CN110255570B - Preparation method of high-purity synthetic quartz sand - Google Patents
Preparation method of high-purity synthetic quartz sand Download PDFInfo
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- CN110255570B CN110255570B CN201910587559.1A CN201910587559A CN110255570B CN 110255570 B CN110255570 B CN 110255570B CN 201910587559 A CN201910587559 A CN 201910587559A CN 110255570 B CN110255570 B CN 110255570B
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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Abstract
The invention belongs to the technical field of chemical production, and particularly relates to a preparation method of high-purity synthetic quartz sand. The method comprises the following steps: diluting a raw water glass material by pure water to prepare a concentrated water glass solution, carrying out dealkalization treatment to obtain a silicic acid aqueous solution, and removing iron ions and alkaline earth metal ions to obtain a high-purity silicic acid aqueous solution; heating to completely gelatinize to obtain hydrated silica gel; cooling the water-containing silica gel along with a furnace after freezing to prepare silica particles; washing and cleaning the silicon dioxide particles to obtain high-purity silicon dioxide powder; the silicon dioxide powder with closed air holes is obtained after melting. The invention adopts the water glass as the raw material, overcomes the defect that the impurity components in the ore bring influence on the quality of the finished product when the ore is adopted as the raw material in the prior art, solves the problem of porosity of the material prepared by sol-gel by utilizing a roasting method, and obtains the high-purity quartz sand with closed pores.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a preparation method of high-purity synthetic quartz sand.
Background
High-purity synthetic quartz sand, which generally refers to quartz powder with a silicon dioxide content higher than 99.99%, is a main raw material of quartz glass, quartz crucibles, quartz tubes, quartz rods and the like. In the prior art, the high-purity quartz sand is mainly obtained by purifying natural ores. Because the ore components are complex, the purification to 99.99 percent is difficult, the requirement on the purity of quartz glass products in semiconductors is higher and higher, and the natural purification method is difficult to improve. In particular, most ores often contain aluminum element, and part of the aluminum element can not be removed by entering the network structure of silicon dioxide, so that the finished product can not meet the requirement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing high-purity quartz sand by using water glass as a raw material and adopting sol-gel synthesis.
The invention is realized by the following technical scheme:
a preparation method of high-purity synthetic quartz sand comprises the following steps:
(1) Diluting with pure water by Na 2 SiO 3 ·9H 2 Preparing a raw water glass material consisting of O into a water glass solution with the concentration of 1-40%, and dealkalizing the water glass solution through an ion exchange column filled with cation exchange resin to obtain a silicic acid aqueous solution;
(2) Removing iron ions and alkaline earth metal ions from the silicic acid aqueous solution obtained in the step (1) through an ion exchange column filled with iron-removing ion exchange resin to obtain a high-purity silicic acid aqueous solution; the content of iron ions and alkaline earth metal ions in the obtained high-purity silicic acid aqueous solution is less than 500ppm;
(3) Keeping the high-purity silicic acid aqueous solution obtained in the step (2) at room temperature for standing or heating to gelatinize the silicic acid aqueous solution to obtain hydrous silica gel; standing for 1-72h, heating at 50-100 deg.C for 1-12h;
(4) Freezing the hydrous silica gel obtained in the step (3) for 3-15h at the temperature of-15 to-2 ℃;
(5) Unfreezing the frozen water-containing silica gel to prepare silica particles;
(6) Removing residual metal ions from the silicon dioxide particles obtained in the step (5) through acid washing and cleaning to obtain high-purity silicon dioxide powder with the metal ion content of less than 50 ppm;
(7) Placing the high-purity silicon dioxide powder obtained in the step (6) in a heating furnace, heating the high-purity silicon dioxide powder to 500 ℃ from room temperature, and then preserving heat for 1h; heating to 600 ℃, then preserving heat for 1h, heating to 700 ℃, then preserving heat for 1h, heating to 800 ℃, then preserving heat for 1h, heating to 900 ℃, then preserving heat for 1h, heating to 1210 ℃, and then preserving heat for 10h, thereby obtaining the silicon dioxide powder with closed pores, wherein the purity of the obtained silicon dioxide powder is more than 99.99%.
