CN115872407A - Preparation method of 4N-grade high-purity quartz sand - Google Patents
Preparation method of 4N-grade high-purity quartz sand Download PDFInfo
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- CN115872407A CN115872407A CN202111131276.XA CN202111131276A CN115872407A CN 115872407 A CN115872407 A CN 115872407A CN 202111131276 A CN202111131276 A CN 202111131276A CN 115872407 A CN115872407 A CN 115872407A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000002386 leaching Methods 0.000 claims abstract description 93
- 239000002253 acid Substances 0.000 claims abstract description 75
- 239000010453 quartz Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 37
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 33
- 239000011707 mineral Substances 0.000 claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000010791 quenching Methods 0.000 claims abstract description 20
- 230000000171 quenching effect Effects 0.000 claims abstract description 20
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000011282 treatment Methods 0.000 claims abstract description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 229910021642 ultra pure water Inorganic materials 0.000 description 12
- 239000012498 ultrapure water Substances 0.000 description 12
- -1 polytetrafluoroethylene Polymers 0.000 description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 7
- 230000007547 defect Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000010433 feldspar Substances 0.000 description 3
- 239000010438 granite Substances 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000010445 mica Substances 0.000 description 3
- 229910052618 mica group Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011044 quartzite Substances 0.000 description 3
- 210000003462 vein Anatomy 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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Abstract
The invention relates to and provides a preparation method of 4N-grade high-purity quartz sand, which comprises the following steps: (1) Calcining a quartz raw material at high temperature, performing water quenching treatment, washing and drying after water quenching to obtain an intermediate mineral; (2) Carrying out ultrasonic acid leaching on the intermediate mineral obtained in the step (1); (3) And (3) carrying out high-temperature leaching on the acid system subjected to ultrasonic acid leaching, and washing and drying a product subjected to high-temperature leaching to obtain a 4N-grade high-purity quartz sand product. The method can obviously reduce the content of impurity elements in the quartz, obtain the quartz sand product with higher purity, has low energy consumption, simple process and easy operation in the preparation process, and solves the technical problems of complex process and high energy consumption of the high-purity quartz sand in the prior art.
Description
Technical Field
The invention belongs to the technical field of processing and purifying of nonmetallic minerals, and particularly relates to a method for preparing 4N-grade high-purity quartz sand.
Background
At present, there are various methods for purifying quartz sand, wherein patent CN111874914A adopts a purification process of "grinding-flotation-roasting water quenching-hot-pressing acid leaching" and the purification process is grinding-flotation-roasting water quenching-hot-pressing acid leachingThe 4N-grade high-purity quartz sand is prepared by the process, the adopted leaching agent is sulfuric acid and hydrofluoric acid mixed acid, hot-pressing acid leaching is adopted for leaching, the leaching temperature is high (220 ℃), the pressure is high during leaching, the leaching process is not easy to operate and control, the energy consumption is high, sulfate radicals remained in the leaching process are not easy to wash and remove in the subsequent process, and the method has a limited effect on removing impurities such as iron, potassium and the like. There are also documents (study on the process of preparing high-purity quartz powder by purifying pegmatite tailings, university of Chongqing science, vol.32, 9 th period, and 9 months in 2018) that a purification process of 'grinding ore, strong magnetic separation, acid leaching, calcining water quenching, secondary acid leaching' is adopted, calcination water quenching is carried out after acid leaching, and secondary acid leaching is introduced, so that the process flow is complex. There is also a document (research on realization of quartz sand high purification by flotation-acid leaching, non-metal ore, no. 36, no. 5, 9 months in 2013) that quartz sand is purified by a simple process of "flotation-acid leaching" to obtain a high-purity quartz sand product of 99.993%, but the quartz sand product of 99.97% purity which has been subjected to beneficiation and calcination is adopted, secondary flotation is performed on the beneficiated ore, the process is more complicated, only iron and aluminum elements are partially removed in the leaching process, and potassium and sodium elements are not effectively removed. Therefore, the method has the advantages of simple process flow, low leaching temperature, low energy consumption and capability of preparing SiO under normal pressure 2 The production method of the high-purity quartz sand with the purity of more than or equal to 99.99 percent has important economic benefit and practical significance.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a preparation method of 4N-grade high-purity quartz sand, which can obviously reduce the content of impurity elements in quartz to obtain a quartz sand product with higher purity, has low energy consumption, simple process and easy operation in the preparation process, and solves the technical problems of complex process and high energy consumption of the high-purity quartz sand in the prior art.
