CN115196644A - Preparation method and application of silicon dioxide - Google Patents

Preparation method and application of silicon dioxide Download PDF

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Publication number
CN115196644A
CN115196644A CN202210931529.XA CN202210931529A CN115196644A CN 115196644 A CN115196644 A CN 115196644A CN 202210931529 A CN202210931529 A CN 202210931529A CN 115196644 A CN115196644 A CN 115196644A
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sodium silicate
silicon dioxide
ion exchange
solid
reaction
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沈家锋
王益庆
邵进
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Anhui Evolutionary Silicon Nanomaterials Technology Co ltd
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Anhui Evolutionary Silicon Nanomaterials Technology Co ltd
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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
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • 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
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • 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
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

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  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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Abstract

The invention relates to the technical field of nano silicon dioxide, in particular to a preparation method and application of silicon dioxide. The preparation method of the silicon dioxide comprises the following steps: the method comprises the following steps of (1) mixing a material obtained by concentrating and crystallizing silicon dioxide production wastewater produced by a carbonization method with quartz sand, and then calcining to obtain a material containing sodium silicate; dissolving a material containing sodium silicate in water, mixing the material with an oxidant, reacting, and then carrying out solid-liquid separation to obtain an iron hydroxide precipitate and a sodium silicate solution; to sodium silicate solutionIntroducing CO into the reaction kettle 2 Carrying out reaction, and carrying out solid-liquid separation after the reaction is finished to obtain a solid material and a mixed solution containing sodium carbonate and sodium bicarbonate; pulping the solid material, adding the pulped solid material into ion exchange resin for ion exchange, and then sequentially carrying out solid-liquid separation and drying to obtain the silicon dioxide. The preparation method takes silicon dioxide production wastewater and quartz sand as raw materials, adopts a precipitation method to prepare the silicon dioxide, and has the advantages of high purity, low cost, simple operation and the like.

Description

Preparation method and application of silicon dioxide
Technical Field
The invention relates to the technical field of nano silicon dioxide, in particular to a preparation method and application of silicon dioxide.
Background
The nano silicon dioxide is white fluffy powder, and has the advantages of porosity, no toxicity, no smell, no pollution, high temperature resistance and the like. The nano silicon dioxide can improve the tensile strength, the tear resistance and the wear resistance of rubber products. In addition, the nano-dioxide can be used as a thixotropic agent, a thickening agent, an anti-settling agent, an anti-sagging agent, a dispersing agent, a grinding aid, a reinforcing agent, an antifoaming agent, a catalyst carrier and the like.
In the prior art, the preparation method of nano-silica comprises chemical vapor deposition, precipitation, sol-gel method, etc. However, the above preparation method has the disadvantages of high cost, complex operation, difficult mass production and the like.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of silicon dioxide, which takes materials and quartz sand obtained by concentrating and crystallizing silicon dioxide production wastewater produced by a carbonization method as raw materials and adopts a precipitation method to prepare the silicon dioxide, and has the advantages of low cost, simplicity, easy operation, mass production and the like.
The second purpose of the invention is to provide the application of the silica prepared by the preparation method in paint, plastic, adhesive and rubber.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a preparation method of silicon dioxide, which comprises the following steps:
(a) And mixing the material obtained by concentrating and crystallizing the silicon dioxide production wastewater produced by the carbonization method with quartz sand, and calcining to obtain the material containing sodium silicate. The main components of the silicon dioxide production wastewater produced by the carbonization method are sodium carbonate and sodium bicarbonate, and the main component of the material obtained by concentrating and crystallizing the silicon dioxide production wastewater produced by the carbonization method is sodium carbonate.
(b) Dissolving the material containing sodium silicate obtained in the step (a) in water, mixing the material with an oxidant, reacting, and then carrying out solid-liquid separation to obtain an iron hydroxide precipitate and a sodium silicate solution.
