CN111320177A - Method for removing hydroxyl in quartz sand powder - Google Patents
Method for removing hydroxyl in quartz sand powder Download PDFInfo
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- CN111320177A CN111320177A CN202010283523.7A CN202010283523A CN111320177A CN 111320177 A CN111320177 A CN 111320177A CN 202010283523 A CN202010283523 A CN 202010283523A CN 111320177 A CN111320177 A CN 111320177A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
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Abstract
The invention relates to a method for removing hydroxyl in quartz sand powder, which comprises the steps of firstly feeding high-purity quartz materials into a high-temperature vacuum furnace, heating to 1000-1050 ℃, and introducing H2Or H2Taking the mixed gas of nitrogen and/or helium as reducing gas, carrying out high-temperature reduction treatment for not less than 2 hours, starting a vacuum system, raising the temperature to 1470-1500 ℃, and raising the vacuum degree to 6.0 × 10‑6～7.0×10‑ 6And pa, carrying out vacuum degassing treatment for 3-4 hours to obtain the high-purity low-hydroxyl quartz sand powder material. The hydroxyl content of the quartz sand powder prepared by the method is lower than 3 ppm.
Description
Technical Field
The invention relates to a method for removing hydroxyl in quartz sand powder, belonging to the non-metal ore deep processing industry.
Background
The transparent quartz glass and its product are produced by using high-purity quartz sand powder as raw material, and melting in high-temperature electric melting furnace by using hydrogen or inert gas or hydrogen + nitrogen + inert gas as protective gas to obtain molten glass, and because of strong hydrogen permeability, it can take away a large amount of silicon vapour, and can play good role in removing quartz glass colouring, raising protection effect and raising product quality, and the molten glass can be mechanically formed, cut, cooled, cleaned, dried and dehydroxylated to obtain the transparent quartz glass product.
JC/T597-2011 provides that the content of hydroxyl groups is less than or equal to 220 × 10-6The content of hydroxyl group in transparent quartz glass rod for semiconductor JC/T2064-2011 is less than or equal to 220 × 10-6In the specification JC/T598-2007 in transparent quartz glass tube for electric light source, a) the hydroxyl group content of the high-pressure mercury lamp tube is less than or equal to 10 × 10-6B) the hydroxyl content of the metal halide lamp tube is less than or equal to 3 × 10-6(ii) a c) Halogen tungsten lamp tube, quartz glass tube for other lamp: agreed by both the supplier and the demand. The source of hydroxyl groups of the quartz glass article comprises essentially two parts: one is hydroxyl contained in the quartz sand, and the other part is protective gas H in the high-temperature melting process2SiO with quartz glass2The hydroxyl group produced by the chemical reaction is higher in proportion than the former one. The hydroxyl groups of the quartz sand are mainly from structural water in the quartz crystal structure and are (OH)-、H+、(H3O)+The ionic form exists in the crystal lattice of quartz crystals as "water", in (OH)-The most common form is that its removal is rather difficult due to the strong bonding forces associated with other particles in the crystal.
In the process of melting quartz glass, gas and liquid wrappings, structural water and hydroxyl groups remained in the raw material quartz sand powder slowly form tiny bubbles in high-temperature glass liquid and gradually increase, and finally escape from the glass liquid. Due to the SiO accompanying the melting process2Because of volatilization, the melting time and melting temperature need to be controlled to a certain extent to reduce the loss of raw materials. In addition, the molten glass still has a certain viscosity at high temperature, and some fine single bubbles are difficult to overcome the viscosity resistance of the molten glass to become large bubbles to escape, which can be homogenizedAnd remain or dissolve in the transparent molten glass and finally exist in the quartz glass product in the form of microbubbles or hydroxyl groups. The hydroxyl groups are usually removed by a high-temperature high-vacuum method, but the hydroxyl group removing effect of the high-temperature vacuum treatment is limited, which seriously limits the quality of high-quality quartz glass and products. In order to solve the problem of hydroxyl in quartz glass raw material quartz sand and improve the qualification rate of quartz glass and products thereof, people need to control the hydroxyl in the quartz glass raw material sand, ensure the purity of the raw material and remove the hydroxyl in the raw material sand to the maximum extent. Therefore, a method for removing hydroxyl groups in quartz sand powder is developed, and the hydroxyl group content in the quartz sand powder prepared by the method is 1-3 ppm.
