A device and method for preparing nano-calcium by integrating atomization reaction and microwave treatment

Abstract

The application discloses a device and a method for preparing nano calcium by atomizing reaction / microwave processing integration, and the device comprises a reaction device, a flange and a vacuum device; one side of the reaction device is provided with a nitrogen storage cavity; the reaction device mainly comprises a microwave module, a circulating module A, an electrostatic adsorption module and a circulating module B which are sequentially connected through the flange; the microwave module, the circulating module A, the electrostatic adsorption module and the circulating module B are all internally provided with airflow nozzles and atomizing nozzles; the nitrogen storage cavity is connected with the airflow nozzles; the vacuum device is connected with one circulating module A; the other circulating module B is provided with a pressure relief device; the calcium source and the carbon source are circulated and reacted in the circular ring-shaped reaction device which is connected by the microwave module, the circulating module and the electrostatic adsorption module, so that nano calcium carbonate is formed; the microwave is used to accelerate the reaction and carry out drying and adsorption; the overall structure is simple, the operation is convenient, and the speed of the reaction can be conveniently controlled.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of chemical material preparation, in particular to a device and method for preparing nano calcium through atomization reaction / microwave treatment integration. BACKGROUND

[0002] Nano calcium carbonate, also known as ultra-fine calcium carbonate, is a new type of ultra-fine solid powder material developed in the 1980s, with a particle size of 0.01-0.1 μm. Due to the ultra-fining of nano calcium carbonate particles, the crystal structure and surface electron structure change, producing quantum size effect, small size effect, surface effect and macroscopic quantum effect that ordinary calcium carbonate does not have. It is widely used in rubber, plastics, papermaking, chemical building materials, ink, paint, sealant and adhesive industries, etc., which can improve product quality, reduce product production cost, and thus improve market competitiveness.

[0003] Currently, the main methods for synthesizing nano calcium carbonate include carbonization method, double decomposition method, jacketed reaction kettle method, emulsion method and electrochemical in-situ carbonization. The main synthesis methods are carbonization method and double decomposition method. Carbonization method has wide raw material sources and is cheap, and can react at low temperature and in aqueous environment, with simple equipment. Double decomposition method can produce excellent products with high purity and good whiteness.

[0004] Carbonization method is a common method for chemically preparing nano calcium carbonate. High-quality limestone is used as raw material, and calcium oxide and kiln gas containing carbon dioxide are obtained by calcination. Calcium oxide is mixed with water in a certain proportion to perform digestion reaction to generate calcium hydroxide suspension, then the kiln gas after purification treatment is introduced, carbonation reaction (carbonization) is performed to generate calcium carbonate precipitate, and nano calcium carbonate product is obtained after dehydration, drying and crushing. The existing carbonization method includes intermittent bubbling carbonization method, intermittent stirring carbonization method, continuous spraying carbonization method and supergravity carbonization method, etc.

[0005] Double decomposition method mainly utilizes the reaction of water-soluble calcium salt and water-soluble carbonate under appropriate process conditions, and the nano calcium carbonate product is prepared by this liquid-solid phase reaction. By controlling the concentration, temperature, feeding rate of reactants, supersaturation of product calcium carbonate and adding appropriate additives, etc., amorphous calcium carbonate product with different morphologies and sizes, such as calcium carbonate spherical particles with particle size ≤0.1 μm, large specific surface area and good solubility, can be prepared. The product has high purity and good whiteness.

[0006] Patent CN201810109767.6 discloses a method for preparing nano calcium carbonate by microreaction, and a device for preparing nano calcium carbonate by microreaction mainly comprises a constant-temperature water tank, a microreactor, a temperature controller, a horizontal flow pump, a mixing and stirring tank, a stirrer, a filtrate regenerator, a mixed gas flow meter, a nitrogen storage tank, a carbon dioxide flow meter, a carbon dioxide storage tank, a pH value measuring instrument, a feed pump, a water washing filter and a dryer, and corresponding connecting pipelines.

[0007] Patent CN202011230771.1 discloses a preparation method of nano calcium carbonate and its application, and belongs to the technical field of medicine. The method specifically comprises the following steps: first, dissolving calcium chloride dihydrate in a solvent, then placing it together with ammonium bicarbonate in a sealed environment, adjusting the environmental temperature to make the ammonium bicarbonate decompose into carbon dioxide gas and ammonia gas, and with the continuous diffusion of the carbon dioxide gas in the sealed environment, when a certain degree is reached, the carbon dioxide gas can be dissolved in the calcium chloride solution, making the solution alkaline and providing CO3 2- , reacting with Ca 2+ to form CaCO3, and finally forming milky white nano calcium carbonate particles.

