pipe work together to cool down the carbonization tank 1. The electric heater converts electrical energy into heat energy to heat the inside of the tank. The overall temperature is easy to adjust, which accelerates the carbonization efficiency and facilitates subsequent heating for drying. The exhaust hole on the sealing cover 2 and the vent hole in the middle of the bottom of the carbonization tank 1 can be used to discharge excess carbon dioxide gas in the carbonization tank 1, maintain the pressure balance inside the tank, and prevent the pressure inside the carbonization tank 1 from being too high.

[0023] The working principle of this embodiment is the same as that of Embodiment 1.

[0024] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. An experimental apparatus for the rapid preparation of nano-calcium carbonate in the laboratory, comprising a carbonization vessel (1), characterized in that: The carbonization tank (1) includes a sealing cover (2), a sliding assembly (3), a microporous breathable membrane (4), and a temperature control assembly (6); one end of the carbonization tank (1) is provided with a carbon dioxide vent pipe (11); the sealing cover (2) is matched with the carbonization tank (1); the sealing cover (2) is provided with a telescopic rod (21); the top end of the telescopic rod (21) is connected to the sealing cover (2), and the bottom end is connected to the carbonization tank (1); the sliding assembly (3) is installed at the bottom end of the sealing cover (2); the microporous breathable membrane (4) is connected to the sealing cover (2) through the sliding assembly (3); The temperature control component (6) includes a heating module (62), a temperature sensor (63), and a controller (64); the heating module (62) is located on the front and rear sides of the bottom of the carbonization tank (1); the temperature sensor (63) is fixedly installed on one side of the carbonization tank (1); the controller (64) is fixedly installed on the outside of the carbonization tank (1) and is electrically connected to the heating module (62), the temperature sensor (63), and the telescopic rod (21).

2. The experimental device for rapidly preparing nano calcium carbonate in a laboratory according to claim 1, characterized in that: The sliding assembly (3) includes several crossbars (31) and slide rails (32); the slide rails (32) are opened on both sides of the bottom end of the sealing cover (2); the two ends of the crossbars (31) are slidably connected to the slide rails (32); the microporous breathable membrane (4) is connected to the sealing cover (2) through the crossbars (31) and the slide rails (32).

3. The experimental apparatus for rapid preparation of nano-calcium carbonate in the laboratory according to claim 1, characterized in that: The carbonization tank (1) is equipped with a circulation system (5); the circulation system (5) consists of two circulating fans, which are installed diagonally at the bottom left and right ends inside the carbonization tank (1).

4. The experimental device for rapidly preparing nano-sized calcium carbonate in a laboratory according to claim 1, characterized in that: The carbonization tank (1) has a drying layer (12) at the bottom inside; the drying layer (12) is filled with a desiccant.

5. The experimental device for rapidly preparing nano-sized calcium carbonate in a laboratory according to claim 1, characterized in that: The temperature control component (6) is provided with a refrigeration module (61) and a connecting pipe (13); the connecting pipe (13) is located in the interlayer on the front and rear sides of the carbonization tank (1); the refrigeration module (61) is located outside the carbonization tank (1) and is connected to the carbonization tank (1) through the connecting pipe (13).

6. The experimental device for rapidly preparing nano-sized calcium carbonate in a laboratory according to claim 1, characterized in that: The carbonization tank (1) has a vent hole at the bottom center; the sealing cover (2) has an exhaust hole.

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