A device for preparing floating hollow microspheres
By designing a preparation device that includes a material container, a water bath, and a cross-linking container, the problem of the lack of equipment for preparing floating hollow microspheres was solved, realizing the mass production and efficient heavy metal adsorption of floating hollow microspheres, and meeting the needs of large-area soil remediation.
Patent Information
- Application Number
- CN202411092614.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-09
- Publication Date
- 2025-12-02
- Estimated Expiration
- 2044-08-09
Smart Images

Figure CN118788316B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of new material preparation technology, and in particular to a device for preparing floating hollow microspheres for reducing heavy metals in soil. Background Technology
[0002] Current technologies for the safe utilization of lightly to moderately polluted farmland are emergency-level technologies and do not reduce the total amount of cadmium in the soil, thus offering limited improvement in soil environmental quality. Existing technologies for reducing total cadmium in the soil, such as phytoremediation, leaching remediation, and magnetic material adsorption removal remediation, have drawbacks such as long cycles, damage to soil structure, and difficulties in material recycling.
[0003] With the development of science and technology, new materials and application technologies for reducing cadmium in soil have emerged. These materials have advantages such as high removal efficiency, short remediation cycle, and no impact on agricultural activities and production seasons. For example, Chinese invention patent CN117244535B discloses the preparation of floating hollow microspheres and their application in reducing cadmium in soil. This material is mainly prepared by cross-linking polyvinyl alcohol, sodium alginate, inorganic minerals, and other materials. It is applied to moist soil and adsorbs heavy metals. After adsorption, water is poured into the field to make the material float and be recovered, achieving the goal of rapid and efficient reduction of cadmium in soil.
[0004] However, there is a lack of production equipment for new materials, especially equipment for the mass production of floating hollow microspheres. To meet the needs of large-scale remediation and regeneration of heavy metal contaminated soil, there is an urgent need for equipment for the large-scale production of floating hollow microspheres. Summary of the Invention
[0005] The purpose of this invention is to provide a floating hollow microsphere preparation device to solve the problem mentioned in the background art of the lack of preparation equipment for mass production of floating hollow microspheres on the market.
[0006] The present invention adopts the following technical solution:
[0007] The present invention discloses a floating hollow microsphere preparation device, comprising a material container including a water bath, a heating and heat preservation tank disposed on the outside of the water bath, a first stirrer disposed inside the water bath, a water bath outlet disposed at the bottom of the water bath, the water bath outlet being connected to a peristaltic pump titration device, and a crosslinking container disposed below the peristaltic pump titration device.
[0008] Furthermore, the crosslinking container has an open structure, the crosslinking container includes a crosslinking barrel, an iron frame is provided at the upper end of the crosslinking barrel, a second stirrer is provided on the iron frame, a crosslinking barrel outlet is provided at the bottom of the crosslinking barrel, and a second support is provided below the crosslinking barrel.
[0009] Furthermore, the second agitator is positioned offset from the first agitator; the second agitator is a slow-speed paddle agitator.
[0010] Furthermore, the water bath has a solution inlet and a solid material inlet at its top. A heating and insulation tank is located on the outer side of the tank wall below the solution inlet and the solid material inlet. A water inlet is located at the top of the heating and insulation tank, and a drain outlet is located at the bottom. The heating and insulation tank includes a tank wall, and an electric heat tracing device is applied to the outer side of the tank wall.
[0011] Furthermore, a thermometer insertion tube is provided on the lower part of the side wall of the water bath, and the outer end of the thermometer insertion tube penetrates through the heating and insulation tank.
[0012] Furthermore, the first agitator is a built-in wall-scraping agitator.
[0013] Furthermore, a first support is provided below the material container.
[0014] Compared with the prior art, the beneficial technical effects of the present invention are as follows:
[0015] In a single batch production, this invention only requires adding materials to the container once. After heating and dissolving the entire mixed solution, and mixing it thoroughly, the solution is discharged from the outlet of the water bath, titrated, and crosslinked. After the mixed material is heated and dissolved in the container, the flow rate of the peristaltic pump titration device is adjusted to allow the mixture to be titrated dropwise into the container. After titration by the peristaltic pump titration device, the material is crosslinked in a neutral boric acid / calcium chloride solution in the crosslinking container to prepare floating hollow microspheres. After settling, the solution and the floating hollow microspheres are collected from the outlet of the crosslinking tank and separated by a filter to obtain the microsphere material. Furthermore, the stirrer in the crosslinking container is a slow-speed paddle stirrer with the blades located in the lower part of the container. This ensures that the material is thoroughly mixed and agitated after being added to the crosslinking solution, allowing for complete crosslinking and achieving sufficient mechanical strength.