[0008] The existing device for preparing nano calcium carbonate mainly uses the carbonation method, and there are few devices for preparing nano calcium carbonate using the double decomposition method. Generally, the preparation steps are separated, and the nano calcium carbonate cannot be prepared integrally, which is complicated and troublesome. SUMMARY

[0009] The purpose of the present application is to provide an atomization reaction / microwave treatment integrated nano calcium carbonate preparation device and method, which is convenient to operate and can integrally prepare nano calcium carbonate, to solve the technical problem of the existing device prepared by the double decomposition method.

[0010] In order to solve the above technical problems, the scheme adopted by the present application is as follows:

[0011] An atomization reaction / microwave treatment integrated nano calcium carbonate preparation device, comprising a reaction device, a flange and a vacuum device; one side of the reaction device is provided with a nitrogen storage cavity; the reaction device comprises a microwave module, a circulation module A, an electrostatic adsorption module and a circulation module B connected in sequence through the flange; the microwave module, the circulation module A, the electrostatic adsorption module and the circulation module B are all provided with airflow nozzles and atomization nozzles inside; the nitrogen storage cavity is connected with the airflow nozzles; the vacuum device is connected with the circulation module A; the circulation module B is provided with a pressure relief device.

[0012] Further, the reaction device is provided with two liquid storage tanks, namely a calcium source liquid storage tank and a carbon source liquid storage tank; the calcium source liquid storage tank is connected with the atomizing nozzles inside the circulation module A and the circulation module B at both ends; the carbon source liquid storage tank is connected with the atomizing nozzles inside the microwave module and the electrostatic adsorption module at both ends.

[0013] Further, both ends of the liquid storage tank are provided with a pressurizing pump; the liquid storage tank is connected with the atomizing nozzle through the pressurizing pump.

[0014] Further, the electrostatic adsorption module is provided with a collection door and an electrostatic device; the collection door is provided with a whistle; one side of the collection door is hinged with the electrostatic adsorption module, and the other side is connected with the electrostatic adsorption module through the whistle; the electrostatic device is located inside the electrostatic adsorption module.

[0015] Further, the vacuum device includes a vacuum pump, a valve and a connecting pipe; the vacuum pump is connected with the circulation module A through the connecting pipe; the valve is located on the connecting pipe.

[0016] Further, the pressure relief device includes a pressure gauge and a one-way pressure relief valve; the one-way pressure relief valve is connected with the circulation module B; the pressure gauge is located above the one-way pressure relief valve.

[0017] Further, the microwave module is provided with a microwave generator inside.

[0018] Further, the reaction device is provided with multiple groups, which are sequentially connected in the order of the microwave module, the circulation module A, the electrostatic adsorption module and the circulation module B.

[0019] Further, the reaction device is in a circular ring shape; the shell of the reaction device is provided with two layers, the inner layer is made of polytetrafluoroethylene material, and the outer layer is made of ordinary carbon steel material.

[0020] A method for preparing nano calcium by atomization reaction / microwave treatment integration, which uses the above-mentioned device to prepare nano calcium, specifically includes the following steps:

[0021] a. Configure calcium source and carbon source with a concentration of 0.01-0.5 mol / L, and respectively fill them into the calcium source liquid storage tank and the carbon source liquid storage tank;

[0022] b. Turn on the vacuum pump of the vacuum device, open the valve to vacuum the inside of the reaction device, and then turn off the vacuum pump and the valve of the vacuum device;

[0023] c. Open the gas flow outlet, control the nitrogen flow rate to be 8-15 m / s, and make the internal gas flow circulation stable;

[0024] d. Open the atomizing nozzle to atomize the quantitative calcium source reaction solution and carbon source reaction solution with a diameter of 10-20 μm, and mix the reaction solution by rapid movement through air circulation, open the microwave generator of the microwave module, control the microwave power at 50-150 W, and process the atomized reaction solution droplets;

[0025] e. After microwave irradiation for 5-10 s, adjust the microwave power to 300-600 W, and rapidly evaporate the water in the reaction product;

[0026] f. Turn on the electrostatic adsorption module, adjust the air jet speed of the air jet outlet, and reduce the gas flow rate to 6-8 m / s, and the electrostatic adsorption module adsorbs the dried reaction product;

[0027] g. After adsorption is completed, restore the normal pressure through the pressure relief device, open the collection door, and collect the adsorbed reaction product.

