Mixed acid for impurity removal of high-purity quartz and impurity removal equipment and process using mixed acid

By using mixed acids with components such as water, oxalic acid, sulfamic acid, etc., combined with microwave and ultrasonic catalytic processes, replacing hydrofluoric acid, the hazards of hydrofluoric acid used in high-purity quartz purification are solved, and efficient and environmentally friendly impurity removal effects are achieved.

CN119683634APending Publication Date: 2025-03-25SHANGRAO ZHONGBIN TONGCHEN TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411861454.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-17
Publication Date
2025-03-25

AI Technical Summary

Technical Problem

In the existing high-purity quartz purification process, the use of hydrofluoric acid has personnel and environmental hazards, and its removal is difficult to replace, affecting the purity and environmental protection requirements of quartz.

Method used

Using a mixed acid, the ingredients include water, oxalic acid, sulfamic acid, penetrant, citric acid and/or hydrochloric acid, the process of synchronous catalysis and pressurization of microwave and ultrasonic waves, replace hydrofluoric acid to achieve impurity removal of high-purity quartz.

Benefits of technology

Effectively remove or replace hydrofluoric acid, ensure the quartz purification effect, reduce the harm of the factory and personnel, and the cost is the same as that of traditional mixed acids, the reaction products are easy to handle, and have good environmental protection.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a mixed acid for impurity removal of high-purity quartz and impurity removal equipment and process using the mixed acid, the mixed acid is used for an acid leaching impurity removal process, and the mixed acid comprises the following components: water, oxalic acid, sulfamic acid, a penetrant, citric acid and / or hydrochloric acid; hydrofluoric acid is effectively removed / replaced by a large amount of inorganic acid, the quartz purification effect can be well guaranteed, the acid cost is relatively mild, the harm coefficient to factories and personnel is greatly reduced, the cost is equal to that of traditional mixed acid, reaction products are easy to treat, and harm to the environment is avoided; the impurity removal equipment applying the acid is provided with the microwave catalysis device and the ultrasonic catalysis device which operate at the same time, effective impurity removal is achieved under the action of the mixed acid, and the equipment is durable and good in impurity removal effect and has the good energy efficiency ratio; according to the technology applying the mixed acid, the acid leaching impurity removal reaction of the mixed acid is effectively promoted in a mode of synchronously catalyzing and pressurizing through microwaves and ultrasonic waves, the impurity removal effect is guaranteed, and energy conservation and environmental protection are achieved.
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Description

Technical Field

[0001] The invention relates to a purification technology of high-purity quartz, in particular to a mixed acid used for removing impurities from high-purity quartz and an impurity removal device and process using the mixed acid. Background Art

[0002] Due to its unique molecular chain structure, lattice shape and lattice change law, high purity quartz has excellent chemical stability, extremely low volume expansion coefficient, extremely high temperature resistance, high insulation and withstand voltage, low and stable ultrasonic delay performance, mechanical properties higher than ordinary glass, ultraviolet spectrum performance, visible light and near infrared spectrum performance. In the preparation process of high purity quartz, the acid leaching and impurity removal process is particularly important. The mixed acid used in the process steps usually includes:

[0003] Hydrofluoric acid: Hydrofluoric acid has a significant dissolving effect on quartz, feldspar, mica, etc., and the more structural defects there are, the faster the dissolution rate. The crystal structure of aluminosilicates such as muscovite and feldspar must be combined with hydrofluoric acid to be effectively destroyed.

[0004] Sulfuric acid: Concentrated sulfuric acid has strong oxidizing properties. Hot concentrated sulfuric acid can react with most metals and convert most sulfide minerals into corresponding high-valent metal sulfates, which have a higher boiling point and a higher leaching temperature can be used under normal pressure.

[0005] Hydrochloric acid: Hydrochloric acid has good metal dissolving ability and good complexing properties for iron ions.

[0006] Nitric acid: Nitric acid has strong oxidizing properties and can effectively oxidize metal elements to form soluble salts. However, its leaching effect alone is not good. It is usually mixed with hydrochloric acid to prepare highly corrosive aqua regia for leaching.

[0007] Oxalic acid: Oxalic acid is an organic acid commonly used in acid leaching. It can form a relatively stable complex with the dissolved metal ions, thereby detaching them from the quartz surface.

