Preparation device and preparation process of high-purity calcium carbonate
By using gas-liquid multi-stage mixing and circulating reaction technology in the preparation process of calcium carbonate, combined with real-time conductivity monitoring, the problems of low carbonization reaction efficiency and cumbersome detection steps are solved, and efficient and rapid preparation of high-purity calcium carbonate is achieved.
Patent Information
- Application Number
- CN202510457500.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-14
- Publication Date
- 2025-05-13
- Estimated Expiration
- 2045-04-14
AI Technical Summary
In the preparation of high-purity calcium carbonate, the gas-liquid mixing reaction efficiency during the carbonization process is low, and the steps to detect the reaction progress are cumbersome, which slows down the reaction process.
The multi-stage gas-liquid mixing method is adopted to achieve real-time monitoring and control of the reaction progress through cyclic reactions combined with real-time monitoring of the conductivity. The specific device includes a refining unit and a carbonization unit. The carbonization unit is equipped with a reaction chamber and a reflow chamber. Multi-stage mixing nozzles and conductors are used to achieve full gas-liquid mixing and real-time monitoring of the reaction progress.
The process of carbonization reaction is accelerated, the reaction progress detection steps are simplified, the reaction efficiency and product purity are improved, and the waste of reaction raw materials is avoided.
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Figure CN119971989A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of preparation of high-purity calcium carbonate, and in particular to a preparation device and a preparation process of high-purity calcium carbonate. Background Art
[0002] Calcium carbonate is an important inorganic chemical product, widely used in plastics, papermaking, coatings, rubber, daily chemicals, chemical building materials, adhesives and sealing materials, food, medicine, feed and other industries. At present, the preparation of high-purity calcium carbonate generally uses limestone or calcium chloride as raw materials. The energy consumption of preparing calcium carbonate with limestone as raw material through calcination, digestion, carbonization, separation, drying and other processes is high, and there are many impurities in lime milk that are difficult to remove. Therefore, calcium chloride is generally used as a 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 a reaction raw material to achieve the carbonization process in an environment where ammonia water or calcium oxide is added. The gas-liquid mixing reaction in the carbonization process is a technical difficulty of this step. In addition, sampling and titration methods are usually used to detect the progress of the reaction, which increases the operating steps and slows down the reaction process. Summary of the invention
[0004] In order to solve the above-mentioned technical problems, the present invention provides a preparation device of high-purity calcium carbonate. The equipment adopts a gas-liquid multi-stage mixing method to achieve sufficient mixing of gas and liquid raw materials, accelerate the reaction progress, and solve the technical difficulties of gas-liquid mixing reaction; through the circulation reaction combined with real-time monitoring of conductivity to monitor the reaction progress, the problems of cumbersome steps and slow reaction progress are solved; specifically, it is achieved through the following technical scheme.
[0005] The present invention discloses a high-purity calcium carbonate preparation device, comprising a refining unit and a carbonization unit; The refining unit comprises a dissolving tank, a first mixing tank, a first filter, a second mixing tank, a second filter and a third mixing tank which are connected in series in sequence, wherein the dissolving tank, the first mixing tank, the second mixing tank and the third mixing tank are all provided with a stirrer, and the outlet of the dissolving tank is provided with a first filter layer; The carbonization unit comprises 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 connecting 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; A plurality of baffles are longitudinally arranged in the reaction chamber to divide the top space into a plurality of compartments. Air holes are arranged on the upper part of the baffles. A mixing nozzle is installed on the top of each compartment to mix the solution prepared by the refining unit with the carbon dioxide gas, atomize and react.
[0006] Preferably, a liquid flow part is provided on the side of the reflux chamber, and the liquid flow part includes a liquid inlet main pipe, a liquid flow return pipe and a circulation pump. The two ends of the liquid flow return pipe are respectively connected to the bottom of the reflux chamber and the liquid inlet main pipe. The liquid inlet main pipe is connected to the mixing nozzle through a plurality of liquid inlet branches, and the liquid flow return pipe is connected to the outlet of the third mixing tank through a solenoid valve.
