Device and method for preparing material by using microbubbles

Abstract

The invention discloses a device and a method for preparing a material by using microbubbles. The device comprises a microbubble generating unit, a gas inlet channel, a reaction chamber, a gas storage unit, a circulating channel and a vacuum pump, gas is driven by the pressure source, and micro-bubbles are formed in the reaction chamber by the gas inlet channel through the micro-bubble generation unit; the reaction chamber provides a place for the action of the microbubbles and the reaction liquid; the gas storage unit collects reacted gas, and the reacted gas can be input into the gas inlet channel through the circulating channel for recycling; the vacuum pump is connected with the gas inlet channel, and residual gas in the channel is pumped out through the vacuum pump before fresh gas is introduced. The device can generate a clean gas reaction atmosphere, improves the reaction efficiency and the gas utilization rate, can be applied to a material preparation reaction in which gas participates, and can remarkably reduce the use amount of harmful gas when the reaction gas is the harmful gas.

Description

Technical Field

[0001] The present invention relates to the technical fields of material preparation and chemical engineering, and particularly relates to a method for preparing materials by generating and recycling microbubbles. Background Art

[0002] Gases are often involved in material preparation. For example, inert gases such as nitrogen are used to remove dissolved oxygen in the reaction solution, carbon monoxide reacts with the methanol solution of Na 2 PdCl 4 to prepare two-dimensional palladium nanosheets, hydrogen sulfide reacts with copper sulfate solution to synthesize copper sulfide chemicals, etc. However, the emission and utilization rate of harmful gases such as carbon monoxide in material preparation have not been taken seriously. Microbubbles have attracted much attention due to their excellent physicochemical properties such as large specific surface area, self-compression effect, surface charge, and surface hydrophobicity. Therefore, it is of great significance to use microbubbles to improve the reaction efficiency in material preparation and design a reaction device to improve gas utilization rate. Summary of the Invention

[0003] In view of the deficiencies of the prior art, the present invention provides a device and method for preparing materials by using microbubbles.

[0004] To achieve the above objectives, one of the technical solutions of the present invention is as follows:

[0005] A device for preparing materials by using microbubbles includes a microbubble generation unit, an intake channel, a reaction chamber, a gas storage unit, a circulation channel, and a vacuum pump; the intake channel is connected to the microbubble generation unit, one end of the reaction chamber is connected to the outlet of the microbubble generation unit, and the other end is connected to the gas storage unit; one end of the circulation channel is connected to the gas storage unit, and the other end is connected to the intake channel as a branch through a three-way valve; the vacuum pump is connected to the intake channel, and the connection point is located in the intake section of the intake channel before the position where the three-way valve is installed. The three-way valve divides the intake channel into an intake section close to the intake end and an outlet section close to the reaction chamber. The two paths of the three-way valve are respectively connected to the intake section and the outlet section, and the other path is connected to the circulation channel.

[0006] Optionally, the method for generating microbubbles by the microbubble generation unit includes at least one of membrane dispersion method, dissolved air-aeration method, and air entrainment-dispersion method.

[0007] Optionally, the intake channel is also connected to a pressure source.

[0008] The present invention also provides the application of the device for preparing materials by using microbubbles in removing oxygen with inert gases.

[0009] The present invention also provides the application of the device for preparing materials by using microbubbles in the material preparation reaction involving gas reactants.

[0010] Another technical solution of the present invention is: a method for preparing materials using microbubbles, adopting the device for preparing materials using microbubbles described above. The method comprises the following steps:

[0011] Step 1, load the reaction liquid into the reaction chamber;

[0012] Step 2, rotate the three-way valve to connect the circulation channel and the intake section of the intake channel, and isolate the outlet section of the intake channel; turn on the vacuum pump to evacuate, and turn off the vacuum pump when the vacuum degree reaches the set vacuum degree; introduce a gas that does not participate in the reaction from the intake section until the vacuum degree returns to 0 and stop; rotate the three-way valve to connect the intake section and the outlet section of the intake channel, and isolate the circulation channel; introduce a gas that does not participate in the reaction from the intake channel at a set flow rate until the set time and stop;

