CN112429740A - Fluorosilane modified silicon dioxide nano material - Google Patents
Fluorosilane modified silicon dioxide nano material Download PDFInfo
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- CN112429740A CN112429740A CN202011351566.0A CN202011351566A CN112429740A CN 112429740 A CN112429740 A CN 112429740A CN 202011351566 A CN202011351566 A CN 202011351566A CN 112429740 A CN112429740 A CN 112429740A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Condensed Matter Physics & Semiconductors (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
A fluorine silane modified silicon dioxide nano material is prepared by graft modifying the particle surface of silicon dioxide by using a modifier, and the raw materials used in the treatment comprise: nano-scale silicon dioxide; and the modifier comprises a silane coupling agent and fluorine modified alkyl silane, wherein the general formula of the silane coupling agent is RSiX3(ii) a The mass part ratio of the modifier to the nano-scale silicon dioxide can be 4-8: 1; the technical key points are that after the silicon dioxide nanometer is modified by the modifier, the product has stable performance and can be stored for a long time; in the operation of extracting the product, the invention can obviously shorten the precipitation time of the product by evaporation and filtration, and simultaneously, the filtered product is uniformly dispersed in a high-speed dispersion machine at a certain temperature, thereby ensuring the perfection of the modification operation and the modificationThe stability and high quality of the material, while the amount of modifier is controllable, allows the data relating to the modified material obtained to be improved at the will of the manufacturer.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a fluorosilane modified silicon dioxide nano material.
Background
The organosilicon material has low surface energy and excellent high and low temperature resistance, aging resistance, hydrophobicity and other performances, and is widely applied to the fields of waterproof protection of building materials, waterproof and antifouling finishing of fabrics and the like; but the organic silicon material is lipophilic in nature and is easy to adsorb oily dirt, so that the cleanliness of the surface of the material is influenced; therefore, in the prior art, the surface of the organic silicon material is modified, so that the surface energy of the material is further reduced while the inherent performance of the organic silicon material is not changed, and the performances of oleophobicity, solvent resistance, antifouling property and the like of the material are enhanced; however, with the improvement of living standard of people, the multifunctional material is more and more emphasized by people, and the performance requirement of the product is higher and higher to adapt to higher and more complex application requirements.
At present, the modified organosilicon material in the prior art has higher cost, complex process and limited applicable base material types; therefore, it is a direction and a subject of research by material workers to modify a material to provide versatility, a simple production process, and a safe use environment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a fluorosilane modified silicon dioxide nano material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a fluorine silane modified silicon dioxide nano material is prepared by graft modifying the particle surface of silicon dioxide by using a modifier, and the raw materials used in the treatment comprise:
nano-scale silicon dioxide; and
the modifier comprises a silane coupling agent and fluorine modified alkyl silane, wherein the general formula of the silane coupling agent is RSiX3(ii) a The mass part ratio of the modifier to the nano-scale silicon dioxide can be 4-8: 1;
the specific modification steps are as follows:
adding the nanoscale silica and water simultaneously to a stirrer; the operations synchronously implemented in the stirring process are as follows: preparing a modifier and a low-boiling point solvent thereof into a spraying solvent;
then putting the mixed liquid in the stirrer into a high-speed centrifuge, and simultaneously carrying out heating treatment in the high-speed centrifuge so as to obtain a filtered product;
and finally, pouring the filtered product into a high-speed dispersion machine for uniform dispersion, connecting an atomizer externally, introducing the atomized spraying solvent into the high-speed dispersion machine for modification treatment, and finally obtaining the modified material.
Preferably, in the general formula of the silane coupling agent, the group represented by R includes one of an amino group, a mercapto group, a vinyl group, an epoxy group, a cyano group, and a methacryloxy group, and the group represented by X includes one of a halogen, an alkoxy group, and an acyloxy group.
Preferably, in the modification step, the specific steps of simultaneously adding the nanoscale silica and water to the stirrer are as follows:
the method comprises the following steps: heating water by using an electric kettle;
step two: selecting the mass part ratio of the nano-scale silicon dioxide to the water as 1: 1-2, and simultaneously pouring water and nano carbon dioxide into a stirrer;
step three: starting a stirrer to stir fully, controlling the stirring time to be 1-2 h, continuously measuring the pH value of the solution in the stirring process, and controlling the pH value of the solution to be 6-7 by adding a neutralizing reagent into the solution.
Preferably, in the first step, the temperature of the heated water is ensured to be 50-70 ℃.
Preferably, in the second step, the rotation speed of the stirrer is 300-.
