Quartz purification method and quartz purification system

Abstract

The application provides an improved quartz purification method, which realizes ultrahigh-purity quartz by adopting a multi-step process assisted by a probe type ultrasonic wave.The purification process comprises the following stages: mechanical grinding, magnetic separation, acid immersion, ultrasonic oscillation assistance and drying, etc.The acid immersion process uses hydrochloric acid, nitric acid, phosphoric acid, hydrogen peroxide and sulfuric acid in any order to selectively remove impurities.Probe type ultrasonic oscillation is used in each acid immersion process to accelerate the reaction kinetics, improve the impurity dissolution efficiency and reduce residual pollutants.The multi-stage process can effectively remove metal and non-metal impurities while maintaining the structural integrity of the quartz.The synergistic effect of ultrasonic oscillation and precise acid treatment not only improves the purification efficiency, but also has high reproducibility and scale characteristics, meeting the high-end application requirements for ultrapure quartz.The quartz purification method provided by the application can improve the purity of quartz to four 9s without using hydrofluoric acid.

Description

Technical Field

[0001] This invention relates to a quartz purification method and a quartz purification system. Background Technology

[0002] In the field of quartz purification, mixed acids are commonly used to treat quartz ore. However, the various acids in a mixed acid solution can easily interfere with each other, making it impossible to completely remove certain impurities and thus affecting the final purity of the quartz. Furthermore, the mixed acid may react with impurities during the reaction to form byproducts that are difficult to remove. These byproducts tend to remain on the surface or inside the quartz, leading to a decrease in purity and failing to achieve the desired purification effect.

[0003] On the other hand, hydrofluoric acid is also commonly used to treat quartz ore in the field of quartz purification. However, although hydrofluoric acid is effective in removing some impurities, its lack of oxidizing properties makes it less effective at removing certain types of impurities, which may leave these impurities in the quartz, preventing the achievement of higher purity standards. Furthermore, hydrofluoric acid is highly toxic; its volatile and corrosive gases pose a significant threat to operators and the environment, increasing the risks and safety management difficulties of the operation process. Its strong etching effect can also damage the surface structure of quartz, further affecting its purity and material stability. Therefore, how to provide a method for obtaining high-purity quartz without using hydrofluoric acid is a topic of active research in the field. Summary of the Invention

[0004] According to one or more embodiments of the present invention, a quartz purification method includes sequentially performing a crushing process, a grinding process, a magnetic separation process, an acid leaching process, a shaking process, and a drying process on quartz, wherein the acid leaching process includes immersing quartz in five acids in any order, the five acids being hydrochloric acid, nitric acid, phosphoric acid, hydrogen peroxide, and sulfuric acid, and each of the five acids being subjected to ultrasonic vibration force.

[0005] In one or more embodiments of the present invention, the first and last acids in the quartz soaking sequence are each selected from any one of the group consisting of hydrochloric acid, nitric acid and sulfuric acid.

[0006] In one or more embodiments of the present invention, the quartz is soaked in the following order: hydrochloric acid, nitric acid, phosphoric acid, hydrogen peroxide, and sulfuric acid.

[0007] In one or more embodiments of the present invention, the molar concentration of each of the five acids is 4M to 6M.

[0008] In one or more embodiments of the present invention, the initial temperature of each of the five acids is 25°C to 35°C.

[0009] In one or more embodiments of the present invention, in the acid leaching process, an ultrasonic probe is used to apply ultrasonic oscillation force to five acids, and the frequency of the ultrasonic oscillation force is 20 kHz to 120 kHz.

[0010] In one or more embodiments of the present invention, the quartz is immersed in each of the five acids for 30 to 60 minutes, and the ultrasonic oscillation force is stopped 10 to 20 minutes before the end of the acid immersion process.

[0011] According to one or more embodiments of the present invention, a quartz purification system includes a crushing device, a grinding device, a magnetic separation device, five ultrasonic acid leaching devices, a shaking device, a drying device, and a conveying device. The five ultrasonic acid leaching devices include a hydrochloric acid tank, a nitric acid tank, a phosphoric acid tank, a hydrogen peroxide tank, and a sulfuric acid tank. The conveying device passes through the crushing device, the grinding device, the magnetic separation device, the five ultrasonic acid leaching devices, the shaking device, and the drying device in sequence.

[0012] In one or more embodiments of the present invention, the conveying device passes through a hydrochloric acid tank, a nitric acid tank, a phosphoric acid tank, a hydrogen peroxide tank, and a sulfuric acid tank in sequence.