The invention provides a preparation method of 4N-grade high-purity quartz sand, which comprises the following steps:
(1) Calcining a quartz raw material at high temperature, performing water quenching treatment, washing and drying after water quenching to obtain an intermediate mineral;
(2) Carrying out ultrasonic acid leaching on the intermediate mineral obtained in the step (1);
(3) And (3) carrying out high-temperature leaching on the acid system subjected to ultrasonic acid leaching, and washing and drying a product subjected to high-temperature leaching to obtain a 4N-grade high-purity quartz sand product.
Further, in the step (3), the leaching pressure of high-temperature leaching is normal pressure, the leaching temperature is 30-95 ℃, and the leaching time is 2-8h.
Further, in the step (1), the high-temperature calcination temperature is 850-950 ℃, and the calcination time is 2-4h.
Further, in the step (2), the mixed acid is adopted for acid leaching, the mixed acid is a combination of hydrofluoric acid and at least one of hydrochloric acid and nitric acid, the concentration of the hydrochloric acid in the mixed acid is 0.5-3mol/L, the concentration of the nitric acid is 0-1mol/L, and the concentration of the hydrofluoric acid is 0.1-1.5mol/L.
Further, in the step (2), the liquid-solid ratio of the mixed acid to the intermediate mineral is 1-5.
Further, in the step (2), ultrasonic acid leaching is carried out at room temperature, and the leaching time is 0.25-2h.
Further, the ultrasonic power is 200-1500W.
Further, siO in the 4N-grade high-purity quartz sand 2 The content of the compound is more than or equal to 99.99wt%, and the granularity is 50-180 meshes.
Further, in the step (1), the quartz raw material is SiO 2 Quartz mineral with content not less than 99.5%. The quartz raw material comprises vein quartz, quartzite, quartz sandstone, granite quartz, etc.
Compared with the prior art, the invention has the following beneficial effects:
(1) The crystal form of quartz is changed under the high-temperature calcination state, so that the volume is increased, the original defect degree in the quartz crystal becomes more serious, meanwhile, impurities such as mica, feldspar and the like mixed in the quartz raw material are beneficial to acid leaching removal through high-temperature mineral phase reconstruction, meanwhile, through instant water quenching treatment, the crystal volume suddenly and rapidly decreases, the internal force of the crystal defect is increased, further, the crystal is promoted to break at the defect, and the impurities in inclusions and cracks in the original quartz are exposed to the particle surface, so that the acid leaching removal is easy.
(2) After calcining and water quenching, the quartz raw material is subjected to normal-temperature normal-pressure ultrasonic assisted acid leaching under a mixed system of hydrochloric acid, nitric acid and hydrofluoric acid, so that acid can be effectively and fully contacted with quartz, the next leaching is facilitated, the leaching efficiency can be greatly improved, the acid consumption and the leaching time can be effectively reduced, and meanwhile, the acid consumption can be remarkably reduced by means of ultrasonic waves, and the contents of iron, calcium and the like in quartz concentrate can be effectively reduced.
(3) And (3) leaching the product subjected to ultrasonic acid leaching at high temperature and normal pressure at the leaching temperature of 30-95 ℃, at low leaching temperature and low energy consumption, simply and efficiently removing associated minerals such as mica, feldspar and the like in quartz, and effectively breaking metal M-O bonds to remove metal impurities among crystal lattices.
(4) Compared with other normal-temperature normal-pressure leaching methods, the method provided by the invention has the advantages of small leaching acid dosage, short leaching time, simple process, easiness in operation and low energy consumption. Compared with other leaching methods, the method has the advantage that the removal rate of metal elements such as iron, sodium, potassium and the like is higher.