[0013] Step 3, rotate the three-way valve to connect the circulation channel and the intake section of the intake channel, and isolate the outlet section of the intake channel; turn on the vacuum pump to evacuate, and turn off the vacuum pump when the vacuum degree reaches the set condition; introduce the microbubble reaction gas from the intake section of the intake channel until the vacuum degree returns to 0 and stop; rotate the three-way valve to connect the intake section and the outlet section of the intake channel, and isolate the circulation channel; introduce the microbubble reaction gas from the intake channel until the set time and stop;

[0014] Step 4, rotate the three-way valve to connect the circulation channel and the intake section of the intake channel, and isolate the outlet section of the intake channel, and input the gas in the gas storage unit into the intake channel; then rotate the three-way valve to connect the intake section and the outlet section of the intake channel, and isolate the circulation channel; introduce the collected gas from the intake channel, and stop after a predetermined time; repeat the above operation until the total gas flow reaches the set flow rate, and then stop the reaction;

[0015] Step 5, collect the liquid after the reaction, and separate to obtain the product.

[0016] Optionally, in each step, the flow rate of the gas in the intake channel is 0.01 L / min to 100 L / min.

[0017] Optionally, in Step 2 and Step 3, the set vacuum degree is -1.5 kg / cm 2 to -0.1 kg / cm 2 .

[0018] Optionally, in Step 2, the gas that does not participate in the reaction is an inert gas.

[0019] Optionally, the set time for each step is 1 min - 60 min.

[0020] The reaction chamber of the present invention provides a place for the microbubbles to act on the reaction liquid; the gas storage unit collects the gas after the reaction, and can be input into the intake channel through the circulation channel for reuse; the vacuum pump is connected to the intake channel, and before introducing new gas, the vacuum pump is used to pump out the residual gas in the channel.

[0021] Optionally, the type of interaction between the bubbles and the reaction solution in the reaction chamber can be a non-chemical reaction such as removing dissolved oxygen by inert gas microbubbles, or a chemical reaction such as the reaction of carbon monoxide microbubbles with a methanol solution of Na 2 PdCl 4 to prepare two-dimensional palladium nanosheets, or the reaction of hydrogen sulfide microbubbles with a copper sulfate solution to synthesize copper sulfide chemicals. In the above methods, before introducing the new gas, the residual gas in the device needs to be evacuated using a vacuum pump, and then the new gas is introduced from the intake channel and reaches the composite membrane. First, an inert gas such as argon is introduced. The microbubbles generated by dispersion through the composite membrane rise in the reaction chamber while continuously removing the dissolved oxygen in the reaction solution, ensuring an anaerobic reaction condition; then the reaction gas is introduced. The microbubbles generated by dispersion through the composite membrane rise in the reaction chamber while reacting with the reaction solution to obtain the reaction product. The tail gas of the reaction is collected by the gas storage unit and can be recycled through the circulation channel and re-introduced into the intake channel for reuse.

[0022] The beneficial effects of the present invention are as follows:

[0023] 1) In the microbubble generation unit of the present invention, methods such as the membrane dispersion method are used to divide the gas into a large number of microbubbles, improving the efficiency of removing dissolved oxygen by inert gas and the mass transfer efficiency of the reaction;

[0024] 2) The present invention recycles the tail gas of the reaction, improving the gas utilization rate and significantly reducing the emission of harmful gas reactant tail gas;

[0025] 3) The materials prepared by the present invention, such as two-dimensional palladium nanosheets, exhibit excellent performance as an anode catalyst for methanol fuel cells;

[0026] 4) The reaction device used in the present invention can expand the application range and has strong practicability. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] The present invention will be further described below in conjunction with the drawings and embodiments.

[0028] Figure 1 is a schematic diagram of the device for preparing materials using microbubbles according to the present invention;

[0029] Figure 2 is the distribution diagram of the microbubble diameter generated by the membrane dispersion method in Example 1, where the composite membrane is the microbubbles generated by the membrane material in a methanol solution of 0.8 mmol / L Na 2 PdCl 4 ;

[0030] Figure 3 is the transmission electron microscope image of the two-dimensional palladium nanosheets prepared under different conditions in Example 1; the scale in the lower right corner of each small figure A, B, and C is 50 nm.