Preferably, in the modification step,
heating the outer wall of a cylinder of the high-speed centrifuge, assembling a filter plate at the outlet end of the cylinder of the high-speed centrifuge, and simultaneously extracting a product from a mixed liquid in the high-speed centrifuge in an evaporation and filtration mode;
the heating temperature is 70-80 ℃, and the rotating speed of the high-speed centrifuge is 10000-30000 r/min.
In the step of the modification,
the diameter of the particles sprayed by the spray solvent through the atomizer is as follows: 0.1-0.5 μm.
Compared with the prior art, the invention provides a fluorine silane modified silicon dioxide nano material, which has the following beneficial effects:
firstly, after the silicon dioxide nanometer is modified by the modifier, the product has stable performance and can be stored for a long time, and meanwhile, the fluorine-containing group exists in the product, so that the integral material has high chemical stability and has certain aging resistance and high and low temperature resistance;
in the operation of extracting the product, the invention can obviously shorten the product precipitation time by evaporation and filtration, simultaneously uniformly disperse the filtered product in a high-speed dispersion machine at a certain temperature, ensure the perfection of modification operation, ensure the stability and high quality of the modified material, and simultaneously control the quantity of the modifier, so that the related data of the modified material can be improved according to the will of a manufacturer.
The preparation steps and the selected modifier can avoid the phenomenon that the hydrophilic and oleophobic surfaces of the silicon dioxide are difficult to soak and disperse in organic media, and are difficult to play the role of the silicon dioxide when the silicon dioxide is directly filled in the material, and the aging resistance of the modified material can be further improved through modification operation.
Detailed Description
The fluorosilane-modified silica nanomaterial of the present invention is not limited to the description of the following examples.
In this embodiment, a specific structure of a fluorinated silane modified silica nanomaterial is provided, and a fluorinated silane modified silica nanomaterial is obtained by performing graft modification on the particle surface of silica by using a modifier, and when performing treatment, the used raw materials include:
nano-scale silicon dioxide; and
the modifier comprises a silane coupling agent and fluorine modified alkyl silane, wherein the general formula of the silane coupling agent is RSiX3(ii) a The mass part ratio of the modifier to the nano-scale silicon dioxide can be 6: 1;
the specific modification steps are as follows:
adding nanoscale silica and water simultaneously into a stirrer; the operations synchronously implemented in the stirring process are as follows: preparing a modifier and a low-boiling point solvent thereof into a spraying solvent;
then putting the mixed liquid in the stirrer into a high-speed centrifuge, and simultaneously carrying out heating treatment in the high-speed centrifuge so as to obtain a filtered product;
and finally, pouring the filtered product into a high-speed dispersion machine for uniform dispersion, connecting an atomizer externally, introducing the atomized spraying solvent into the high-speed dispersion machine for modification treatment, and finally obtaining the modified material.
After the silicon dioxide nanometer is modified by the modifier, the product has stable performance and can be stored for a long time, and meanwhile, the fluorine-containing group exists in the product, so that the integral material has high chemical stability and has certain aging resistance and high and low temperature resistance;
the preparation steps and the selected modifier can avoid the phenomenon that the hydrophilic and oleophobic surfaces of the silicon dioxide are difficult to soak and disperse in organic media and are difficult to play the role of the silicon dioxide when the silicon dioxide is directly filled into the material, and the aging resistance of the modified material can be further improved through modification operation.
In the general formula of the silane coupling agent, the group represented by R comprises one of amino, mercapto, vinyl, epoxy, cyano and methyl-propyl-vinyl-oxy, and the group represented by X comprises one of halogen, alkoxy and acyloxy.
In the modification step, the specific steps of simultaneously adding the nanoscale silica and water into the stirrer are as follows:
the method comprises the following steps: heating water by using an electric kettle;
step two: selecting the mass part ratio of the nano-scale silicon dioxide to the water as 1: 1-2, and simultaneously pouring water and nano carbon dioxide into a stirrer;
step three: starting a stirrer to stir fully, controlling the stirring time to be 1-2 h, continuously measuring the pH value of the solution in the stirring process, and controlling the pH value of the solution to be 6-7 by adding a neutralizing reagent into the solution.
In step one, the temperature of the heated water is ensured to be 50-70 ℃.
In the second step, the rotation speed of the stirrer is 300-500 r/min.
In the step of modification, the reaction mixture is subjected to a reaction,
heating the outer wall of a cylinder of the high-speed centrifuge, assembling a filter plate at the outlet end of the cylinder of the high-speed centrifuge, and simultaneously extracting a product from a mixed liquid in the high-speed centrifuge in an evaporation and filtration mode;
the heating temperature is 70-80 ℃, and the rotating speed of the high-speed centrifuge is 10000-30000 r/min.
