Preparation method and device of porous silicon dioxide integral material

Abstract

The invention relates to the technical field of silicon dioxide material preparation, in particular to a preparation method and device of a porous silicon dioxide monolithic material.The preparation method comprises the following specific operation steps that a hydrochloric acid aqueous solution is prepared, then a surfactant is dissolved in the hydrochloric acid aqueous solution, and a transparent aqueous phase solution is obtained; the preparation method comprises the following steps: ultrasonically dispersing a silicon dioxide emulsifier into an organic solvent to obtain an oil phase, mixing a water phase solution and the oil phase solution, intensely stirring by a preparation device to obtain a water-in-oil Pickering emulsion, adding a silane coupling agent into the Pickering emulsion, carrying out hydrothermal reaction to remove the residual organic solution, washing with ethanol for several times to remove the redundant silane coupling agent and acid on the surface, and drying to obtain the water-in-oil Pickering emulsion. Calcining to obtain a three-dimensional porous silicon dioxide block material; and the wheel disc, the stirring blades and the inner wall of the separation fixed ring seat are all in an exposed state, so that the homogeneous stirring part can be conveniently and quickly cleaned from the outer side after each use, and no cleaning dead angle is ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of silicon dioxide material preparation, and in particular to a method and a device for preparing a porous silicon dioxide monolithic material. Background Art

[0002] With the rapid development of industrialization, the problem of dye wastewater has become increasingly prominent, causing serious pollution to the water environment. Dye wastewater usually contains a large amount of organic dyes and heavy metal ions. These pollutants are difficult to be naturally degraded and pose a serious threat to the ecological environment and human health. As a new type of porous material, three-dimensional porous silica block material has the characteristics of high specific surface area, high adsorption capacity and good mechanical strength, and has broad application prospects in the field of environmental protection.

[0003] When preparing three-dimensional porous silica bulk materials, the existing preparation methods are usually cumbersome and time-consuming, which is not conducive to large-scale production; moreover, it is difficult to achieve precise control of the pore size, shape and distribution in controlling the pore structure of the three-dimensional porous silica bulk material, which affects the adsorption performance and mechanical strength of the material; and, since the relatively single pore structure will also affect the adsorption performance of the three-dimensional porous silica bulk material; therefore, it is very necessary to design a three-dimensional porous silica bulk material with controllable internal structure and its preparation method and application;

[0004] At the same time, when the solution is homogenously stirred by the preparation device, since the specifications of the device are fixed and the sizes of the containers for storing the solutions are different, when the size of the container is much larger than the homogenous stirring part, the homogenous stirring efficiency of the homogenous stirring part that only moves up and down is low. At the same time, after each use, the homogenous stirring part needs to be cleaned manually. The internal cleaning of the homogenous stirring part is difficult and is prone to contamination residues, which affects subsequent use. Summary of the invention

[0005] The problem to be solved by the present invention is to provide a method for preparing a porous silicon dioxide monolithic material and a device thereof, thereby solving the above-mentioned technical problems.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] A method for preparing a porous silicon dioxide monolithic material, the specific steps of the preparation method are as follows:

[0008] Step 1: prepare a hydrochloric acid aqueous solution, and then dissolve the surfactant in the hydrochloric acid aqueous solution to obtain a transparent aqueous phase solution;

[0009] Step 2: Ultrasonic dispersion of the silica emulsifier in the organic solvent to obtain an oil phase;

