Device and preparation process for preparing high-purity calcium carbonate

Abstract

The present invention relates to the field of preparation of high-purity calcium carbonate, and particularly to a preparation device and a preparation process for high-purity calcium carbonate. The preparation device includes a refining unit and a carbonization unit. The refining unit sequentially removes impurities such as Mg<supgt;2+< / supgt; and Fe<supgt;2+< / supgt; in the calcium chloride solution through a dissolution tank, a multi-stage mixing tank and a filter. The carbonization unit is provided with a reaction chamber and a reflux chamber, and realizes the circulating filtration of the reaction liquid through a partition plate, a reflux hole and a second filter layer. The mixing nozzle integrates the gas-liquid two-phase atomization function, and combines with an annular gas chamber, a conical cylinder structure and an air flow pump to promote the full mixing and secondary reaction of carbon dioxide and the reaction liquid. At the same time, the circulation pump is used to realize the recycling of the unreacted liquid. The present invention significantly improves the purity, reaction efficiency and resource utilization rate of calcium carbonate preparation through multi-stage filtration and efficient gas-liquid mixing.

Description

Technical Field

[0001] The present invention relates to the field of preparation of high-purity calcium carbonate, and particularly to a preparation device and a preparation process for high-purity calcium carbonate. Background Art

[0002] Calcium carbonate is an important inorganic chemical product, which is widely used in industries such as plastics, papermaking, coatings, rubber, daily chemicals, chemical building materials, adhesives and sealing materials, food, medicine, feed, etc. At present, limestone or calcium chloride is generally used as the raw material for preparing high-purity calcium carbonate. When using limestone as the raw material, the preparation of calcium carbonate through processes such as calcination, digestion, carbonization, separation, and drying has high energy consumption, and there are many impurities in lime milk that are difficult to remove. Therefore, calcium chloride is generally used as the raw material to prepare high-purity calcium carbonate.

[0003] In the process of preparing high-purity calcium carbonate from calcium chloride, carbon dioxide is generally used as the reaction raw material in an environment where ammonia water or calcium oxide is added to achieve the carbonization process. The gas-liquid mixing reaction in the carbonization process is a technical problem in this step. In addition, the sampling method and titration method are usually used to detect the reaction progress, which increases the operation steps and slows down the reaction process. Summary of the Invention

[0004] In order to solve the foregoing technical problems, the present invention provides a preparation device for high-purity calcium carbonate. This device adopts a multi-stage gas-liquid mixing method to achieve full mixing of gas-liquid raw materials, accelerate the reaction progress, and solve the technical problem of gas-liquid mixing reaction. By combining cyclic reaction with real-time monitoring of conductivity to monitor the reaction progress, the problems of cumbersome steps and slow reaction process are solved. Specifically, it is achieved through the following technical solutions.

[0005] A preparation device for high-purity calcium carbonate according to the present invention includes a refining unit and a carbonization unit;

[0006] The refining unit includes a dissolution tank, a first mixing tank, a first filter, a second mixing tank, a second filter, and a third mixing tank connected in series in sequence. Stirrers are provided in the dissolution tank, the first mixing tank, the second mixing tank, and the third mixing tank, and a first filter layer is provided at the outlet of the dissolution tank;

[0007] The carbonization unit includes a carbonization box. The interior of the carbonization box is divided into a reaction chamber and a reflux chamber by a partition plate. A reflux hole communicating the two chambers is provided at the bottom of the partition plate. A second filter layer is provided at the bottom of the reaction chamber, and a conductivity meter is provided on the side wall of the reflux chamber;

[0008] A plurality of baffles are longitudinally provided in the reaction chamber, dividing the top space into several compartments. Air holes are provided in the upper part of the baffles, and a mixing nozzle is installed at the top of each compartment for mixing and atomizing the solution obtained by the refining unit with carbon dioxide gas and reacting.

