Preparation process of medical nanoscale ultra-high-purity high-surface-area mesoporous silica material

Through hydrothermal reaction and multiple calcination of nano-adjusted agent materials with ethyl orthosilicate, ammonium bicarbonate, etc., mesoporous silica is prepared with high surface area, small particle size, and low drug loading and slow removal speed of existing mesoporous silica materials, and the application of high-efficiency drug carriers is achieved.

CN120398076AActive Publication Date: 2025-08-01WUXI GUANGWEI SEMICONDUCTOR MATERIALS CO LTD
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Patent Information

Application Number
CN202510609024.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-13
Publication Date
2025-08-01
Estimated Expiration
2045-05-13

AI Technical Summary

Technical Problem

The existing mesoporous silica materials have small specific surface area and large particle size, which leads to low drug load and slow removal speed in the body, which may cause potential harm to the body.

Method used

The nano-adjusting material is combined with ethyl orthosilicate, ammonium bicarbonate, etc., and a high surface area mesoporous silica is formed through hydrothermal reaction and multiple calcination. The carbon nanotubes and graphene oxide nanosheets in the nano-adjusting material are used to form a supporting framework to increase porosity and stabilize the structure.

Benefits of technology

Prepare small-particle mesoporous silica with high purity and high surface area to increase the load of drugs, easily remove in the body, and reduce the harm to the body.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of preparation of nano materials, in particular to a preparation process of a medical nanoscale ultra-high-purity high-surface-area mesoporous silica material, which specifically comprises the following steps: adding a nano auxiliary material into a template agent, fully mixing, adding the mixture, a silicon source and a basic catalyst into deionized water, and carrying out heating reaction to obtain the nano-grade ultra-high-purity high-surface-area mesoporous silica material. And after centrifugal drying, transferring into a tubular furnace for calcining, then carrying out secondary calcining under the condition of sufficient oxygen and under the action of oscillation, and then carrying out magnetic separation and screening. The prepared mesoporous silica is high in purity, large in surface area and small in particle size, has very high loading capacity when being applied to a medicine carrier, and does not cause potential harm to an organism due to the fact that the mesoporous silica is small in particle size and relatively high in in-vivo clearing speed.
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Description

Technical Field

[0001] The present invention relates to the technical field of the preparation of nanomaterials, and particularly to a preparation process of a medical nano-level ultra-high purity and high surface area mesoporous silica material. Background Art

[0002] The rapid development of nanobiology has promoted the preparation of various nanomaterial systems with different morphologies and compositions that can be used as nano-drugs. Mesoporous silica nanoparticles have been widely used in research fields such as drug delivery, bioimaging, biosensing, and the combined treatment of cancer due to their advantages such as large specific surface area, high pore volume, uniformly adjustable pore size, easily chemically modified inner and outer surfaces, excellent thermal / chemical stability, and good biosafety. At present, being used as a drug carrier is one of the most important applications of mesoporous silica in the medical field. Various drugs such as anticancer drugs, antibiotics, and anti-inflammatory drugs can be loaded into the mesoporous channels to achieve the slow release and controlled release of drugs, improve the efficacy of drugs, and reduce the toxic and side effects of drugs. It is also possible to make the drug carrier specifically recognize and bind to the surface of diseased cells by surface modification of targeting molecules such as antibodies, polypeptides, and nucleic acid aptamers to achieve targeted drug delivery.

[0003] For example, Chinese Patent CN102992329A uses sodium dodecylbenzenesulfonate (SDBS) as a surfactant and utilizes the three-dimensional guiding template effect during the polymerization of urea-formaldehyde resin to synthesize a urea-formaldehyde resin-silica composite microsphere. After the composite microsphere is soaked in a tetraethyl orthosilicate alcohol solution, it is calcined at 600 °C to obtain a mesoporous silica microsphere, but the particle size is relatively large, between 2.0 - 7.2 μm, and the specific surface area is only about 500 m 2 / g; when this mesoporous silica is used as a drug carrier, due to its small specific surface area, the drug loading amount is low, and its relatively large particle size results in a relatively slow clearance rate in the body, and long-term accumulation may cause potential harm to the body. Summary of the Invention

[0004] Aiming at the technical problems existing in the prior art, the purpose of the present invention is to provide a preparation process of a medical nano-level ultra-high purity and high surface area mesoporous silica material, which has a high surface area and a small particle size. When used as a drug carrier, it not only has a high loading amount, but also is easily cleared in the body and will not cause harm to the body.