[0007] Preferably, an airflow portion is provided on the top of the reaction chamber, the airflow portion includes an air intake manifold, the air intake manifold is connected to an external carbon dioxide supply pipe through a one-way valve, the air intake manifold is fixedly connected to the reaction chamber and faces the air hole; The intake manifold is fixedly connected to the intake branch pipe, the intake branch pipe is fixedly connected to a plurality of flow dividers, and the plurality of flow dividers are fixedly connected to each mixing nozzle one by one; One end of the reaction chamber away from the air intake main pipe is fixedly connected to the air flow return pipe, the air flow return pipe is fixedly connected to the air intake main pipe, and an air flow pump is installed on the air flow return pipe.
[0008] Preferably, the mixing nozzle comprises an annular air chamber, the annular air chamber is coaxially fixed with the air inlet branch pipe, the annular air chamber is fixedly connected with the liquid inlet branch pipe, the annular air chamber is coaxially fixed with the first conical cylinder, and the bottom of the first conical cylinder is provided with a first nozzle; The outer side of the annular air chamber is threadedly connected to the sealing nut, and a second conical cylinder is rotatably mounted on the sealing nut. A second nozzle is opened at the bottom of the second conical cylinder, and an annular chamber is formed between the second conical cylinder and the first conical cylinder. The annular chamber is connected to the inside of the annular air chamber through a plurality of air passages.
[0009] Preferably, the airflow pump comprises a motor, fan blades and an annular shell, the fan blades are radially arranged in the annular shell, and the airflow return pipe is connected to a tangential position of the annular shell.
[0010] Preferably, ends of the reaction chamber and the reflux chamber are both fixedly connected with solenoid valves.
[0011] The present invention also provides a process for preparing high-purity calcium carbonate, comprising the following steps: S1, adding calcium chloride and water into a dissolving tank, starting the agitator in the dissolving tank to stir until the calcium chloride is dissolved, filtering through the first filter layer and then conveying to the first mixing tank; S2, adding calcium oxide into the first mixing tank, starting the agitator in the first mixing tank and stirring for 10 to 20 minutes, and then transferring to the second mixing tank; S3, adding hydrogen peroxide solution into the second mixing tank, starting the agitator in the second mixing tank for stirring, reacting for 10 minutes to 20 minutes, and then transferring to the third mixing tank; S4, adding ammonia water into the third mixing tank, starting the agitator in the third mixing tank for stirring, and conveying the ammonia water into the liquid inlet main pipe, and conveying carbon dioxide gas into the gas inlet main pipe; S5. When the conductivity meter detects that the conductivity of the solution in the reflux chamber no longer changes, the solenoid valve at the end face of the reaction chamber is opened to collect the mixture inside the reaction chamber, and the CaCO3 product is obtained after dehydration and washing.
[0012] After adopting the above technical solution, the beneficial effects of the present invention are: 1. The present invention accelerates the process of carbonization reaction by mixing carbon dioxide gas with the reaction liquid twice in succession.
[0013] 2. The present invention realizes the recycling of airflow and liquid flow through the airflow part and the liquid flow part respectively, so that the reactants can be fully utilized and the waste of reaction raw materials can be avoided.
[0014] 3. The present invention can centrally collect the calcium carbonate products after the reaction, which is convenient for subsequent processing of the products.
[0015] 4. The present invention can timely know the progress of the carbonization reaction through real-time monitoring of the conductivity, which facilitates the collection of the product. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0017] Figure 1 It is a schematic diagram of the installation of a high-purity calcium carbonate preparation device; Figure 2 is a stereogram of the carbonization unit; Figure 3 is a forward cross-sectional view of the carbonization unit; Figure 4 is a longitudinal cross-sectional view of a carbonization unit; Figure 5 is a cross-sectional view of a mixing nozzle; Figure 6 It is a partial cutaway schematic diagram of the air flow pump.