Wherein, the main component of the solid material obtained after the solid-liquid separation comprises ferric hydroxide precipitate, and the main component of the liquid material comprises sodium silicate.
The oxidant can completely oxidize the iron in the material containing the sodium silicate to generate ferric hydroxide precipitate, thereby filtering and removing iron impurities.
(c) Introducing CO into the sodium silicate solution obtained in the step (b) 2 And (3) carrying out reaction, and carrying out solid-liquid separation after the reaction is finished to obtain a solid material and a mixed solution containing sodium carbonate and sodium bicarbonate.
Wherein, CO is introduced 2 The reaction principle of (2) is as follows:
CO 2 +Na 2 SiO 3 +H 2 O＝＝H 2 SiO 3 ↓+Na 2 CO 3 ；
2CO 2 +Na 2 SiO 3 +2H 2 O＝＝H 2 SiO 3 ↓+2NaHCO 3 。
therefore, the main component of the solid material obtained after the solid-liquid separation in the step includes silicic acid precipitate, and the main component of the liquid material includes sodium carbonate and sodium bicarbonate.
(d) Pulping the solid material obtained in the step (c), adding the pulped solid material into ion exchange resin for ion exchange, and then sequentially carrying out solid-liquid separation and drying to obtain silicon dioxide;
wherein, pulping is to make into slurry, which is the process of adding a certain amount of water into the solid to make the solid into thick slurry mixed liquid.
The ion exchange resin is used for removing residual sodium carbonate and sodium bicarbonate, and converting the residual sodium carbonate and sodium bicarbonate into carbon dioxide and water, thereby achieving the purpose of removing impurities and purifying.
According to the preparation method provided by the invention, the material obtained by concentrating and crystallizing the silicon dioxide production wastewater produced by a carbonization method and quartz sand are used as raw materials, and the precipitation method is adopted to prepare the silicon dioxide, so that the preparation method has the advantages of low cost, simplicity in operation, easiness in realizing mass production and the like.
In addition, the nano silicon dioxide prepared by the preparation method has high purity and good quality.
Wherein the quartz sand is quartz particles formed by crushing quartz stones. Quartz sand is a silicate mineral with high hardness, wear resistance and stable chemical property, and the main mineral component of the quartz sand is SiO 2 The color of the quartz sand is milky white or colorless and semitransparent.
In some embodiments of the invention, the silica sand has a particle size of 0.1 to 2mm.
Preferably, in step (a), the temperature of the calcination is 1200 to 1500 ℃.
Preferably, in the step (a), the ratio of the volume of the material obtained by concentrating and crystallizing the silicon dioxide production wastewater produced by the carbonization method to the mass of the quartz sand is 1.8-1.
Preferably, in step (b), the oxidizing agent comprises hydrogen peroxide solution and/or ozone.
Preferably, the mass fraction of the hydrogen peroxide solution is 5-50%.
Preferably, the mass ratio of the oxidizing agent in step (b) to the sodium silicate in step (a) is 0.01% to 0.1%.
Preferably, in step (c), the temperature of the mixture during the reaction is 40-98 ℃.
Preferably, in step (c), the pH of the mixture during the reaction is between 8 and 10.5, including but not limited to the values of any one of 8.5, 9, 9.5, 10 or a range between any two.
Preferably, in step (c), the reaction time is 30 to 240min.
Preferably, the step (c) further comprises a step of recycling the mixed solution containing sodium carbonate and sodium bicarbonate.
Preferably, the recycling method specifically includes: concentrating and crystallizing the mixed solution containing sodium carbonate and sodium bicarbonate, mixing with quartz sand, and calcining to obtain sodium silicate; then adding the sodium silicate into the material containing the sodium silicate in the step (b) for use, or adding the sodium silicate into the sodium silicate solution in the step (c) for use.
Preferably, in step (c), the temperature of the calcination is 1200 to 1500 ℃.
Preferably, step (d) further comprises the step of washing the solid material obtained in step (c) before the pulping.
