CN114634186A - Preparation method of nano silicon dioxide dispersion liquid - Google Patents
Preparation method of nano silicon dioxide dispersion liquid Download PDFInfo
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- CN114634186A CN114634186A CN202011485701.0A CN202011485701A CN114634186A CN 114634186 A CN114634186 A CN 114634186A CN 202011485701 A CN202011485701 A CN 202011485701A CN 114634186 A CN114634186 A CN 114634186A
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- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention provides a preparation method of nano silicon dioxide dispersion liquid, which is high in stability, quality and solid content by adjusting the conditions of concentration, pH value, average particle size of silicon dioxide and the like of silicon dioxide slurry. The preparation method of the nano silicon dioxide dispersion liquid provided by the invention has the advantages of high maturity of equipment, low cost, easiness in industrialization, high solid content of the prepared product and good stability, and can be used for preparing latex products, wet mixing rubber products, coatings, printing ink, adhesives and the like.
Description
Technical Field
The invention relates to the field of preparation of nano silicon dioxide dispersion liquid, and particularly relates to a preparation method of nano silicon dioxide dispersion liquid.
Background
Colloidal silica dispersions are often used as coating materials to improve the adhesion properties of the coating and to increase the wear resistance and water resistance of various materials. However, highly concentrated colloidal silica compositions have poor stability and are prone to gelation or precipitation in the material, shortening the storage time of the material.
The prior art currently provides some methods for the dispersion of silane-modified silicas. However, the stability of the dispersion is poor, most of the raw materials used are fumed silica, and the fumed silica is used together with a silane coupling agent, a dispersing agent and the like, so that the production cost of the prepared nano silica dispersion is high, and the application of the silica dispersion is greatly limited.
Mixing an anionic polymeric dispersant and an aminosilane compound into an aqueous medium, and mixing silica particles into an aqueous medium containing an anionic polymeric dispersant and an aminosilane compound; and reacting, or reacting, the aminosilane compound with the silica particles to provide an aqueous silica dispersion.
The silica dispersion provided in the prior art is realized by reducing the average particle size of silica particles to less than 100nm, thereby improving the technical difficulty of grinding and the production cost. Or adding a stabilizer such as biogel or a dispersion system consisting of an aluminum compound and anions to the dispersion system, the cost is high, and the co-storage of the stabilizer and the silica particles is not favorable for the long-term storage of the silica dispersion and the storage stability is poor. Alternatively, a highly concentrated colloidal silica dispersion is provided, particularly for use in the coating art, but such products suffer from the problem of easy settling.
In summary, the storage stability of the silica dispersions (dispersions) is a major problem which limits their use. At present, since it is difficult for the silica dispersion (dispersion) to maintain good stability during storage, most users of the application fields of silica dispersions (e.g. paper industry, construction industry) still need to purchase silica powder and prepare the silica dispersion themselves. For the user of the dispersion, this not only means an increased amount of labor, but also requires a long-term storage of the silica powder in large quantities, resulting in an increased cost.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The preparation method of the nano-silica dispersion provided by the invention is used for completely or partially solving the problems of high cost, easy sedimentation, poor quality and the like of the existing silica nano-dispersion, and the nano-silica dispersion with high stability, high quality and high solid content is obtained by adjusting the conditions of the concentration, the pH value, the average particle size of silica and the like of silica slurry.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a preparation method of nano silicon dioxide dispersion liquid comprises the following steps:
(a) carrying out first filter pressing on the silicon dioxide slurry, cleaning to obtain a filter cake with the solid content of 20-22%, carrying out first pulping on the filter cake, and then carrying out second filter pressing to obtain a filter cake with the solid content of 30-50%;
(b) and pulping the filter cake with the solid content of 30-50% for the second time, adjusting the pH of the pulp to 8-10 after pulping, grinding the pulp until the particle size of the silicon dioxide is 20-1000nm, and filtering to obtain the nano silicon dioxide dispersion liquid.
Preferably, in step (a), the silica slurry is prepared by a precipitation process, and more preferably, the precipitation process comprises at least one of a sulfuric acid process, a hydrochloric acid process, or a carbonic acid process.
Preferably, in the step (a), the first filter pressing is performed by plate and frame filter pressing, wherein the pressing pressure of the plate and frame filter pressing is 0.6-1.2MPa, and the washing pressure is 0.6-1.0 MPa.