[0018] Description of reference numerals: 100-refining unit, 101-dissolving tank, 102-first filter layer, 103-agitator, 104-first mixing tank, 105-first filter, 106-second mixing tank, 107-second filter, 108-third mixing tank; 200-carbonization unit, 201-carbonization box, 202-partition plate, 203-reaction chamber, 204-reflux chamber, 205-reflux hole, 206-second filter layer, 207-conductivity meter, 208-baffle, 209-air hole, 210-air flow section, 211-air intake main pipe, 212-air intake branch pipe, 213-dividing pipe, 214-air flow return pipe, 220-liquid flow section, 221-liquid intake main pipe, 222-liquid intake branch pipe, 223-liquid flow return pipe, 224-circulation pump, 230-check valve, 240-solenoid valve; 300 - mixing nozzle, 301 - annular air chamber, 302 - first conical barrel, 303 - first nozzle, 304 - sealing nut, 305 - second conical barrel, 306 - air channel, 307 - second nozzle; 400-air flow pump, 401-motor, 402-fan blades, 403-annular shell. DETAILED DESCRIPTION
[0019] The features and exemplary embodiments of various aspects of the present invention will be described in detail below. In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction 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 the need for some of these specific details. The following description of the embodiments is only to provide a better understanding of the present invention by illustrating examples of the present invention.
[0020] The directional words appearing in the following description are all 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, or a detachable connection or an integral connection; it can be directly connected or indirectly connected. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to the specific circumstances.
[0021] The embodiment of the present invention provides a device for preparing high-purity calcium carbonate. Figure 1 to Figure 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 which are connected in series in sequence.
[0022] Among them, the dissolving tank 101, the first mixing tank 104, the second mixing tank 106 and the third mixing tank 108 are respectively equipped with a stirrer 103 for stirring and mixing the mixtures inside each. The outlet of the dissolving tank 101 is fixedly equipped with a first filter layer 102 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 filtering impurities in the second mixing tank 106. The first mixing tank 104 and the first filter 105 are used to achieve Mg in the calcium chloride solution. 2+ The second mixing tank 106 and the second filter 107 are used to remove Fe in the calcium chloride solution. 2+ The third mixing tank 108 is used to add ammonia water to the calcium chloride solution and mix it well, paving the way for the carbonization process of calcium chloride.
[0023] The carbonization unit 200 includes a carbonization box 201, in which a reaction chamber 203 and a reflux chamber 204 are provided. A partition plate 202 fixed to the inner wall of the carbonization box 201 is provided 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 fixedly installed at the ends of the reaction chamber 203 and the reflux chamber 204, respectively, for discharging the mixture in the reaction chamber 203 and the reflux chamber 204 to the outside.
[0024] See also Figure 4 A plurality of reflux holes 205 are provided at the bottom of the partition plate 202, and the reflux holes 205 connect the reaction chamber 203 and the reflux chamber 204. A second filter layer 206 is fixedly installed at the bottom of the reaction chamber 203 close to the side of 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 be filtered by 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 of 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.
[0025] A plurality of baffles 208 are evenly arranged longitudinally inside the reaction chamber 203 to divide the top of the reaction chamber 203 into a plurality of compartments. An air hole 209 is provided on the upper portion of the baffle 208 to achieve communication between the compartments. A mixing nozzle 300 is fixedly installed on the top of each compartment to achieve sufficient mixing and reaction of the gas-liquid two phases.
[0026] Through the above structure, the present invention simultaneously introduces the solution prepared by the refining unit 100 and the carbon dioxide gas into the mixing nozzle 300, and the mixing action of the mixing nozzle 300 realizes a sufficient mixing reaction of the gas-liquid two phases. The reaction products are collected at the bottom of the reaction chamber 203 and filtered by the second filter layer 206, so that the solid products remain in the reaction chamber 203. 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.