[0010] Step 3: The aqueous solution obtained in step 1 and the oil solution obtained in step 2 are mixed, and after strong stirring by the preparation device, an oil-in-water type Pickering emulsion is obtained. The hydraulic cylinder drives the sliding arm to rise and fall in the adjustment groove of the column, and then the height of the wheel disc, the stirring blade and the separation fixed ring seat are adjusted. The aqueous solution obtained in step 1 and the oil solution obtained in step 2 are added to the container, and the container is placed on the base. At this time, the wheel disc, the stirring blade and the separation fixed ring seat are moved down into the solution, and the wheel disc and the stirring blade are driven to rotate by the third motor, and cooperate with the separation fixed ring seat to complete the mixing of the aqueous solution and the oil solution. During homogenous stirring, the sliding seat is driven to rotate by the first motor, and the threaded rod is driven to rotate by the second motor, thereby driving the threaded slider to translate in the sliding groove. The two cooperate, and the wheel disc and the stirring blade are driven to rotate in the sliding groove. The disc, stirring blades and separation fixed ring seat move along a spiral path in the container, and after the homogenization and stirring are completed, the container is moved out of the device. At this time, the first rotating tooth is driven to rotate by the fourth motor, and cooperates with the meshing first external tooth to drive the rotating ring seat to rotate on the fixed ring seat. During the rotation of the fixed ring seat, the arc groove acts on the support rod to drive the support rod to move along the translation groove. At this time, the separation fixed ring seats are separated from each other until the second rotating tooth at the top of the support rod moves to mesh with the inner tooth of the adjustment ring. At this time, the third rotating tooth is driven to rotate by the fifth motor to cooperate with the meshing second external tooth to drive the adjustment ring to rotate. The rotating adjustment ring drives the second rotating tooth to rotate through the internal tooth, and is driven by the support rod to rotate 180°. At this time, the wheel disc, stirring blades and the inner wall of the separation fixed ring seat are all in an exposed state, which is convenient for cleaning with a spray gun.

[0011] Step 4: Add silane coupling agent to the Pickering emulsion obtained in step 3. After the hydrothermal reaction, remove the remaining organic solution, wash with ethanol several times to remove excess silane coupling agent and acid on the surface, dry, and calcine at 550°C for 5h to obtain a three-dimensional porous silica bulk material.

[0012] Preferably, the surfactant is any one of Pluronic F127, Pluronic P123 and TX-10;

[0013] The concentration of the hydrochloric acid aqueous solution is 0.1 to 3.0 mol / L;

[0014] The mass fraction of the surfactant in the aqueous solution is 0.01 to 0.15.

[0015] Preferably, the particle size of the silicon dioxide emulsifier is 20 nm to 60 nm, and the contact angle is 80° to 100°;

[0016] The organic solvent is any one of n-hexane, cyclohexane, toluene and n-octane;

[0017] The mass fraction of the silicon dioxide emulsifier in the organic solvent is 0.01 to 0.2.

[0018] Preferably, the mass ratio of the aqueous phase solution to the oil phase solution is 1:1-5;

[0019] The stirring rate of the preparation device is 200-20000 rpm / min.

[0020] Preferably, the silane coupling agent is any one of methyl orthosilicate, ethyl orthosilicate, and butyl orthosilicate;

[0021] The mass ratio of the silane coupling agent to the silica emulsifier in step 2 is 2 to 8:1.

[0022] The slidable cylinder pressure sensor is installed on the bottom of the support frame, and the slidable cylinder pressure sensor is installed on the bottom of the support frame, and the slidable cylinder pressure sensor is installed on the bottom of the support frame, and the slidable cylinder pressure sensor is installed on the bottom of the support frame, and the slidable cylinder pressure sensor is installed on the bottom of the support frame.

[0023] Preferably, a first motor is installed on the slide arm, and an output end of the first motor is connected to the slide seat;

[0024] A second motor is installed at the end of the slide seat, and a threaded rod is installed at the output end of the second motor located in the slide groove, and the threaded rod is threadedly connected to the slide block.

[0025] Preferably, a third motor is installed on the motor seat, and an output end of the third motor is connected to the stirring shaft.

[0026] Preferably, the outer side of the fixed ring seat is provided with a first outer tooth, the bottom side of the fixed ring seat is provided with a plurality of translation grooves at equal angles, the bottom side of the fixed ring seat is provided with a plurality of T-shaped rails parallel to the translation grooves at equal angles, and the adjustment block is slidably mounted on the T-shaped rails;

[0027] A rotating ring seat is rotatably mounted on the bearing of the fixed ring seat, a fourth motor is mounted on the rotating ring seat, a first rotating tooth is mounted on the output end of the fourth motor, and the first rotating tooth is meshed with the first external tooth.