Disclosure of Invention
The invention aims to provide a method for removing hydroxyl groups in quartz sand as a raw material of quartz glass, and the quartz sand after the hydroxyl groups are removed is used as a high-quality raw material of the quartz glass.
The scheme adopted by the invention for solving the technical problems is as follows:
a method for removing hydroxyl in quartz sand powder comprises the following steps:
(1) feeding a high-purity quartz material into a high-temperature vacuum furnace, heating to 1000-1050 ℃, and introducing H2Or H2Performing high-temperature reduction treatment with one or two of nitrogen and helium as reducing gas for at least 2 hr;
(2) starting a vacuum system, raising the temperature to 1470-1500 ℃, and raising the vacuum degree to 6.0 × 10-6～7.0×10-6And pa, carrying out vacuum degassing treatment for 3-4 hours to obtain the high-purity low-hydroxyl quartz sand powder material.
Preferably, the hydroxyl content in the high-purity low-hydroxyl quartz sand powder material obtained in the step (2) is not more than 3 ppm.
Preferably, the high-purity quartz material in the step (1) is prepared from vein quartz of igneous rock, and the preparation process comprises the following steps: selecting SiO2The% (m/m) ≧ 99.90% igneous rock vein quartz is processed by mineral dressing → crushing → acid washing → calcining → water quenching → sand making → magnetic separation → classification → flotation → acid washing→ pure water washing → drying to obtain high-purity quartz sand; and then the obtained high-purity quartz sand is subjected to high-temperature chlorination at the temperature of 1000-1100 ℃ for 1-1.5 h to obtain the high-purity quartz sand.
Preferably, the metal and nonmetal impurities in the high-purity quartz material in the step (1) are less than or equal to 20 ppm.
Preferably, the reducing gas in the step (1) is introduced under the condition of micro negative pressure, and the vacuum degree of the micro negative pressure environment is 0.001-0.01 MPa.
The invention also aims to provide a method for melting a low-hydroxyl quartz glass device, which comprises the steps of firstly preparing a high-purity low-hydroxyl quartz sand powder material by adopting the method, and then melting the required quartz glass device at the temperature of 1800-.
α -Quartz (Low temperature Quartz) is converted to β -Quartz (high temperature Quartz) at 573 deg.C, β -Quartz is stable at 573-870 deg.C under atmospheric pressure β -Quartz is converted to tridymite at temperatures above 870 deg.C, tridymite is SiO2The tridymite is transformed into high-temperature cristobalite at the temperature of 1470 ℃ and the high-temperature cristobalite is an isometric crystal system variant stable at the temperature of 1470 ℃ and 1728 ℃ under normal pressure, the transformation of β -quartz into tridymite is reconstruction phase change, when the quartz material is subjected to high-temperature reconstruction phase change, Si-O bonds are firstly broken and then reconstructed, the crystal lattice of the quartz crystal is opened when the Si-O bonds of the quartz crystal are broken, so that hydroxyl groups in the original crystal lattice can be fully exposed, the Si-O bonds in the crystal are in a transition state before reconstruction before the reconstruction of the Si-O bonds, and hydrogen can permeate into OH exposed from the reduced crystal lattice in the quartz material by selecting a proper temperature range for hydrogen reduction-And the generated water vapor is volatilized, thereby achieving the purpose of removing the hydroxyl. The hydroxyl groups which are not removed and residual reducing hydrogen can be removed in the environment of 1470 ℃ and 1500 ℃ in high vacuum. The final product is a low-hydroxyl or hydroxyl-free quartz material.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
The hydroxyl content in the invention is all in GB/T12442-2019The method is used for inspection; SiO 22The purity is checked according to the method GB/T3284-2015; the impurity elements are tested according to the method GB/T32650-2016.