[0005] To achieve the above purpose, the present invention provides the following technical solutions: A preparation process of a medical nano-level ultra-high purity and high surface area mesoporous silica material specifically includes the following steps: The nano-additive material is added to the template, mixed thoroughly, and then added to deionized water together with a silicon source and an alkaline catalyst for heating reaction. After centrifugal drying, it is transferred to a tube furnace for calcination, and then a second calcination is carried out under sufficient oxygen conditions and oscillation, and finally it is sieved by magnetic separation.

[0006] As a further preferred embodiment of the present invention, the ratio of the nano-auxiliary material, template, silicon source, alkaline catalyst and deionized water is (1-2) g: (18-26) mL: (4-7) mL: (0.36-0.45) g: (25-35) mL.

[0007] As a further preferred embodiment of the present invention, the heating reaction temperature is 70-75°C and the reaction time is 3-5h; The calcination temperature is 550-560°C and the calcination time is 6-8h; The secondary calcination temperature is 700-720°C and the calcination time is 8-10h; The oscillation speed is 1500-200r / min.

[0008] As a further preferred embodiment of the present invention, the silicon source is selected from tetraethyl orthosilicate; The alkaline catalyst is selected from ammonium bicarbonate; The template agent is composed of hexadecyltrimethylammonium bromide, cyclohexane, and isopropyl alcohol in a ratio of (1.0-1.6) g: (16-20) mL: (2-3) mL.

[0009] As a further preferred embodiment of the present invention, the preparation method of the nano auxiliary material is as follows: 1) Dissolve ferric chloride hexahydrate, anhydrous sodium acetate, and polyethylene glycol in ethylene glycol. After complete dissolution, add deionized water and stir evenly to obtain a reaction solution. 2) Adding carbon nanotubes to the reaction solution, stirring and dispersing for 10-15 minutes, then transferring to a reactor, sealing, and heating at 198-200°C for 12-15 hours under intermittent ultrasonication. After the reaction is completed, naturally cooling to room temperature, centrifuging, collecting the product with a magnet, repeatedly washing with ethanol and deionized water, and drying to obtain a magnetic carbon nanotube composite material; 3) adding graphene oxide to deionized water and ultrasonically dispersing the mixture for 30-50 minutes, then adding ferrous chloride tetrahydrate and ferric chloride hexahydrate, stirring for 40-60 minutes, heating the mixture to 90-93°C, adding sodium hydroxide solution, and continuing to stir and react for 60-90 minutes. After the reaction is complete, the mixture is naturally cooled to room temperature, separated, washed, and then dried to obtain magnetic graphene nanosheets; 4) Add 3 - 5 g of magnetic carbon nanotube composite material into 200 - 500 mL of deionized water. After sufficient stirring, add 5 - 10 g of magnetic graphene nanosheets. After mechanical stirring at 1000 - 1500 r / min for 1 - 2 h, then perform ultrasonic treatment at 500 - 800 W for 1 - 2 h. After the treatment is completed, centrifuge and separate the product, and dry it to obtain the nano - additive material.

[0010] Furthermore, in step 1), the ratio of the reaction solution, ferric chloride hexahydrate, sodium acetate anhydrous, polyethylene glycol, ethylene glycol, and deionized water is (2.0 - 2.8) g : (2.8 - 3.5) g : (1.5 - 1.9) g : (70 - 100) mL : (10 - 15) mL.

[0011] Furthermore, in step 2), the ratio of the carbon nanotubes to the reaction solution is (2 - 3) g : (60 - 80) mL; For the stirring and dispersion, the rotation speed is 300 - 500 r / min.