[0028] The beneficial effects of the present application are as follows:

[0029] 1. The present application forms nanometer calcium carbonate by circulating the calcium source and the carbon source in the internal reaction device connected by the microwave module, the circulation module A / electrostatic adsorption module and the circulation module B, and performs drying adsorption, and the reaction in the vacuum environment is less disturbed by external impurities.

[0030] 2. The reaction of the calcium source and the carbon source in the present application is dispersed in the air flow in the form of atomized droplets, and the diameter of the single atomized droplet is small, which facilitates the reaction of the reaction solution, and the reaction solution is in a high-speed motion state by nitrogen circulation, which limits the growth environment of the crystal.

[0031] 3. The present application is uniformly, efficiently and quickly processed by microwave irradiation, which is more conducive to the formation of nanometer calcium; increasing the microwave power can rapidly dry and dehydrate the microdroplets, and stop the crystallization reaction process.

[0032] 4. The one-way pressure relief valve and the pressure gauge of the circulation module A facilitate pressure relief when the air pressure in the reaction device is too high, so as to ensure the pressure in the device.

[0033] 5. The reaction device of the present application has a double-layer structure, and the inner layer of polytetrafluoroethylene material has excellent chemical stability and corrosion resistance, which can avoid corrosion by the carbon source.

[0034] 6. The present application has a simple overall structure and is easy to operate, and the speed of the reaction can be easily controlled by adjusting the power of the microwave and the flow rate of the air jet outlet. BRIEF DESCRIPTION OF DRAWINGS

[0035] Figure 1 is a top view structural schematic diagram of the present application;

[0036] Figure 2A schematic diagram of a top view structure of the present application;

[0037] Figure 3 A schematic diagram of a top view structure of the present application; Figure 2 A schematic diagram of an enlarged structure at A in the middle;

[0038] Figure 4 A schematic diagram of a front view structure of the present application;

[0039] Figure 5 A schematic diagram of a front view structure of the present application.

[0040] In the figure: 1, reaction device; 101, flange; 102, gas flow outlet; 103, atomizing nozzle; 2, microwave module; 201, microwave generator; 3, circulating module A; 301, circulating module B; 4, electrostatic adsorption module; 401, collection door; 402, whistle; 403, electrostatic device; 5, vacuum device; 501, vacuum pump; 502, valve; 503, connecting pipe; 6, nitrogen storage cavity; 7, liquid storage tank; 701, calcium source liquid storage tank; 702, carbon source liquid storage tank; 703, pressure pump; 8, pressure relief device; 801, pressure gauge; 802, one-way pressure relief valve. DETAILED DESCRIPTION

[0041] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0042] In the description of the present application, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application; the terms "first", "second", "third" are only for the purpose of description, and cannot be understood as indicating or implying relative importance; in addition, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connection" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be mechanically connected, or it can be electrically connected; it can be directly connected, or it can be indirectly connected through an intermediate medium; it can be the communication between two elements inside. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0043] The application further discloses a device and method for preparing nano calcium by integrating atomization reaction and microwave treatment. EMBODIMENT