[0016] The floating hollow microsphere preparation device provided by the present invention has the advantage of being able to produce floating hollow microspheres in batches and on a large scale. Attached Figure Description
[0017] The present invention will be further described below with reference to the accompanying drawings.
[0018] Figure 1 This is a front view of a floating hollow microsphere preparation device according to the present invention;
[0019] Figure 2 This is a schematic diagram of the material container structure of a floating hollow microsphere preparation device according to the present invention;
[0020] Figure 3This is a schematic diagram of the crosslinking container structure of a floating hollow microsphere preparation device according to the present invention;
[0021] Figure 4 This is a top view of the crosslinking container of a floating hollow microsphere preparation device according to the present invention.
[0022] Explanation of reference numerals in the attached drawings: 1. Material container; 101. Drain of the insulated tank; 102. Heated insulated tank; 102-1. Tank wall; 102-2. Electric heat tracing; 103. Water inlet of the insulated tank; 104. Solution inlet; 105. First stirrer; 106. Solid material inlet; 107. Water bath; 108. Thermometer insertion tube; 109. First support; 110. Water bath outlet; 2. Crosslinking container; 201. Second stirrer; 202. Crosslinking tank; 203. Crosslinking tank outlet; 204. Second support; 205. Iron frame; 3. Peristaltic pump titration device; 3-1. Valve. Detailed Implementation
[0023] To make the technical problems, technical solutions, and beneficial effects of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments.
[0024] like Figure 1 and Figure 2 As shown, this embodiment discloses a floating hollow microsphere preparation device, including a material container 1, which includes a water bath 107. A heating and insulation tank 102 is arranged on the outside of the water bath 107. A first stirrer 105 is arranged inside the water bath 107. A water bath outlet 110 is arranged at the bottom of the water bath 107, and the water bath outlet 110 is connected to a peristaltic pump titration device 3. A crosslinking container 2 is arranged below the peristaltic pump titration device 3. A first support 109 is arranged below the material container 1. In this embodiment, three water bath outlets 110 are provided, and all three water bath outlets 110 are connected to the peristaltic pump titration device 3 through pipes. The design of three water bath outlets 110 allows multiple peristaltic pumps to be connected simultaneously without mutual interference, and also ensures normal operation even if one water bath outlet 110 is blocked.
[0025] A solution inlet 104 and a solid material inlet 106 are provided above the water bath 107. A heating and insulation tank 102 is provided on the outer side of the tank wall below the solution inlet 104 and the solid material inlet 106. A water inlet 103 is provided on the top of the heating and insulation tank 102, and a drain outlet 101 is provided on the bottom of the heating and insulation tank 102.
[0026] The heating and insulation tank 102 includes a tank wall 102-1, and an electric heat tracing device 102-2 is applied to the outer side of the tank wall 102-1. The electric heat tracing device 102-2 can heat and maintain the temperature when energized. In addition, water is added between the tank wall 102-1 and the water bath 107 for auxiliary insulation. The electric heat tracing device 102-2 is existing technology and will not be described in detail here.
[0027] The main body of the peristaltic pump titration device 3 is a peristaltic pump. A valve 3-1 is installed at the outlet of the peristaltic pump. Adjusting the valve 3-1 can control the titration speed. The peristaltic pump is an existing technology and will not be described in detail here.
[0028] In this embodiment, a thermometer insertion tube 108 is provided on the lower part of the side wall of the water bath 107, and the outer end of the thermometer insertion tube 108 penetrates through the heating and insulation tank 102. The thermometer insertion tube 108 is 20 to 40 centimeters away from the outlet 110 of the water bath, and a thermometer can be placed inside the thermometer insertion tube 108 for real-time monitoring of the temperature of the mixed materials.