[0031] Figure 4 Cyclic voltammetry test diagrams of two-dimensional palladium nanosheets prepared under different conditions in Example 1 and commercial 10% palladium-carbon catalyst in 1 mol / L KOH solution;

[0032] Figure 5 Cyclic voltammetry test diagrams of two-dimensional palladium nanosheets prepared under different conditions in Example 1 and commercial 10% palladium-carbon catalyst in a mixed solution of 1 mol / L KOH and 1 mol / L methanol;

[0033] Figure 6 Current-time test diagrams of two-dimensional palladium nanosheets prepared under different conditions in Example 1 and commercial 10% palladium-carbon catalyst in a mixed solution of 1 mol / L KOH and 1 mol / L methanol;

[0034] Figure 7 Calculation results of the catalytic efficiency of two-dimensional palladium nanosheets prepared under different conditions in Example 1 and commercial 10% palladium-carbon catalyst;

[0035] Figure 8 Calculation results of the catalyst stability of two-dimensional palladium nanosheets prepared under different conditions in Example 1 and commercial 10% palladium-carbon catalyst;

[0036] Figure 9 Comparison of the carbon monoxide consumption for preparing two-dimensional palladium nanosheets using large bubbles and circulating microbubbles in Example 1. Detailed implementation manners

[0037] In order to better illustrate the technical features, technical content and achieved technical effects of the present invention, the accompanying drawings of the present invention will be described in more detail in combination with embodiments. However, the shown drawings are only for better illustrating the technical solution of the present invention and cannot limit the protection scope of the claims of the present invention. The technical solution of the present invention will be further described and described below through specific implementation manners in combination with the drawings.

[0038] Schematic diagram of the reaction device for preparing materials using microbubbles in the present invention is as Figure 1As shown in the figure, it includes an intake channel 1, a microbubble generation unit 2, a reaction chamber 3, a gas storage unit 4, a circulation channel 5, a vacuum pump 6, and a three-way valve 7. The microbubble generation unit 2 is located on the connection path between the intake channel 1 and the reaction chamber 3. Gas forms microbubbles in the reaction chamber 3 through the microbubble generation unit 2 from the intake channel 1, and the reaction chamber 3 is filled with a reaction liquid. The front end of the circulation channel 5 is connected to the gas storage unit 4, and the rear end is connected to the intake channel 1 as a branch through the three-way valve 7. The function of the three-way valve 7 is to rotate the three-way valve 7 to make the arrow face down before the vacuum pump 6 evacuates, isolating the part above the three-way valve 7 to prevent the reaction liquid in the reaction chamber 3 from being sucked back into the vacuum pump 6 through the microbubble generation unit 2. After the pressure in the device returns above atmospheric pressure, rotate the three-way valve 7 to make the arrow face left, connect the intake channel 1, and isolate the circulation channel 5.

[0039] The bottom port of the intake channel 1 is connected to a pressure source.

[0040] When it is necessary to recycle the gas, rotate the three-way valve 7 to make the arrow face down, connect the circulation channel 5 and the lower end of the intake channel 1, and input the gas in the gas storage unit 4 into the pressure source through the intake channel. Then rotate the three-way valve 7 to make the arrow face left, connect the intake channel 1, and isolate the circulation channel 5, so that the gas can be recycled.

[0041] Example 1

[0042] Adopt Figure 1 The device for preparing microbubbles uses a nylon membrane with a film thickness of 100 μm and a pore diameter of 0.8 μm, which is covered with a stainless steel rigid skeleton with a thickness of 250 μm, a central 37*37 square hole array, a side length of the square hole of 250 μm, and a center distance of the holes of 300 μm to form a composite membrane. That is, the membrane dispersion method is used as the method for generating microbubbles in the microbubble generation unit. Select a 70 mL methanol solution of 0.8 mmol / L Na 2 PdCl 4 as the reaction liquid to fill the reaction chamber.