[0012] Furthermore, in step 2), for the intermittent ultrasonic action, the power is 200 - 300 W, the intermittent interval is 10 - 15 min, and the intermittent action time is 20 - 30 min.

[0013] Furthermore, in step 3), the ratio of graphene oxide, deionized water, ferrous chloride tetrahydrate, ferric chloride hexahydrate, and sodium hydroxide solution is (1 - 2) g : (100 - 200) mL : (1 - 2) g : (3 - 6) g : (3.5 - 7.0) mL; [[ID=and the concentration of the sodium hydroxide solution is 0.1 - 0.3 mol / L; For the ultrasonic dispersion, the power is 200 - 300 W; For the stirring, the rotation speed is 300 - 500 r / min.

[0014] Furthermore, in step 4), the ratio of the magnetic carbon nanotube composite material, deionized water, and magnetic graphene nanosheets is (3 - 5) g : (200 - 500) mL : (5 - 10) g; For the mechanical stirring, the rotation speed is 1000 - 1500 r / min; For the ultrasonic treatment, the power is 500 - 800 W.

[0015] Compared with the prior art, the beneficial effects of the present invention are: In the present invention, tetraethyl orthosilicate is used as the silicon source, ammonium bicarbonate is used as the basic catalyst, cetyltrimethylammonium bromide, cyclohexane and isopropanol form the template agent, and a nano additive material is added. The reaction is carried out under hydrothermal conditions, and the template agent is removed by primary calcination of the product to obtain mesoporous nano-silica. Then, secondary calcination is carried out under sufficient air and oscillation conditions, so that the carbon-containing components in the nano additive material are combusted and decomposed, thereby causing the structure of the nano additive material to collapse inside the mesoporous nano-silica. Moreover, through subsequent magnetic separation and screening, the residual magnetic iron tetroxide can be removed. Also, due to the fact that in the secondary calcination, the carbon-containing components are fully combusted, the generated gases such as carbon dioxide cause an increase in the internal pressure of the mesoporous nano-silica. At the same time, the residual magnetic iron tetroxide will continuously collide with the inner wall of the mesoporous nano-silica under the action of high-speed oscillation, which leads to the easy collapse of the structure of the mesoporous nano-silica, forming small particle products, so that nano-sized mesoporous silica with high purity and high specific surface area can be obtained.

[0016] In the nano - additive material of the present invention, carbon nanotubes are used as the matrix material. A large amount of nano - magnetite is deposited on the matrix material by the hydrothermal method. And because there are a large number of small - hole - like defects on the wall of the carbon nanotubes, it just provides sites for the deposition and embedding of nano - magnetite, so that the generated nano - magnetite can be embedded into the defects on the tube wall, improving the bonding strength between the two. Thus, a firm and stable nano - particle deposition layer is formed on the wall of the carbon nanotubes, greatly increasing the surface roughness of the carbon nanotubes. And by using intermittent ultrasonic action, a local high - pressure environment can be generated, promoting the progressive batch - by - batch embedding of nano - magnetite into the tube - wall defects of the carbon nanotubes. This not only makes the formed deposition layer more regular, but also makes the structure more stable, which is beneficial to the subsequent embedding and combination of nano - sheets. Then, by using the chemical co - precipitation method, nano - magnetite is deposited on the sheet - like structure of graphene oxide to prepare magnetic graphene oxide nano - sheets. With deionized water as the medium, through high - speed mechanical stirring and ultrasonic treatment, the generated impact force causes the two to collide. The sheet - like structure of the magnetic graphene oxide nano - sheets is easily embedded into the nano - particle deposition layer on the surface of the magnetic carbon nanotube composite material, so that physical combination is likely to occur between the two, forming a nano - additive material with a stable structure. By introducing this nano - additive material into the hydrothermal reaction, the nano - additive material can form a network structure through the mutual entanglement of carbon nanotubes, thus forming a support framework in the mesoporous nano - silica of the reaction product. After subsequent secondary calcination, the carbon nanotubes in the framework structure will burn and decompose, forming pores in the mesoporous nano - silica, which helps to increase the porosity of the product. At the same time, the graphene oxide nano - sheets in the framework structure will burn and decompose, forming sheet - like pore defects on the pore walls of the product. With the formation of a large number of sheet - like pore defects, not only the porosity of the product is further increased, but also the pore - wall thickness is reduced, resulting in the mesoporous nano - silica structure being more likely to collapse, making the particle size of the mesoporous silica miniaturized, and thus it is easier to obtain small - particle - size mesoporous silica with a high surface area. Detailed implementation mode

[0017] The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.