[0013] In one or more embodiments of the present invention, each of the five ultrasonic acid leaching devices further includes an ultrasonic probe, and the ultrasonic probe is disposed in each of the hydrochloric acid tank, nitric acid tank, phosphoric acid tank, hydrogen peroxide tank and sulfuric acid tank.

[0014] According to the above embodiments of the present invention, the quartz purification method of the present invention can improve the purity of quartz to four nines (99.9 ... Attached Figure Description

[0015] To make the above and other objects, features, advantages and embodiments of the present invention more apparent and understandable, the accompanying drawings are described below:

[0016] Figure 1 This is a schematic flowchart of a quartz purification method according to some embodiments of the present invention;

[0017] Figure 2 A scanning electron microscope (SEM) image of purified quartz according to some embodiments of the present invention; and

[0018] Figure 3 This is a schematic diagram of the configuration of a quartz purification system according to some embodiments of the present invention.

[0019] Figure label:

[0020] S10~S60: Steps

[0021] 100: Quartz Purification System

[0022] 110: Crushing device

[0023] 120: Grinding device

[0024] 130: Ultrasonic acid leaching device

[0025] 130a: Hydrochloric acid tank

[0026] 130b: Nitric acid tank

[0027] 130c: Phosphate tank

[0028] 130d:Hydrogen oxygen tank

[0029] 130e: Sulfuric acid tank

[0030] 140: Oscillating device

[0031] 150: Drying device

[0032] 160: Conveying device

[0033] 170: Magnetic separation device

[0034] P: Ultrasonic probe

[0035] C: Controller

[0036] AR: Arrow Detailed Implementation

[0037] The following describes several embodiments of the present invention with reference to the accompanying drawings. For clarity, many practical details will be described in the following description. However, it should be understood that these practical details are not intended to limit the invention. That is, in some embodiments of the invention, these practical details are not essential and therefore are not intended to limit the invention. Furthermore, for the sake of simplicity, some known and conventional structures and components will be shown in the drawings in a simple schematic manner. In addition, for the reader's convenience, the dimensions of the components in the drawings are not drawn to scale.

[0038] It should be understood that although the terms "first," "second," and "third," etc., may be used herein to describe various components, parts, regions, layers, and / or portions, these components, parts, regions, and / or portions should not be limited by these terms. These terms are used only to distinguish one component, part, region, layer, or portion from another component, part, region, layer, or portion. Therefore, "first component," "part," "region," "layer," or "part" as used below may also be referred to as a second component, part, region, layer, or portion without departing from the teachings of this document.

[0039] This invention provides a quartz purification method that can improve the purity of quartz to Four Nines Purity without using hydrofluoric acid (HF). This achieves high-purity quartz while reducing operator safety risks, minimizing environmental pollution, extending equipment lifespan, and lowering purification costs. Furthermore, this invention provides a quartz purification system to implement the quartz purification method.

[0040] Please see Figure 1 This is a flowchart of a quartz purification method according to some embodiments of the present invention. The quartz purification method includes steps S10 to S60. In step S10, the quartz is pulverized (process). In step S20, the pulverized quartz is ground (process). In step S30, the ground quartz is magnetically separated (process). In step S40, the magnetically separated quartz is acid-leached (process), including placing the magnetically separated quartz in five acids (acid solutions) in any order, wherein the five acid solutions are hydrochloric acid solution, nitric acid solution, phosphoric acid solution, hydrogen peroxide solution, and sulfuric acid solution, and each of the five acid solutions is subjected to ultrasonic vibration. In step S50, the acid-leached quartz is agitated (process). In step S60, the agitated quartz is dried (process). In the following description, the above steps will be described sequentially.

[0041] First, in step S10, the quartz is crushed. In some embodiments, single-step crushing can be performed, directly crushing large pieces of quartz ore to a suitable grinding particle size (e.g., 0.5 mm to 15 mm). Single-step crushing simplifies the process and improves efficiency, and is suitable for cases where the original quartz ore is brittle. In other embodiments, multi-step crushing can be performed, progressively crushing large pieces of quartz ore to a suitable grinding particle size. For example, multi-step crushing may include a coarse crushing step, an intermediate crushing step, and a fine crushing step, wherein the coarse crushing step can crush the quartz to a particle size of 10 mm to 15 mm, the intermediate crushing step can crush the quartz to a particle size of 5 mm to 9 mm, and the fine crushing step can crush the quartz to a particle size of 0.5 mm to 3 mm. Multi-step crushing can effectively reduce equipment wear and energy waste caused by processing too much material at once or by a large particle size range of the material. In addition, multi-step operation can help to accurately control particle size distribution, reduce the risk of over-grinding of materials, thereby improving the quality of the final quartz and production efficiency.