Preferably, in the step (a), the washing is carried out until the conductivity is lower than 800 mus/cm in the process of washing the filter cake with the solid content of 20-22%.
Preferably, in the step (a), the time for the first beating is 0.1-0.5 h.
Preferably, in the step (a), the second filter pressing is performed by plate and frame filter pressing, and the compression pressure of the plate and frame filter pressing is 6-20 MPa.
Preferably, in the step (b), the time for the second beating is 0.1-0.5 h.
Preferably, an activating agent is added in the second pulping process, and the addition amount of the activating agent is 0.1-5% of the mass of the dry powder in the silicon dioxide slurry, and more preferably 2-4%;
more preferably, the activating agent comprises one or more of sodium hexametaphosphate, ethylenediamine phosphate, sodium tripolyphosphate, sodium metaaluminate, sodium pyrophosphate, sodium polyacrylate and fatty alcohol-polyoxyethylene ether.
Preferably, in step (b), the grinding process specifically comprises:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 5-9 μm, and then sanding until the particle size of the silicon dioxide is 20-1000nm, preferably 50-500 nm.
Preferably, the medium for ball milling is zirconia beads, and more preferably, the particle size of the zirconia beads is 1-5 mm.
Preferably, the sanded media are zirconia beads, and more preferably, the zirconia beads have a particle size of 0.05 to 0.6 μm.
Preferably, in step (b), the filter element has a pore size of less than 1000 nm.
Preferably, in the step (b), the pH is adjusted by using a lye, and more preferably, the lye is one or more selected from the group consisting of sodium hydroxide solution, sodium carbonate solution and ammonia water solution.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the preparation method of the nano silicon dioxide dispersion liquid, provided by the invention, the nano silicon dioxide dispersion liquid with high stability, high quality and high solid content is obtained by adjusting the conditions such as the concentration, the pH value, the average particle size of silicon dioxide and the like of the silicon dioxide slurry.
(2) The preparation method of the nano silicon dioxide dispersion liquid provided by the invention has the advantages of high maturity of equipment, low cost and easiness in industrialization.
(3) The nano silicon dioxide dispersion liquid product provided by the invention has high solid content and good stability, and can be used for preparing latex products, wet mixing rubber products, coatings, printing ink, adhesives, paper, textile coatings and the like.
Detailed Description
While the technical solutions of the present invention will be described clearly and completely with reference to the specific embodiments, those skilled in the art will understand that the following described examples are some, but not all, examples of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The preparation method of the nano silicon dioxide dispersion liquid provided by the invention specifically comprises the following steps:
(a) carrying out first filter pressing on the silicon dioxide slurry, cleaning to obtain a filter cake with the solid content of 20% -22% (20%, 21%, 22%), carrying out first pulping on the filter cake, and then carrying out second filter pressing to obtain a filter cake with the solid content of 30% -50%;
(b) and second beating the filter cake with the solid content of 30-50% (30%, 35%, 40%, 45%, 50%), adjusting the pH of the slurry to 8-10 (for example, 8, 8.5, 9, 9.5, 10) after beating, grinding the slurry until the particle size of silica is 20-1000nm (20, 50, 80, 100, 200, 300, 400, 500, 600, 700, 800, 900, 1000nm), and filtering to obtain a nano silica dispersion.
The preparation method of the nano-silica dispersion liquid provided by the invention completely or partially solves the problems of high cost, easy sedimentation, poor quality and the like of the existing silica nano-dispersion liquid, and obtains the nano-silica dispersion liquid with high stability, high quality and high solid content by adjusting factors such as the concentration, the pH value, the average particle size of silica and the like of silica slurry.
In some preferred embodiments of the present invention, in the step (a), the silica slurry is prepared by a precipitation method using water glass as a raw material, and further, the precipitation method includes at least one of a sulfuric acid method, a hydrochloric acid method, and a carbonic acid method.
In some preferred embodiments of the present invention, in step (a), the first press filtration is performed by plate and frame press filtration to increase the solid content and facilitate subsequent grinding, wherein the pressure of the plate and frame press filtration is 0.6-1.2MPa (e.g., 0.6, 0.7, 0.8, 1, 1.2MPa), and the washing pressure is 0.6-1.0MPa (e.g., 0.6, 0.7, 0.8, 1 MPa).
In some preferred embodiments of the present invention, in step (a), the washing step is carried out until the conductivity of the filter cake is less than 800 μ s/cm during the washing step to obtain a filter cake with a solid content of 20% -22%, and the conductivity is measured by dissolving the filter cake in water.