[0009] Preferably, a liquid flow part is arranged on the side of the reflux chamber. The liquid flow part includes a main liquid inlet pipe, a liquid flow return pipe and a circulation pump. Two ends of the liquid flow return pipe are respectively connected to the bottom of the reflux chamber and the main liquid inlet pipe. The main liquid inlet pipe is communicated with the mixing nozzle through a plurality of liquid inlet branch pipes. The liquid flow return pipe is communicated with the outlet of the third mixing tank through an electromagnetic valve.

[0010] Preferably, an air flow part is arranged at the top of the reaction chamber. The air flow part includes a main air inlet pipe. The main air inlet pipe is communicated with an external carbon dioxide supply pipe through a one-way valve. The main air inlet pipe is fixedly communicated with the reaction chamber and is opposite to the air holes.

[0011] The main air inlet pipe is fixedly communicated with an air inlet branch pipe. The air inlet branch pipe is fixedly communicated with a plurality of shunt pipes. A plurality of the shunt pipes are fixedly communicated with each mixing nozzle one by one.

[0012] One end of the reaction chamber far away from the main air inlet pipe is fixedly communicated with an air flow return pipe. The air flow return pipe is fixedly communicated with the main air inlet pipe. An air flow pump is installed on the air flow return pipe.

[0013] Preferably, the mixing nozzle includes an annular air chamber. The annular air chamber is coaxially fixed with the air inlet branch pipe. The annular air chamber is fixedly communicated with the liquid inlet branch pipe. The annular air chamber is coaxially fixed with a first conical cylinder. A first spray port is formed at the bottom of the first conical cylinder.

[0014] The outside of the annular air chamber is in threaded connection with a sealing nut. A second conical cylinder is rotatably installed on the sealing nut. A second spray port is formed at the bottom of the second conical cylinder. An annular chamber is formed between the second conical cylinder and the first conical cylinder. The annular chamber is communicated with the inside of the annular air chamber through a plurality of air channels.

[0015] Preferably, the air flow pump includes a motor, a fan blade and an annular shell. The fan blade is arranged in the annular shell along the radial direction. The air flow return pipe is connected to the tangential position of the annular shell.

[0016] Preferably, electromagnetic valves are fixedly communicated with the ends of the reaction chamber and the reflux chamber.

[0017] The present invention also provides a preparation process of high-purity calcium carbonate, including the following steps:

[0018] S1. Add calcium chloride medicine and water into a dissolution tank, start a stirrer in the dissolution tank to stir until the calcium chloride medicine is dissolved, and then filter it through a first filter layer and transport it into a first mixing tank.

[0019] S2. Add calcium oxide into the first mixing tank, start the stirrer in the first mixing tank to stir for 10 min to 20 min, and then transport it into a second mixing tank.

[0020] S3. Add hydrogen peroxide solution into the second mixing tank, start the stirrer in the second mixing tank to stir, and transfer it into the third mixing tank after reacting for 10 min to 20 min;

[0021] S4. Add ammonia water into the third mixing tank, start the stirrer in the third mixing tank to stir, and transfer it into the liquid inlet main pipe, and transfer carbon dioxide gas into the gas inlet main pipe;

[0022] S5. When the conductivity of the solution in the reflux chamber no longer changes detected by the conductivity meter, open the solenoid valve at the end face of the reaction chamber, collect the mixture inside the reaction chamber, and obtain the CaCO3 product after dehydration and washing.

[0023] After adopting the above technical solution, the beneficial effects of the present invention are as follows:

[0024] 1. Through the two successive mixing reactions of carbon dioxide gas with the reaction liquid, the present invention accelerates the process of the carbonization reaction.

[0025] 2. By respectively realizing the recycling of gas flow and liquid flow through the gas flow part and the liquid flow part, the present invention enables the reactants to be fully utilized and avoids the waste of reaction raw materials.

[0026] 3. The present invention can centrally collect the calcium carbonate product after the reaction, which is convenient for the subsequent treatment of the product.