[0028] Preferably, the rotating ring seat is provided with a plurality of arc grooves at equal angles, and the bottom end of the support rod penetrates the translation groove and the arc groove and is provided with a second rotating tooth;

[0029] The rotating ring seat bearing is rotatably mounted with an adjusting ring, the inner side of the adjusting ring is provided with inner teeth, the outer side of the adjusting ring is provided with second outer teeth, the bottom side of the rotating ring seat is mounted with a fifth motor, the output end of the fifth motor is mounted with a third rotating tooth, and the third rotating tooth is meshed with the second outer tooth.

[0030] The beneficial effects of the present invention are:

[0031] A three-dimensional porous silica bulk material is prepared by a droplet template method. The preparation process is simple, the operation is simple, and large-scale production is easy to achieve. The size and shape of the three-dimensional porous silica bulk material can be adjusted according to demand and the container used, and the mechanical strength is as high as 5.0 to 50N. Such high mechanical strength is due to the hydrolysis-polymerization reaction of the silane coupling agent in the internal space of the droplet and between the droplets to obtain silicon oxide with a three-dimensional network structure. The internal structure of the prepared three-dimensional porous silica bulk material can be adjusted, and a bulk material with a foamy internal structure, a cavity and a hollow structure can be prepared. The control can be achieved by controlling the acid concentration and the hydrothermal temperature. The porosity of the three-dimensional porous silica bulk material can be controlled by adjusting the amount of silicon source and the reaction time. The prepared three-dimensional porous silica bulk material has a multi-level pore structure due to the presence of surfactant assembly and gaps in and between the droplets, which can accelerate the diffusion rate and is beneficial to the adsorption of pollutants.

[0032] The preparation device realizes height adjustment of the homogenizing and stirring part through the operation of the hydraulic cylinder, realizes rotation of the slide seat through the operation of the first motor, and drives the slider to translate in the slide seat through the operation of the second motor. During homogenizing and stirring, the homogenizing and stirring part realizes spiral movement in the container, and fully homogenizes and stirs the solutions in containers of different specifications, thereby greatly improving the efficiency of homogenizing and stirring.

[0033] The fourth motor is used to realize the assembly and separation of multiple separation fixed ring seats. After the multiple separation fixed ring seats are separated, the fifth motor is used to realize the synchronous rotation of the multiple separation fixed ring seats, so that the wheel, stirring blades and the inner wall of the separation fixed ring seat are all in an exposed state, which is convenient for quick cleaning of the homogenization and stirring part from the outside after each use, and ensures that there are no dead angles in the cleaning. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 This is a schematic diagram of the first structure of the preparation device of the present invention;

[0035] Figure 2 This is a second structural schematic diagram of the preparation device of the present invention;

[0036] Figure 3 This is a schematic diagram of the installation structure of the fixed ring seat of the present invention;

[0037] Figure 4 This is a schematic diagram of the installation structure of the rotating ring seat of the present invention;

[0038] Figure 5 This is a schematic diagram of the installation structure of the wheel disc, stirring blades and separation fixed ring seat of the present invention;

[0039] Figure 6 It is a line graph of the absorption rate of the three-dimensional porous silica block material of the present invention.

[0040] Legend:

[0041] 1. Base; 2. Column; 3. Adjustment slot; 4. Slide arm; 5. Hydraulic cylinder; 6. Slide seat; 7. First motor; 8. Slide slot; 9. Sliding block; 10. Second motor; 11. Threaded rod; 12. Fixed frame; 13. Motor seat; 14. Third motor; 15. Stirring shaft; 16. Wheel; 17. Stirring blade; 18. Connecting arm; 19. Fixed ring seat; 20. Adjustment block; 21. Support rod; 22. Separation fixed ring seat; 23. Homogenizing hole; 24. First outer tooth; 25. Translation slot; 26. T-rail; 27. Rotating ring seat; 28. Fourth motor; 29. ​​First rotating tooth; 30. Arc groove; 31. Second rotating tooth; 32. Adjusting ring; 33. Internal tooth; 34. Second outer tooth; 35. Fifth motor; 36. Third rotating tooth. DETAILED DESCRIPTION

[0042] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0043] Specific examples are given below.

