CN113526512A - Silica sol and preparation method thereof - Google Patents
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- CN113526512A CN113526512A CN202110958247.4A CN202110958247A CN113526512A CN 113526512 A CN113526512 A CN 113526512A CN 202110958247 A CN202110958247 A CN 202110958247A CN 113526512 A CN113526512 A CN 113526512A
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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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/141—Preparation of hydrosols or aqueous dispersions
- C01B33/142—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates
- C01B33/143—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates of aqueous solutions of silicates
- C01B33/1435—Preparation of hydrosols or aqueous dispersions by acidic treatment of silicates of aqueous solutions of silicates using ion exchangers
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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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a silica sol and a preparation method thereof, wherein the silica sol comprises hollow silica nanoparticles, the hollow silica nanoparticles are spherical structures and comprise an inner layer and an outer layer, the inner layer is a hollow structure, and the outer layer is a silica shell layer; the diameter of the inner layer cavity is 55 nm-100 nm; the hollow silica sol comprises the following components in percentage by weight: 5 to 10 percent of hollow silicon dioxide nano particles, 0.1 to 0.5 percent of sodium hydroxide and the balance of solvent water. Polyacrylic acid and ammonia water are mixed to form a cation template, a silicon source precursor initiator generates particle growing points on the surface of the template, and finally the addition of active silicic acid is regulated and controlled to realize the controllability of the inner diameter of the cavity and the thickness of the shell layer. The method can prepare the silica sol in one step, and the aqueous dispersion liquid of the silica sol is pollution-free. Meanwhile, the silicon dioxide particle has controllable inner diameter of a cavity and thickness of a shell layer, has good performance, and has wide application prospect in the fields of anti-reflection film products, drug carriers, catalysts and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of functional inorganic nano materials, and relates to a silica sol and a preparation method thereof.
Background
The silica sol has many excellent properties, such as large specific surface area, high adsorptivity, high dispersity, high fire resistance, high insulation, high temperature resistance, oxidation resistance and the like, and in addition, the production raw materials have wide sources, are convenient to produce and have low price. In the field of coatings, silica sol as an inorganic coating and an organic high molecular polymer emulsion have achieved satisfactory effects, and thus have attracted the attention of coating researchers worldwide. By introducing inorganic nano-silica into polymer emulsion, inorganic-organic nano-composite materials with excellent performance can be prepared, which becomes one of the research directions of material workers.
According to the demand of the silica sol market, the gap between China and developed countries in the world in the technical field is found out, and the advanced preparation method of the high-quality silica sol is further researched, so that the method is necessary for expanding the application of the silica sol. Due to the potential application of the inorganic hollow material in white light emitting diodes, medicine controlled release, catalysis and antireflection films, the synthesis of the inorganic hollow material with a novel morphology has gained wide attention worldwide, and the preparation of a hollow silica sol becomes a new research hotspot. In order to meet some of the above application requirements, researchers have synthesized hollow SiO with different sizes and shapes2Many efforts are made in materials.
The template method and the template-free method are two most commonly used methods for synthesizing the hollow SiO2Methods of nanoparticles (HSNs). The templateless approach is generally based on the synthesis of HSNs by some novel mechanism, such as nucleation and growth of pores. The template method is widely known because of the narrow size distribution and the various shapes of the synthesized HSNs. More templates are used, including emulsion droplets, inorganic nanoparticles, macromolecules and surfactant aggregates. TheThe method mainly involves two steps: first, by SiO2The precursor is rapidly hydrolyzed and condensed on the template, usually Tetraethoxysilane (TEOS) reacts to form SiO in alkaline environment2A shell layer forming a core-shell structured particle; the templates are then removed by high temperature calcination, washing or acid etching to finally form the HSNs.
Generally, HSNs of desired size can be prepared by carefully controlling the size of the plates. However, most of the HSNs prepared by the templating method are spherical due to the difficulty in obtaining uniform non-spherical templates. In addition, the existing method for controllably synthesizing the non-spherical monodisperse HSNs is more complicated. The existing method comprises the following steps: using polymer nano rod as template, depositing SiO on it2To prepare hollow SiO2Nanotubes (HSNTs); and (3) synthesizing the HSNTs containing the nickel nanoparticles by taking the nonionic surfactant as a template. These methods all involve high temperature calcination or chemical etching, which is expensive, time consuming and causes environmental and energy problems. Therefore, a convenient method for preparing HSNs with different morphologies is urgently needed to be found, and it is very challenging to develop a simple, effective and environment-friendly method for synthesizing HSNs with adjustable morphologies.