[0027] 4. By real-time monitoring of the conductivity, the present invention can timely know the progress of the carbonization reaction and is convenient for the collection of the product. Description of the Drawings

[0028] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0029] Figure 1 It is an installation schematic diagram of a preparation device for high-purity calcium carbonate;

[0030] Figure 2 It is a three-dimensional view of the carbonization unit;

[0031] Figure 3 It is a front sectional view of the carbonization unit;

[0032] Figure 4 It is a longitudinal sectional view of the carbonization unit;

[0033] Figure 5 It is a sectional view of the mixing nozzle;

[0034] Figure 6 It is a partial sectional view of an air flow pump.

[0035] Explanation of reference numerals:

[0036] 100 - Refining unit, 101 - Dissolving tank, 102 - First filter layer, 103 - Stirrer, 104 - First mixing tank, 105 - First filter, 106 - Second mixing tank, 107 - Second filter, 108 - Third mixing tank;

[0037] 200 - Carbonization unit, 201 - Carbonization box, 202 - Partition board, 203 - Reaction chamber, 204 - Reflux chamber, 205 - Reflux hole, 206 - Second filter layer, 207 - Conductivity meter, 208 - Baffle, 209 - Air hole, 210 - Air flow part, 211 - Main air inlet pipe, 212 - Air inlet branch pipe, 213 - Shunt pipe, 214 - Air flow return pipe, 220 - Liquid flow part, 221 - Main liquid inlet pipe, 222 - Liquid inlet branch pipe, 223 - Liquid flow return pipe, 224 - Circulation pump, 230 - Check valve, 240 - Solenoid valve;

[0038] 300 - Mixing nozzle, 301 - Annular air chamber, 302 - First conical cylinder, 303 - First nozzle, 304 - Sealing nut, 305 - Second conical cylinder, 306 - Air duct, 307 - Second nozzle;

[0039] 400 - Air flow pump, 401 - Motor, 402 - Fan blade, 403 - Annular shell. Detailed implementation manners

[0040] The features and exemplary embodiments of various aspects of the present invention will be described in detail below. In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below in combination with the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are only configured to explain the present invention and are not configured to limit the present invention. For those skilled in the art, the present invention can be implemented without some of these specific details. The following description of the embodiments is only to provide a better understanding of the present invention by showing examples of the present invention.

[0041] The orientation terms appearing in the following description are all the directions shown in the figures and do not limit the specific structure of the present invention. In the description of the present invention, it should also be noted that unless otherwise clearly specified and limited, the terms "installation, connection" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection or an integral connection; it can be directly connected or indirectly connected. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0042] An embodiment of the present invention provides a preparation device for high-purity calcium carbonate. Refer to Figures 1 to 4 , the preparation device includes a refining unit 100 and a carbonization unit 200. The refining unit 100 includes a dissolving tank 101, a first mixing tank 104, a first filter 105, a second mixing tank 106, a second filter 107, and a third mixing tank 108 connected in series in sequence.

[0043] Among them, stirrers 103 are respectively installed and configured in the dissolving tank 101, the first mixing tank 104, the second mixing tank 106, and the third mixing tank 108 for stirring and mixing the internal mixtures. A first filter layer 102 is fixedly installed at the outlet position of the dissolving tank 101 for filtering impurities in the mixture in the dissolving tank 101. The first filter 105 and the second filter 107 have the same structure and are respectively used for filtering impurities in the first mixing tank 104 and the second mixing tank 106. The first mixing tank 104 and the first filter 105 are used to remove Mg 2+ in the calcium chloride solution, and the second mixing tank 106 and the second filter 107 are used to remove Fe 2+ in the calcium chloride solution. The third mixing tank 108 is used to add ammonia water to the calcium chloride solution and mix it evenly, laying a foundation for the carbonization process of calcium chloride.