[0044] See also Figure 6 , a method for preparing a porous silicon dioxide monolithic material, the specific operation steps of the preparation method are as follows:

[0045] Step 1: preparing a hydrochloric acid aqueous solution, and then dissolving a surfactant in the hydrochloric acid aqueous solution to obtain a transparent aqueous phase solution, wherein the surfactant is any one of Pluronic F127, Pluronic P123 and TX-10, the concentration of the hydrochloric acid aqueous solution is 0.1 to 3.0 mol / L, and the mass fraction of the surfactant in the aqueous solution is 0.01 to 0.15;

[0046] Step 2: ultrasonically dispersing a silica emulsifier into an organic solvent to obtain an oil phase, wherein the particle size of the silica emulsifier is 20 nm to 60 nm, the contact angle is 80° to 100°, the organic solvent is any one of n-hexane, cyclohexane, toluene, and n-octane, and the mass fraction of the silica emulsifier in the organic solvent is 0.01 to 0.2;

[0047] Step 3: the aqueous solution obtained in step 1 and the oil solution obtained in step 2 are mixed, and after strong stirring by a preparation device, a water-in-oil type Pickering emulsion is obtained, wherein the mass ratio of the aqueous solution to the oil solution is 1:1-5, and the stirring rate of the preparation device is 200-20000 rpm / min;

[0048] Step 4: Add a silane coupling agent to the Pickering emulsion obtained in step 3. After the hydrothermal reaction, remove the remaining organic solution, wash with ethanol several times to remove excess silane coupling agent and acid on the surface, dry, and calcine at 550°C for 5 hours to obtain a three-dimensional porous silica bulk material. The silane coupling agent is any one of methyl orthosilicate, ethyl orthosilicate, and butyl orthosilicate. The mass ratio of the silane coupling agent to the silica emulsifier in step 2 is 2 to 8:1.

[0049] The adsorption amount of methyl blue in the patent document Emulsion-Templated Monoliths Based on PlM-1Monomers: Hierarchical Porosity and Dye Adsorption is 28 mg / g, while the adsorption amount of the present application reaches 76 mg / g.

[0050] See also Figure 1 to Figure 5 The preparation device includes a base 1, a column 2 is installed on the base 1, an adjustment groove 3 is provided on the column 2, a hydraulic cylinder 5 is installed on the side wall of the base 1, and the telescopic end of the hydraulic cylinder 5 is connected to a slide arm 4 slidably installed in the adjustment groove 3, a slide seat 6 is rotatably installed on the bottom side of the outer end of the slide arm 4, a slide groove 8 is provided in the slide seat 6, a slide block 9 is slidably installed in the slide groove 8, a fixed frame 12 is installed on the bottom side of the slide block 9, a motor seat 13 is installed in the fixed frame 12, and a stirring shaft 15 is rotatably installed on the bottom side of the motor seat 13, and the stirring shaft 15 bottom A wheel disc 16 is installed at the end, and a plurality of stirring blades 17 are arranged on the bottom side of the wheel disc 16. A fixed ring seat 19 is installed on the bottom side of the fixed frame 12 through a plurality of connecting arms 18. A plurality of adjusting blocks 20 are slidably installed at equal angles on the bottom side of the fixed ring seat 19, and a support rod 21 is rotatably installed through the adjusting block 20. A separation fixed ring seat 22 is installed at the bottom end of the support rod 21, and a plurality of homogenizing holes 23 are opened on the separation fixed ring seat 22. A plurality of separation fixed ring seats 22 are installed in combination on the outside of the wheel disc 16 and the stirring blade 17.

[0051] A first motor 7 is installed on the slide arm 4, and the output end of the first motor 7 is connected to the slide seat 6. A second motor 10 is installed at the end of the slide seat 6. The output end of the second motor 10 is located in the slide groove 8 and is installed with a threaded rod 11, and the threaded rod 11 is threadedly connected to the slider 9. A third motor 14 is installed on the motor seat 13, and the output end of the third motor 14 is connected to the stirring shaft 15. The height adjustment of the homogenizing and stirring part is achieved through the operation of the hydraulic cylinder 5, the slide seat 6 is rotated through the operation of the first motor 7, and the slider 9 is driven to translate in the slide seat 6 through the operation of the second motor 10. During homogenizing and stirring, the homogenizing and stirring part realizes spiral movement in the container, and fully homogenizes and stirs the solutions in containers of different specifications, thereby greatly improving the efficiency of homogenizing and stirring.