Example 1
SiO of Xinyang place in Henan province2Taking vein quartz with the purity of 99.98 percent as a raw material, and obtaining high-purity quartz sand through mineral dressing → crushing → acid washing → calcining → water quenching → sand making → magnetic separation → classification → flotation → acid washing → pure water washing → drying; and then the obtained high-purity quartz sand is subjected to high-temperature chlorination for 1 hour at the temperature of 1000 ℃ to obtain 70-120-mesh initial raw material high-purity quartz sand powder. The hydroxyl group content of the initial raw material was measured to be 400ppm, SiO2The purity is 99.98%.
The initial raw materials are processed according to the following steps:
1. placing the initial raw materials after high-temperature chlorination into a vertical metal tungsten high-temperature vacuum furnace with the temperature of 1050 ℃, calcining for 2 hours in a micro-negative pressure (0.001 Mpa shown in a vacuum table), and then introducing 5% H from the bottom of the furnace at the temperature2Carrying out high-temperature reduction treatment on the mixed gas (V/V) of + 95% He for 2 hours, stopping ventilation, and preparing for vacuum degassing;
2. starting a vacuum system, heating to 1470 ℃, and keeping the vacuum degree at 6.0-7.0 × 10-6pa, removing the mixed gas for 4 hours, and then feeding the obtained material into a storage bin of a continuous melting furnace for melting quartz for later use;
3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz tube drawing furnace to melt quartz glass liquid at 1800 plus 2000 ℃, and drawing the transparent quartz glass tube for the electric light source by using high-purity nitrogen of 4N or above as protective gas according to a conventional process method. Hydroxyl group content of the drawn transparent quartz glass tube product was 1ppm, SiO2The purity is 99.999%.
Example 2
SiO in certain place of Huanggang in Hubei province2Taking vein quartz with the purity of 99.96% as a raw material, and obtaining high-purity quartz sand through mineral dressing → crushing → acid washing → calcining → water quenching → sand making → magnetic separation → classification → flotation → acid washing → pure water washing → drying; then the obtained high-purity quartz sand is subjected to high-temperature chlorination for 1.5 hours at 1050 ℃ to obtainThe high-purity quartz sand powder is used as the initial raw material of 40-70 meshes. The hydroxyl content of the initial raw material was measured to be 600ppm, SiO2The purity is 99.96%.
The initial raw materials are processed according to the following steps:
1. placing the initial raw materials after high-temperature chlorination into a vertical metal tungsten high-temperature vacuum furnace at 1050 ℃, calcining for 2 hours under a micro-negative pressure bar (shown as 0.003Mpa in a vacuum table), and then introducing 10% H from the bottom of the furnace at the temperature2+90％N2The mixed gas (V/V) is reduced at high temperature for 3 hours, the introduction of the mixed gas containing hydrogen is stopped, and the preparation for vacuum degassing is started;
2. starting a vacuum system, heating to 1500 ℃, and keeping the vacuum degree at 6.0-7.0 × 10-6pa, removing the hydrogen-containing mixed gas for 3 hours, and then feeding the materials into a storage bin of a continuous melting furnace for melting quartz for later use;
3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz tube drawing rod to melt quartz glass liquid at the temperature of 1800 plus 2100 ℃, and drawing the transparent quartz glass rod for the semiconductor by using high-purity nitrogen of 4N or more as protective gas according to a conventional process method. Hydroxyl group content of the drawn transparent quartz glass tube product was 3ppm, SiO2％：99.998％。
Example 3
SiO in certain place of Shaanxi Han2Purity: 99.97 percent of vein quartz is used as a raw material, and high-purity quartz sand is obtained through mineral dressing → crushing → acid washing → calcining → water quenching → sand making → magnetic separation → classification → flotation → acid washing → pure water washing → drying; and then the obtained high-purity quartz sand is subjected to high-temperature chlorination for 1 hour at 1100 ℃ to obtain 70-120-mesh initial raw material high-purity quartz sand powder. The hydroxyl group content of the initial raw material is measured to be 500ppm, SiO2The purity is 99.97%.