[0044] The carbonization unit 200 includes a carbonization box 201. A reaction chamber 203 and a reflux chamber 204 are provided in the carbonization box 201. A partition plate 202 fixed to the inner wall of the carbonization box 201 is arranged between the reaction chamber 203 and the reflux chamber 204. The partition plate 202 divides the reaction chamber 203 and the reflux chamber 204 into two independent spaces. Solenoid valves 240 are respectively fixedly installed at the ends of the reaction chamber 203 and the reflux chamber 204 for discharging the mixtures in the reaction chamber 203 and the reflux chamber 204 to the outside.

[0045] Refer to Figure 4 , a number of reflux holes 205 are opened at the bottom of the partition plate 202. The reflux holes 205 connect the reaction chamber 203 and the reflux chamber 204. A second filter layer 206 is fixedly installed on the side of the bottom of the reaction chamber 203 close to the partition plate 202, so that when the solution in the reaction chamber 203 circulates to the reflux chamber 204 through the reflux holes 205, it needs to pass through the second filter layer 206, thereby ensuring the purity of the solution entering the reflux chamber 204. A conductivity meter 207 is fixedly installed on the side wall at the bottom of the reflux chamber 204, and the conductivity meter 207 can monitor the conductivity of the solution inside the reflux chamber 204 in real time.

[0046] Inside the reaction chamber 203, a number of baffles 208 are longitudinally and uniformly arranged, dividing the top of the reaction chamber 203 into several compartments. Air holes 209 are opened in the upper part of the baffles 208 to achieve communication between the compartments. A mixing nozzle 300 is fixedly installed at the top of each compartment, and the mixing nozzle 300 is used to achieve sufficient mixing and reaction of the gas-liquid two phases.

[0047] With the above structure of the present invention, the solution prepared by the refining unit 100 and carbon dioxide gas are simultaneously introduced into the mixing nozzle 300. Through the mixing action of the mixing nozzle 300, sufficient mixing reaction of the gas-liquid two phases is achieved. The product after the reaction is collected at the bottom of the reaction chamber 203 and, through the filtering action of the second filter layer 206, the solid product remains in the reaction chamber 203, and the liquid enters the reflux chamber 204 through the reflux hole 205. The conductivity of the liquid is detected in real time by the conductivity meter 207 installed on the side wall of the reflux chamber 204, so as to know the reaction progress of the reactants in the reaction chamber 203.

[0048] As a further explanation of the above embodiment, refer to Figures 2 to 4 , a liquid flow part 220 is installed on the side of the reflux chamber 204. The liquid flow part 220 includes a main liquid inlet pipe 221. The middle part of the main liquid inlet pipe 221 is fixedly communicated with the first end of the liquid flow return pipe 223. A circulation pump 224 is fixedly installed on the liquid flow return pipe 223. The second end of the liquid flow return pipe 223 is fixedly communicated with the bottom of the reflux chamber 204. The side of the main liquid inlet pipe 221 is fixedly communicated with a number of liquid inlet branch pipes 222, and the number of liquid inlet branch pipes 222 is fixedly communicated with each group of mixing nozzles 300 one by one.

[0049] In addition, the liquid flow return pipe 223 is also communicated with the outlet of the third mixing tank 108 through an electromagnetic valve 240, so that the reaction stock solution in the third mixing tank 108 can be transported into the mixing nozzle 300 to participate in the reaction.

[0050] With the above structure, after the gas-liquid mixing reaction is achieved in the mixing nozzle 300, part of the reaction liquid is not completely consumed by the reaction. This part of the reaction liquid is re-collected in the reflux chamber 204 after passing through the filtering action of the second filter layer 206. The reaction liquid in the reflux chamber 204 can be transported along the liquid flow return pipe 223 to the main liquid inlet pipe 221 under the pumping action of the circulation pump 224 and then branched to each mixing nozzle 300, and further gas-liquid mixing reaction is achieved in the mixing nozzle 300.