[0042] Next, in step S20, the pulverized quartz undergoes a grinding step. Specifically, grinding after pulverizing the quartz further refines the particles and improves particle size uniformity, thereby enhancing mixability and the reaction rate of the quartz in the subsequent acid leaching step. During grinding, the surface area of ​​the particles increases, which helps remove impurities from the quartz in the subsequent acid leaching step. In some embodiments, the ground quartz can be passed through a 100-mesh to 200-mesh sieve (e.g., 120-mesh, 140-mesh, 160-mesh, and 180-mesh). This results in fine and uniform particles and an increased surface area, improving magnetic separation efficiency in the subsequent magnetic separation step and promoting contact between the quartz and acid in the subsequent acid leaching step, thereby increasing the purity of the quartz.

[0043] Subsequently, in step S30, the ground quartz undergoes a magnetic separation step. Specifically, a strong external magnetic field can be used to adsorb iron-based substances from the quartz. In some embodiments, a magnetic separator can be used for the magnetic separation step, and the strength of the magnetic field used can be from 0.1 texela to 1.5 texela (e.g., 0.2 texela, 0.4 texela, 0.6 texela, 0.8 texela, 1.0 texela, 1.2 texela, 1.4 texela). The specific strength depends on the content and nature of iron impurities in the quartz ore; generally, a higher iron content requires a higher magnetic field strength. In some embodiments, the preliminary cleaning and magnetic separation steps can be carried out at room temperature to increase the magnetization of the magnetic substances (impurities). Overall, after completing the magnetic separation step, the content of iron-based substances (iron impurities) in the quartz can be significantly reduced. In some embodiments, before performing the magnetic separation step on the quartz, a preliminary cleaning step (process) can be performed with pure water on the quartz.

[0044] Subsequently, in step S40, the magnetically separated quartz undergoes an acid leaching step. The acid leaching step primarily utilizes the chemical properties of acid to remove impurities and impurities from the quartz material. During acid leaching, the magnetically separated quartz is immersed in an acid solution (i.e., an aqueous solution containing acid). The impurities and impurities react with the acid in the solution to form soluble compounds, thereby being removed. Furthermore, the acid leaching step also helps improve the surface smoothness of the quartz and modify the particle morphology, further enhancing the quality of the purified quartz.

[0045] In this invention, by immersing magnetically separated quartz in a single acid solution while simultaneously applying ultrasonic vibration to each acid solution, the purity of quartz can be increased to four nines (99.99%) without using highly toxic hydrofluoric acid. Specifically, this invention uses five acid solutions—hydrochloric acid, nitric acid, phosphoric acid, hydrogen peroxide, and sulfuric acid—for the acid leaching step of the magnetically separated quartz. The magnetically separated quartz is placed in these five acid solutions in any order, ensuring that the quartz is exposed to only one acid solution at a time. For example, the quartz can be placed in the following order: hydrochloric acid, nitric acid, phosphoric acid, hydrogen peroxide, and sulfuric acid. Alternatively, it can be placed in the following order: sulfuric acid, nitric acid, phosphoric acid, hydrogen peroxide, and hydrochloric acid. Compared to directly immersing the quartz in a mixed acid solution, this invention, by immersing the quartz in only one acid solution at a time, has many advantages, listed below.

[0046] [Control Reactivity]

[0047] Soaking in a single acid allows for more precise control of reactivity. Specifically, since each acid has a different dissolution rate for different impurities in quartz, selecting the appropriate single acid not only removes specific impurities and adjusts the reaction rate as needed, but also avoids uneven reactions and optimizes soaking time and concentration, thereby achieving better cleaning or impurity removal results.

[0048] [Avoid adverse reactions]

[0049] Soaking in a single acid can avoid adverse reactions. Specifically, chemical reactions between different acids can lead to precipitation, gas release, or other side reactions, resulting in the formation of undesirable products and affecting the pickling effect. By using only a single acid at a time, the probability of these potential adverse reactions can be reduced.