[0018] In the embodiments of the present invention, the silicon source is selected from tetraethyl orthosilicate; the basic catalyst is selected from ammonium bicarbonate; the template agent is composed of cetyltrimethylammonium bromide, cyclohexane, and isopropanol in a ratio of 1.2 g: 18 mL: 2.6 mL.

[0019] Example 1 A preparation process for medical nano-scale ultra-high purity and high surface area mesoporous silica material comprises the following steps: 1 g of nano-additive material was added to 18 mL of template agent, mixed thoroughly, and then added to 25 mL of deionized water together with 4 mL of silicon source and 0.36 g of alkaline catalyst. The mixture was heated at 70 ° C for 3 h, and then centrifuged and dried. The mixture was transferred to a tube furnace and calcined at 550 ° C for 6 h. Then, under sufficient oxygen conditions, the mixture was oscillated at 1500 r / min and calcined for a second time at 700 ° C for 8 h. The mixture was then sieved by magnetic separation. Wherein, the preparation method of nano auxiliary material is as follows: 1) Dissolve 2.0 g of ferric chloride hexahydrate, 2.8 g of anhydrous sodium acetate, and 1.5 g of polyethylene glycol in 70 mL of ethylene glycol. After complete dissolution, add 10 mL of deionized water and stir to obtain a reaction solution. 2) Add 2 g of carbon nanotubes to 60 mL of the reaction solution, stir and disperse at 300 rpm for 10 min, then transfer to a reactor, seal, and heat at 198°C for 12 h under 200 W intermittent ultrasonication. After the reaction is completed, naturally cool to room temperature, centrifuge, collect the product with a magnet, repeatedly wash with ethanol and deionized water, and dry to obtain a magnetic carbon nanotube composite material. The intermittent ultrasonication interval is 10 min, and the intermittent action time is 20 min. 3) 1 g of graphene oxide was added to 100 mL of deionized water and ultrasonically dispersed at 200 W for 30 minutes. Then, 1 g of ferrous chloride tetrahydrate and 3 g of ferric chloride hexahydrate were added. After stirring at 300 r / min for 40 minutes, the temperature was raised to 90°C, and 3.5 mL of 0.1 mol / L sodium hydroxide solution was added. The stirring reaction was continued for 60 minutes. After the reaction was completed, the mixture was naturally cooled to room temperature, separated, washed, and dried to obtain magnetic graphene nanosheets. 4) Add 3 g of magnetic carbon nanotube composite material to 200 mL of deionized water, stir thoroughly, then add 5 g of magnetic graphene nanosheets. After mechanical stirring at 1000 rpm for 1 hour, ultrasonic treatment at 500 W for 1 hour is performed. After the treatment is completed, the product is centrifuged and dried to obtain the nano-additive material.