[0051] With this structure, on the one hand, the full utilization of the reaction liquid is achieved, and on the other hand, through the circulation of the reaction liquid, the solid reaction product can be retained in the reaction chamber 203 for collection.

[0052] In addition, the reaction liquid inside the carbonization chamber 201 can only be replenished by opening the solenoid valve 240 installed on the main liquid inlet pipe 221. Therefore, by monitoring the conductivity of the solution in the reflux chamber 204 in real time and replenishing the reaction liquid in a timely manner, the reaction process and reaction efficiency can be effectively controlled.

[0053] As a further explanation of the above embodiment, refer to Figures 2 to 4 , an air flow part 210 is installed at the top of the reaction chamber 203. The air flow part 210 includes a main air inlet pipe 211. The first end of the main air inlet pipe 211 is connected to an external carbon dioxide supply pipe through a check valve 230, the second end of the main air inlet pipe 211 is fixedly connected to the reaction chamber 203, and the second end of the main air inlet pipe 211 faces the air hole 209.

[0054] The side of the main air inlet pipe 211 is fixedly connected to an air inlet branch pipe 212, the air inlet branch pipe 212 is fixedly connected to a number of shunt pipes 213, and the number of shunt pipes 213 is fixedly connected to each group of mixing nozzles 300 one by one.

[0055] One end of the reaction chamber 203 away from the main air inlet pipe 211 at the top is fixedly connected to the first end of an air flow return pipe 214, the second end of the air flow return pipe 214 is fixedly connected to the side of the main air inlet pipe 211, and an air flow pump 400 is installed on the air flow return pipe 214 to realize the flow of gas from the first end of the air flow return pipe 214 to the second end of the air flow return pipe 214.

[0056] With the above structure in this embodiment, a secondary mixing reaction of carbon dioxide gas and the reaction liquid is realized. First, a part of the carbon dioxide gas is shunted through the main air inlet pipe 211 and enters the inside of the mixing nozzle 300 along the air inlet branch pipe 212 and the shunt pipes 213, mixes and reacts with the reaction liquid, and then the reaction liquid is atomized and sprayed out through the mixing nozzle 300. Another part of the gas enters the inside of the reaction chamber 203 through the main air inlet pipe 211, and successively passes through the air holes 209 formed in a number of baffles 208 and fills the compartments separated by the number of baffles 208, and makes a secondary contact reaction with the atomized reaction liquid. The remaining gas of the reaction is transported to the inside of the main air inlet pipe 211 through the air flow return pipe 214 for recycling.

[0057] In addition, when the air pressure in the reaction chamber 203 decreases, that is, after the carbon dioxide gas is consumed, the check valve 230 installed on the main air inlet pipe 211 is opened under the action of negative pressure, and then carbon dioxide gas is replenished into the reaction chamber 203 to maintain the reaction demand of this carbonization process.

[0058] Through the secondary contact of carbon dioxide gas and the reaction liquid, and the atomization of the reaction liquid, the contact area between the gas and the liquid is effectively increased, thereby accelerating the progress of the reaction.

[0059] As a further explanation of the above embodiment, refer to Figure 5 , the mixing nozzle 300 includes an annular air chamber 301. The inner side of the annular air chamber 301 is coaxially fixed with the intake branch pipe 212, and the outer side of the annular air chamber 301 is fixedly communicated with the liquid intake branch pipe 222. The bottom of the inner side of the annular air chamber 301 is coaxially fixed with a first conical cylinder 302, and a first nozzle 303 is provided at the bottom of the first conical cylinder 302.

[0060] The bottom of the outer side of the annular air chamber 301 is threadedly connected with a sealing nut 304. A second conical cylinder 305 is rotatably installed at the bottom of the sealing nut 304. A second nozzle 307 is provided at the bottom of the second conical cylinder 305. An annular chamber is formed between the second conical cylinder 305 and the first conical cylinder 302, and this conical chamber is communicated with the inside of the annular air chamber 301 through a plurality of air passages 306 provided at the bottom of the annular air chamber 301.