[0050] [Increase purity]

[0051] Soaking in a single acid can improve the final purity of the quartz. Specifically, each acid has a specific solubility for different types of impurities, and using a single acid allows for targeted removal of the desired impurities, thus reducing the risk of secondary contamination, which is especially important in applications requiring high purity. Furthermore, mixed acids can affect the crystal structure of quartz, leading to changes in the material's physical and chemical properties, while a single acid does not affect the chemical structure of quartz.

[0052] [Simplified process]

[0053] Single-acid immersion simplifies the process. Specifically, using mixed acids requires precise calculation of the proportions of each acid to avoid uneven mixing or over-reaction, while using a single acid only requires controlling its concentration and dosage. This makes immersion conditions easier to standardize and adjust, further reducing process variables and the complexity of parameter settings. Furthermore, single-acid systems are simpler to manage and monitor, eliminating the need for compatibility with multi-acid systems and contributing to improved overall process reliability and production efficiency.

[0054] [Improve security]

[0055] Soaking in a single acid can improve operational safety. Specifically, mixed acids may release toxic gases or trigger thermal reactions during operation, increasing the danger of the experiment. Using a single acid can reduce this risk, making the experiment safer.

[0056] [Improve repeatability]

[0057] Single-acid immersion improves process repeatability. Specifically, in mixed-acid systems, interactions between different acids can cause fluctuations in multiple variables, such as reaction rate, temperature, and acidity, affecting the results of each batch. A single acid, with its stable and highly controllable chemical properties, eliminates these variables, allowing for precise control of acid concentration, temperature, and reaction time in each treatment, ensuring consistent and stable results across batches. Furthermore, in single-acid systems, experimental parameters and operating conditions are easier to standardize, which is crucial for quality control in industrial production. This helps reduce quality fluctuations caused by impurities or material inhomogeneities, ultimately improving the predictability and reproducibility of process results.

[0058] Overall, as mentioned above, immersing quartz in only one acid solution at a time allows for better control of reactivity, avoids adverse reactions, improves quartz purity, simplifies the process, enhances operational safety, and improves process repeatability. On the other hand, immersing quartz in an acid solution subjected to ultrasonic oscillation (i.e., acid leaching combined with ultrasonic oscillation) effectively improves acid penetration, ultimately increasing quartz purity. Specifically, the cavitation effect generated by high-frequency ultrasonic oscillation causes the rapid generation and instantaneous disintegration of tiny bubbles in the acid solution, releasing intense energy that directly acts on the quartz surface. The micro-shock waves formed by this cavitation effect help break down the bonds of surface contaminants, gradually detaching particles from the quartz surface for highly efficient cleaning. In this process, physical removal and chemical acid leaching occur simultaneously, resulting in more uniform purification of the quartz surface and improved overall purity.

[0059] Under the influence of ultrasonic oscillation, microcracks appearing on the quartz surface further enhance purification efficiency. These microcracks allow acid solution to penetrate the inner structure of the quartz, removing hidden contaminants remaining below the surface. These microcracks effectively increase the active area on the quartz surface, allowing the acid to contact a wider area and achieving multi-layered contaminant removal. The opening of these microcracks exposes a new quartz surface layer to the acid solution, accelerating the efficiency of chemical etching and thus promoting a deeper purification process, which is crucial for achieving ultra-high purity quartz powder. For a detailed structural representation of the microcracks, please refer to [link to relevant documentation]. Figure 2 The image is a scanning electron microscope (SEM) image of purified quartz according to some embodiments of the present invention, in which microcracks in the quartz are visible at the location indicated by arrow AR.

[0060] Furthermore, the localized heating effect induced by ultrasonic oscillation also helps accelerate the acid leaching reaction. When the oscillation energy is transferred to the acid solution, the local temperature in the acid solution rises. Although this heating is localized and brief, it helps improve reaction kinetics. The high temperature increases the diffusion rate of active molecules in the acid solution, making the reaction between the acid and the quartz surface more efficient, further increasing the etching rate and shortening the processing time. The instantaneous high temperature generated by this localized heating is particularly suitable for removing tightly adhered impurities that are difficult to remove with conventional acid leaching, thereby improving the overall effect of acid leaching for impurity removal.

[0061] Furthermore, regarding surface roughness, the ultrasonic vibration force alters the surface structure of the quartz particles, creating fine, irregular textures on the outer layer. These textures increase the total surface area of ​​the quartz particles, allowing the acid solution to distribute more evenly across the quartz surface, enhancing the chemical contact between the acid and the quartz, and improving the efficiency of dissolving and removing contaminants. Compared to smooth surfaces, rough surfaces can more effectively trap acid molecules, making the quartz purification process more thorough and enabling a more comprehensive removal of tiny particles and impurities.