In the step of modification, the reaction mixture is subjected to a reaction,
the diameter of the particles sprayed by the spray solvent through the atomizer is as follows: 0.1-0.5 μm.
In the operation of extracting the product, the invention can obviously shorten the precipitation time of the product by evaporation and filtration, simultaneously uniformly disperse the filtered product in a high-speed dispersion machine at a certain temperature, ensure the perfection of the modification operation, ensure the stability and high quality of the modified material, and simultaneously control the quantity of the modifier, so that the related data of the modified material can be improved according to the will of a manufacturer.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (7)
1. A fluorine silane modified silicon dioxide nano material is characterized in that: the particle surface of the silicon dioxide is subjected to graft modification by using a modifier, and when the modification is carried out, the raw materials used comprise:
nano-scale silicon dioxide; and
the modifier comprises a silane coupling agent and fluorine modified alkyl silane, wherein the general formula of the silane coupling agent is RSiX3(ii) a The mass part ratio of the modifier to the nano-scale silicon dioxide can be 4-8: 1;
the specific modification steps are as follows:
adding the nanoscale silica and water simultaneously to a stirrer; the operations synchronously implemented in the stirring process are as follows: preparing a modifier and a low-boiling point solvent thereof into a spraying solvent;
then putting the mixed liquid in the stirrer into a high-speed centrifuge, and simultaneously carrying out heating treatment in the high-speed centrifuge so as to obtain a filtered product;
and finally, pouring the filtered product into a high-speed dispersion machine for uniform dispersion, connecting an atomizer externally, introducing the atomized spraying solvent into the high-speed dispersion machine for modification treatment, and finally obtaining the modified material.
2. The fluorosilane-modified silica nanomaterial according to claim 1, wherein: in the general formula of the silane coupling agent, the group represented by R comprises one of amino, mercapto, vinyl, epoxy, cyano and methyl-propyl-vinyl-oxy, and the group represented by X comprises one of halogen, alkoxy and acyloxy.
3. The fluorosilane-modified silica nanomaterial according to claim 1, wherein: in the modification step, the specific steps of simultaneously adding the nanoscale silica and water into the stirrer are as follows:
the method comprises the following steps: heating water by using an electric kettle;
step two: selecting the mass part ratio of the nano-scale silicon dioxide to the water as 1: 1-2, and simultaneously pouring water and nano carbon dioxide into a stirrer;
step three: starting a stirrer to stir fully, controlling the stirring time to be 1-2 h, continuously measuring the pH value of the solution in the stirring process, and controlling the pH value of the solution to be 6-7 by adding a neutralizing reagent into the solution.
4. The fluorosilane-modified silica nanomaterial according to claim 3, wherein: in the first step, the temperature of the heated water is ensured to be 50-70 ℃.
5. The fluorosilane-modified silica nanomaterial according to claim 3, wherein: in the second step, the rotation speed of the stirrer is 300-500 r/min.
6. The fluorosilane-modified silica nanomaterial according to claim 1, wherein: in the step of the modification,
heating the outer wall of a cylinder of the high-speed centrifuge, assembling a filter plate at the outlet end of the cylinder of the high-speed centrifuge, and simultaneously extracting a product from a mixed liquid in the high-speed centrifuge in an evaporation and filtration mode;
the heating temperature is 70-80 ℃, and the rotating speed of the high-speed centrifuge is 10000-30000 r/min.
7. The fluorosilane-modified silica nanomaterial according to claim 1, wherein: in the step of the modification,
the diameter of the particles sprayed by the spray solvent through the atomizer is as follows: 0.1-0.5 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011351566.0A CN112429740A (en) | 2020-11-26 | 2020-11-26 | Fluorosilane modified silicon dioxide nano material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011351566.0A CN112429740A (en) | 2020-11-26 | 2020-11-26 | Fluorosilane modified silicon dioxide nano material |
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| Publication Number | Publication Date |
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| CN112429740A true CN112429740A (en) | 2021-03-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202011351566.0A Withdrawn CN112429740A (en) | 2020-11-26 | 2020-11-26 | Fluorosilane modified silicon dioxide nano material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116190616A (en) * | 2023-03-30 | 2023-05-30 | 河北坤天新能源股份有限公司 | Silicon-oxygen-carbon composite material for power battery and preparation method thereof |
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2020
- 2020-11-26 CN CN202011351566.0A patent/CN112429740A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116190616A (en) * | 2023-03-30 | 2023-05-30 | 河北坤天新能源股份有限公司 | Silicon-oxygen-carbon composite material for power battery and preparation method thereof |
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Application publication date: 20210302 |