Preferably, the wash is performed until the conductivity of the wash liquor is below 1000 μ s/cm, including but not limited to values of any one or a range between any two of 900 μ s/cm, 800 μ s/cm, 700 μ s/cm, 600 μ s/cm, 500 μ s/cm, 400 μ s/cm, 300 μ s/cm, 200 μ s/cm, 100 μ s/cm.
Preferably, in step (d), the ion exchange resin comprises a strong acid cation resin and/or a weak acid cation resin.
Preferably, in step (d), during the ion exchange, carbon dioxide is also obtained and the carbon dioxide is recycled.
Preferably, in step (d), the ion exchange resin is subjected to a regeneration treatment after the use is completed.
Preferably, in step (D), the silica has a D50 particle size of 4 to 12 μm.
Preferably, in step (d), the temperature of the drying is 120 to 200 ℃.
The invention also provides application of the silica prepared by the preparation method of the silica in paint, plastic, adhesive and rubber.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the preparation method of the silicon dioxide, the material and the quartz sand obtained by concentrating and crystallizing the silicon dioxide production wastewater produced by a carbonization method are used as raw materials, and the silicon dioxide is prepared by adopting a precipitation method, so that the preparation method has the advantages of low cost, simplicity in operation, easiness in realizing mass production and the like.
(2) The nano silicon dioxide prepared by the preparation method of the silicon dioxide provided by the invention has high purity and good quality.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following detailed description, but those skilled in the art will understand that the following described examples are some, not all, of the 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.
Example 1
The embodiment provides a preparation method of silicon dioxide, which comprises the following steps:
(1) 100kg of silicon dioxide production wastewater produced by a carbonization method is concentrated and crystallized to obtain a material (the main component is sodium carbonate), and the material is mixed with 200kg of quartz sand with the particle size of 2mm and then calcined to obtain a material containing sodium silicate. Wherein the temperature of calcination is 1400 ℃.
(2) Adding the material containing sodium silicate obtained in the step (1) into 400kg of water, dissolving at high temperature and high pressure to obtain a sodium silicate solution, then adding 0.6kg of hydrogen peroxide solution with the mass fraction of 10% into the sodium silicate solution for reaction (impurity removal), and filtering after the reaction is finished to obtain ferric hydroxide precipitate (solid material) and the sodium silicate solution (liquid material);
(3) Introducing CO into the sodium silicate solution obtained in the step (2) 2 And filtering after reacting for 120min to obtain a solid material and a mixed solution containing sodium carbonate and sodium bicarbonate. Wherein the temperature of the mixed materials in the reaction process is 90 ℃, and the pH value is 8-10.5.
And the mixed solution containing sodium carbonate and sodium bicarbonate is recycled, and the specific method comprises the following steps: and (3) after concentrating and crystallizing the mixed solution containing sodium carbonate and sodium bicarbonate, mixing with quartz sand and calcining (at the temperature of 1400 ℃), so as to obtain sodium silicate for later use (which can be added into the material containing sodium silicate in the step (2) for next preparation of silicon dioxide or added into the sodium silicate solution in the step (3).
(4) And (4) washing the solid material obtained in the step (3) until the conductivity of the washing liquid is lower than 1000 mu s/cm, pulping, adding the solid material into strong-acid ion exchange resin, performing ion exchange, recycling the released carbon dioxide, and sequentially filtering and drying (at the temperature of 150 ℃) to obtain the silicon dioxide.
Wherein, after the strong acid ion exchange resin is used, acid is added for regeneration treatment and recycling.
The silica prepared in this example was found to have a D50 particle size of 5.3 μm and a purity of 99.88%.
Example 2
The embodiment provides a preparation method of silicon dioxide, which comprises the following steps:
(1) 100kg of silicon dioxide production wastewater produced by a carbonization method is concentrated and crystallized to obtain a material (the main component is sodium carbonate), and the material is mixed with 200kg of quartz sand with the grain diameter of 1mm and then calcined to obtain a material containing sodium silicate. Wherein the temperature of calcination is 1200 ℃.