[0062] Overall, the application of ultrasonic oscillation in acid leaching simultaneously promotes both physical and chemical cleaning, providing multiple mechanisms for improving quartz purity. Physical processes such as cavitation, crack formation, and localized acid heating constitute a multi-layered removal process, enabling thorough purification in a relatively short time. Furthermore, increasing surface roughness optimizes the acid contact area, making the overall leaching process more efficient. These multifaceted synergistic effects allow quartz to achieve a purity of nine out of ten.

[0063] It should be noted that regardless of the order in which quartz is immersed in these five acid solutions, a purity of four nines can be achieved. Hydrochloric acid solution primarily removes metal oxide impurities from quartz, such as iron, copper, nickel, aluminum, and chromium, and can also partially remove alkaline earth metals such as calcium and magnesium. Nitric acid solution primarily removes reduced metal impurities from quartz, such as copper, manganese, tin, and lead, and can also effectively remove organic matter and some non-metallic impurities. Phosphoric acid solution is effective in removing elements such as titanium, aluminum, calcium, and potassium. Phosphoric acid can form stable phosphate compounds with these metals, thereby reducing their content in quartz. Phosphoric acid also has a certain effect on removing alkali metals such as lithium and sodium. Hydrogen peroxide solution primarily removes reduced metal impurities from quartz, such as manganese, chromium, lithium, and boron. Hydrogen peroxide can oxidize these metals to higher valence ions, which can then be removed in conjunction with other acids. Hydrogen peroxide is also very effective in removing organic matter and carbon residues from the surface of quartz. Sulfuric acid solution can mainly remove impurities such as iron, aluminum, calcium and magnesium from quartz. Sulfuric acid can form soluble sulfate compounds with these metals and can be used in combination with oxidizing agents to improve the removal efficiency of some difficult-to-remove metal impurities (such as aluminum and titanium). Sulfuric acid also has a certain ability to remove alkali metal impurities such as sodium and potassium.

[0064] In some embodiments, the order in which the quartz is immersed in the five acid solutions can be adjusted so that the acid solutions with relatively higher acidity are placed first and last to achieve better purification results. For example, the first and last acid solutions can each be selected from the group consisting of hydrochloric acid, nitric acid, and sulfuric acid solutions, and the first and last acid solutions are different acid solutions. In detail, placing the highly acidic acid solution first can remove most of the impurities in a short time, ensuring improved purity in subsequent processing. This is because the highly acidic acid solution can quickly dissociate and react with the metal to form easily soluble salts, thereby achieving a preliminary deep purification effect. Placing the highly acidic acid solution last can further remove residual trace metal impurities to ensure high purity of the quartz. This is because the highly acidic acid solution can attack residual and difficult-to-remove metals after the quartz has undergone multiple acid treatments, thereby further improving the purification effect. Overall, this operational sequence (soaking in strong acid → weak acid → strong acid) can form an effective purification loop, minimizing the content of residual impurities, thereby improving the purification efficiency and final purity of quartz.

[0065] In some embodiments, the two acid solutions with relatively lower acidity (phosphoric acid solution and hydrogen peroxide solution) among the five acid solutions can be arranged in the third and fourth order, or in the second and third order. In a preferred embodiment, quartz can be placed sequentially in hydrochloric acid solution, nitric acid solution, phosphoric acid solution, hydrogen peroxide solution, and sulfuric acid solution. It should be understood that although not all arrangements of the five acid solutions are listed herein, any arrangement of the five acid solutions falls within the scope of this invention and can achieve a purity of four nines for quartz.

[0066] In some embodiments, the molar concentration of each of the five acid solutions (i.e., the molar concentration of each of the five acids in water) can be from 4M to 6M (e.g., 4.5M, 5M, 5.5M), and the quartz can be immersed in each of the five acid solutions for 30 minutes to 60 minutes (e.g., 35 minutes, 40 minutes, 45 minutes, 50 minutes, 55 minutes). Immersing the quartz in an acid of appropriate concentration for an appropriate time can improve the purification effect and the final quality of the quartz. Specifically, the concentration of the acid solution determines the efficiency of impurity removal from the quartz surface; too high a concentration may cause corrosion of the quartz surface and damage its structure, while too low a concentration may not be able to effectively remove deep impurities. In addition, the immersion time can be coordinated with the acid concentration; too short a time may not achieve the desired impurity removal effect, while too long a time may lead to unnecessary material loss.