[0008] In summary, in the acid leaching process of high-purity quartz, the components of the mixed acid generally include hydrofluoric acid, sulfuric acid, hydrochloric acid, nitric acid and oxalic acid, etc. The selection and ratio of these acids depends on the type of impurities to be removed and the required quartz purity. In the prior art, the above-mentioned mixed acid components are indispensable, and any reduction will directly lead to incomplete impurity removal, and the prepared finished quartz cannot reach the purity of high-purity quartz. In particular, hydrofluoric acid is particularly important, but hydrofluoric acid is also strictly controlled in industrial use. There are huge personnel and environmental hazards in the process of its use, and it is extremely difficult for by-products to meet environmental protection standards. Summary of the invention

[0009] The main technical problem to be solved by the present invention is to provide a mixed acid for removing impurities from high-purity quartz and an impurity removal device and process using the mixed acid, which can effectively remove / replace hydrofluoric acid and ensure the quartz purification effect.

[0010] In order to solve the above technical problems, the present invention provides a mixed acid for removing impurities from high-purity quartz, which is used in the acid leaching and impurity removal process, and its components include: water, oxalic acid, aminosulfonic acid, a penetrant, citric acid and / or hydrochloric acid.

[0011] Preferably, the penetrant is silicate or sodium oleate.

[0012] Preferably, the concentration of the mixed acid is 25-35%.

[0013] During implementation, the molar ratio of each component in the mixed acid is: 1-7 oxalic acid, 3-10 aminosulfonic acid, 1-5 penetrant, and 1-5 citric acid or hydrochloric acid.

[0014] Preferably, the molar ratio of the components of the mixed acid is: 1-2 oxalic acid, 1 sulfamic acid, 1-5 penetrant, and 1 citric acid or hydrochloric acid.

[0015] Preferably, the mixed acid also includes one or more of sulfuric acid, nitric acid, tartaric acid, fulvic acid, silicic acid, perchloric acid, and benzoic acid.

[0016] During implementation, the molar ratio of each component in the mixed acid is: oxalic acid 1-7, aminosulfonic acid 3-10, penetrant 1-5, citric acid or hydrochloric acid 1-5, and other acids 2-8.

[0017] A device for removing impurities from high-purity quartz uses the mixed acid for removing impurities from high-purity quartz as described above; the device includes an acid leaching chamber with a closed cover, on which a microwave catalytic device and an ultrasonic catalytic device operating simultaneously, an air pressure regulating mechanism, and an ore disturbance mechanism are arranged; the inner cavity wall of the acid leaching chamber and the inner wall of the closed cover are made of polyetheretherketone, polyimide or polytetrafluoroethylene.

[0018] A process for removing impurities from high-purity quartz, using the mixed acid for removing impurities from high-purity quartz as described above; in the acid leaching and impurity removal process, microwaves and ultrasound are used simultaneously for catalysis and pressurization, the temperature is controlled at 60-80 degrees Celsius, the process is carried out in a closed cavity, and the ore is kept rolling, and the pressure in the cavity is controlled at 1-5 Pa in the middle of the acid leaching; the power ratio of microwave heating and ultrasound is maintained at 1:3 to 5:1 (whether it is accurate).

[0019] Preferably, at the beginning of the acid leaching and impurity removal process, the quartz ore material is first placed in a closed cavity, and then the ore is kept in a rolling state, and then the components of the mixed acid for high-purity quartz impurity removal are sequentially injected into the closed cavity.

[0020] Preferably, the quartz ore material is a powder with a particle size of 40-160 mesh; in the acid leaching and impurity removal process, the pressure in the chamber is controlled at 3 Pa.

[0021] During implementation, after the acid leaching and impurity removal process is completed, the finished product needs to be washed, dried, color sorted, and chlorinated to remove impurities in sequence, and then the finished product is obtained.

[0022] The beneficial effects of the present invention are as follows: a mixed acid for removing impurities from high-purity quartz and impurity removal equipment and process using the mixed acid, which are used for acid leaching impurity removal process, and the components thereof include: water, oxalic acid, aminosulfonic acid, a penetrant, citric acid and / or hydrochloric acid; the mixed acid effectively removes / replaces hydrofluoric acid through a large amount of inorganic acid, and can better ensure the quartz purification effect, the cost of each acid is relatively moderate, the hazard coefficient to the plant and personnel is greatly reduced, and the cost is the same as that of the traditional mixed acid, the reaction product is easy to handle, and will not cause harm to the environment; the impurity removal equipment using the acid is provided with a microwave catalytic device and an ultrasonic catalytic device operating simultaneously, and effective impurity removal is achieved under the action of the mixed acid, and the equipment is durable, has a good impurity removal effect, and has a good energy efficiency ratio; the process using the mixed acid effectively promotes the acid leaching impurity removal reaction of the mixed acid by simultaneously catalyzing and pressurizing with microwaves and ultrasonic waves, ensures the impurity removal effect, and is energy-saving and environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic structural diagram of an embodiment of the impurity removal equipment of the present invention. DETAILED DESCRIPTION

[0024] The present invention will be further described in detail below through specific implementation modes in conjunction with the accompanying drawings.