Drawings
FIG. 1 is a process flow diagram of a method for preparing high-purity N-grade silica sand according to example 4.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, in an embodiment of the present invention, a method for preparing 4N-grade high-purity quartz sand includes the following steps:
(1) Calcining a quartz raw material at high temperature, performing water quenching treatment, washing and drying after water quenching to obtain intermediate minerals;
(2) Carrying out ultrasonic acid leaching on the intermediate mineral obtained in the step (1);
(3) And (3) carrying out high-temperature leaching on the acid system subjected to ultrasonic acid leaching, and washing and drying a product subjected to high-temperature leaching to obtain a 4N-grade high-purity quartz sand product.
Wherein in the step 1, the quartz raw material is SiO 2 The quartz minerals with content of 99.5% or more include vein quartz, quartzite, quartz sandstone, granite quartz, etc.
In one embodiment, the calcination temperature is 850-950 ℃, and the calcination time is 2-4h. The advantage of selecting the temperature range is that the quartz can be promoted to generate crystal form transformation, the volume is increased, the original defect degree in the quartz crystal becomes more serious, and meanwhile, mica, feldspar and other impurities mixed in the quartz raw material are beneficial to acid leaching removal through high-temperature ore phase reconstruction. Further, the calcination temperature may be 850 ℃, 875 ℃, 900 ℃, 925 ℃ and 950 ℃. Further, the calcination time may be 2h, 3h, or 4h.
In the step 1, the washing and drying are ultra-pure washing with the conductivity of more than 18 MOmega, and the drying is ordinary pollution-free drying. The washing mode, time and drying time can be set according to requirements, namely, the washing is ensured to be clean, and the washing is fully dried without pollution.
In the step 2, the acid leaching adopts mixed acid, the mixed acid is a mixed system of two or more than two types of monovalent acid, and the monovalent acid is easy to remove in the subsequent washing process.
In one embodiment, the mixed acid is a combination of at least one of hydrochloric acid and nitric acid and hydrofluoric acid. In the mixed acid, the concentration of hydrochloric acid is 0.5-3mol/L, the concentration of nitric acid is 0-1mol/L, and the concentration of hydrofluoric acid is 0.1-1.5mol/L. Further, the concentration of the hydrochloric acid may be 0.5mol/L, 1mol/L, 1.5mol/L, or the like. Further, the concentration of the nitric acid may be 0mol/L, 0.5mol/L, 1mol/L, or the like. Further, the concentration of the hydrofluoric acid may be 0.1mol/L, 0.5mol/L, 1mol/L, or the like.
In one embodiment, the liquid-solid ratio of the mixed acid to the intermediate mineral is 1-5. Further, the liquid-solid ratio can be 1, 2.
In the step 2, the ultrasonic acid leaching is leaching under an ultrasonic environment, and an ultrasonic field is generated by an ultrasonic generator. The power of the ultrasonic wave generating device can be selected from 200-1500W, and can be selected by one skilled in the art according to the needs.
In one embodiment, the ultrasonic leaching temperature is room temperature, and the leaching time is 0.25-2h. Further, the leaching time may be 0.25h,0.5h,0.75h,1h, etc.
In the step 2, carrying out ultrasonic acid leaching on the intermediate minerals: firstly, mixing mixed acid and intermediate minerals, and then leaching under the assistance of ultrasonic waves; the mixing mode is to add the mixed acid into the polytetrafluoroethylene container and then add the intermediate mineral, or to add the quartz into the polytetrafluoroethylene container and then add the mixed acid, the reaction container is a corrosion-resistant container, the specific mixing mode is set according to the requirement, and the invention is not limited further.
In the step 3, after the ultrasonic acid leaching is finished, the acid reaction system is transferred to high temperature for high temperature normal pressure leaching without pressurization, and the high temperature leaching is relative to the normal temperature in the ultrasonic acid leaching stage.