[0067] In some embodiments, the initial temperature of each of the five acid solutions can be, for example, room temperature (25°C to 35°C). As mentioned earlier, since the ultrasonic oscillation force can induce localized heating, high-temperature acid solutions are unnecessary, which helps improve operational safety. Furthermore, because the temperatures of the aforementioned acid solutions are relatively low, excessive corrosion of the quartz surface structure, increased material loss, or alteration of the quartz's microstructure can be avoided, thus preventing impacts on its physical properties and subsequent application stability. In short, by adjusting the temperature of the acid solutions, impurity removal can be accelerated while avoiding unnecessary damage to the quartz itself, achieving optimal purification results.

[0068] In some embodiments, during the acid leaching step, an ultrasonic probe is used to apply ultrasonic oscillation force to five solutions, wherein the frequency of the ultrasonic oscillation force is 20 kHz to 120 kHz, and the amplitude of the ultrasonic oscillation force is 10 micrometers to 70 micrometers. When the frequency and energy of the ultrasonic oscillation force fall within the above range, the proportion of cracks generated in the quartz by the ultrasonic probe is about 15% to 20%. Such a number of cracks does not affect the integrity of the quartz structure and can significantly increase the acid penetration effect, achieving a deep cleaning purpose. In some embodiments, the ultrasonic oscillation force can be stopped 10 to 20 minutes before the end of the acid leaching step. More specifically, considering the overall time of the acid leaching step (30 minutes to 60 minutes), the ultrasonic oscillation force accounts for 1 / 6 to 2 / 3 of the acid leaching step time (e.g., 1 / 2, 1 / 3, 1 / 4, 1 / 5), preferably 1 / 3 to 1 / 2. This effectively avoids potential damage to the quartz material from excessive oscillation. In detail, ultrasonic oscillation promotes surface etching and impurity removal in the early and middle stages of acid leaching. However, excessive oscillation over time can lead to excessive propagation of microcracks or overheating, causing structural damage. Therefore, stopping oscillation before the acid leaching process is complete allows the acid solution to undergo final reaction and cleaning under stable conditions, ensuring purification while protecting the structural integrity of the quartz. Furthermore, this approach reduces energy consumption and equipment wear, optimizing the overall processing cost and efficiency.

[0069] In some embodiments, after immersing the quartz in each acid solution, the quartz can be placed in pure water for a rinsing step to prevent residual acid solution from the previous solution from interacting with subsequent acid solutions and causing fluctuations in multiple variables such as reaction rate, temperature, and acidity, or leading to the formation of unexpected products. For example, in embodiments where the quartz is sequentially immersed in hydrochloric acid solution, nitric acid solution, phosphoric acid solution, hydrogen peroxide solution, and sulfuric acid solution, the quartz can be rinsed with pure water after immersion in hydrochloric acid solution, followed by immersion in nitric acid solution, and then rinsed with pure water. This immersion and rinsing process is repeated until all acid immersion steps are completed. In some embodiments, the water temperature for the rinsing step can be 25°C to 35°C, and the rinsing time can be 15 minutes to 30 minutes. Next, in step S50, the acid-immersed quartz is subjected to an agitation step. In some embodiments, the acid-immersed and rinsed quartz can be placed in pure water and subjected to ultrasonic agitation. Ultrasonic oscillation generates high-frequency pressure changes in a liquid, producing microbubbles. The localized high pressure and high-speed microfluidic motion generated when these bubbles burst effectively break the bond between impurities and the quartz surface, causing them to completely desorb. This physical action compensates for the shortcomings of chemical cleaning, achieving a more thorough cleaning effect and improving the purity and quality of the quartz. In some embodiments, the ultrasonic oscillation power can be from 250 watts to 350 watts (e.g., 260 watts, 270 watts, 280 watts, 290 watts, 300 watts, 310 watts, 320 watts, 330 watts, 340 watts). An appropriate oscillation power can be selected based on the properties of the quartz material, the type of impurities, and the cleaning objective, thereby achieving optimal cleaning results and improved purity while protecting the material structure.