[0025] The invention provides a mixed acid for removing impurities from high-purity quartz and impurity removal equipment and a process using the mixed acid.

[0026] The present invention discloses a mixed acid for high-purity quartz impurity removal, which is used in an acid leaching impurity removal process, and its components include: water, oxalic acid, aminosulfonic acid, a penetrant, citric acid and / or hydrochloric acid. The component can effectively remove / replace hydrofluoric acid and ensure the quartz purification effect.

[0027] During implementation, preferably, the concentration of the mixed acid is 25-35%, so that the acid has the best activity.

[0028] During implementation, the molar ratio of each component in the mixed acid is: 1-7 oxalic acid, 3-10 aminosulfonic acid, 1-5 penetrant, and 1-5 citric acid or hydrochloric acid. This ratio can maximize the impurity removal effect of the mixed acid. During implementation, each ratio can be appropriately adjusted according to the impurity situation of the treated quartz.

[0029] In practice, preferably, the penetrant is silicate or sodium oleate. The two components, when added in a mixed form, can produce a better superposition effect and ensure the acid leaching impurity removal effect.

[0030] During implementation, preferably, the molar ratio of the components of the mixed acid is: 1-2 oxalic acid, 1 sulfamic acid, 1-5 penetrant, and 1 citric acid or hydrochloric acid.

[0031] Preferably, the mixed acid also comprises one or more of sulfuric acid, nitric acid, tartaric acid, fulvic acid, silicic acid, perchloric acid and benzoic acid. After addition, the effect of the mixed acid can be optimal.

[0032] The specific mixed ingredients can be:

[0033] Example 1: water, oxalic acid, aminosulfonic acid, penetrant, citric acid.

[0034] Example 2: water, oxalic acid, aminosulfonic acid, penetrant, hydrochloric acid.

[0035] Example 3: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid, hydrochloric acid.

[0036] Example 4: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid.

[0037] Example 5: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, nitric acid.

[0038] Example 6: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid.

[0039] Example 7: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid, nitric acid.

[0040] Example 8: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid, fulvic acid.

[0041] Example 9: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, fulvic acid.

[0042] Example 10: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, fulvic acid, sulfuric acid.

[0043] Example 11: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, perchloric acid, sulfuric acid.

[0044] Example 12: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, perchloric acid.

[0045] Example 13: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, benzoic acid.

[0046] Example 14: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid, nitric acid.

[0047] Example 15: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, fulvic acid, benzoic acid.

[0048] Example 16: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, perchloric acid, benzoic acid.

[0049] Example 17: Water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid, sulfuric acid, benzoic acid.

[0050] Example 18: water, oxalic acid, aminosulfonic acid, penetrant, citric acid and / or hydrochloric acid, silicic acid, perchloric acid, benzoic acid.

[0051] Example 19: water, oxalic acid, aminosulfonic acid, penetrant, citric acid and / or hydrochloric acid, silicic acid, sulfuric acid, benzoic acid.

[0052] Example 20: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid, nitric acid, tartaric acid, silicic acid, benzoic acid.

[0053] Example 21: Water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid, tartaric acid, silicic acid, benzoic acid.

[0054] Of course, during implementation, a small amount of hydrofluoric acid can also be added to the mixed acid of the present invention to improve the effect. However, compared with the traditional mixed acid formula, the amount of hydrofluoric acid used can be greatly reduced under the same effect.

[0055] During implementation, preferably, specifically, the molar ratio of each component in the mixed acid is: 1-7 of oxalic acid, 3-10 of aminosulfonic acid, 1-5 of penetrant, 1-5 of citric acid or hydrochloric acid, and 2-8 of other acids.

[0056] In the above-mentioned various implementations, the concentration of the mixed acid is finally controlled to be 25-35% by mixing with water, so that the acid has the best activity.

[0057] The following is a comparison of the application of the mixed acid of the present invention and the traditional mixed acid with hydrofluoric acid:

[0058] (1) Old formula (containing hydrofluoric acid): raw ore SiO 2 The content is 99.8%. After roasting, it is sequentially quenched, ground, classified, and iron removed by high gradient. After acid leaching and impurity removal, the agent is heated for 48 hours, and then washed, floated, dried, color sorted, and chlorinated for impurity removal. The finished product is tested for SiO2 Content 99.99%.