[0052] A first external tooth 24 is arranged on the outer side of the fixed ring seat 19, a plurality of translation grooves 25 are arranged at equal angles on the bottom side of the fixed ring seat 19, a plurality of T-shaped rails 26 parallel to the translation grooves 25 are arranged at equal angles on the bottom side of the fixed ring seat 19, and the adjustment block 20 is slidably mounted on the T-shaped rails 26, a rotating ring seat 27 is rotatably mounted on the fixed ring seat 19, a fourth motor 28 is mounted on the rotating ring seat 27, a first rotating tooth 29 is mounted on the output end of the fourth motor 28, and the first rotating tooth 29 is meshed with the first external tooth 24, a plurality of arc grooves 30 are arranged at equal angles on the rotating ring seat 27, and a second rotating tooth 31 is mounted on the bottom end of the support rod 21 penetrating the translation groove 25 and the arc groove 30, and the rotating ring seat 27 is rotatably mounted on the bearing There is an adjusting ring 32, an inner tooth 33 is arranged on the inner side of the adjusting ring 32, a second outer tooth 34 is arranged on the outer side of the adjusting ring 32, a fifth motor 35 is installed on the bottom side of the rotating ring seat 27, a third rotating tooth 36 is installed on the output end of the fifth motor 35, and the third rotating tooth 36 is meshed with the second outer tooth 34, and the fourth motor 28 is operated to realize the assembly and separation of multiple separation fixed ring seats 22. After the multiple separation fixed ring seats 22 are separated, the fifth motor 35 is operated to realize the synchronous rotation of the multiple separation fixed ring seats 22, and the wheel 16, the stirring blade 17 and the inner wall of the separation fixed ring seat 22 are all in an exposed state, so that the homogenization stirring part can be quickly cleaned from the outside after each use, and it is ensured that there is no dead angle in the cleaning.

[0053] The working principle of the configuration device is as follows: the hydraulic cylinder 5 drives the sliding arm 4 to rise and fall in the adjusting slot 3 of the column 2, thereby adjusting the height of the wheel disc 16, the stirring blade 17 and the separation fixed ring seat 22, and adding the aqueous solution obtained in step 1 and the oil solution obtained in step 2 into the container, and placing the container on the base 1. At this time, the wheel disc 16, the stirring blade 17 and the separation fixed ring seat 22 are moved down into the solution, and the third motor 14 drives the wheel disc 16 and the stirring blade 17 to rotate, and cooperates with the separation fixed ring seat 22 to complete the mixing of the aqueous solution and the oil solution. During homogenous stirring, the first motor 7 drives the sliding seat 6 to rotate, and the second motor 10 drives the threaded rod 11 to rotate, thereby driving the threaded slider 9 to translate in the sliding slot 8. The two cooperate, and the wheel disc 16, the stirring blade 17 and the separation fixed ring seat 22 move along a spiral path in the container, and after the homogenous stirring is completed. After completion, the container is removed from the device. At this time, the first rotating tooth 29 is driven to rotate by the fourth motor 28, and cooperates with the meshing first external tooth 24 to drive the rotating ring seat 27 to rotate on the fixed ring seat 19. During the rotation of the fixed ring seat 19, the arc groove 30 acts on the support rod 21 to drive the support rod 21 to move along the translation groove 25. At this time, the separation fixed ring seat 22 is separated from each other until the second rotating tooth 31 at the top of the support rod 21 moves to mesh with the inner tooth 33 of the adjustment ring 32. At this time, the third rotating tooth 36 is driven to rotate by the fifth motor 35 to cooperate with the meshing second external tooth 34 to drive the adjustment ring 32 to rotate. The rotating adjustment ring 32 drives the second rotating tooth 31 to rotate through the inner tooth 33, and is transmitted through the support rod 21 to drive the separation fixed ring seat 22 to rotate 180°. At this time, the wheel 16, the stirring blade 17 and the inner wall of the separation fixed ring seat 22 are all in an exposed state, which is convenient for cleaning with a spray gun.