[0070] Subsequently, in step S60, the agitated quartz undergoes a drying process to obtain high-purity quartz (purity of four nines). In some embodiments, the drying temperature can be between 80°C and 120°C, and the drying time can be between 2 and 6 hours. An appropriate drying temperature can effectively remove residual moisture and volatile substances from the quartz surface and pores, preventing them from re-adhering or agglomerating into new impurities during the drying process. If the drying temperature is too low, incomplete moisture evaporation may lead to surface contamination or crystallization defects; if the drying temperature is too high, it may cause thermal stress deformation of the quartz or generate microcracks, affecting the physical properties and purity of the material. Therefore, based on the characteristics of the quartz and the purification target, an appropriate drying temperature can be selected within the above temperature range to balance moisture removal and material stability, ensuring the high purity and structural integrity of the product. On the other hand, the drying time can be coordinated with the drying temperature.

[0071] Please see Figure 3This is a schematic diagram of the configuration of a quartz purification system 100 according to some embodiments of the present invention. The quartz purification system 100 includes a pulverizing device 110, a grinding device 120, a magnetic separation device 170, five ultrasonic acid leaching devices 130, a shaking device 140, a drying device 150, and a conveying device 160. The conveying device 160 sequentially passes through the pulverizing device 110, the grinding device 120, the magnetic separation device 170, each of the five ultrasonic acid leaching devices 130, the shaking device 140, and the drying device 150, and is configured to sequentially convey quartz into these devices. The ultrasonic acid leaching devices 130 provide ultrasonic vibration force, allowing the quartz to be subjected to ultrasonic vibration force during the acid leaching step. In addition, the five ultrasonic acid leaching devices include a hydrochloric acid tank 130a, a nitric acid tank 130b, a phosphoric acid tank 130c, a hydrogen peroxide tank 130d, and a sulfuric acid tank 130e. In some embodiments, each ultrasonic acid leaching device 130 may, for example, include an ultrasonic probe P, and may be positioned and immersed in each of the hydrochloric acid tank 130a, nitric acid tank 130b, phosphoric acid tank 130c, hydrogen peroxide tank 130d, and sulfuric acid tank 130e, wherein the five ultrasonic probes P can be operated independently by a separate controller C. Furthermore, in some embodiments, the pulverizing device 110, the grinding device 120, the magnetic separation device 170, the five ultrasonic acid leaching devices 130, the shaking device 140, the drying device 150, and the conveying device 160 may be arranged adjacent to each other. In some embodiments, the quartz purification system 100 may further include a preliminary cleaning device (not shown), positioned and connected between the grinding device 120 and the magnetic separation device 170.

[0072] In some embodiments, the quartz purification method described above can be achieved through... Figure 2The quartz purification system 100 is used to achieve this. Specifically, the quartz undergoes a crushing step in the crushing device 110, a grinding step in the grinding device 120, a magnetic separation step in the magnetic separation device 170, an acid leaching step in the ultrasonic acid leaching device 130 with ultrasonic vibration, a vibration step in the vibration device 140, and a drying step in the drying device 150. In some embodiments, the conveying device 160 can be an adjustable conveying pipeline, and the configuration path of the conveying pipeline can be adjusted according to the requirements of the acid leaching sequence. For example, the conveying device 160 can sequentially pass through a hydrochloric acid tank 130a, a nitric acid tank 130b, a phosphoric acid tank 130c, a hydrogen peroxide tank 130d, and a sulfuric acid tank 130e. In some embodiments, the oscillating device may be an ultrasonic oscillator of 250 to 350 watts (e.g., 260 watts, 270 watts, 280 watts, 290 watts, 300 watts, 310 watts, 320 watts, 330 watts, 340 watts). In some embodiments, the ground quartz may undergo a preliminary cleaning step in a preliminary cleaning device before the magnetic separation step.

[0073] In the following description, several embodiments will be listed to demonstrate the effectiveness of the invention. It should be understood that the invention should not be interpreted as limiting by the embodiments described below.

[0074] In this experiment, steps S10 to S60 described above were used to purify quartz. In the pulverization step, a single-step pulverization process was used to pulverize the quartz to a particle size of 0.5 mm to 15 mm. In the preliminary cleaning and magnetic separation steps, a magnetic separator was used to perform magnetic separation on the quartz at room temperature. In the grinding step, the ground quartz passed through a 100-200 mesh sieve. In the acid leaching step, the molar concentration of each of the five acid solutions was 5M, and the temperature of each acid solution was room temperature. The quartz was placed in each of the five acid solutions for 45 minutes, and the ultrasonic oscillation frequency was 20 kHz, with the ultrasonic oscillation stopping 10 minutes before the end of the acid leaching step. In the washing step (a total of 5 washes), the temperature of the pure water was room temperature, and the total washing time was 100 minutes (each wash lasting 20 minutes). In the shaking step, the quartz was ultrasonically shaken using a power of 300 watts. In the drying step, the drying temperature was 100°C, and the drying time was 120 minutes. The results of the quartz purification are recorded in Table 1.