Patents CN109071239B, CN103272543B, and CN103359743B all propose different methods for preparing hollow silica particles, and the prepared particles can reach the control technology with controllable inner diameter of the cavity and thickness of the shell layer, but these methods all have complicated processes, and do not leave template removal means such as calcination and etching, which often affect the quality of the product particles. In the application of an anti-reflection film, drug slow release and a catalyst, factors such as production cost, particle structure, compatibility with related solvents, particle size and dispersion degree, green and pollution-free are all important. In order to solve the defects of the prior art, the invention aims to provide a convenient, cheap, controllable-size, green and pollution-free hollow silica sol product and a preparation method thereof.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a silica sol and a preparation method thereof. The method can complete the preparation of the silica sol by a one-step method, realize the accurate control of the inner diameter of the particle cavity and the thickness of the shell layer, and simultaneously prepare the aqueous dispersion sol to ensure that the product is green and pollution-free.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a silica sol comprises hollow silica nanoparticles, wherein the hollow silica nanoparticles are spherical structures and comprise an inner layer and an outer layer, the inner layer is a hollow structure, and the outer layer is a silica shell layer; the diameter of the inner layer cavity is 55 nm-100 nm, and the hollow silica sol comprises the following components in percentage by weight: 5 to 10 percent of hollow silica nano particles, 0.1 to 0.5 percent of sodium hydroxide and the balance of solvent water.
Further, the thickness of the silicon dioxide shell layer is 20 nm-40 nm.
The invention adopts polyacrylic acid and ammonia water to mix and disperse in ethanol solvent to form a cation template, initiator is hydrolyzed and condensed on the surface of the cation template to form a growth site, and finally silicic acid is added to continue to grow on the growth site to form a shell structure. The addition concentration of polyacrylic acid determines the size of the cation template, namely the diameter of the cavity of the inner layer. The addition of silicic acid determines the degree of silica growth, i.e. the shell thickness. The higher the porosity and the lower the refractive index, the combination of different cavity diameters and shell thicknesses together determining the refractive index of the hollow silica.
The invention also provides a preparation method of the silica sol, which comprises the following steps:
s1, adding water and water glass into a reaction container, uniformly stirring to obtain a mixed solution, and allowing the mixed solution to pass through a filled hydrogen type strong acid cation exchange resin column to obtain silicic acid A, wherein the concentration of the water glass is 40 degrees Be;
s2, at room temperature, dissolving polyacrylic acid in ammonia water to obtain a solution B;
s3, mixing the solution B with ethanol and stirring vigorously, and then adding an initiator alkoxy silane into the vigorously stirred reaction liquid;
s4, equally dividing silicic acid A into four equal parts, dropwise adding one part of silicic acid A into the violently stirred reaction liquid obtained in the step S3, dropwise adding one part of silicic acid A every 2 hours, and continuing to react for 7 hours after the dropwise adding is finished to obtain sol C;
s5, concentrating the sol C to 5% -10% by a reduced pressure distillation or ultrafiltration method, replacing ethanol with deionized water by solvent replacement, adding sodium hydroxide solution to adjust the pH value to 10, and uniformly stirring to finally obtain the hollow silica sol.
Further, the volume ratio of water to water glass in the step S1 is 4: 1. And (3) diluting the water glass, and facilitating cation resin exchange to obtain a silicic acid solution.
Further, in the step S2, the polyacrylic acid has an average molecular weight of 3000, the addition amount is 0.4 g-0.75 g, and the diameter of the inner layer cavity of the hollow silica nanoparticle is 55 nm-100 nm. The amount of polyacrylic acid added determines the size of the cationic template, i.e., the inner cavity diameter.
Further, the initiator alkoxysilane in the step S3 is any one of tetramethoxysilane, tetraethoxysilane or tetrabutoxysilane, and is preferably tetraethoxysilane. The initiator is used for generating the silicon dioxide growth sites on the surface of the cationic template through hydrolytic polycondensation.