[0043] Rotate the three-way valve 7 to make the arrow face down to connect the circulation channel and the lower end of the intake channel (i.e., the intake section), and isolate the upper end of the intake channel (i.e., the outlet section). Turn on the vacuum pump to evacuate. When the vacuum degree reaches -1 kg / cm 2 , turn off the vacuum pump, and introduce argon into the intake channel at a flow rate of 10 mL / min until the vacuum degree returns to 0 and stop. Repeat the above operation 3 times. Rotate the three-way valve to make the arrow face left to connect the upper and lower ends of the intake channel and isolate the circulation channel. Introduce argon into the intake channel at a flow rate of 10 mL / min and stop after 15 minutes. The bubble diameter distribution when introducing argon is as Figure 2 shown.

[0044] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolating the upper end of the intake channel. Turn on the vacuum pump to evacuate, and when the vacuum reaches -1 kg / cm 2 , turn off the vacuum pump, and introduce carbon monoxide gas into the intake channel at a flow rate of 10 mL / min until the vacuum returns to 0 and then stop. Rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel, isolating the circulation channel. Introduce carbon monoxide gas into the intake channel at a flow rate of 10 mL / min, and stop after 5 min.

[0045] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolating the upper end of the intake channel. Input the gas in the gas storage unit into the pressure source through the intake channel, then rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel, isolating the circulation channel. Introduce the collected gas into the intake channel at a flow rate of 10 mL / min, and stop after 5 min. Repeat the above operation 7 times until the total gas flow is 400 mL, and then stop the reaction.

[0046] Collect the liquid after the reaction, and centrifuge to obtain the solid. Ultrasonically wash it with a mixed solution of ethanol and water and then centrifuge. Repeat three times, and then put the solid into a freeze dryer for freeze-drying for 24 h to obtain two-dimensional palladium nanosheets. Its transmission electron microscope characterization is as shown in Figure 3 (A).

[0047] Mix the two-dimensional palladium nanosheets with Vulcan xc-72 conductive carbon black to prepare a sample with a palladium content of 10% wt and load it on a glassy carbon electrode with a diameter of 5 mm. Select a 10*10*0.2 mm platinum electrode as the counter electrode and a saturated calomel electrode as the reference electrode. Set the potential range from -0.9 V to 0.3 V and the scan rate at 0.05 V / s, and perform cyclic voltammetry tests in 1 mol / L KOH solution. The obtained results are as shown in Figure 4 . Perform cyclic voltammetry tests under the same conditions in a mixed solution of 1 mol / L KOH and 1 mol / L methanol, and the obtained results are as shown in Figure 5 . Subsequently, in the same solution, select the Figure 5 oxidation half-wave potential in as the potential for the current-time test, and the obtained results are as shown in Figure 6 . Calculate the catalytic efficiency from the ratio of the two peak potentials in Figure 5 , and the results are as shown in Figure 7 . Calculate the catalyst stability from the ratio of the initial current and the current at the last second in Figure 6 , and the results are as shown in Figure 8 .

[0048] Change the time for introducing carbon monoxide to 40 min, and do not recycle the gas. Keep other preparation, washing treatment methods and test conditions unchanged. The transmission electron microscope characterization of the prepared two-dimensional palladium nanosheets is as shown in Figure 3 (B), and the electrochemical test data are as shown in Figures 4 - 8 .

[0049] Prepare two-dimensional palladium nanosheets using a conventional method. In a beaker containing 70 mL of a 0.8 mmol / L methanol solution of Na 2 PdCl 4 , generate large bubbles at a flow rate of 80 mL / min through a silica gel tube with an inner diameter of 10 mm and an outer diameter of 13 mm. First, introduce argon and then carbon monoxide for 5 minutes each. Keep other washing treatment methods and test conditions unchanged. The transmission electron microscope characterization of the prepared two-dimensional palladium nanosheets is as shown in Figure 3 (C), and the electrochemical test data is as shown in Figures 4 - 8 .

[0050] Load a purchased 10% wt commercial palladium-carbon catalyst onto a glassy carbon electrode with a diameter of 5 mm. Keep other test conditions unchanged. The electrochemical test data is as shown in Figures 4 - 8 .

[0051] Use the two-dimensional palladium nanosheets prepared by the present invention as the anode catalyst of a methanol fuel cell. The catalytic efficiency and catalyst stability are both superior to the materials prepared by conventional methods and commercial catalysts. As shown in Figure 9 , the amount of harmful carbon monoxide gas used in this method is about 50 mL, which is significantly less than the 400 mL used in the large bubble preparation method.