The initial raw materials are processed according to the following steps:
1. placing the above initial raw materials after high temperature chlorination into a vertical high temperature vacuum furnace made of metal tungsten at 1000 deg.C, calcining under micro negative pressure (vacuum table shows 0.006Mpa) for 2 hr, and introducing H from the bottom of the furnace at the above temperature2Carrying out high-temperature reduction treatment for 2 hours, stopping introducing gas, and starting to prepare vacuum degassing;
2. starting a vacuum system, heating to 1480 ℃ and vacuum degree of 6.0-7.0 × 10-6pa, removing hydrogen-containing gas for 3.5 hours, and then feeding the materials into a storage bin of a continuous melting furnace for melting quartz for later use;
3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz tube drawing furnace to melt quartz glass liquid at 1800-2100 ℃, and drawing the transparent quartz glass tube for the semiconductor by using high-purity nitrogen gas of 4N or above as protective gas according to a conventional process method. Hydroxyl group content of the drawn transparent quartz glass tube product was 2ppm, SiO2％：99.998％。
Example 4
SiO of certain place in the Hunan Yueyang2Purity: 99.97 percent of vein quartz is used as a raw material, and high-purity quartz sand is obtained through mineral dressing → crushing → acid washing → calcining → water quenching → sand making → magnetic separation → classification → flotation → acid washing → pure water washing → drying; and then the obtained high-purity quartz sand is subjected to high-temperature chlorination for 1 hour at 1100 ℃ to obtain 70-120-mesh initial raw material high-purity quartz sand powder. The hydroxyl group content of the initial raw material was measured to be 550ppm, SiO2The purity is 99.97%.
The initial raw materials are processed according to the following steps:
1. placing the above initial raw materials after high temperature chlorination into a vertical high temperature vacuum furnace made of metal tungsten at 1000 deg.C, calcining under micro negative pressure (vacuum table shows 0.006Mpa) for 2 hr, and introducing 10% H from the bottom of the furnace at the above temperature2+40％He+40％N2(V/V/V) carrying out high-temperature reduction treatment for 2 hours, stopping introducing gas, and starting to prepare vacuum degassing;
2. starting a vacuum system, heating to 1480 ℃ and vacuum degree of 6.0-7.0 × 10-6pa, removing residual gas for 3.5 hours, and then feeding the materials into a storage bin of a continuous melting furnace for melting quartz for later use;
3, feeding the quartz glass raw material sand powder obtained in the step 2 into a continuous quartz pulling tube furnace for melting quartz glass liquid at 1800-2100 ℃ for4N or more high-purity nitrogen is used as protective gas, and the transparent quartz glass tube for the semiconductor is drawn according to the conventional process method. Hydroxyl group content of the drawn transparent quartz glass tube product was 2ppm, SiO2％：99.998％。
Example 5
The same starting materials as in example 1, and the same manner of treating the starting materials and the same melting method were used, except that the reducing gas was 50% H2+50％N2The composition of the mixed gas.
Hydroxyl group content of the final drawn transparent quartz glass tube product was 2ppm, SiO2The purity is 99.998%.
Example 6
The same starting materials as in example 1, the same manner of treating the starting materials, and the same manner of melting were used, except that the composition of the reduced mixed gas was: 30% H2+35％He+35％N2(V/V/V)。
Hydroxyl group content of the final drawn transparent quartz glass tube product was 2ppm, SiO2The purity is 99.998%.
Comparative example 1
The same starting materials as in example 1, the same manner of treating the starting materials, and the same manner of melting were used, except that the temperature of the high-temperature reduction treatment was 900 ℃.
Hydroxyl group content of final pulled transparent quartz glass tube finished product for electric light source is 8ppm, SiO2The purity is 99.996%.
Comparative example 2
The same starting materials as in example 1, the same manner of treating the starting materials, and the same manner of melting were used, except that the temperature of the high-temperature reduction treatment was 1100 ℃.