Further, the amount of silicic acid A used in step S4 is 30-70 mL. The shell thickness is determined by the adding amount of silicic acid, and the silica shell thickness of the obtained hollow silica nanoparticles is 20-40 nm.
Compared with the traditional hollow silica sol, the hollow silica sol prepared by the method has the advantages of convenient preparation method, safe and pollution-free preparation process and capability of being used for industrial large-scale production.
The invention has the following beneficial effects:
1. the inner diameter of the particle cavity and the thickness of the shell layer are controllable, the porosity of the particle sol with large inner diameter and thin shell layer is high, the refractive index of the particle sol with small inner diameter and thick shell layer is large, and thus the corresponding hollow silica sol can be prepared according to the requirements of different porosities and refractive indexes.
2. Due to the lower refractive index of the hollow silica, the sol of the hollow silica can be excellently and directly applied to single-layer and multi-layer anti-reflection film products; in addition, in the fields of drug carriers, catalysts and the like, the hollow silica sol has wide application prospect due to the characteristics of green and pollution-free products.
3. The method provided by the invention is simple and effective, the water glass is used as the raw material, the cost of the raw material is greatly reduced, the preparation process is simple and mild, and the industrial large-scale production is expected to be realized.
Drawings
FIG. 1 is a transmission electron micrograph of a hollow silica sol obtained in example 1 of the present invention.
FIG. 2 is a particle size distribution diagram of a hollow silica sol obtained in example 5 of the present invention.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a preparation method of silica sol, which provides the following practical specific invention examples according to the hollow particle cavity diameter and the shell thickness range:
example 1
The specific implementation method of the hollow silica sol with the average cavity diameter of 55nm and the average shell thickness of 20nm mainly comprises the following operation steps:
s1, adding water and water glass into a reaction container, mixing the water and the water glass in a volume ratio of 4:1, uniformly stirring to obtain a mixed solution, and allowing the obtained mixed solution to pass through a packed hydrogen type strong acid cation exchange resin column to obtain silicic acid A;
s2, dissolving 0.4g of polyacrylic acid in 7.5mL of ammonia water at room temperature to obtain a solution B;
s3, mixing the solution B with 150mL of ethanol in a 250mL conical flask, and stirring vigorously (the rotating speed is more than or equal to 300 rpm). Then adding 0.5mL of initiator tetraethoxysilane into the vigorously stirred reaction liquid, and reacting for 2 h;
s4, equally dividing 30mL of silicic acid A into four equal parts, dropwise adding one part of silicic acid A into the violently stirred reaction liquid obtained in the step S3, dropwise adding one part of silicic acid A every 2 hours, and continuing to react for 7 hours after the dropwise addition is finished to obtain sol C;
s5, purifying and concentrating the sol C by a reduced pressure distillation method, replacing ethanol by deionized water by solvent replacement, adding a stabilizer sodium hydroxide solution (0.5mol/L) to adjust the pH value to 10, and uniformly stirring to finally obtain the hollow silica sol with the solid content of 5.1%.
Example 2
The specific implementation method of the hollow silica sol with the average cavity diameter of 55nm and the average shell thickness of 40nm mainly comprises the following operation steps:
s1, adding water and water glass into a reaction container, mixing the water and the water glass in a volume ratio of 4:1, uniformly stirring to obtain a mixed solution, and allowing the obtained mixed solution to pass through a packed hydrogen type strong acid cation exchange resin column to obtain silicic acid A;
s2, dissolving 0.4g of polyacrylic acid in 7.5mL of ammonia water at room temperature to obtain a solution B;
s3, mixing the solution B with 150mL of ethanol in a 250mL conical flask, and stirring vigorously (the rotating speed is more than or equal to 300 rpm). Then adding 0.5mL of initiator tetraethoxysilane into the vigorously stirred reaction liquid, and reacting for 2 h;
s4, equally dividing 70mL of silicic acid A into four equal parts, dropwise adding one part of silicic acid A into the violently stirred reaction liquid obtained in the step S3, dropwise adding one part of silicic acid A every 2 hours, and continuing to react for 7 hours after the dropwise addition is finished to obtain sol C;
s5, purifying and concentrating the sol C by a reduced pressure distillation method, replacing ethanol by deionized water by solvent replacement, adding a stabilizer sodium hydroxide solution (0.5mol/L) to adjust the pH value to 10, and uniformly stirring to finally obtain the hollow silica sol with the solid content of 9.8%.