[0052] Example 2

[0053] Adopt Figure 1 The device for preparing materials using microbubbles, select a ceramic membrane with a membrane thickness of 300 μm and a pore size of 0.8 μm, that is, use the membrane dispersion method as the method for generating microbubbles in the microbubble generation unit. Select 70 mL of a 10 mmol / L CuSO 4 solution as the reaction solution to fill the reaction chamber.

[0054] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolating the upper end of the intake channel. Turn on the vacuum pump to evacuate. When the vacuum reaches -1 kg / cm 2 , turn off the vacuum pump. Introduce argon into the intake channel at a flow rate of 10 mL / min until the vacuum returns to 0 and stop. Repeat the above operation 3 times. Rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel, isolating the circulation channel. Introduce argon into the intake channel at a flow rate of 10 mL / min and stop after 15 minutes.

[0055] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolating the upper end of the intake channel. Turn on the vacuum pump to evacuate. When the vacuum reaches -1 kg / cm 2Turn off the vacuum pump, and introduce hydrogen sulfide gas into the intake channel at a flow rate of 10 mL / min until the vacuum degree returns to 0 and then stop. Rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel and isolate the circulation channel. Introduce hydrogen sulfide gas into the intake channel at a flow rate of 10 mL / min and stop after 5 minutes.

[0056] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolate the upper end of the intake channel, input the gas in the gas storage unit into the pressure source through the intake channel, and then rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel and isolate the circulation channel. Introduce the collected gas into the intake channel at a flow rate of 10 mL / min and stop after 5 minutes. Repeat the above operation 7 times until the total gas flow is 400 mL and then stop the reaction.

[0057] Collect the liquid after the reaction and centrifuge to obtain a solid. Wash the solid ultrasonically with water and then centrifuge. Repeat three times and then put the solid into a freeze dryer for freeze-drying for 24 h to obtain CuS particles.

[0058] Example 3

[0059] Adopt Figure 1 the device for preparing materials using microbubbles, select a ceramic membrane with a membrane thickness of 300 μm and a pore size of 0.8 μm, that is, use the membrane dispersion method as the method for generating microbubbles in the microbubble generation unit. Select 70 mL of 0.1 mol / L Al(NO 3 ) 3 solution as the reaction solution to fill the reaction chamber.

[0060] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolate the upper end of the intake channel. Turn on the vacuum pump to evacuate, and when the vacuum degree reaches -1 kg / cm 2 , turn off the vacuum pump, introduce argon gas into the intake channel at a flow rate of 10 mL / min until the vacuum degree returns to 0 and then stop. Repeat the above operation 3 times. Rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel and isolate the circulation channel. Introduce argon gas into the intake channel at a flow rate of 10 mL / min and stop after 15 minutes.

[0061] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolate the upper end of the intake channel. Turn on the vacuum pump to evacuate, and when the vacuum degree reaches -1 kg / cm 2 , turn off the vacuum pump, introduce ammonia gas into the intake channel at a flow rate of 10 mL / min until the vacuum degree returns to 0 and then stop. Rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel and isolate the circulation channel. Introduce ammonia gas into the intake channel at a flow rate of 10 mL / min and stop after 5 minutes.

[0062] Rotate the three-way valve so that the arrow points downward to connect the circulation channel and the lower end of the intake channel, isolate the upper end of the intake channel, and input the gas in the gas storage unit into the pressure source through the intake channel. Then rotate the three-way valve so that the arrow points to the left to connect the upper and lower ends of the intake channel and isolate the circulation channel. Introduce the collected gas into the intake channel at a flow rate of 10 mL / min, and stop after 5 minutes. Repeat the above operation 7 times until the total gas flow is 400 mL, and then stop the reaction.

[0063] Collect the liquid after the reaction, adjust the pH to 4 - 5 with 0.1 mol / L dilute hydrochloric acid, and then centrifuge to obtain a solid. Wash the solid ultrasonically with water and then centrifuge, repeat three times, and then heat the solid at 500 °C for 3 h to obtain Al 2 O 3 particles.