[0044] The device for preparing nano calcium by integrating atomization reaction and microwave treatment comprises a circular ring-shaped reaction device 1, a flange 101 and a vacuum device 5. The reaction device 1 is provided with a nitrogen storage cavity 6 on one side, and comprises a microwave module 2, a circulation module A 3, an electrostatic adsorption module 4 and a circulation module B 301 which are sequentially connected through the flange 101. The microwave module 2, the circulation module A 3, the electrostatic adsorption module 4 and the circulation module B 301 are all internally provided with an airflow outlet 102 and an atomization nozzle 103. The nitrogen storage cavity 6 is connected with the airflow outlet 102. The atomization nozzle 103 and the airflow outlet 102 both spray counterclockwise. The vacuum device 5 is connected with one circulation module A 3. The circulation module B 301 is provided with a pressure relief device 8. The reaction device 1 is provided with two liquid storage tanks 7, i.e. The two ends of the calcium source liquid storage tank 701 are connected with the atomization nozzles 103 in the circulation module A 3 and the circulation module B 301. The two ends of the carbon source liquid storage tank 702 are connected with the atomization nozzles 103 in the microwave module 2 and the electrostatic adsorption module 4. The two ends of the liquid storage tank 7 are both provided with a pressurizing pump 703. The liquid storage tank 7 is connected with the atomization nozzle 103 through the pressurizing pump 703. The electrostatic adsorption module 4 is provided with a collection door 401 and an electrostatic device 403. The collection door 401 is hinged to the electrostatic adsorption module 4 on one side and connected with the electrostatic adsorption module 4 through the whistle on the other side. The electrostatic device 403 is located in the electrostatic adsorption module 4. The vacuum device 5 comprises a vacuum pump 501, a valve 502 and a connecting pipe 503. The vacuum pump 501 is connected with the circulation module A 3 through the connecting pipe 503. The valve 502 is located on the connecting pipe 503. The pressure relief device 8 comprises a pressure gauge 801 and a one-way pressure relief valve 802. The one-way pressure relief valve 802 is connected with the circulation module B 301. The pressure gauge 801 is located above the one-way pressure relief valve 802. The microwave module 2 is internally provided with a microwave generator 201. The shell of the reaction device 1 is provided with two layers, the inner layer is made of polytetrafluoroethylene material, and the outer layer is made of ordinary carbon steel material.

[0045] The application further discloses a method for preparing nano calcium by integrating atomization reaction and microwave treatment.

[0046] a. The calcium chloride and the ammonium carbonate with a concentration of 0.2 mol / L are respectively filled into the calcium source liquid storage tank 701 and the carbon source liquid storage tank 702;

[0047] b. Open the vacuum pump 501 of the vacuum device 5, open the valve 502, the vacuum pump 501 draws the inside of the reaction device 1 into a vacuum state through the connecting pipe 503, then close the vacuum pump 501 and the valve 502 of the vacuum device 5;

[0048] c. Open the air flow outlet 102, control the nitrogen flow rate at 12 m / s, and make the air flow in the reaction device 1 circulate stably;

[0049] d. Open the atomizing nozzle 103 to atomize and spray calcium chloride and ammonium carbonate with a volume ratio of 1:1, the calcium chloride and ammonium carbonate are mixed and reacted to generate nano calcium carbonate and hydrogen chloride through the rapid movement of the air flow circulation, open the microwave generator 201 of the microwave module 2, control the microwave power at 80 W, process the atomized reaction droplets, accelerate the generation of nano calcium carbonate, and at the same time, the hydrogen chloride is decomposed into chlorine and ammonia gas, which is discharged from the reaction device through the one-way pressure relief valve 802;

[0050] e. After microwave irradiation for 10 s, adjust the microwave power to 450 W for drying, and quickly evaporate the moisture inside the nano calcium carbonate;

[0051] f. Open the electrostatic adsorption module 4, adjust the air jet speed of the air flow outlet 102, and reduce the gas flow rate to 7 m / s, and the electrostatic adsorption module 4 adsorbs the dry nano calcium carbonate;

[0052] g. After the adsorption is completed, the one-way pressure relief valve 802 of the pressure relief device 8 is used for pressure relief, the inside of the device returns to normal pressure, the collection door 401 is opened, and the nano calcium carbonate adsorbed in the inner cavity of the electrostatic adsorption module 4 is collected.

[0053] Finally, it should be noted that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application 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 replacements to some technical features, as long as they are within the spirit and principles of the present application. Any modification, equivalent replacement, improvement, etc. made within the scope of the present application should be included in the protection scope of the present application.