[0020] Example 2 A preparation process for medical nano-scale ultra-high purity and high surface area mesoporous silica material comprises the following steps: Add 1.5 g of nano-additive material to 23 mL of template agent. After thorough mixing, add it together with 5 mL of silicon source and 0.42 g of alkaline catalyst to 30 mL of deionized water. Heat and react at 72 °C for 4 h. Then, after centrifugal drying, transfer it to a tubular furnace and calcine at 555 °C for 7 h. Then, under sufficient oxygen conditions, perform secondary calcination at 710 °C for 9 h under the oscillation of 1800 r / min. After that, perform magnetic separation and screening to obtain the product; Among them, the preparation method of the nano-additive material is as follows: 1) Dissolve 2.5 g of ferric chloride hexahydrate, 3.2 g of anhydrous sodium acetate, and 1.7 g of polyethylene glycol in 80 mL of ethylene glycol. After complete dissolution, add 13 mL of deionized water and stir evenly to obtain a reaction solution; 2) Add 2.5 g of carbon nanotubes to 70 mL of the reaction solution, stir and disperse at 400 r / min for 13 min, then transfer it to a reaction kettle, seal it, and heat and react at 200 °C for 13 h under the action of 260 W intermittent ultrasound. After the reaction is completed, naturally cool to room temperature. After centrifugal separation, collect the product with a magnet, wash it repeatedly with ethanol and deionized water, and dry it to obtain a magnetic carbon nanotube composite material. Among them, the intermittent interval of the intermittent ultrasound is 15 min, and the intermittent action time is 25 min; 3) Add 1.5 g of graphene oxide to 150 mL of deionized water, disperse it by ultrasound at 260 W for 40 min, then add 1.5 g of ferrous chloride tetrahydrate and 5 g of ferric chloride hexahydrate, stir at 400 r / min for 50 min, then raise the temperature to 92 °C, and add 5.8 mL of sodium hydroxide solution with a concentration of 0.2 mol / L, continue to stir and react for 70 min. After the reaction is completed, naturally cool to room temperature, separate, wash, and dry to obtain magnetic graphene nanosheets; 4) Add 4 g of magnetic carbon nanotube composite material to 300 mL of deionized water, stir thoroughly, add 7 g of magnetic graphene nanosheets, mechanically stir at 1200 r / min for 1.5 h, and then perform ultrasonic treatment at 700 W for 1.5 h. After the treatment is completed, centrifuge and separate the product, and dry it to obtain the nano-additive material.

[0021] Example 3 A preparation process of a medical nano-level ultra-high purity and high surface area mesoporous silica material specifically includes the following steps: Add 2 g of nano-additive material to 26 mL of template agent. After thorough mixing, add it together with 7 mL of silicon source and 0.45 g of alkaline catalyst to 35 mL of deionized water. Heat and react at 75 °C for 5 h. Then, after centrifugation and drying, transfer it to a tubular furnace and calcine at 560 °C for 8 h. Then, under sufficient oxygen conditions, carry out secondary calcination at 720 °C for 10 h under the oscillation of 2000 r / min, and then perform magnetic separation and screening; Among them, the preparation method of the nano-additive material is as follows: 1) Dissolve 2.8 g of ferric chloride hexahydrate, 3.5 g of anhydrous sodium acetate, and 1.9 g of polyethylene glycol in 100 mL of ethylene glycol. After complete dissolution, add 15 mL of deionized water and stir evenly to obtain a reaction solution; 2) Add 3 g of carbon nanotubes to 80 mL of the reaction solution, stir and disperse at 500 r / min for 15 min, then transfer it to a reaction kettle, seal it, and heat and react at 200 °C for 15 h under the action of 300 W intermittent ultrasound. After the reaction is completed, naturally cool to room temperature. After centrifugal separation, collect the product with a magnet, wash it repeatedly with ethanol and deionized water, and dry it to obtain a magnetic carbon nanotube composite material. Among them, the intermittent interval of the intermittent ultrasound action is 15 min, and the intermittent action time is 30 min; 3) Add 2 g of graphene oxide to 200 mL of deionized water, disperse it by ultrasound at 300 W for 50 min, then add 2 g of ferrous chloride tetrahydrate and 6 g of ferric chloride hexahydrate. After stirring at 500 r / min for 60 min, raise the temperature to 93 °C, and add 7.0 mL of sodium hydroxide solution with a concentration of 0.3 mol / L. Continue to stir and react for 90 min. After the reaction is completed, naturally cool to room temperature. After separation and washing, dry it to obtain magnetic graphene nanosheets; 4) Add 5 g of the magnetic carbon nanotube composite material to 500 mL of deionized water, stir well, add 10 g of magnetic graphene nanosheets, stir mechanically at 1500 r / min for 2 h, and then perform ultrasonic treatment at 800 W for 2 h. After the treatment is completed, centrifuge and separate the product, and dry it to obtain the nano-additive material.