[0054] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing a porous silicon dioxide monolithic material, characterized in that: The specific steps of the preparation method are as follows: Step 1: prepare a hydrochloric acid aqueous solution, and then dissolve the surfactant in the hydrochloric acid aqueous solution to obtain a transparent aqueous phase solution; Step 2: Ultrasonic dispersion of the silica emulsifier in the organic solvent to obtain an oil phase; Step 3: The aqueous solution obtained in step 1 and the oil solution obtained in step 2 are mixed, and after being vigorously stirred by a preparation device, an oil-in-water type Pickering emulsion is obtained. The hydraulic cylinder (5) drives the sliding arm (4) to rise and fall in the adjustment groove (3) of the column (2), and then the height of the wheel disc (16), the stirring blade (17) and the separation fixed ring seat (22) are adjusted. The aqueous solution obtained in step 1 and the oil solution obtained in step 2 are added to the container, and the container is placed on the base (1). At this time, the wheel disc (16), the stirring blade (17) and the separation fixed ring seat (22) are adjusted. The third motor (14) drives the wheel disc (16) and the stirring blade (17) to rotate, and cooperates with the separation fixed ring seat (22) to complete the mixing of the aqueous phase solution and the oil phase solution. During homogenous stirring, the first motor (7) drives the slide seat (6) to rotate, and the second motor (10) drives the threaded rod (11) to rotate, thereby driving the threaded slider (9) to translate in the slide groove (8). The two cooperate, and the wheel disc (16), the stirring blade (17) and the separation fixed ring seat (22) are driven to rotate. The device moves along a spiral path in the container, and after homogenization and stirring are completed, the container is removed from the device. At this time, the first rotating tooth (29) is driven to rotate by the fourth motor (28), and cooperates with the meshing first external tooth (24), driving the rotating ring seat (27) to rotate on the fixed ring seat (19). During the rotation of the fixed ring seat (19), the arc groove (30) acts on the support rod (21), driving the support rod (21) to move along the translation groove (25). At this time, the separation fixed ring seats (22) are separated from each other until the second rotating tooth (29) at the top of the support rod (21) is engaged. 31) moves to mesh with the inner teeth (33) of the adjusting ring (32), at which time the third rotating teeth (36) are driven to rotate by the fifth motor (35), and cooperate with the meshed second outer teeth (34) to drive the adjusting ring (32) to rotate, and the rotating adjusting ring (32) drives the second rotating teeth (31) to rotate through the inner teeth (33), and drives the separation fixed ring seat (22) to rotate 180° through the support rod (21), at which time the wheel disc (16), the stirring blade (17) and the inner wall of the separation fixed ring seat (22) are all in an exposed state, which is convenient for cleaning with a spray gun; Step 4: Add silane coupling agent to the Pickering emulsion obtained in step 3. After the hydrothermal reaction, remove the remaining organic solution, wash with ethanol several times to remove excess silane coupling agent and acid on the surface, dry, and calcine at 550°C for 5h to obtain a three-dimensional porous silica bulk material.

2. The method for preparing a porous silicon dioxide monolithic material according to claim 1, characterized in that: The surfactant is any one of Pluronic F127, Pluronic P123 and TX-10; The concentration of the hydrochloric acid aqueous solution is 0.1 to 3.0 mol / L; The mass fraction of the surfactant in the aqueous solution is 0.01 to 0.

15.

3. The method for preparing a porous silicon dioxide monolithic material according to claim 2, characterized in that: The particle size of the silicon dioxide emulsifier is 20nm to 60nm, and the contact angle is 80° to 100°; The organic solvent is any one of n-hexane, cyclohexane, toluene and n-octane; The mass fraction of the silicon dioxide emulsifier in the organic solvent is 0.01 to 0.

2.

4. The method for preparing a porous silicon dioxide monolithic material according to claim 3, characterized in that: The mass ratio of the aqueous phase solution to the oil phase solution is 1:1-5; The stirring rate of the preparation device is 200-20000 rpm / min.