(2) Adding the material containing sodium silicate obtained in the step (1) into 400kg of water, dissolving at high temperature and high pressure to obtain a sodium silicate solution, then adding 0.6kg of hydrogen peroxide solution with the mass fraction of 10% into the sodium silicate solution for reaction (impurity removal), and filtering after the reaction is finished to obtain ferric hydroxide precipitate (solid material) and the sodium silicate solution (liquid material);
(3) Introducing CO into the sodium silicate solution obtained in the step (2) 2 After reacting for 150min, filtering to obtain solid materials and mixed liquid containing sodium carbonate and sodium bicarbonate. Wherein the temperature of the mixed materials in the reaction process is 95 ℃, and the pH value is 8-10.5.
And the mixed solution containing sodium carbonate and sodium bicarbonate is recycled, and the specific method comprises the following steps: and (3) after concentrating and crystallizing the mixed solution containing sodium carbonate and sodium bicarbonate, mixing with quartz sand and calcining (at the temperature of 1400 ℃), so as to obtain sodium silicate for later use (which can be added into the material containing sodium silicate in the step (2) for next preparation of silicon dioxide or added into the sodium silicate solution in the step (3).
(4) And (3) washing the solid material obtained in the step (3) until the conductivity of a washing liquid is lower than 1000 mu s/cm, pulping, adding the pulped solid material into a strong-acid ion exchange resin, carrying out ion exchange, simultaneously recycling the released carbon dioxide, and then sequentially filtering and drying (at the temperature of 150 ℃) to obtain the silicon dioxide.
Wherein, after the strong acid ion exchange resin is used, acid is added for regeneration treatment and recycling.
The silica prepared in this example was found to have a D50 particle size of 6.2 μm and a purity of 99.85%.
Example 3
The embodiment provides a preparation method of silicon dioxide, which comprises the following steps:
(1) 100kg of silicon dioxide production wastewater produced by a carbonization method is concentrated and crystallized to obtain a material (the main component is sodium carbonate), and the material is mixed with 200kg of quartz sand with the particle size of 1mm and then calcined to obtain a material containing sodium silicate. Wherein the temperature of calcination is 1500 ℃.
(2) Adding the material containing sodium silicate obtained in the step (1) into 400kg of water, dissolving at high temperature and high pressure to obtain a sodium silicate solution, then adding 0.6kg of hydrogen peroxide solution with the mass fraction of 10% into the sodium silicate solution for reaction (impurity removal), and filtering after the reaction is finished to obtain ferric hydroxide precipitate (solid material) and the sodium silicate solution (liquid material);
(3) Introducing CO into the sodium silicate solution obtained in the step (2) 2 After reacting for 240min, filtering to obtain solid materials and mixed liquid containing sodium carbonate and sodium bicarbonate. Wherein the temperature of the mixed materials in the reaction process is 98 ℃, and the pH value is 8-10.5.
(4) And (3) washing the solid material obtained in the step (3) until the conductivity of a washing liquid is lower than 1000 mu s/cm, pulping, adding the pulped solid material into a strong-acid ion exchange resin, carrying out ion exchange, simultaneously recycling the released carbon dioxide, and then sequentially filtering and drying (at the temperature of 150 ℃) to obtain the silicon dioxide.
Wherein, after the strong acid ion exchange resin is used, acid is added for regeneration treatment and recycling.
The silica prepared in this example was found to have a D50 particle size of 4.8 μm and a purity of 99.89%.
Example 4
The embodiment provides a preparation method of silicon dioxide, which comprises the following steps:
(1) 100kg of silicon dioxide production wastewater produced by a carbonization method is concentrated and crystallized to obtain a material (the main component is sodium carbonate), and the material is mixed with 200kg of quartz sand with the particle size of 0.5mm and then calcined to obtain a material containing sodium silicate. Wherein the temperature of calcination is 1400 ℃.