[0029] In this embodiment, the first stirrer 105 is a built-in wall-scraping stirrer, which is used to prevent the viscous mixed solution from sticking to the wall after heating. The rotation speed of the first stirrer 105 is set to 100-150 r / min.
[0030] like Figure 3 and Figure 4 As shown, the crosslinking container 2 has an open structure. The crosslinking container 2 includes a crosslinking barrel 202. An iron frame 205 is provided at the upper port of the crosslinking barrel 202. A second stirrer 201 is provided on the iron frame 205. A crosslinking barrel outlet 203 is provided at the bottom of the crosslinking barrel 202. A second support 204 is provided below the crosslinking barrel 202.
[0031] The second stirrer 201 is placed in a staggered manner from the first stirrer 105, with the second stirrer 201 10 to 30 centimeters away from the outer wall of the heating and insulation tank 102. The staggered placement design can prevent the second stirrer 201 from causing the viscous mixed solution dripping from the water bath outlet 110 of the material container 1 and the peristaltic pump titration device 3 to not drip into the cross-linking solution, thus preventing the microspheres from forming.
[0032] In this embodiment, the second agitator 201 is a slow-speed paddle agitator with a distance of 20 to 40 centimeters between the paddle blades and the discharge port, and a rotation speed of 50-100 r / min.
[0033] The method of using the floating hollow microsphere preparation device provided by the present invention includes the following steps:
[0034] Polyvinyl alcohol, sodium alginate, attapulgite / biochar, and other materials are added to material container 1 through the solid material inlet 106, while water and other materials are added to material container 1 through the solution inlet 104. Polyvinyl alcohol and sodium alginate are heated and dissolved in material container 1, and then stirred evenly with other materials using the first stirrer 105. The mixed materials are titrated by a peristaltic pump titration device 3, and then cross-linked in a boric acid / calcium chloride solution in cross-linking container 2 to prepare floating hollow microspheres. After settling, the solution and the floating hollow microspheres are collected through the cross-linking tank outlet 203, then separated by a filter, washed with water, and dried or sun-dried below 50°C to obtain the microsphere material.
[0035] Combination Figures 1 to 4 The working principle of this invention is as follows:
[0036] The microsphere material mainly comprises a hollow cross-linked polymer microsphere framework obtained by cross-linking polyvinyl alcohol and sodium alginate, and adsorbent materials such as attapulgite / biochar loaded inside the hollow cross-linked polymer microsphere framework. In the preparation apparatus of this invention, after adding the cross-linking agent and adsorbent material to the material container 1, the mixture is dissolved by heating the insulated tank 102 and stirred and mixed by the first stirrer 105, so that the adsorbent material is uniformly loaded onto the cross-linking agent. That is, the main function of the material container 1 is to dissolve the polyvinyl alcohol and sodium alginate framework material and successfully load the adsorbent material. The mixed material is added dropwise into the cross-linking solution in the cross-linking container 2 via the peristaltic pump titration device 3. That is, the main function of the peristaltic pump titration device 3 is to allow the material to slowly form drops for further cross-linking. The dripped mixed material is stirred and allowed to stand in the cross-linking solution to allow the material to fully cross-link and form, so as to achieve sufficient mechanical strength. That is, the main function of the cross-linking container 2 is to allow the material to fully cross-link, form, and achieve sufficient mechanical strength through the ion exchange of calcium ions and sodium ions. Thus, a floating hollow microsphere material with heavy metal adsorption properties is prepared.
[0037] The specific process flow of this embodiment is as follows:
[0038] 1. Dissolve 8.5 kg of sodium carbonate in 5 L of water to prepare a sodium carbonate solution; add 1500 L of water, 55 kg of boric acid, and 15 kg of calcium chloride to crosslinking container 2, turn on the second stirrer 201 in crosslinking container 2 to dissolve all the reagents, then add the prepared sodium carbonate solution and continue stirring for 10 minutes, then turn off the second stirrer 201.
[0039] 2. Add 1185L of water to material container 1 through solution inlet 104. Add 115.2kg of polyvinyl alcohol (PVA) and 2.28kg of sodium alginate to material container 1 through solid material inlet 106. Turn on the first stirrer 105 in material container 1. After the electric heating element 102-2 is energized, raise the temperature of water bath 107 to 90℃, and then continue heating for 2 hours to dissolve and mix the materials.