5. The method for preparing a porous silicon dioxide monolithic material according to claim 4, characterized in that: The silane coupling agent is any one of methyl orthosilicate, ethyl orthosilicate and butyl orthosilicate; The mass ratio of the silane coupling agent to the silica emulsifier in step 2 is 2 to 8:

1.

6. The device for preparing a porous silicon dioxide monolithic material according to claim 5, characterized in that: The preparation device is applied to step 3 of claim 1, and the preparation device comprises a base (1), a column (2) is installed on the base (1), an adjustment slot (3) is provided on the column (2), a hydraulic cylinder (5) is installed on the side wall of the base (1), and the telescopic end of the hydraulic cylinder (5) is connected to a slide arm (4) slidably installed in the adjustment slot (3), a slide seat (6) is rotatably installed on the bottom side of the outer end of the slide arm (4), a slide slot (8) is provided in the slide seat (6), a slider (9) is slidably installed in the slide slot (8), a fixed frame (12) is installed on the bottom side of the slider (9), a motor seat (13) is installed in the fixed frame (12), and the bottom side of the motor seat (13) is rotatable. A stirring shaft (15) is installed, a wheel disc (16) is installed at the bottom end of the stirring shaft (15), a plurality of stirring blades (17) are arranged on the bottom side of the wheel disc (16), a fixed ring seat (19) is installed on the bottom side of the fixed frame (12) through a plurality of connecting arms (18), a plurality of adjustment blocks (20) are equiangularly slidably installed on the bottom side of the fixed ring seat (19), and a support rod (21) is rotatably installed in the adjustment block (20), a separation fixed ring seat (22) is installed at the bottom end of the support rod (21), and a plurality of homogenizing holes (23) are opened on the separation fixed ring seat (22), and a plurality of the separation fixed ring seats (22) are assembled and installed on the outside of the wheel disc (16) and the stirring blades (17).

7. A method and device for preparing a porous silicon dioxide monolithic material according to claim 6, characterized in that: A first motor (7) is installed on the slide arm (4), and an output end of the first motor (7) is connected to the slide seat (6); A second motor (10) is installed at the end of the slide seat (6); a threaded rod (11) is installed at the output end of the second motor (10) in the slide groove (8); and the threaded rod (11) is threadedly connected to the slide block (9).

8. A method for preparing a porous silicon dioxide monolithic material and a device thereof according to claim 7, characterized in that: A third motor (14) is mounted on the motor seat (13), and an output end of the third motor (14) is connected to a stirring shaft (15).

9. A method for preparing a porous silicon dioxide monolithic material and a device thereof according to claim 8, characterized in that: The fixed ring seat (19) is provided with a first external tooth (24) on the outside, the fixed ring seat (19) is provided with a plurality of translation grooves (25) at equal angles on the bottom side, the fixed ring seat (19) is provided with a plurality of T-shaped rails (26) parallel to the translation grooves (25) at equal angles on the bottom side, and the adjustment block (20) is slidably mounted on the T-shaped rails (26); A rotating ring seat (27) is rotatably mounted on a bearing on the fixed ring seat (19), a fourth motor (28) is mounted on the rotating ring seat (27), a first rotating tooth (29) is mounted on an output end of the fourth motor (28), and the first rotating tooth (29) is meshed with the first external tooth (24).

10. A method for preparing a porous silicon dioxide monolithic material and a device thereof according to claim 9, characterized in that: The rotating ring seat (27) is provided with a plurality of arc-shaped grooves (30) at equal angles, and the bottom end of the support rod (21) penetrates the translation groove (25) and the arc-shaped groove (30) and is provided with a second rotating tooth (31); The rotating ring seat (27) is rotatably mounted with an adjusting ring (32) on a bearing, the inner side of the adjusting ring (32) is provided with an inner tooth (33), the outer side of the adjusting ring (32) is provided with a second outer tooth (34), a fifth motor (35) is mounted on the bottom side of the rotating ring seat (27), the output end of the fifth motor (35) is provided with a third rotating tooth (36), and the third rotating tooth (36) is meshed with the second outer tooth (34).

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