[0064] The above embodiments are only used to further illustrate an apparatus and method for preparing materials using microbubbles according to the present invention. However, the present invention is not limited to the embodiments. Any simple modification, equivalent change, and modification made to the above embodiments based on the technical essence of the present invention shall fall within the protection scope of the technical solution of the present invention.

Claims

1. A device for preparing materials using microbubbles, characterized in that: The invention comprises a microbubble generating unit, an air inlet channel, a reaction chamber, an air storage unit, a circulation channel and a vacuum pump; the air inlet channel is connected to the microbubble generating unit, one end of the reaction chamber is connected to the outlet of the microbubble generating unit, and the other end is connected to the air storage unit; one end of the circulation channel is connected to the air storage unit, and the other end is connected to the air inlet channel as a branch through a three-way valve; the vacuum pump is connected to the air inlet channel, and the connection is located at the air inlet section before the position where the three-way valve is installed in the air inlet channel, the three-way valve divides the air inlet channel into an air inlet section close to the air inlet end and an air outlet section close to the reaction chamber, two paths of the three-way valve are respectively connected to the air inlet section and the air outlet section, and the other path is connected to the circulation channel.

2. The device for preparing materials using microbubbles according to claim 1, characterized in that: The microbubble generating unit generates microbubbles in a manner including at least one of a membrane dispersion method, a dissolved air-aeration method, and an air entrainment-dispersion method.

3. The device for preparing materials using microbubbles according to claim 1, characterized in that: The air intake passage is also connected to a pressure source.

4. Use of the device for preparing materials using microbubbles according to any one of claims 1 to 3 in inert gas deoxygenation.

5. Use of the device for preparing materials using microbubbles according to any one of claims 1 to 3 in a material preparation reaction involving gaseous reactants.

6. A method for preparing a material using microbubbles, characterized in that: The device for preparing a material using microbubbles according to any one of claims 1 to 3 comprises the following steps: Step 1: loading a reaction liquid into a reaction chamber; Step 2: Rotate the three-way valve to connect the air inlet section of the circulation channel and the air inlet channel, and isolate the air outlet section of the air inlet channel; turn on the vacuum pump to evacuate, and turn off the vacuum pump when the vacuum degree reaches the set vacuum degree; introduce a gas that does not participate in the reaction from the air inlet section until the vacuum degree returns to 0; rotate the three-way valve to connect the air inlet section and the air outlet section of the air inlet channel, and isolate the circulation channel; introduce a gas that does not participate in the reaction from the air inlet channel at a set flow rate, and stop at a set time; Step 3: Rotate the three-way valve to connect the circulation channel and the air inlet section of the air inlet channel, and isolate the air outlet section of the air inlet channel; turn on the vacuum pump to evacuate, and turn off the vacuum pump when the vacuum degree reaches the set condition; introduce microbubble reaction gas from the air inlet section of the air inlet channel until the vacuum degree returns to 0; rotate the three-way valve to connect the air inlet section and the air outlet section of the air inlet channel, and isolate the circulation channel; introduce microbubble reaction gas from the air inlet channel until the set time stops; Step 4: Rotate the three-way valve to connect the circulation channel and the air inlet section of the air inlet channel, isolate the air outlet section of the air inlet channel, and input the gas in the gas storage unit into the pressure source through the air inlet channel; rotate the three-way valve again to connect the air inlet section and the air outlet section of the air inlet channel, and isolate the circulation channel; introduce the collected gas from the air inlet channel, and stop after a predetermined time; repeat the above operation until the total gas flow reaches the set flow, and then stop the reaction; Step 5: Collect the liquid after the reaction and separate the product.

7. The method for preparing a material using microbubbles according to claim 6, characterized in that: In each step, the flow rate of the gas in the air inlet channel is 0.01-100 L / min.

8. The method for preparing a material using microbubbles according to claim 6, characterized in that: In step 2 and step 3, the vacuum degree is set to -1.5kg / cm 2 To -0.1kg / cm 2 .

9. The method for preparing a material using microbubbles according to claim 6, characterized in that: In step 2, the gas that does not participate in the reaction is an inert gas.

10. The method for preparing a material using microbubbles according to claim 6, characterized in that: The setting time of each step is 1min-60min.

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