[0061] In the above structure, the reaction liquid enters the annular air chamber 301 through the liquid intake branch pipe 222, and enters the conical chamber between the second conical cylinder 305 and the first conical cylinder 302 through a plurality of air passages 306 at the bottom of the annular air chamber 301. The carbon dioxide gas inside the intake branch pipe 212 enters the conical chamber between the second conical cylinder 305 and the first conical cylinder 302 through the first nozzle 303 to impact and mix the reaction liquid, and is atomized and sprayed outwards through the second nozzle 307.

[0062] In the above process, on the one hand, the first mixing reaction of carbon dioxide and the reaction liquid is carried out before atomization, and after atomization, the reaction liquid is made to fully contact and react with the carbon dioxide gas. At the same time, the atomized reaction liquid enters the compartment at the top of the reaction chamber 203 to further react with the carbon dioxide gas in the compartment, and the reaction is accelerated in this way.

[0063] As a further explanation of the above embodiment, refer to Figure 6 , the air flow pump 400 includes a motor 401. The top of the carbonization box 201 is fixed to the motor 401. The output end of the motor 401 passes through the side of the annular shell 403 and is fixed to a plurality of fan blades 402. The plurality of fan blades 402 are arranged radially in the annular shell 403, and the side of the fan blade 402 is in sealing lap with the inner surface of the annular shell 403. The annular shell 403 is fixed to the air flow return pipe 214, and the air flow return pipe 214 is located at the tangential position of the annular shell 403.

[0064] With the above structure of the present invention, after the motor 401 is started, the fan blades 402 are driven to rotate by its output shaft, so that a pressure difference is formed between the two ends of the air flow return pipe 214, and thus the carbon dioxide gas in the reaction chamber 203 is circulated through the air flow return pipe 214.

[0065] The embodiment of the present invention further provides a preparation process of high-purity calcium carbonate, which uses the preparation device provided in the above embodiment to complete the preparation of high-purity calcium carbonate, and specifically includes the following steps:

[0066] S1. Add industrial calcium chloride and water into the dissolving tank 101, start the agitator 103 in the dissolving tank 101 to stir fully until the calcium chloride is completely dissolved, and prepare a calcium chloride stock solution, which is filtered through the first filter layer 102 and then transported to the first mixing tank 104 through a pipeline equipped with a pump body.

[0067] In this process, water and industrial calcium chloride are fully stirred and mixed by the agitator 103 installed inside the dissolving tank 101 to prepare a calcium chloride stock solution, and impurities in the stock solution are filtered out by the first filter layer 102, laying a foundation for subsequent impurity removal.

[0068] S2, adding calcium oxide into the first mixing tank 104, and fully stirring it with the agitator 103 installed in the first mixing tank 104, reacting for 10 minutes to 20 minutes, and then transporting it into the second mixing tank 106 through the pipeline equipped with the first filter 105.

[0069] Industrial calcium chloride contains more iron and magnesium, so it needs to be refined and impurity-removed to obtain refined calcium chloride solution. Taking advantage of the large difference in the solubility product of Ca(OH)2 and Mg(OH)2, a precipitation conversion reaction is used to achieve the purpose of removing magnesium.

[0070] The reaction principle is as follows:

[0071] Ca(OH)2+Mg 2＋ =Mg(OH)2↓+Ca 2＋

[0072] The equilibrium constant K of this reaction is:

[0073]

[0074] According to the principle of chemical equilibrium shift, when [Ca 2＋ ] / [Mg 2＋ ]<K, the equilibrium shifts to the right, making Mg 2＋ Removed in the form of Mg(OH)2 precipitation, when the solution [Mg 2＋ ]<10 －5 mol / L, requiring [Ca 2＋ ]<[Mg 2 ＋ ]·K=3.50×10 5 .