In some preferred embodiments of the present invention, in step (a), the first beating time is 0.1-0.5h, and the filter cake structure is destroyed by shearing force.
In some preferred embodiments of the invention, in step (a), the second press filtration is performed using a plate and frame press filtration having a packing pressure of 0.6 to 1.2MPa (e.g., 6, 7, 8, 10, 12, 14, 15, 16, 18, 20 MPa).
In some preferred embodiments of the present invention, in step (b), the second beating time is 0.1-0.5h, and the filter cake structure is destroyed again by the shearing force;
further, an activating agent is added in the second pulping process, and the adding amount of the activating agent is 0.1-5% (preferably 0.1-1%, 1-3%, 1-2%, 2-3%, such as 0.1%, 0.5%, 0.8%, 1%, 2%, 3%, 4%, 5%) of the mass of the dry powder in the silicon dioxide slurry, and more preferably 2-4%;
further, the activating agent can reduce the viscosity of the silicon dioxide slurry system and is beneficial to grinding treatment, and the activating agent comprises one or a combination of several of sodium hexametaphosphate, ethylenediamine phosphate, sodium tripolyphosphate, sodium metaaluminate, sodium pyrophosphate, sodium polyacrylate and fatty alcohol-polyoxyethylene ether.
In some preferred embodiments of the present invention, in step (b), the grinding is performed to refine the silica particles, and in order to improve the stability of the silica dispersion during storage, the grinding specifically comprises:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 5-9 μm, and then sanding until the particle size of the silicon dioxide is 20-1000nm, preferably 50-500 nm.
The ball milling medium and the particle size are further preferably selected from zirconia beads with the particle size of 1-5 mm.
It is further preferable that the medium to be sanded and the particle diameter are 0.05 to 0.6 μm, wherein the medium to be sanded is zirconia beads.
In some preferred embodiments of the invention, in step (b), the filter element has a pore size of less than 1000 nm.
In some preferred embodiments of the present invention, in step (b), the pH is adjusted by using a lye, more preferably, the lye is selected from one or a combination of several of sodium hydroxide solution, sodium carbonate solution and ammonia solution.
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Examples
A preparation method of nano silicon dioxide dispersion liquid comprises the following steps:
(1) carrying out first filter pressing on the silicon dioxide slurry by adopting a plate-and-frame filter press, wherein the pressure of the plate-and-frame filter pressing is 6-20MPa, then cleaning until the conductivity is lower than 800 mu s/cm to obtain a filter cake with the solid content of 20-22%, carrying out first pulping on the filter cake for 0.1-0.5h, then carrying out second filter pressing by adopting the plate-and-frame filter press, wherein the compaction pressure of the plate-and-frame filter pressing is 0.6-1.2MPa, and the washing pressure is 0.6-1.0MPa to obtain a filter cake with the solid content of 30-50%;
wherein, the silicon dioxide slurry is prepared by a precipitation method, and the precipitation method comprises at least one of a sulfuric acid method, a hydrochloric acid method or a carbonic acid method;
(2) adding an activating agent into the filter cake with the solid content of 30-50% obtained in the step (1), wherein the adding amount of the activating agent is 0.1-5% of the mass of the dry powder in the silicon dioxide slurry, then carrying out second pulping for 0.1-0.5h, adjusting the pH value of the slurry to 8-10 by adopting an alkali liquor after pulping, grinding the slurry until the particle size of the silicon dioxide is 20-1000nm, and then filtering by adopting a filter element with the pore diameter smaller than 1000nm to obtain a nano silicon dioxide dispersion liquid;
wherein the activating agent is selected from one or more of sodium hexametaphosphate, ethylenediamine phosphate, sodium tripolyphosphate, sodium metaaluminate, sodium pyrophosphate, sodium polyacrylate and fatty alcohol-polyoxyethylene ether.
The grinding process specifically comprises the following steps:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 5-9 μm, and then sanding until the particle size of the silicon dioxide is 20-1000nm, preferably 50-500 nm;
the ball-milled media are zirconia beads of 1-5mm and the sanded media are zirconia beads of 0.05-0.6 μm, more preferably the zirconia beads have a particle size of 0.05-0.1 μm.