[0022] Comparative Example 1: This comparative example is basically the same as Example 1, except that it does not contain nano-additive material.

[0023] Comparative Example 2: This comparative example is basically the same as Example 1, except that in the preparation of the nano-additive material, carbon nanofibers are used to replace the carbon nanotubes in step 2).

[0024] Comparative Example 3: This comparative example is basically the same as Example 1, except that in the preparation of the nano-additive material, the intermittent ultrasound action in step 2) is omitted.

[0025] Comparative Example 4: This comparative example is basically the same as Example 1, except that in the preparation of the nano-additive material, step 3) is omitted.

[0026] Comparative Example 5: This comparative example is basically the same as Example 1, except that in the preparation of the nano-additive material, mechanical stirring and ultrasonic treatment in step 4) are omitted.

[0027] Test experiment: Weigh 20 mg of the mesoporous silica materials prepared in the above Examples 1-3 and Comparative Examples 1-5 respectively and place them in a conical flask. Pour 15 mL of PBS (pH = 7. ) into the conical flask and disperse it by ultrasonic for 10 min; then weigh 20 mg of human lipase (LIP, average enzyme activity 2000 U / g) and add it to the conical flask, seal and stir at room temperature for 4 h; centrifuge at 4000 rpm, take the supernatant, measure the absorbance at 285 nm with a UV spectrophotometer, and calculate the adsorption rate of the mesoporous silica material to human lipase.

[0028] Calculation of adsorption rate: Absorbance of blank PBS is A1; Prepare a PBS solution of 20 mg of human lipase and measure the absorbance A2; Absorbance of the supernatant is A3; Adsorption rate % = (A3 - A1) / (A2 - A1) × 100%. The specific results are as follows: Results of in vitro lipase adsorption rate As can be seen from the above table, the mesoporous silica prepared in the present invention has a high surface area, small particle size, large loading capacity, and high adsorption rate. When used as a pharmaceutical carrier, it has broad application prospects.

[0029] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor limit the invention to the specific embodiments described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments to better explain the principle and practical application of the present invention, so that those skilled in the relevant art can understand and utilize the present invention well. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A preparation process of a medical nano-level ultra-high purity and high surface area mesoporous silica material, characterized in that, Specifically, it includes the following steps: Add the nano - additive material to the template agent. After thorough mixing, add it together with the silicon source and the alkaline catalyst to deionized water for heating reaction. Then, after centrifugal drying, transfer it to a tubular furnace for calcination. Then, under sufficient oxygen conditions, perform secondary calcination under the action of oscillation, and finally, perform magnetic separation and screening.

2. The preparation process of a medical nano-scale ultra-high purity and high surface area mesoporous silica material according to claim 1, characterized in that, The ratio of the nano - additive material, template agent, silicon source, alkaline catalyst, and deionized water is (1 - 2) g:(18 - 26) mL:(4 - 7) mL:(0.36 - 0.45) g:(25 - 35) mL.

3. The preparation process of a medical nano-level ultra-high purity and high surface area mesoporous silica material according to claim 1, characterized in that, For the heating reaction, the temperature is 70 - 75 °C and the reaction time is 3 - 5 h. For the calcination, the temperature is 550 - 560 °C and the calcination time is 6 - 8 h. For the secondary calcination, the temperature is 700 - 720 °C and the calcination time is 8 - 10 h. For the oscillation, the rotation speed is 1500 - 200 r / min.

4. The preparation process of a medical nano-scale ultra-high purity and high surface area mesoporous silica material according to claim 1, characterized in that, The silicon source is selected from tetraethyl orthosilicate. The alkaline catalyst is selected from ammonium bicarbonate. The template agent is composed of cetyltrimethylammonium bromide, cyclohexane, and isopropanol in a ratio of (1.0 - 1.6) g:(16 - 20) mL:(2 - 3) mL.