[0075] It can be seen that when CaO is added to the solution, the [Ca2＋ ]<3.05mol / L, which can ensure that the magnesium precipitation in the solution is relatively complete.

[0076] S3, adding hydrogen peroxide solution into the second mixing tank 106, and fully stirring it by using the stirrer 103 installed in the second mixing tank 106, reacting for 10 minutes to 20 minutes, and then transporting it to the third mixing tank 108 through the pipeline equipped with the second filter 107.

[0077] The main form of iron in calcium chloride solution is Fe 2＋ In the form of Fe 2＋ Oxidized to Fe 3＋ Then it is removed in the form of Fe(OH)3. The reaction principle is as follows:

[0078] H2O2+2Fe(OH)2=2Fe(OH)3↓

[0079] The concentration of H2O2 added to the second mixing tank 106 in this step is 30%, and the amount of Fe 2＋ 1.0 to 1.5 times the theoretical amount.

[0080] S4, adding ammonia water into the third mixing tank 108, and fully stirring by the agitator 103 installed in the third mixing tank 108, so that the ammonia water and the calcium chloride solution are mixed and transported to the liquid inlet main pipe 221 as reactants, and carbon dioxide gas is transported into the gas inlet main pipe 211, so that the two undergo carbonization reaction in the reaction chamber 203 to generate a calcium carbonate product.

[0081] The reaction principle in the above steps is as follows:

[0082] CaCl2+2NH3·H2O+CO2=CaCO3↓+2NH4Cl+H2O

[0083] In this reaction, NH4Cl can act as a catalyst to ensure that the carbonization reaction proceeds rapidly.

[0084] S5. When the conductivity meter 207 detects that the conductivity of the solution in the reflux chamber 204 no longer changes, the solenoid valve 240 at the end face of the reaction chamber 203 is opened to collect the mixture inside the reaction chamber 203, and obtain the CaCO3 product after dehydration and washing.

[0085] When the conductivity of the solution in the centralized reflux chamber 204 no longer changes, it indicates that the carbonization reaction in step S4 has ended. At this time, the mixture collected in the reaction chamber 203 is the remaining CaCO3 product and NH4Cl solution after filtering through the second filter layer 206. Therefore, the final CaCO3 product can be obtained by dehydrating and washing the mixture.

[0086] In accordance with the embodiments of the present invention as described above, these embodiments do not describe all the details in detail, nor do they limit the invention to only the specific embodiments. Obviously, many modifications and variations can be made based on the above description. The present specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can make good use of the present invention and its modified use. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A preparation device for high-purity calcium carbonate, characterized in that: It includes a refining unit (100) and a carbonization unit (200); The refining unit (100) includes a dissolution tank (101), a first mixing tank (104), a first filter (105), a second mixing tank (106), a second filter (107), and a third mixing tank (108) connected in series in sequence. Stirrers (103) are provided in the dissolution tank (101), the first mixing tank (104), the second mixing tank (106), and the third mixing tank (108). A first filter layer (102) is provided at the outlet of the dissolution tank (101); The carbonization unit (200) includes a carbonization box (201). The interior of the carbonization box (201) is separated by a partition plate (202) into a reaction chamber (203) and a reflux chamber (204). A reflux hole (205) communicating the two chambers is provided at the bottom of the partition plate (202). A second filter layer (206) is provided at the bottom of the reaction chamber (203). A conductivity meter (207) is provided on the side wall of the reflux chamber (204); A plurality of baffles (208) are longitudinally provided in the reaction chamber (203), dividing the top space into several compartments. Air holes (209) are provided in the upper part of the baffles (208). A mixing nozzle (300) is installed at the top of each compartment for mixing and atomizing the solution prepared by the refining unit (100) with carbon dioxide gas and reacting; An air flow part (210) is provided at the top of the reaction chamber (203). The air flow part (210) includes an intake main pipe (211). The intake main pipe (211) is connected to an external carbon dioxide supply pipe through a one-way valve (230). The intake main pipe (211) is fixedly connected to the reaction chamber (203) and is directly opposite to the air hole (209); The intake main pipe (211) is fixedly connected to intake branch pipes (212). The intake branch pipes (212) are fixedly connected to a plurality of shunt pipes (213). The plurality of shunt pipes (213) are fixedly connected to each mixing nozzle (300) one by one; One end of the reaction chamber (203) away from the intake main pipe (211) is fixedly connected to an air flow return pipe (214). The air flow return pipe (214) is fixedly connected to the intake main pipe (211). An air flow pump (400) is installed on the air flow return pipe (214).