[0075] Table 1

[0076]

[0077]

[0078] [Note 1]

[0079] Purity is calculated as follows: 1 - [(total impurities) / 1000000] × 100%.

[0080] [Note 2]

[0081] Acid leaching sequence:

[0082] Example 1: Hydrochloric acid → Nitric acid → Phosphoric acid → Hydrogen peroxide → Sulfuric acid

[0083] Example 2: Sulfuric acid → Nitric acid → Phosphoric acid → Hydrogen peroxide → Hydrochloric acid

[0084] Example 3: Phosphoric acid → Hydrochloric acid → Nitric acid → Hydrogen peroxide → Sulfuric acid

[0085] Example 4: Hydrogen peroxide → Nitric acid → Hydrochloric acid → Phosphoric acid → Sulfuric acid

[0086] It should be understood that the impurity content in Table 1 was obtained by inductively coupled plasma mass spectrometry (ICP-MS), and the results of Examples 1-3 were obtained by repeating the same experiment three times (each result was identical). As shown in Table 1, the quartz purification method of the present invention can indeed achieve a purity of four nines that is difficult to achieve, and does not use highly toxic hydrofluoric acid. Therefore, the present invention can obtain high-purity quartz while reducing operator safety risks, reducing environmental pollution, extending equipment life, and reducing purification costs.

[0087] Although the present invention has been described above with reference to embodiments, it is not intended to limit the present invention. Anyone skilled in the art can make various modifications and refinements without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention shall be determined by the appended claims.

Claims

1. A method for purifying quartz, characterized in that, include: The quartz is subjected to a series of processes including crushing, grinding, magnetic separation, acid leaching, vibration, and drying. The acid leaching process involves immersing the quartz in five acids in any order: hydrochloric acid, nitric acid, phosphoric acid, hydrogen peroxide, and sulfuric acid. Each of the five acids is subjected to ultrasonic vibration.

2. The quartz purification method as described in claim 1, characterized in that, The first and last acids in the immersion sequence of the quartz are each selected from any one of the groups consisting of hydrochloric acid, nitric acid, and sulfuric acid.

3. The quartz purification method as described in claim 1, characterized in that, The quartz was soaked in the following order: hydrochloric acid, nitric acid, phosphoric acid, hydrogen peroxide, and sulfuric acid.

4. The quartz purification method as described in claim 1, characterized in that, The molar concentrations of the five acids range from 4 M to 6 M.

5. The quartz purification method as described in claim 1, characterized in that, The initial temperature for each of the five acids is between 25°C and 35°C.

6. The quartz purification method according to claim 1, characterized in that, In this acid leaching process, an ultrasonic probe is used to apply ultrasonic oscillation force to the five acids, and the frequency of the ultrasonic oscillation force is 20 kHz to 120 kHz.

7. The quartz purification method according to claim 1, characterized in that, The quartz is immersed in each of the five acids for 30 to 60 minutes, and the ultrasonic vibration stops 10 to 20 minutes before the end of the acid immersion process.

8. A quartz purification system, characterized in that, include: The device includes a crushing device, a grinding device, a magnetic separation device, five ultrasonic acid leaching devices, a vibration device, a drying device, and a conveying device. The five ultrasonic acid leaching devices include a hydrochloric acid tank, a nitric acid tank, a phosphoric acid tank, a hydrogen peroxide tank, and a sulfuric acid tank. The conveying device passes through the crushing device, the grinding device, the magnetic separation device, the five ultrasonic acid leaching devices, the vibration device, and the drying device in sequence.

9. The quartz purification system as described in claim 8, characterized in that, The conveying device passes sequentially through the hydrochloric acid tank, the nitric acid tank, the phosphoric acid tank, the hydrogen peroxide tank, and the sulfuric acid tank.

10. The quartz purification system as described in claim 8, characterized in that, Each of the five ultrasonic acid leaching devices further includes an ultrasonic probe disposed in each of the hydrochloric acid tank, the nitric acid tank, the phosphoric acid tank, the hydrogen peroxide tank, and the sulfuric acid tank.

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