Example 1
The preparation method of the nano-silica dispersion provided by the embodiment specifically includes the following steps:
(1) carrying out first filter pressing on the silicon dioxide slurry by adopting a plate-and-frame filter press, wherein the pressure of the plate-and-frame filter pressing is 6MPa, then cleaning until the conductivity is lower than 800 mu s/cm to obtain a filter cake with the solid content of 20%, carrying out first pulping on the filter cake for 0.1h, then carrying out second filter pressing by adopting the plate-and-frame filter press, wherein the pressing pressure of the plate-and-frame filter pressing is 0.6MPa, and the washing pressure is 0.6MPa to obtain a filter cake with the solid content of 30%;
wherein, the silicon dioxide slurry is prepared by a precipitation method;
(2) adding an activating agent into the filter cake with the solid content of 30% obtained in the step (1), wherein the adding amount of the activating agent is 0.1% of the mass of the dry powder in the silicon dioxide slurry, then carrying out second pulping for 0.1-0.5h, adjusting the pH value of the pulp to 8 by adopting an alkali liquor after pulping, grinding the pulp until the particle size of the silicon dioxide is 20nm, and then filtering by adopting a filter element with the pore size of less than 20nm to obtain 20nm nano-silicon dioxide dispersion liquid;
wherein the activating agent is sodium hexametaphosphate;
the grinding process specifically comprises the following steps:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 5 μm, and then sanding until the particle size of the silicon dioxide is 20 nm;
the ball-milled media were 1mm zirconia beads and the sanded media were 0.05 μm zirconia beads.
Example 2
The preparation method of the nano-silica dispersion provided by the embodiment specifically includes the following steps:
(1) carrying out first filter pressing on the silicon dioxide slurry by adopting a plate-and-frame filter press, wherein the pressure of the plate-and-frame filter pressing is 20MPa, then cleaning until the conductivity is lower than 800 mu s/cm to obtain a filter cake with the solid content of 22%, carrying out first pulping on the filter cake for 0.5h, then carrying out second filter pressing by adopting the plate-and-frame filter press, wherein the pressing pressure of the plate-and-frame filter pressing is 1.2MPa, and the washing pressure is 1.0MPa to obtain a filter cake with the solid content of 50%;
wherein, the silicon dioxide slurry is prepared by a precipitation method;
(2) adding an activating agent into the filter cake with the solid content of 50% obtained in the step (1), wherein the adding amount of the activating agent is 5% of the mass of the dry powder in the silicon dioxide slurry, then carrying out second pulping for 0.1-0.5h, adjusting the pH value of the slurry to 10 by adopting alkali liquor after pulping, grinding the slurry until the particle size of the silicon dioxide is 1000nm, and then filtering by adopting a filter element with the pore diameter smaller than 1000nm to obtain 1000nm nano silicon dioxide dispersion liquid;
wherein the activating agent is ethylene diamine phosphate;
the grinding process specifically comprises the following steps:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 9 μm, and then sanding until the particle size of the silicon dioxide is 1000 nm;
the ball-milled media were 5mm zirconia beads and the sanded media were 0.6 μm zirconia beads.
Example 3
The preparation method of the nano-silica dispersion provided by the embodiment specifically includes the following steps:
(1) carrying out first filter pressing on the silicon dioxide slurry by adopting a plate-and-frame filter press, wherein the pressure of the plate-and-frame filter pressing is 10MPa, then cleaning until the conductivity is lower than 800 mu s/cm to obtain a filter cake with the solid content of 21%, carrying out first pulping on the filter cake by 0.2, then carrying out second filter pressing by adopting the plate-and-frame filter press, wherein the pressing pressure of the plate-and-frame filter pressing is 0.8MPa, and the washing pressure is 0.8MPa to obtain a filter cake with the solid content of 40%;
wherein, the silicon dioxide slurry is prepared by a precipitation method;
(2) adding an activating agent into the filter cake with the solid content of 40% obtained in the step (1), wherein the adding amount of the activating agent is 2% of the mass of the dry powder in the silicon dioxide slurry, then carrying out second pulping for 0.2h, adjusting the pH value of the pulp to 9 by adopting alkali liquor after pulping, grinding the pulp until the particle size of silicon dioxide is 100nm, and then filtering by adopting a filter element with the pore size smaller than 100nm to obtain 100nm nano-silicon dioxide dispersion liquid;
wherein the activating agent is fatty alcohol-polyoxyethylene ether;
the grinding process specifically comprises the following steps:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 6 μm, and then sanding until the particle size of the silicon dioxide is 100 nm;
the ball-milled media were 3mm zirconia beads and the sanded media were 0.1 μm zirconia beads.