Example 3
The specific implementation method of the hollow silica sol with the average cavity diameter of 100nm and the average shell thickness of 20nm mainly comprises the following operation steps:
s1, adding water and water glass into a reaction container, mixing the water and the water glass in a volume ratio of 4:1, uniformly stirring to obtain a mixed solution, and allowing the obtained mixed solution to pass through a packed hydrogen type strong acid cation exchange resin column to obtain silicic acid A;
s2, dissolving 0.75g of polyacrylic acid in 7.5mL of ammonia water at room temperature to obtain a solution B;
s3, mixing the solution B with 150mL of ethanol in a 250mL conical flask, and stirring vigorously (the rotating speed is more than or equal to 300 rpm). Then adding 0.5mL of initiator tetraethoxysilane into the vigorously stirred reaction liquid, and reacting for 2 h;
s4, equally dividing 30mL of silicic acid A into four equal parts, dropwise adding one part of silicic acid A into the violently stirred reaction liquid obtained in the step S3, dropwise adding one part of silicic acid A every 2 hours, and continuing to react for 7 hours after the dropwise addition is finished to obtain sol C;
s5, purifying and concentrating the sol C by a reduced pressure distillation method, replacing ethanol by deionized water by solvent replacement, adding a stabilizer sodium hydroxide solution (0.5mol/L) to adjust the pH value to 10, and uniformly stirring to finally obtain the hollow silica sol with the solid content of 5.2%.
Example 4
The specific implementation method of the hollow silica sol with the average cavity diameter of 100nm and the average shell thickness of 40nm mainly comprises the following operation steps:
s1, adding water and water glass into a reaction container, mixing the water and the water glass in a volume ratio of 4:1, uniformly stirring to obtain a mixed solution, and allowing the obtained mixed solution to pass through a packed hydrogen type strong acid cation exchange resin column to obtain silicic acid A;
s2, dissolving 0.75g of polyacrylic acid in 7.5mL of ammonia water at room temperature to obtain a solution B;
s3, mixing the solution B with 150mL of ethanol in a 250mL conical flask, and stirring vigorously (the rotating speed is more than or equal to 300 rpm). Then adding 0.5mL of initiator tetraethoxysilane into the vigorously stirred reaction liquid, and reacting for 2 h;
s4, equally dividing 70mL of silicic acid A into four equal parts, dropwise adding one part of silicic acid A into the violently stirred reaction liquid obtained in the step S3, dropwise adding one part of silicic acid A every 2 hours, and continuing to react for 7 hours after the dropwise addition is finished to obtain sol C;
s5, purifying and concentrating the sol C by a reduced pressure distillation method, replacing ethanol by deionized water by solvent replacement, adding a stabilizer sodium hydroxide solution (0.5mol/L) to adjust the pH value to 10, and uniformly stirring to finally obtain the hollow silica sol with the solid content of 9.7%.
Example 5
The specific implementation method of the hollow silica sol with the average cavity diameter of 75nm and the average shell thickness of 30nm mainly comprises the following operation steps:
s1, adding water and water glass into a reaction container, mixing the water and the water glass in a volume ratio of 4:1, uniformly stirring to obtain a mixed solution, and allowing the obtained mixed solution to pass through a packed hydrogen type strong acid cation exchange resin column to obtain silicic acid A;
s2, dissolving 0.58g of polyacrylic acid in 7.5mL of ammonia water at room temperature to obtain a solution B;
s3, mixing the solution B with 150mL of ethanol in a 250mL conical flask, and stirring vigorously (the rotating speed is more than or equal to 300 rpm). Then adding 0.5mL of initiator tetraethoxysilane into the vigorously stirred reaction liquid, and reacting for 2 h;
s4, equally dividing 50mL of silicic acid A into four equal parts, dropwise adding one part of silicic acid A into the violently stirred reaction liquid obtained in the step S3, dropwise adding one part of silicic acid A every 2 hours, and continuing to react for 7 hours after the dropwise addition is finished to obtain sol C;
s5, purifying and concentrating the sol C by an ultrafiltration method, replacing ethanol by deionized water by solvent replacement, adding a stabilizer sodium hydroxide solution (0.5mol/L) to adjust the pH value to 10, and uniformly stirring to finally obtain the hollow silica sol with the solid content of 5.5%.