The cation exchange resin in the step (1) is acidic cation exchange resin.
The acid washing method in the step (6) is as follows: adding silica particles to HF, HCl and HNO 3 The mixed solution is filtered after being stirred for 1 to 48 hours at normal temperature or under heating condition, and the heating temperature is 50 to 100 ℃.
The cleaning method in the step (6) is as follows: and cleaning the silicon dioxide particles obtained after acid cleaning with ultrapure water, wherein the resistivity of the ultrapure water is more than 17 megaohms.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the water glass as the raw material, and overcomes the defect that the impurity components in the ore bring influence on the quality of the finished product when the ore is adopted as the raw material in the prior art.
2. The invention adopts sol-gel synthesis to prepare high-purity quartz sand, solves the problem of porosity of a material prepared from sol-gel by a roasting method, and obtains the high-purity quartz sand with closed pores.
3. The process for preparing silicic acid by using water glass adopts acidic cation exchange resin, and is milder and easier to control than the reaction of hydrochloric acid and sulfuric acid.
4. The method can control the granularity and the shape of the prepared quartz sand by controlling the concentration of the water glass solution, thereby meeting the requirements of different quartz glass production processes, such as 100-200 meshes of quartz sand required by a gas smelting quartz glass process and 40-160 meshes of quartz sand required by an electric connection melting quartz glass process.
5. The shape of the quartz sand particles prepared by the invention is similar to the shape of crushed natural ores, and because the shape is not spherical, bubbles can be removed in the melting process, thereby preparing quartz glass with good internal quality.
Drawings
FIG. 1 is a schematic view showing the shape of quartz sand produced in example 3 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited by the examples.
Example 1
A preparation method of high-purity synthetic quartz sand comprises the following steps:
(1) Diluting with pure water to remove Na 2 SiO 3 ·9H 2 Making raw water glass material composed of O into water glass solution with concentration of 5%, and mixing water glassDealkalizing the solution through an ion exchange column filled with weak acid cation exchange resin to obtain a silicic acid aqueous solution;
(2) Removing iron ions and alkaline earth metal ions from the silicic acid aqueous solution obtained in the step (1) through an ion exchange column filled with iron-removing ion exchange resin to obtain a high-purity silicic acid aqueous solution; the content of iron ions and alkaline earth metal ions in the obtained high-purity silicic acid aqueous solution is less than 500ppm;
(3) Keeping the high-purity silicic acid aqueous solution obtained in the step (2) at room temperature, and standing to completely gelatinize the silicic acid aqueous solution to obtain hydrous silica gel; standing for 36.4h;
(4) Freezing the hydrous silica gel obtained in the step (3) for 8.6h at-9 ℃;
(5) Keeping the frozen water-containing silica gel at 250 ℃ for 1h, and then cooling the silica gel along with the furnace to prepare silica particles;
(6) Washing and cleaning the silica particles obtained in the step (5), wherein the silica particles are added to HF, HCl and HNO during acid washing 3 The mixed solution is stirred for 46 hours at normal temperature and then filtered, and the silicon dioxide particles obtained after filtering are washed by ultrapure water, wherein the resistivity of the ultrapure water is more than 17 megaohms. Removing residual metal ions through acid washing and cleaning to obtain high-purity silicon dioxide powder with the metal ion content of less than 50 ppm;
(8) Placing the high-purity silicon dioxide powder obtained in the step (6) in a heating furnace, heating the high-purity silicon dioxide powder to 500 ℃ from room temperature, and then preserving heat for 1h; and (3) heating to 600 ℃, then preserving heat for 1h, heating to 700 ℃, then preserving heat for 1h, heating to 800 ℃, then preserving heat for 1h, heating to 900 ℃, then preserving heat for 1h, heating to 1210 ℃, and then preserving heat for 10h, so that silicon dioxide powder with closed air holes is obtained, and the purity of the obtained silicon dioxide powder is more than 99.99%.