[0040] 3. After heating is complete, turn off the first agitator 105 in material container 1 and turn off the electric heating tracing 102-2 for fifteen minutes to allow the material in the heating and insulation tank 102 to cool down slightly. Open the solid material inlet 106, add 48 kg of biochar, turn on the first agitator 105 to continue stirring, and use the heating and insulation tank 102 to maintain the temperature of material container 1 at about 65°C. Specifically, when the temperature reaches 65°C, turn off the electric heating tracing 102-2 and keep the temperature warm by the water between the tank wall 102-1 and the water bath 107. When the temperature drops below 65°C, turn on the electric heating tracing 102-2 to reheat and raise the temperature to 65°C.
[0041] 4. Turn on the second stirrer 201 in crosslinking container 2, and open the water bath outlet 110 at the bottom of material container 1 to allow the mixed viscous solution in material container 1 to enter the peristaltic pump titration device 3 and drip into crosslinking container 2. Control the dripping rate through valve 3-1 to ensure that the material drips in droplets and does not form a continuous stream. After all the material in material container 1 has dripped, close the water bath outlet 110. After the second stirrer 201 in crosslinking container 2 continues stirring for another hour, turn off the second stirrer 201.
[0042] 5. Continue to let the material stand in crosslinking container 2 for 24 hours. Open the discharge port 203 of the crosslinking tank. The solution and the floatable hollow microsphere material are collected through the discharge port 203. After separation by a filter, the microsphere material can be obtained. Rinse the collected microsphere material twice with water, and finally dry it at 50°C to obtain floatable hollow microspheres for reducing heavy metals in soil. In this embodiment, the equipment capacity is 170 kg / day. The hardness of the prepared material and its performance in removing heavy metals from soil both meet the requirements of patent CN117244535B.
[0043] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims
1. A device for preparing floating hollow microspheres, characterized in that: The material container (1) includes a water bath (107), a heating and heat preservation tank (102) is provided on the outside of the water bath (107), a first stirrer (105) is provided inside the water bath (107), a water bath outlet (110) is provided at the bottom of the water bath (107), the water bath outlet (110) is connected to a peristaltic pump titration device (3), and a crosslinking container (2) is provided below the peristaltic pump titration device (3). The crosslinking container (2) has an open structure. The crosslinking container (2) includes a crosslinking barrel (202). An iron frame (205) is provided at the upper port of the crosslinking barrel (202). A second stirrer (201) is provided on the iron frame (205). A crosslinking barrel outlet (203) is provided at the bottom of the crosslinking barrel (202). A second support (204) is provided below the crosslinking barrel (202). The second stirrer (201) is placed in a staggered position from the first stirrer (105); the second stirrer (201) is a slow-speed paddle stirrer; The water bath (107) is provided with a solution inlet (104) and a solid material inlet (106) above it. The heating and heat preservation tank (102) is provided on the outer side of the tank wall below the solution inlet (104) and the solid material inlet (106) of the water bath (107). The heating and heat preservation tank (102) is provided with a heat preservation tank water inlet (103) at the top and a heat preservation tank drain outlet (101) at the bottom. The heating and heat preservation tank (102) includes a tank wall (102-1), and an electric heat tracing (102-2) is applied to the outer side of the tank wall (102-1). A thermometer insertion tube (108) is provided on the lower side wall of the water bath (107), and the outer end of the thermometer insertion tube (108) penetrates the heating and heat preservation barrel (102). The first agitator (105) is a built-in wall-scraping agitator; A first support (109) is provided below the material container (1); There are three water bath outlets (110), and all three water bath outlets (110) are connected to the peristaltic pump titration device (3) through pipes.
Citation Information
Patent Citations
Preparation of floating hollow microsphere materials and their application in soil cadmium reduction
CN117244535B
Preparation of floatable hollow microsphere material and application of floatable hollow microsphere material in soil cadmium reduction
CN117244535A
Dissolving and stirring device for coating material
CN210964765U
Full-automatic sodium alginate immobilized microsphere preparation device
CN219482599U
Polyacrylate synthesis reaction kettle
CN221334155U