Example 4
The preparation method of the nano-silica dispersion provided by the embodiment specifically includes the following steps:
(1) carrying out first filter pressing on the silicon dioxide slurry by adopting a plate-and-frame filter press, wherein the pressure of the plate-and-frame filter pressing is 15MPa, then cleaning until the conductivity is lower than 800 mu s/cm to obtain a filter cake with the solid content of 22%, carrying out first pulping on the filter cake for 0.3h, then carrying out second filter pressing by adopting the plate-and-frame filter press, wherein the pressing pressure of the plate-and-frame filter pressing is 1MPa, and the washing pressure is 0.9MPa to obtain a filter cake with the solid content of 35%;
wherein, the silicon dioxide slurry is prepared by a precipitation method;
(2) adding an activating agent into the filter cake with the solid content of 35% obtained in the step (1), wherein the adding amount of the activating agent is 2% of the mass of the dry powder in the silicon dioxide slurry, then carrying out second pulping for 0.4h, adjusting the pH value of the pulp to 8 by using alkali liquor after pulping, grinding the pulp until the particle size of silicon dioxide is 50nm, and then filtering by using a filter element with the pore size smaller than 50nm to obtain 50nm nano silicon dioxide dispersion liquid;
wherein the activating agent is sodium tripolyphosphate;
the grinding process specifically comprises:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 8 μm, and then sanding until the particle size of the silicon dioxide is 50 nm;
the ball-milled media were 4mm zirconia beads and the sanded media were 0.4 μm zirconia beads.
Example 5
The preparation method of the nano-silica dispersion provided by the embodiment specifically includes the following steps:
(1) carrying out first filter pressing on the silicon dioxide slurry by adopting a plate-and-frame filter press, wherein the pressure of the plate-and-frame filter pressing is 12MPa, then cleaning until the conductivity is lower than 800 mu s/cm to obtain a filter cake with the solid content of 22%, carrying out first pulping on the filter cake for 0.3h, then carrying out second filter pressing by adopting the plate-and-frame filter press, wherein the pressing pressure of the plate-and-frame filter pressing is 0.7MPa, and the washing pressure is 1.0MPa to obtain a filter cake with the solid content of 45%;
wherein, the silicon dioxide slurry is prepared by a precipitation method;
(2) adding an activating agent into the filter cake with the solid content of 45% obtained in the step (1), wherein the adding amount of the activating agent is 4% of the mass of dry powder in the silicon dioxide slurry, then carrying out second pulping for 0.4h, adjusting the pH value of the slurry to 9 by adopting alkali liquor after pulping, grinding the slurry until the particle size of silicon dioxide is 500nm, and then filtering by adopting a filter element with the pore size of less than 500nm to obtain 500nm nano-silicon dioxide dispersion liquid;
wherein the activating agent is sodium polyacrylate;
the grinding process specifically comprises the following steps:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 8 μm, and then sanding until the particle size of the silicon dioxide is 500 nm;
the ball-milled media were 5mm zirconia beads and the sanded media were 0.6 μm zirconia beads.
Comparative example 1
(1) Carrying out first filter pressing on the silicon dioxide slurry by adopting a plate-and-frame filter press, wherein the pressure of the plate-and-frame filter pressing is 12MPa, then cleaning until the conductivity is lower than 800 mu s/cm to obtain a filter cake with the solid content of 22%, carrying out first pulping on the filter cake for 0.3h, then carrying out second filter pressing by adopting the plate-and-frame filter press, wherein the pressing pressure of the plate-and-frame filter pressing is 0.7MPa, and the washing pressure is 1.0MPa to obtain a filter cake with the solid content of 45%;
wherein, the silicon dioxide slurry is prepared by a precipitation method;
(2) the grinding process specifically comprises the following steps:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 8 μm, and then sanding until the particle size of the silicon dioxide is 500 nm; the ball-milled media were 5mm zirconia beads and the sanded media were 0.6 μm zirconia beads.
Comparative example 2
(1) Adding water into the silicon dioxide powder, mixing to obtain a suspension with the solid content of 40%, uniformly stirring, and carrying out ball milling treatment;
(2) the grinding process specifically comprises the following steps:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 8 mu m, and then sanding until the particle size of the silicon dioxide is 1000 nm; the ball-milled media were 5mm zirconia beads and the sanded media were 0.6 μm zirconia beads.