The obtained silica powder is quartz sand particles, and the particle size of the quartz sand particles obtained in the embodiment is 140-160 meshes according to measurement.
Example 2
A preparation method of high-purity synthetic quartz sand comprises the following steps:
(1) Diluting with pure waterNa 2 SiO 3 ·9H 2 Preparing a raw water glass material consisting of O into a water glass solution with the concentration of 40%, and dealkalizing the water glass solution through an ion exchange column filled with strong-base cation exchange resin to obtain a silicic acid aqueous solution;
(2) Removing iron ions and alkaline earth metal ions from the silicic acid aqueous solution obtained in the step (1) through an ion exchange column filled with iron-removing ion exchange resin to obtain a high-purity silicic acid aqueous solution; the content of iron ions and alkaline earth metal ions in the obtained high-purity silicic acid aqueous solution is less than 500ppm;
(3) Heating the high-purity silicic acid aqueous solution obtained in the step (2) to completely gelatinize the silicic acid aqueous solution to obtain hydrated silica gel; the heating temperature is 87 ℃, and the heating time is 6h.
(4) Freezing the hydrous silica gel obtained in the step (3) for 6 hours at the temperature of minus 3 ℃;
(5) Keeping the frozen water-containing silica gel at 250 ℃ for 1h, and then cooling the silica gel along with the furnace to prepare silica particles;
(6) Washing and cleaning the silica particles obtained in the step (5), wherein the silica particles are added to HF, HCl and HNO during acid washing 3 Stirring the mixed solution at 85 ℃ for 23 hours, filtering, washing the silicon dioxide particles obtained after filtering with ultrapure water, wherein the resistivity of the ultrapure water is more than 17 megaohms, and removing residual metal ions by acid washing and washing to obtain high-purity silicon dioxide powder with the metal ion content of less than 50 ppm;
(7) Placing the high-purity silicon dioxide powder obtained in the step (6) in a heating furnace, heating the high-purity silicon dioxide powder to 500 ℃ from room temperature, and then preserving heat for 1h; heating to 600 ℃, then preserving heat for 1h, heating to 700 ℃, then preserving heat for 1h, heating to 800 ℃, then preserving heat for 1h, heating to 900 ℃, then preserving heat for 1h, heating to 1210 ℃, and then preserving heat for 10h, thereby obtaining the silicon dioxide powder with closed pores, wherein the purity of the obtained silicon dioxide powder is more than 99.99%.
The obtained silica powder is quartz sand particles, and the particle size of the quartz sand particles obtained in the embodiment is 40-60 meshes according to measurement.
Example 3
A preparation method of high-purity synthetic quartz sand comprises the following steps:
(1) Diluting with pure water to remove Na 2 SiO 3 ·9H 2 Preparing a raw water glass material consisting of O into a water glass solution with the concentration of 25%, and dealkalizing the water glass solution through an ion exchange column filled with weak acid cation exchange resin to obtain a silicic acid aqueous solution;
(2) Removing iron ions and alkaline earth metal ions from the silicic acid aqueous solution obtained in the step (1) through an ion exchange column filled with iron-removing ion exchange resin to obtain a high-purity silicic acid aqueous solution; the content of iron ions and alkaline earth metal ions in the obtained high-purity silicic acid aqueous solution is less than 500ppm;
(3) Heating the high-purity silicic acid aqueous solution obtained in the step (2) to completely gelatinize the silicic acid aqueous solution to obtain hydrated silica gel; the heating temperature is 98 ℃, and the heating time is 1.3h;
(4) Freezing the hydrous silica gel obtained in the step (3) for 3h at-15 ℃;
(5) Keeping the frozen water-containing silica gel at 250 ℃ for 1h, and then cooling the silica gel along with the furnace to prepare silica particles;
(6) Removing residual metal ions from the silicon dioxide particles obtained in the step (5) through acid washing and cleaning to obtain high-purity silicon dioxide powder with the metal ion content of less than 50 ppm;
(7) Placing the high-purity silicon dioxide powder obtained in the step (6) in a heating furnace, heating the high-purity silicon dioxide powder to 500 ℃ from room temperature, and then preserving heat for 1h; heating to 600 ℃, then preserving heat for 1h, heating to 700 ℃, then preserving heat for 1h, heating to 800 ℃, then preserving heat for 1h, heating to 900 ℃, then preserving heat for 1h, heating to 1210 ℃, and then preserving heat for 10h, thereby obtaining the silicon dioxide powder with closed pores, wherein the purity of the obtained silicon dioxide powder is more than 99.99%.