In conclusion, the inner diameter of the particle cavity and the thickness of the shell layer are accurate and controllable, and the hollow silica sol can be prepared according to different requirements. The difference of different embodiments of the invention mainly lies in the difference of the prepared cavity inner diameter, shell thickness and solid content, and the specific application can be selected according to the specific use environment, such as: the hollow silica sol product in example 3 can be selected if a product with large particle size and thin wall thickness is required; due to the lower refractive index of the hollow silica, the sol of the hollow silica can be excellently and directly applied to an anti-reflection film product, and has wide application prospects in the fields of drug carriers, catalysts and the like.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The silica sol comprises hollow silica nanoparticles, and is characterized in that the hollow silica nanoparticles are spherical structures and comprise an inner layer and an outer layer, wherein the inner layer is a hollow structure, and the outer layer is a silica shell layer; the diameter of the inner layer cavity is 55 nm-100 nm, and the silica sol comprises the following components in percentage by weight:
5 to 10 percent of hollow silicon dioxide nano particles,
0.1 to 0.5 percent of sodium hydroxide,
the balance being solvent water.
2. The silica sol according to claim 1, wherein the silica shell layer has a thickness of 20 to 40 nm.
3. A method for producing the silica sol according to claim 1, comprising the steps of:
s1, adding water and water glass into a reaction container, uniformly stirring to obtain a mixed solution, and allowing the mixed solution to pass through a filled hydrogen type strong acid cation exchange resin column to obtain silicic acid A, wherein the concentration of the water glass is 40 degrees Be;
s2, at room temperature, dissolving polyacrylic acid in ammonia water to obtain a solution B;
s3, mixing the solution B with ethanol and stirring vigorously, and then adding an initiator alkoxy silane into the vigorously stirred reaction liquid;
s4, equally dividing silicic acid A into four equal parts, dropwise adding one part of silicic acid A into the violently stirred reaction liquid obtained in the step S3, dropwise adding one part of silicic acid A every 2 hours, and continuing to react for 7 hours after the dropwise adding is finished to obtain sol C;
s5, concentrating the sol C to 5% -10% by a reduced pressure distillation or ultrafiltration method, replacing ethanol with deionized water by solvent replacement, adding sodium hydroxide solution to adjust the pH value to 10, and uniformly stirring to finally obtain the hollow silica sol.
4. The method for producing a silica sol according to claim 3, wherein the volume ratio of water to water glass in the step S1 is 4: 1.
5. The method for producing a silica sol according to claim 3, wherein the polyacrylic acid having an average molecular weight of 3000 is added in an amount of 0.4 to 0.75g in step S2.
6. The method of preparing a silica sol according to claim 3, wherein the alkoxysilane in the step S3 is any one of tetramethoxysilane, tetraethoxysilane, or tetrabutoxysilane.
7. The method for producing a silica sol according to claim 4, wherein the amount of silicic acid A used in step S4 is 30 to 70 mL.
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| CN116496647A (en) * | 2022-11-11 | 2023-07-28 | 无锡普天铁心股份有限公司 | Insulation coating liquid for surface modification of oriented silicon steel and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517217A (en) * | 2016-11-16 | 2017-03-22 | 嘉兴昊特新材料科技有限公司 | Preparation method of core-shell type silica sol |
| CN109502987A (en) * | 2018-12-17 | 2019-03-22 | 常州大学 | A method of high rigidity antireflective film is prepared based on hollow silica |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106517217A (en) * | 2016-11-16 | 2017-03-22 | 嘉兴昊特新材料科技有限公司 | Preparation method of core-shell type silica sol |
| CN109502987A (en) * | 2018-12-17 | 2019-03-22 | 常州大学 | A method of high rigidity antireflective film is prepared based on hollow silica |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116496647A (en) * | 2022-11-11 | 2023-07-28 | 无锡普天铁心股份有限公司 | Insulation coating liquid for surface modification of oriented silicon steel and preparation method thereof |
| CN116496647B (en) * | 2022-11-11 | 2024-01-16 | 无锡普天铁心股份有限公司 | Insulation coating liquid for surface modification of oriented silicon steel and preparation method thereof |
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