[0027] As a further explanation of the above embodiments, see Figure 2 to Figure 4 A liquid flow portion 220 is installed on the side of the reflux chamber 204, and the liquid flow portion 220 includes a liquid inlet main pipe 221. The middle part of the liquid inlet main pipe 221 is fixedly connected to the first end of the liquid flow return pipe 223. A circulating pump 224 is fixedly installed on the liquid flow return pipe 223. The second end of the liquid flow return pipe 223 is fixedly connected to the bottom of the reflux chamber 204. The side of the liquid inlet main pipe 221 is fixedly connected to a plurality of liquid inlet branch pipes 222, and the plurality of liquid inlet branch pipes 222 are fixedly connected to each group of mixing nozzles 300 one by one.
[0028] In addition, the liquid return pipe 223 is also connected to the outlet of the third mixing tank 108 through the solenoid valve 240, so that the reaction stock solution in the third mixing tank 108 can be transported to the mixing nozzle 300 to participate in the reaction.
[0029] Through the above structure, after the gas-liquid mixing reaction is realized in the mixing nozzle 300, part of the reaction liquid is not completely reacted and consumed, and this part of the reaction liquid is filtered by the second filter layer 206 and then collected again in the reflux chamber 204. The reaction liquid in the reflux chamber 204 can be transported to the liquid inlet main pipe 221 along the liquid flow return pipe 223 under the pumping action of the circulation pump 224 and then diverted to each mixing nozzle 300, and further gas-liquid mixing reaction is realized in the mixing nozzle 300.
[0030] This structure not only realizes full utilization of the reaction liquid, but also enables solid reaction products to be retained in the reaction chamber 203 for collection through the circulation of the reaction liquid.
[0031] In addition, the reaction liquid inside the carbonization box 201 can only be replenished by opening the solenoid valve 240 installed on the liquid inlet main pipe 221. Therefore, by real-time monitoring the conductivity of the solution in the reflux chamber 204 and replenishing the reaction liquid in time, the reaction process and reaction efficiency can be effectively controlled.
[0032] As a further explanation of the above embodiments, see Figure 2 to Figure 4An airflow section 210 is installed on the top of the reaction chamber 203, and the airflow section 210 includes an air intake manifold 211. A first end of the air intake manifold 211 is connected to an external carbon dioxide supply pipe through a one-way valve 230, and a second end of the air intake manifold 211 is fixedly connected to the reaction chamber 203, and the second end of the air intake manifold 211 is directly opposite to the air hole 209.
[0033] The side of the intake manifold 211 is fixedly connected to the intake branch pipe 212 , the intake branch pipe 212 is fixedly connected to a plurality of flow dividers 213 , and the plurality of flow dividers 213 are fixedly connected to each group of mixing nozzles 300 one by one.
[0034] One end of the top of the reaction chamber 203 away from the air intake manifold 211 is fixedly connected to the first end of the air flow return pipe 214, and the second end of the air flow return pipe 214 is fixedly connected to the side of the air intake manifold 211. 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.
[0035] The present embodiment realizes a secondary mixing reaction of carbon dioxide gas and reaction liquid through the above structure. First, a part of carbon dioxide gas is diverted through the intake main pipe 211 and then enters the mixing nozzle 300 along the intake branch pipe 212 and the diverter pipe 213, and after mixing and reacting with the reaction liquid, the reaction liquid is atomized and sprayed out through the mixing nozzle 300. Another part of the gas enters the reaction chamber 203 through the intake main pipe 211, and passes through the air holes 209 opened on the baffles 208 in turn, and then fills the compartments separated by the baffles 208, and undergoes a secondary contact reaction with the atomized reaction liquid. The remaining gas of the reaction is transported to the intake main pipe 211 through the air flow return pipe 214 for recycling.