Hydroxyl group content of the final drawn transparent quartz glass tube product was 8ppm, SiO2Purity 99.995%, where a small amount of SiO was detected.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (6)
1. A method for removing hydroxyl in quartz sand powder is characterized by comprising the following steps:
(1) feeding a high-purity quartz material into a high-temperature vacuum furnace, heating to 1000-1050 ℃, and introducing H2Or H2The mixed gas of the nitrogen and/or helium is used as reducing gas to carry out high-temperature reduction treatment for not less than 2 hours;
(2) starting a vacuum system, raising the temperature to 1470-1500 ℃, and raising the vacuum degree to 6.0 × 10-6～7.0×10-6And pa, carrying out vacuum degassing treatment for 3-4 hours to obtain the high-purity low-hydroxyl quartz sand powder material.
2. The method for removing hydroxyl groups from quartz sand powder as claimed in claim 1, wherein the hydroxyl group content of the high-purity low-hydroxyl quartz sand powder material obtained in the step (2) is not more than 3 ppm.
3. The method for removing hydroxyl groups from quartz sand powder according to claim 1, wherein the high-purity quartz material obtained in step (1) is prepared from vein quartz of igneous rock by the following steps: selecting SiO2The method comprises the following steps of (m/m) ≧ 99.90% of igneous rock vein quartz, and obtaining high-purity quartz sand through mineral dressing → crushing → acid washing → calcining → water quenching → sand preparation → magnetic separation → classification → flotation → acid washing → pure water washing → drying; and then the obtained high-purity quartz sand is subjected to high-temperature chlorination at the temperature of 1000-1100 ℃ for 1-1.5 h to obtain the high-purity quartz sand.
4. The method for removing hydroxyl groups from quartz sand powder according to claim 1, wherein the metal and non-metal impurities in the high-purity quartz material obtained in step (1) are less than or equal to 20 ppm.
5. The method for removing hydroxyl groups in quartz sand powder according to claim 1, wherein the reducing gas in step (1) is introduced under a micro-negative pressure environment with a vacuum degree of 0.001-0.01 MPa.
6. A method for melting a low-hydroxyl quartz glass device is characterized in that firstly, a high-purity low-hydroxyl quartz sand powder material is prepared by the method of any one of claims 1 to 5, and then the required quartz glass device is melted at 1800-.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112010317A (en) * | 2020-09-14 | 2020-12-01 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN112479560A (en) * | 2020-12-24 | 2021-03-12 | 连云港福东正佑照明电器有限公司 | Preparation method of radiation-resistant anti-crystallization high-transmittance quartz tube for ultra-high-power light source |
| CN112624580A (en) * | 2020-12-03 | 2021-04-09 | 东海县奥兰石英科技有限公司 | Method for removing impurities of optical fiber quartz target rod by continuous melting and intermediate frequency furnace integration method |
| CN114368757A (en) * | 2022-01-21 | 2022-04-19 | 成都光华科技发展有限公司 | Purification method of high-purity quartz sand |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112010317A (en) * | 2020-09-14 | 2020-12-01 | 昆明理工大学 | Method for purifying quartz sand by microwave-vacuum combined roasting |
| CN112624580A (en) * | 2020-12-03 | 2021-04-09 | 东海县奥兰石英科技有限公司 | Method for removing impurities of optical fiber quartz target rod by continuous melting and intermediate frequency furnace integration method |
| CN112624580B (en) * | 2020-12-03 | 2021-12-14 | 东海县奥兰石英科技有限公司 | Method for removing impurities of optical fiber quartz target rod by continuous melting and intermediate frequency furnace integration method |
| CN112479560A (en) * | 2020-12-24 | 2021-03-12 | 连云港福东正佑照明电器有限公司 | Preparation method of radiation-resistant anti-crystallization high-transmittance quartz tube for ultra-high-power light source |
| CN114368757A (en) * | 2022-01-21 | 2022-04-19 | 成都光华科技发展有限公司 | Purification method of high-purity quartz sand |
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