The pickling method in the step (6) is as follows: adding silica particles to HF, HCl and HNO 3 The mixed solution of (1) was stirred under heating for 2 hours and then filtered off, the heating temperature being 100 ℃. The cleaning method in the step (6) is as follows: and cleaning the silicon dioxide particles obtained after acid cleaning with ultrapure water, wherein the resistivity of the ultrapure water is more than 17 megaohms.
The obtained silica powder is quartz sand particles, and the particle size of the quartz sand particles obtained in the embodiment is 60-80 meshes according to measurement. The shape of the obtained quartz sand can be seen by microscopic observation, and is shown in figure 1.
Claims (1)
1. The preparation method of the high-purity synthetic quartz sand is characterized by comprising the following steps of:
(1) Diluting with pure water to remove Na 2 SiO 3 ·9H 2 Preparing a raw water glass material consisting of O into a water glass solution with the concentration of 40%, and dealkalizing the water glass solution through an ion exchange column filled with cation exchange resin to obtain a silicic acid aqueous solution, wherein the cation exchange resin is acidic cation exchange resin;
(2) Removing iron ions and alkaline earth metal ions from the silicic acid aqueous solution obtained in the step (1) through an ion exchange column filled with iron-removing ion exchange resin to obtain a high-purity silicic acid aqueous solution; the content of iron ions and alkaline earth metal ions in the obtained high-purity silicic acid aqueous solution is less than 500ppm;
(3) Keeping the high-purity silicic acid aqueous solution obtained in the step (2) at room temperature for standing or heating to gelatinize the silicic acid aqueous solution to obtain hydrous silica gel; standing for 1-72h, heating at 50-100 deg.C for 1-12h;
(4) Freezing the hydrous silica gel obtained in the step (3) for 3-15h at the temperature of-15 to-2 ℃;
(5) Unfreezing the frozen water-containing silica gel to prepare silica particles;
(6) Removing residual metal ions from the silicon dioxide particles obtained in the step (5) through acid washing and cleaning to obtain high-purity silicon dioxide powder with the metal ion content of less than 50 ppm;
the pickling method comprises the following steps: adding silica particles to HF, HCl and HNO 3 Stirring the mixed solution at normal temperature or under heating condition for 1-48h, and filtering, wherein the heating temperature is 50-100 ℃; the cleaning method comprises the following steps: washing the silicon dioxide particles obtained after acid washing with ultrapure water, whereinThe resistivity of the ultrapure water is more than 17 megaohms;
(7) Placing the high-purity silicon dioxide powder obtained in the step (6) in a heating furnace, heating the high-purity silicon dioxide powder to 500 ℃ from room temperature, and then preserving heat for 1h; heating to 600 ℃, then preserving heat for 1h, heating to 700 ℃, then preserving heat for 1h, heating to 800 ℃, then preserving heat for 1h, heating to 900 ℃, then preserving heat for 1h, heating to 1210 ℃, and then preserving heat for 10h, thereby obtaining the silicon dioxide powder with closed pores, wherein the purity of the obtained silicon dioxide powder is more than 99.99%.
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