(2) Adding the material containing sodium silicate obtained in the step (1) into 400kg of water, dissolving at high temperature and high pressure to obtain a sodium silicate solution, then adding 0.6kg of a hydrogen peroxide solution with the mass fraction of 10% into the sodium silicate solution to perform reaction (impurity removal), and filtering after the reaction is finished to obtain an iron hydroxide precipitate (solid material) and a sodium silicate solution (liquid material);
(3) Introducing CO into the sodium silicate solution obtained in the step (2) 2 Reacting for 60min, and filtering to obtain solid material and mixed liquid containing sodium carbonate and sodium bicarbonate. Wherein the temperature of the mixed materials in the reaction process is 70 ℃, and the pH value is 8-10.5.
(4) And (3) washing the solid material obtained in the step (3) until the conductivity of a washing liquid is lower than 1000 mu s/cm, pulping, adding the pulped solid material into a strong-acid ion exchange resin, carrying out ion exchange, simultaneously recycling the released carbon dioxide, and then sequentially filtering and drying (at the temperature of 150 ℃) to obtain the silicon dioxide.
Wherein, after the strong acid ion exchange resin is used, acid is added for regeneration treatment and recycling.
The silica prepared in this example was found to have a D50 particle size of 5.6 μm and a purity of 99.91%.
Example 5
The embodiment provides a preparation method of silicon dioxide, which comprises the following steps:
(1) 100kg of silicon dioxide production wastewater produced by a carbonization method is concentrated and crystallized to obtain a material (the main component is sodium carbonate), and the material is mixed with 200kg of quartz sand with the particle size of 0.1mm and then calcined to obtain a material containing sodium silicate. Wherein the temperature of calcination is 1300 ℃.
(2) Adding the material containing sodium silicate obtained in the step (1) into 400kg of water, dissolving at high temperature and high pressure to obtain a sodium silicate solution, then adding 0.6kg of hydrogen peroxide solution with the mass fraction of 10% into the sodium silicate solution for reaction (impurity removal), and filtering after the reaction is finished to obtain ferric hydroxide precipitate (solid material) and the sodium silicate solution (liquid material);
(3) Introducing CO into the sodium silicate solution obtained in the step (2) 2 And reacting for 120min, and filtering to obtain a solid material and a mixed solution containing sodium carbonate and sodium bicarbonate. Wherein the temperature of the mixed materials in the reaction process is 50 ℃, and the pH value is 8-10.5.
(4) And (3) washing the solid material obtained in the step (3) until the conductivity of a washing liquid is lower than 1000 mu s/cm, pulping, adding the pulped solid material into a strong-acid ion exchange resin, carrying out ion exchange, simultaneously recycling the released carbon dioxide, and then sequentially filtering and drying (at the temperature of 150 ℃) to obtain the silicon dioxide.
Wherein, after the strong acid ion exchange resin is used, acid is added for regeneration treatment and recycling.
The silica prepared in this example was found to have a D50 particle size of 5.7 μm and a purity of 99.87%.
Comparative example 1
The comparative example provides silica prepared substantially the same as example 1 except that the temperature in step (1) was replaced with 1800 ℃.
The silica prepared by this comparative example was found to have a particle size of 10.7 μm and a purity of 99.80%.
Comparative example 2
This comparative example provides silica having substantially the same preparation method as example 1 except that the pH in step (3) was replaced with 7.5.
The silica prepared by this comparative example was found to have a particle size of 11.4 μm and a purity of 99.83%.
Comparative example 3
The preparation method of silica provided in this comparative example is substantially the same as that of example 1 except that step (4) is not provided, that is, ion exchange is not performed.
The silica prepared by this comparative example was found to have a particle size of 5.5 μm and a purity of 95.2%.