2. The preparation device for high-purity calcium carbonate according to claim 1, characterized in that: A liquid flow part (220) is provided on the side of the reflux chamber (204). The liquid flow part (220) includes a liquid intake main pipe (221), a liquid flow return pipe (223), and a circulation pump (224). The two ends of the liquid flow return pipe (223) are respectively connected to the bottom of the reflux chamber (204) and the liquid intake main pipe (221). The liquid intake main pipe (221) is communicated with the mixing nozzle (300) through a plurality of liquid intake branch pipes (222). The liquid flow return pipe (223) is communicated with the outlet of the third mixing tank (108) through a solenoid valve (240).

3. The preparation device for high-purity calcium carbonate according to claim 1, characterized in that: The mixing nozzle (300) includes an annular gas chamber (301), which is coaxially fixed to the intake branch pipe (212). The annular gas chamber (301) is fixedly communicated with the liquid inlet branch pipe (222). The annular gas chamber (301) is coaxially fixed to the first conical cylinder (302), and a first nozzle (303) is provided at the bottom of the first conical cylinder (302). The outer side of the annular gas chamber (301) is threadedly connected to a sealing nut (304). A second conical cylinder (305) is rotatably mounted on the sealing nut (304). A second nozzle (307) is provided at the bottom of the second conical cylinder (305). An annular chamber is formed between the second conical cylinder (305) and the first conical cylinder (302), and the annular chamber is communicated with the inside of the annular gas chamber (301) through a plurality of air channels (306).

4. The preparation device of high-purity calcium carbonate according to claim 1, wherein: The air flow pump (400) includes a motor (401), a fan blade (402) and an annular shell (403). The fan blade (402) is arranged radially in the annular shell (403). The air flow return pipe (214) is connected to the tangential position of the annular shell (403).

5. The preparation device of high-purity calcium carbonate according to claim 1, wherein: Solenoid valves (240) are fixedly communicated with the ends of the reaction chamber (203) and the reflux chamber (204).

6. A preparation process of high-purity calcium carbonate, characterized in that: Using the preparation device of high-purity calcium carbonate according to any one of claims 1 to 5 to complete the preparation of high-purity calcium carbonate, including the following steps: S1. Add calcium chloride medicine and water into the dissolution tank (101), start the stirrer (103) in the dissolution tank (101) to stir until the calcium chloride medicine is dissolved, and then filter it through the first filter layer (102) and transport it into the first mixing tank (104). S2. Add calcium oxide into the first mixing tank (104), start the stirrer (103) in the first mixing tank (104) to stir for 10 min to 20 min, and then transport it into the second mixing tank (106). S3. Add hydrogen peroxide solution into the second mixing tank (106), start the stirrer (103) in the second mixing tank (106) to stir, and after reacting for 10 min to 20 min, transport it into the third mixing tank (108). S4. Add ammonia water into the third mixing tank (108), start the stirrer (103) in the third mixing tank (108) to stir, and transport it into the liquid inlet main pipe (221), and transport carbon dioxide gas into the gas inlet main pipe (211). S5. When the conductivity meter (207) detects that the conductivity of the solution in the reflux chamber (204) no longer changes, open the solenoid valve (240) at the end face of the reaction chamber (203), collect the mixture inside the reaction chamber (203), dehydrate and wash it to obtain the CaCO3 product.

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