In one embodiment, the high temperature is 30-95 ℃ and the leaching time is 2-8h. Further, the leaching temperature can be 30 ℃, 40 ℃, 50 ℃, 60 ℃ and the like. Further, the leaching time can be 2h, 3h, 4h, 5h and the like.
In step 3, stirring and enhanced leaching may be added during the leaching process, and the specific stirring manner and heating manner may be selected by those skilled in the art as required, and the present invention is not further limited.
In step 3, siO in the prepared 4N-grade high-purity quartz sand 2 The content is more than or equal to 99.99wt%, and the granularity is 50-180 meshes.
In order to make the objects and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The quartz material used in the examples of the present invention was SiO 2 The quartz minerals with content of 99.5% or more include vein quartz, quartzite, quartz sandstone, granite quartz, etc. The contents of the respective impurity elements of a certain quartz raw material are shown in Table 1.
TABLE 1 impurity element content of Quartz raw Material
Example 1
(1) Placing a certain quartz raw material in a crucible, calcining for 4h at 875 ℃, taking out, directly pouring into ultrapure water for water quenching treatment, washing with ultrapure water after water quenching, and drying to obtain an intermediate mineral;
(2) Adding the intermediate mineral into a polytetrafluoroethylene reactor filled with mixed acid, wherein the mixed acid is mixed acid of hydrochloric acid and hydrofluoric acid, the concentration of the hydrochloric acid is 2mol/L, the concentration of the hydrofluoric acid is 1mol/L, the liquid-solid ratio of the mixed acid to the intermediate mineral is 3;
(3) And pouring the solid-liquid mixture subjected to ultrasonic-assisted leaching into a thermal reaction kettle with a polytetrafluoroethylene lining for heating leaching reaction at the leaching temperature of 95 ℃ for 3 hours. And after the leaching reaction is finished, carrying out solid-liquid separation, washing the quartz sand solid by adopting ultrapure water until no chloride ion exists, and drying to prepare a 4N-grade high-purity quartz sand product.
Example 2
(1) Placing a certain quartz raw material in a crucible, calcining for 2 hours at 950 ℃, taking out, directly pouring the quartz raw material into ultrapure water for water quenching treatment, washing with ultrapure water after water quenching, and drying to obtain intermediate minerals;
(2) Adding the intermediate mineral into a polytetrafluoroethylene reactor filled with mixed acid, wherein the mixed acid is mixed acid of hydrochloric acid, nitric acid and hydrofluoric acid, the concentration of the hydrochloric acid is 2.5mol/L, the concentration of the nitric acid is 0.5mol, the concentration of the hydrofluoric acid is 1mol/L, the liquid-solid ratio of the mixed acid to the intermediate mineral is 4;
(3) And pouring the solid-liquid mixture subjected to ultrasonic-assisted leaching into a thermal reaction kettle with a polytetrafluoroethylene lining for heating leaching reaction at the leaching temperature of 85 ℃ for 5 hours. And after the leaching reaction is finished, carrying out solid-liquid separation, washing the quartz sand solid by adopting ultrapure water until no chloride ion exists, and drying to prepare a 4N-grade high-purity quartz sand product.
Example 3
(1) Placing a certain quartz raw material in a crucible, calcining for 3h at 900 ℃, taking out, directly pouring into ultrapure water for water quenching treatment, washing with ultrapure water after water quenching, and drying to obtain an intermediate mineral;
(2) Adding the intermediate mineral into a polytetrafluoroethylene reactor filled with mixed acid, wherein the mixed acid is mixed acid of hydrochloric acid and hydrofluoric acid, the concentration of the hydrochloric acid is 3mol/L, the concentration of the hydrofluoric acid is 0.5mol/L, the liquid-solid ratio of the mixed acid to the intermediate mineral is 5;
(3) And pouring the solid-liquid mixture subjected to ultrasonic-assisted leaching into a thermal reaction kettle with a polytetrafluoroethylene lining for heating leaching reaction at the leaching temperature of 80 ℃ for 6 hours. And after the leaching reaction is finished, carrying out solid-liquid separation, washing the quartz sand solid by adopting ultrapure water until no chloride ion exists, and drying to prepare a 4N-grade high-purity quartz sand product.