Experimental example 1 silica stability and particle size testing
The stability and particle size of the nano-silica dispersions prepared in examples 1 to 5 and comparative examples 1 to 2 are shown in Table 1.
Table 1 silica stability and particle size test results
| Item | Stability (/ day) | Particle size (nm) | Sedimentation condition |
| Example 1 | 223 | 20 | Is composed of |
| Example 2 | 255 | 1000 | Is composed of |
| Example 3 | 244 | 100 | Is free of |
| Example 4 | 210 | 50 | Is free of |
| Example 5 | 238 | 500 | Is free of |
| Comparative example 1 | 110 | 2200 | Small amount of |
| Comparative example 2 | 60 | 2800 | Much more |
In conclusion, the nano silicon dioxide dispersion liquid prepared by the preparation method provided by the application has the advantages of high stability, high quality and high solid content.
While particular embodiments of the present invention have been illustrated and described, it will be appreciated that the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit it; those of ordinary skill in the art will understand that: modifications may be made to the teachings of the foregoing embodiments without departing from the spirit or scope of the present invention, or equivalents may be substituted for some or all of the features thereof; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; it is therefore intended to cover in the appended claims all such alternatives and modifications that are within the scope of the invention.
Claims (10)
1. A preparation method of nano silicon dioxide dispersion liquid is characterized by comprising the following steps:
(a) carrying out first filter pressing on the silicon dioxide slurry, cleaning to obtain a filter cake with the solid content of 20-22%, carrying out first pulping on the filter cake, and then carrying out second filter pressing to obtain a filter cake with the solid content of 30-50%;
(b) and pulping the filter cake with the solid content of 30-50% for the second time, adjusting the pH of the pulp to 8-10 after pulping, grinding the pulp until the particle size of the silicon dioxide is 20-1000nm, and filtering to obtain the nano silicon dioxide dispersion liquid.
2. The method for preparing a nano silica dispersion according to claim 1, wherein the silica slurry is prepared by a precipitation method in the step (a), preferably, the precipitation method comprises at least one of a sulfuric acid method, a hydrochloric acid method or a carbonic acid method.
3. The method for preparing a nano-silica dispersion according to claim 1, wherein in the step (a), the first filter pressing is performed by plate-and-frame filter pressing, and the pressing pressure of the plate-and-frame filter pressing is 0.6 to 1.2MPa and the washing pressure is 0.6 to 1.0 MPa.
4. The method for preparing a nano-silica dispersion according to claim 1, wherein in the step (a), the washing is carried out until the conductivity is less than 800 μ s/cm during the washing to obtain a filter cake with a solid content of 20-22%.
5. The method for preparing a nano silica dispersion according to claim 1, wherein the time of the first beating is 0.1 to 0.5h in the step (a).
6. The method for preparing a nano-silica dispersion according to claim 1, wherein in the step (a), the second press filtration is performed by plate-and-frame press filtration, and the compression pressure of the plate-and-frame press filtration is 6 to 20 MPa.
7. The method for preparing a nano silica dispersion according to claim 1, wherein in the step (b), the time for the second beating is 0.1 to 0.5 h;
preferably, an activating agent is added in the second pulping process, and the addition amount of the activating agent is 0.1-5% of the mass of the dry powder in the silicon dioxide slurry, and more preferably 2-4%;
more preferably, the activating agent comprises one or more of sodium hexametaphosphate, ethylenediamine phosphate, sodium tripolyphosphate, sodium metaaluminate, sodium pyrophosphate, sodium polyacrylate and fatty alcohol-polyoxyethylene ether.
8. The method for preparing a nano silica dispersion according to claim 1, wherein in the step (b), the grinding specifically comprises:
ball-milling the slurry by a ball mill until the particle size of the silicon dioxide is 5-9 μm, and then sanding until the particle size of the silicon dioxide is 20-1000nm, preferably 50-500 nm;
preferably, the medium for ball milling is zirconia beads, and more preferably, the particle size of the zirconia beads is 1-5 mm;
preferably, the sanded media are zirconia beads, and more preferably, the zirconia beads have a particle size of 0.05 to 0.6 μm.
9. The method of preparing a nano-silica dispersion according to claim 1, wherein the pore size of the filtered cartridge is less than 1000nm in step (b).
10. The method for preparing nano-silica dispersion according to claim 1, wherein in the step (b), the pH is adjusted by using alkali solution, preferably, the alkali solution is selected from one or more of sodium hydroxide solution, sodium carbonate solution and ammonia water solution.
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