While particular embodiments of the present invention have been illustrated and described, it will be appreciated that the above embodiments are merely illustrative of the technical solution of the present invention and are not restrictive; those of ordinary skill in the art will understand that: modifications may be made to the above-described embodiments, or equivalents may be substituted for some or all of the features thereof without departing from the spirit and scope of the present invention; 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 silicon dioxide is characterized by comprising the following steps:
(a) The material obtained by concentrating and crystallizing the silicon dioxide production wastewater produced by the carbonization method is mixed with quartz sand and then calcined to obtain a material containing sodium silicate;
(b) Dissolving the material containing sodium silicate obtained in the step (a) in water, mixing the material with an oxidant, reacting, and then carrying out solid-liquid separation to obtain an iron hydroxide precipitate and a sodium silicate solution;
(c) The step of(b) Introducing CO into the sodium silicate solution obtained in the step (2) 2 Carrying out reaction, and carrying out solid-liquid separation after the reaction is finished to obtain a solid material and a mixed solution containing sodium carbonate and sodium bicarbonate;
(d) Pulping the solid material obtained in the step (c), adding the pulped solid material into ion exchange resin for ion exchange, and then sequentially carrying out solid-liquid separation and drying to obtain silicon dioxide.
2. The method for preparing silica according to claim 1, wherein the calcination temperature in the step (a) is 1200 to 1500 ℃;
preferably, in the step (a), the mass ratio of the material obtained by concentrating and crystallizing the silicon dioxide production wastewater produced by the carbonization method to the quartz sand is 1.
3. The method for preparing silica according to claim 1, wherein in the step (b), the oxidizing agent comprises hydrogen peroxide solution and/or ozone; preferably, the mass fraction of the hydrogen peroxide solution is 5-50%;
preferably, the mass ratio of the oxidizing agent in step (b) to the sodium silicate in step (a) is 0.01% to 0.1%.
4. The method for preparing silica according to claim 1, wherein in the step (c), the temperature of the mixture during the reaction is 40-98 ℃;
preferably, the pH value of the mixed materials in the reaction process is 8-10.5;
preferably, the reaction time is 30 to 240min.
5. The method for producing silica according to claim 1, further comprising a step of recycling the mixed solution containing sodium carbonate and sodium hydrogencarbonate in step (c);
preferably, the recycling method specifically includes: concentrating and crystallizing the mixed solution containing sodium carbonate and sodium bicarbonate, mixing with quartz sand, and calcining to obtain sodium silicate; adding the sodium silicate into the material containing the sodium silicate in the step (b) for use, or adding the sodium silicate into the sodium silicate solution in the step (c) for use;
preferably, the temperature of the calcination is 1200 to 1500 ℃.
6. The method for producing silica according to claim 1, wherein in the step (d), before the beating, a step of washing the solid matter obtained in the step (c) is further included;
preferably, the washing is carried out until the conductivity of the washing solution is less than 1000. Mu.s/cm.
7. The method for producing silica according to claim 1, wherein in the step (d), the ion exchange resin comprises a strongly acidic cation resin and/or a weakly acidic cation resin;
preferably, in the step (d), during the ion exchange, carbon dioxide is also obtained and is recycled;
preferably, in step (d), the ion exchange resin is subjected to a regeneration treatment after the use is completed.
8. The method for preparing silica according to claim 1, wherein the silica has a D50 particle size of 4 to 12 μm in the step (D).
9. The method for preparing silica according to any one of claims 1 to 8, wherein the drying temperature in the step (d) is 120 to 200 ℃.
10. Use of the silica obtained by the process according to any one of claims 1 to 9 in coatings, plastics, adhesives and rubbers.
CN202210931529.XA 2022-08-04 2022-08-04 Preparation method and application of silicon dioxide Pending CN115196644A (en)

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Citations (6)

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JP2011153044A (en) * 2010-01-27 2011-08-11 Taiheiyo Cement Corp Method for manufacturing high purity silica
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