Example 4
(1) Placing a certain quartz raw material in a crucible, calcining at 925 ℃ for 4h, taking out, directly pouring the quartz raw material into ultrapure water for water quenching treatment, washing with ultrapure water after water quenching, and drying to obtain intermediate minerals;
(2) Adding the intermediate mineral into a polytetrafluoroethylene reactor filled with mixed acid, wherein the mixed acid is mixed acid of hydrochloric acid, nitric acid and hydrofluoric acid, the concentration of the hydrochloric acid is 1.5mol/L, the concentration of the nitric acid is 1mol/L, the concentration of the hydrofluoric acid is 1.5mol/L, the liquid-solid ratio of the mixed acid to the intermediate mineral is 2;
(3) And pouring the solid-liquid mixture subjected to ultrasonic-assisted leaching into a thermal reaction kettle with a polytetrafluoroethylene lining for heating leaching reaction at the leaching temperature of 90 ℃ for 4 hours. And after the leaching reaction is finished, carrying out solid-liquid separation, washing the quartz sand solid by adopting ultrapure water until no chloride ion exists, and then drying to prepare a 4N-grade high-purity quartz sand product.
The results of ICP-MS testing of the 4N grade high purity silica sand products of examples 1-4 are shown in Table 2.
TABLE 2 4N grade high purity Quartz Sand products with each impurity element content (mug/g)
As can be seen from Table 2, siO of the 4N-grade high-purity quartz sand prepared in examples 1 to 4 of the present invention 2 The content can reach at least more than 99.992wt%, the prepared high-purity quartz sand can meet the requirement of the industry on the high-purity quartz sand, and the process flow in the preparation process is simple and the energy consumption is low.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (9)
1. A preparation method of 4N-grade high-purity quartz sand is characterized by comprising the following steps:
(1) Calcining a quartz raw material at high temperature, performing water quenching treatment, washing and drying after water quenching to obtain intermediate minerals;
(2) Carrying out ultrasonic acid leaching on the intermediate mineral obtained in the step (1);
(3) And (3) carrying out high-temperature leaching on the acid system subjected to ultrasonic acid leaching, and washing and drying a product subjected to high-temperature leaching to obtain a 4N-grade high-purity quartz sand product.
2. The method for preparing high-purity quartz sand of 4N grade according to claim 1, wherein in the step (3), the leaching pressure of the high-temperature leaching is normal pressure, the leaching temperature is 30-95 ℃, and the leaching time is 2-8h.
3. The method for preparing 4N-grade high-purity quartz sand according to claim 1, wherein in the step (1), the high-temperature calcination temperature is 850-950 ℃ and the calcination time is 2-4h.
4. The method for preparing high purity quartz sand of 4N grade according to claim 1, wherein in the step (2), the acid is dipped with mixed acid, the mixed acid is a combination of hydrofluoric acid and at least one of hydrochloric acid and nitric acid, the concentration of hydrochloric acid in the mixed acid is 0.5-3mol/L, the concentration of nitric acid is 0-1mol/L, and the concentration of hydrofluoric acid is 0.1-1.5mol/L.
5. The method for preparing 4N-grade high-purity quartz sand according to claim 4, wherein in the step (2), the liquid-solid ratio of the mixed acid to the intermediate mineral is 1-5.
6. The method for preparing high purity quartz sand of 4N grade according to claim 1, wherein in the step (2), the ultrasonic acid leaching is performed at room temperature, and the leaching time is 0.25-2h.
7. The method for preparing high-purity quartz sand of 4N grade according to claim 6, wherein the ultrasonic power is 200-1500W.
8. The method for preparing 4N and high-purity quartz sand according to claim 1, wherein SiO in the 4N grade high-purity quartz sand is 2 The content of (A) is more than or equal to 99.99wt%.
9. The method for preparing 4N-grade high-purity quartz sand according to claim 1, wherein in the step (1), the quartz material is SiO 2 Quartz mineral with content not less than 99.5%.
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