[0036] In addition, when the gas pressure in the reaction chamber 203 decreases, that is, after the carbon dioxide gas is consumed, the one-way valve 230 installed on the intake manifold 211 opens under the action of negative pressure, thereby replenishing carbon dioxide gas into the reaction chamber 203 to maintain the reaction requirements of the carbonization process.
[0037] Through the secondary contact between 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 reaction.
[0038] As a further explanation of the above embodiments, see 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 air inlet branch 212, the outer side of the annular air chamber 301 is fixedly connected with the liquid inlet branch 222, the inner bottom of the annular air chamber 301 is coaxially fixed with the first conical tube 302, and the bottom of the first conical tube 302 is provided with a first nozzle 303.
[0039] The outer bottom of the annular air chamber 301 is threadedly connected to the sealing nut 304, and 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 the conical chamber is connected to the inside of the annular air chamber 301 through a plurality of air channels 306 opened at the bottom of the annular air chamber 301.
[0040] In the above structure, the reaction liquid enters the annular air chamber 301 through the liquid inlet 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 air inlet 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 outward through the second nozzle 307.
[0041] In the above process, on the one hand, the first mixing reaction of carbon dioxide and reaction liquid is carried out before atomization, and after atomization, the reaction liquid is allowed 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, thereby accelerating the reaction.
[0042] As a further explanation of the above embodiments, see Figure 6 The airflow 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 blades 402. The plurality of blades 402 are radially arranged in the annular shell 403, and the side of the blades 402 is sealed and overlapped with the inner surface of the annular shell 403. The annular shell 403 is fixed to the airflow return pipe 214, and the airflow return pipe 214 is located at a tangential position of the annular shell 403.
[0043] Through the above structure, after the motor 401 is started, the fan blade 402 is driven to rotate through its output shaft, so that a pressure difference is formed between the two ends of the airflow return pipe 214, so that the carbon dioxide gas in the reaction chamber 203 can circulate through the airflow return pipe 214.
[0044] 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: 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.
[0045] 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.
[0046] 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.
[0047] 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.
[0048] The reaction principle is as follows: Ca(OH)2+Mg 2+ =Mg(OH)2↓+Ca 2+ The equilibrium constant K of this reaction is:
[0049] According to the principle of chemical equilibrium shift, when [Ca 2+ ] / [Mg 2+ ]<K, the equilibrium shifts to the right, making the Mg in the solution 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 .
[0050] It can be seen that when CaO is added to the solution, the [Ca 2+ ]<3.05mol / L, which can ensure that the magnesium precipitation in the solution is relatively complete.
[0051] 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.
[0052] 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: H2O2+2Fe(OH)2=2Fe(OH)3↓ 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.
[0053] 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.
[0054] The reaction principle in the above steps is as follows: CaCl2+2NH3·H2O+CO2=CaCO3↓+2NH4Cl+H2O In this reaction, NH4Cl can act as a catalyst to ensure that the carbonization reaction proceeds rapidly.
[0055] 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.
[0056] 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.
[0057] According to 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 the only specific embodiments. Obviously, based on the above description, many modifications and changes can be made. This 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 the modified use based on the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A device for preparing high-purity calcium carbonate, characterized in that: It includes a refining unit (100) and a carbonization unit (200); The refining unit (100) comprises 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) which are sequentially connected in series, wherein the dissolving tank (101), the first mixing tank (104), the second mixing tank (106) and the third mixing tank (108) are each provided with an agitator (103), and the outlet of the dissolving tank (101) is provided with a first filter layer (102); The carbonization unit (200) comprises a carbonization box (201), the interior of the carbonization box (201) being divided into a reaction chamber (203) and a reflux chamber (204) by a partition plate (202), a reflux hole (205) connecting the two chambers being provided at the bottom of the partition plate (202), a second filter layer (206) being provided at the bottom of the reaction chamber (203), and a conductivity meter (207) being provided on the side wall of the reflux chamber (204); A plurality of baffles (208) are longitudinally arranged in the reaction chamber (203) to divide the top space into a plurality of compartments. An air hole (209) is arranged on the top of the baffle (208). A mixing nozzle (300) is installed on the top of each compartment to mix the solution produced by the refining unit (100) with carbon dioxide gas for atomization and reaction.