5. The preparation process of a medical nano-scale ultra-high purity and high surface area mesoporous silica material according to claim 1, characterized in that, The preparation method of the nano - additive material is as follows: 1) Dissolve ferric chloride hexahydrate, sodium acetate anhydrous, and polyethylene glycol in ethylene glycol. After complete dissolution, add deionized water and stir evenly to obtain a reaction solution. 2) Add carbon nanotubes to the reaction solution, stir and disperse for 10 - 15 min, then transfer it to a reaction kettle, seal it, and under the action of intermittent ultrasound, heat - react at 198 - 200 °C for 12 - 15 h. After the reaction ends, naturally cool to room temperature. After centrifugal separation, collect the product with a magnet, wash it repeatedly with ethanol and deionized water, and dry it to obtain a magnetic carbon nanotube composite material. 3) Add graphene oxide to deionized water, disperse it by ultrasound for 30 - 50 min, then add ferrous chloride tetrahydrate and ferric chloride hexahydrate. After stirring for 40 - 60 min, raise the temperature to 90 - 93 °C, and add sodium hydroxide solution. Continue to stir and react for 60 - 90 min. After the reaction ends, naturally cool to room temperature, separate, wash, and dry to obtain magnetic graphene nanosheets. 4) Add 3 - 5 g of the magnetic carbon nanotube composite material to 200 - 500 mL of deionized water, stir well, then add 5 - 10 g of magnetic graphene nanosheets. After mechanical stirring at 1000 - 1500 r / min for 1 - 2 h, then perform ultrasonic treatment at 500 - 800 W for 1 - 2 h. After the treatment ends, centrifuge and separate the product, and dry it to obtain the nano - additive material.

6. The preparation process of a medical nano-scale ultra-high purity and high surface area mesoporous silica material according to claim 5, characterized in that, In step 1), the ratio of the reaction solution, ferric chloride hexahydrate, sodium acetate anhydrous, polyethylene glycol, ethylene glycol, and deionized water is (2.0 - 2.8) g:(2.8 - 3.5) g:(1.5 - 1.9) g:(70 - 100) mL:(10 - 15) mL.

7. The preparation process of a medical nano-scale ultra-high purity and high surface area mesoporous silica material according to claim 5, characterized in that, In step 2), the ratio of the carbon nanotubes to the reaction solution is (2 - 3) g:(60 - 80) mL. For the stirring and dispersion, the rotation speed is 300 - 500 r / min.

8. The preparation process of a medical nano-level ultra-high purity and high surface area mesoporous silica material according to claim 5, characterized in that, In step 2), for the intermittent ultrasonic action, the power is 200 - 300 W, the intermittent interval is 10 - 15 min, and the intermittent action time is 20 - 30 min.

9. The preparation process of a medical nano-scale ultra-high purity and high surface area mesoporous silica material according to claim 5, characterized in that, In step 3), the ratio of graphene oxide, deionized water, ferrous chloride tetrahydrate, ferric chloride hexahydrate, and sodium hydroxide solution is (1 - 2) g : (100 - 200) mL : (1 - 2) g : (3 - 6) g : (3.5 - 7.0) mL; For the sodium hydroxide solution, the concentration is 0.1 - 0.3 mol / L; For the ultrasonic dispersion, the power is 200 - 300 W; For the stirring, the rotation speed is 300 - 500 r / min.

10. The preparation process of a medical nano-scale ultra-high purity and high surface area mesoporous silica material according to claim 5, characterized in that, In step 4), the ratio of the magnetic carbon nanotube composite material, deionized water, and magnetic graphene nanosheets is (3 - 5) g : (200 - 500) mL : (5 - 10) g; For the mechanical stirring, the rotation speed is 1000 - 1500 r / min; For the ultrasonic treatment, the power is 500 - 800 W.

Citation Information

Patent Citations

  • Mesoporous silica nanosphere, preparation method thereof, and application of nanosphere in drug load

    CN109896528A

  • Preparation method and application method of silicon dioxide nano microspheres

    CN110255573A

  • Ultralow dielectric constant hollow silicon dioxide material for 5G high-frequency and preparation method thereof

    CN111232993A

  • Preparation and application of chitosan modified magnetic nano material

    CN111458429A

  • Method for producing fine silica powder

    JP2016160154A