Claims

1. An apparatus for preparing nano-calcium using an integrated atomization reaction / microwave treatment method, characterized in that: The application relates to a reaction device for preparing nano calcium, which comprises a ring-shaped reaction device (1), a flange (101) and a vacuum device (5); one side of the reaction device (1) is provided with a nitrogen storage cavity (6), the reaction device (1) comprises a microwave module (2), a circulation module A (3), an electrostatic adsorption module (4) and a circulation module B (301) which are sequentially connected by the flange (101); the microwave module (2), the circulation module A (3), the electrostatic adsorption module (4) and the circulation module B (301) are internally provided with airflow nozzles (102) and atomizing nozzles (103); the nitrogen storage cavity (6) is connected with the airflow nozzles (102); the vacuum device (5) is connected with the circulation module A (3); the circulation module B (301) is provided with a pressure relief device (8). 2.The device for preparing nano-calcium by atomizing reaction and microwave processing according to claim 1, characterized in that: The reaction device (1) is provided with two liquid storage tanks (7), namely a calcium source liquid storage tank (701) and a carbon source liquid storage tank (702); the two ends of the calcium source liquid storage tank (701) are connected with the atomizing nozzles (103) in the circulation module A (3) and the circulation module B (301); the two ends of the carbon source liquid storage tank (702) are connected with the atomizing nozzles (103) in the microwave module (2) and the electrostatic adsorption module (4) respectively. 3.The device for preparing nano-calcium by atomizing reaction / microwave processing integration according to claim 2, characterized in that: The two ends of the liquid storage tank (7) are provided with pressurizing pumps (703); the liquid storage tank (7) is connected with the atomizing nozzles (103) through the pressurizing pumps (703).

4. The device for preparing nano-calcium by atomizing reaction / microwave processing integration according to claim 1, characterized in that: The electrostatic adsorption module (4) is provided with a collecting door (401) and an electrostatic device (403); the collecting door (401) is provided with a plug whistle (402); one side of the collecting door (401) is hinged with the electrostatic adsorption module (4), and the other side is connected with the electrostatic adsorption module (4) through the plug whistle; the electrostatic device (403) is located in the interior of the electrostatic adsorption module (4).

5. The device for preparing nano-calcium by atomizing reaction / microwave processing integration according to claim 1, characterized in that: The vacuum device (5) comprises a vacuum pump (501), a valve (502) and a connecting pipe (503); the vacuum pump (501) is connected with the circulation module A (3) through the connecting pipe (503); the valve (502) is located on the connecting pipe (503).

6. The device for preparing nano-calcium by atomizing reaction / microwave processing integration according to claim 1, characterized in that: The pressure relief device (8) comprises a pressure gauge (801) and a one-way pressure relief valve (802); the one-way pressure relief valve (802) is connected with the circulation module B (301); the pressure gauge (801) is located above the one-way pressure relief valve (802).

7. The device for preparing nano-calcium by atomizing reaction / microwave processing integration according to claim 1, characterized in that: The microwave module (2) is internally provided with a microwave generator (201). 8.The device for preparing nano-calcium by atomizing reaction and microwave processing according to claim 1, characterized in that: The reaction device (1) is provided with multiple groups which are sequentially connected according to the microwave module (2), the circulation module A (3), the electrostatic adsorption module (4) and the circulation module B (301).

9. The device for preparing nano-calcium by atomizing reaction / microwave processing integration according to claim 1, characterized in that: The shell of the reaction device (1) is provided with two layers, the inner layer is made of polytetrafluoroethylene material, and the outer layer is made of ordinary carbon steel material.

10. A method for preparing nano-calcium by integrating atomization reaction and microwave treatment, characterized in that: The application further discloses a preparation method of the nano calcium by using the device. a. The calcium source and carbon source with concentration in the range of 0.01-0.5 mol / L are filled into the calcium source storage tank (701) and carbon source storage tank (702); b. The vacuum pump (501) of the vacuum device (5) is opened, the valve (502) is opened to vacuumize the inside of the reaction device (1), and then the vacuum pump (501) and valve (502) of the vacuum device (5) are closed; c. The gas flow outlet (102) is opened, the nitrogen flow rate is controlled in the range of 8-15 m / s, and the internal gas flow is circulated and stabilized; d. The atomizing nozzle (103) is opened to atomize and spray the quantitative calcium source reaction liquid and carbon source reaction liquid with a diameter in the range of 10-20 μm, the atomized reaction liquid droplets are mixed and reacted by the rapid movement of the gas flow, the microwave generator of the microwave module (2) is opened, and the microwave power is controlled in the range of 50-150 W; e. After microwave irradiation for 5-10 s, the microwave power is adjusted to 300-600 W to rapidly evaporate the water in the reaction product; f. The electrostatic adsorption module (4) is opened, the gas flow speed of the gas flow outlet (102) is adjusted, the gas flow rate is reduced to 6-8 m / s, and the electrostatic adsorption module (4) adsorbs the dried reaction product; g. After adsorption is completed, the normal pressure is restored by the pressure relief device (8), the collection door (401) is opened, and the adsorbed reaction product is collected.

Images