2. The preparation device of high-purity calcium carbonate according to claim 1, characterized in that: A liquid flow portion (220) is provided on the side of the reflux chamber (204), and the liquid flow portion (220) comprises a liquid inlet main pipe (221), a liquid flow return pipe (223) and a circulation pump (224); two ends of the liquid flow return pipe (223) are respectively connected to the bottom of the reflux chamber (204) and the liquid inlet main pipe (221); the liquid inlet main pipe (221) is connected to the mixing nozzle (300) via a plurality of liquid inlet branch pipes (222); and the liquid flow return pipe (223) is connected to the outlet of the third mixing tank (108) via a solenoid valve (240).
3. The preparation device of high-purity calcium carbonate according to claim 2, characterized in that: An airflow section (210) is provided at the top of the reaction chamber (203), the airflow section (210) comprising an air intake manifold (211), the air intake manifold (211) being connected to an external carbon dioxide supply pipe via a one-way valve (230), the air intake manifold (211) being fixedly connected to the reaction chamber (203) and facing the air hole (209); The intake manifold (211) is fixedly connected to the intake branch pipe (212), the intake branch pipe (212) is fixedly connected to a plurality of flow dividers (213), and the plurality of flow dividers (213) are fixedly connected to the mixing nozzles (300) one by one; One end of the reaction chamber (203) away from the air intake main pipe (211) is fixedly connected to the air flow return pipe (214), the air flow return pipe (214) is fixedly connected to the air intake main pipe (211), and an air flow pump (400) is installed on the air flow return pipe (214).
4. The preparation device of high-purity calcium carbonate according to claim 3, characterized in that: The mixing nozzle (300) comprises an annular air chamber (301), the annular air chamber (301) is coaxially fixed with the air inlet branch pipe (212), the annular air chamber (301) is fixedly connected with the liquid inlet branch pipe (222), the annular air chamber (301) is coaxially fixed with the first conical tube (302), and the bottom of the first conical tube (302) is provided with a first nozzle (303); The outer side of the annular air 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 air chamber (301) through a plurality of air passages (306).
5. The preparation device of high-purity calcium carbonate according to claim 3, characterized in that: The airflow pump (400) comprises a motor (401), a fan blade (402) and an annular shell (403); the fan blade (402) is radially arranged inside the annular shell (403); and the airflow return pipe (214) is connected to a tangential position of the annular shell (403).
6. The preparation device of high-purity calcium carbonate according to claim 1, characterized in that: The ends of the reaction chamber (203) and the reflux chamber (204) are both fixedly connected to a solenoid valve (240).
7. A process for preparing high-purity calcium carbonate, characterized in that: The preparation of high-purity calcium carbonate is completed by using the high-purity calcium carbonate preparation device described in any one of claims 1 to 6, comprising the following steps: S1, adding calcium chloride and water into a dissolving tank (101), starting the agitator (103) in the dissolving tank (101) to stir until the calcium chloride is dissolved, filtering through a first filter layer (102), and then conveying to a first mixing tank (104); S2, adding calcium oxide into the first mixing tank (104), starting the stirrer (103) in the first mixing tank (104) to stir for 10 minutes to 20 minutes, and then transferring the calcium oxide into the second mixing tank (106); S3, adding hydrogen peroxide solution into the second mixing tank (106), starting the agitator (103) in the second mixing tank (106) for stirring, reacting for 10 minutes to 20 minutes, and then transferring the solution into the third mixing tank (108); S4, adding ammonia water into the third mixing tank (108), starting the agitator (103) in the third mixing tank (108) for stirring, and conveying the ammonia water into the liquid inlet main pipe (221), and conveying 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, 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 the CaCO3 product is obtained after dehydration and washing.
Citation Information
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