[0059] (2) New formula of the present invention: raw ore SiO 2 The content is 99.8%. After roasting, it is sequentially quenched, ground, classified, and iron removed by high gradient. After acid leaching and impurity removal, the agent is heated for 48 hours, and then washed, floated, dried, color sorted, and chlorinated for impurity removal. The finished product is tested for SiO 2 The content is 99.89%. It can be seen that the mixed acid of the present invention basically achieves the impurity removal effect of the traditional formula.

[0060] Reference Figure 1 As shown, the present invention also discloses a device for removing impurities from high-purity quartz, using the mixed acid for removing impurities from high-purity quartz as described above; the device includes an acid leaching chamber with a closed cover, on which a microwave catalytic device 5 and an ultrasonic catalytic device 4 operating simultaneously, an air pressure regulating mechanism 8 and an ore disturbance mechanism are arranged; the inner cavity wall of the acid leaching chamber and the inner wall of the closed cover are made of polyetheretherketone, polyimide or polytetrafluoroethylene.

[0061] During implementation, the ore disturbance mechanism can be a rotation drive mechanism, a shaking mechanism or a vibration mechanism of the acid leaching chamber. In the embodiment of the present patent, the preferred structure is a structure in which the roasting chamber is driven to rotate by a motor.

[0062] like Figure 1 As shown, a device for removing impurities from high-purity quartz is a horizontal reactor, which includes a horizontally placed U-shaped reactor body 1 and a quick-opening reactor cover 2 for closing the opening of the reactor body. The reactor body and the quick-opening reactor cover are detachably connected through a safety buckle (or bolt 3), and a sealing ring 14 made of acid- and alkali-resistant polymer material is also provided on the contact surface between the reactor body and the quick-opening reactor cover. An ultrasonic catalytic device 4 penetrating the reactor body is provided at the bottom of the U-shaped structure of the reactor body 1; a microwave catalytic device 5 radiating into the tube is provided on the outer wall of the reactor body 1; a microwave isolation layer is also provided to envelop the outer wall of the reactor body to prevent the aforementioned microwave from leaking; and an ore turning mechanism is also provided to drive the processed ore in the reactor body 1 to turn over.

[0063] like Figure 1 As shown, it is preferred that the bottom edge of the horizontal reactor body 1 is at an angle of -5 to -15 degrees with the horizontal. There are three schemes to achieve the angle: 1. The two sides of the U-shaped reactor body 1 are at an angle of 10-30 degrees, and the central axis of the inner cavity tube body of the reactor body 1 is located in the horizontal plane; 2. Or the two sides of the U-shaped reactor body 1 are parallel, and the central axis of the inner cavity tube body of the reactor body 1 is at an angle of -5 to -15 degrees with the horizontal plane; 3. The reactor body 1 can also be provided with a tilting mechanism, which drives the reactor body 1 to tilt from the horizontal to an angle of -5 to -15 degrees with the horizontal during the cleaning stage (maintaining the horizontal during the conventional acid leaching and impurity removal stage).

[0064] like Figure 1 As shown, it is preferred that the ultrasonic catalytic device 4 includes an ultrasonic main unit 4a, an ultrasonic transducer 4b and a transducer head anti-corrosion layer 4c, the ultrasonic main unit 4a is arranged on the outside of the reactor body 1, and the ultrasonic transducer 4b penetrates the bottom center of the U-shaped structure of the reactor body 1 and is arranged on the central axis of the inner cavity tube body of the reactor body 1.

[0065] like Figure 1 As shown, during implementation, the inner wall of the reaction kettle body 1 and the inner wall of the quick-opening kettle cover 2 are made of polymer acid- and alkali-resistant materials; the anti-corrosion layer 4c is an anti-corrosion ceramic protective layer or a polymer acid- and alkali-resistant material protective layer on the surface of the ultrasonic transducer head 4b; the polymer acid- and alkali-resistant material is polyetheretherketone, polyimide or polytetrafluoroethylene.

[0066] like Figure 1 As shown, during implementation, the microwave catalytic device 5 includes a microwave variable frequency power supply 5c, a variable frequency magnetron 5b and a waveguide cavity 5a. The waveguide cavity 5a is close to the outer wall of the reactor body 1 to introduce microwaves into the inner cavity of the reactor body 1.

[0067] like Figure 1 As shown, it is preferred that during implementation, the outer wall of the reactor body 1 has a cylindrical profile, and the microwave isolation layer is a metal isolation cover 6 with a cylindrical inner cavity. The metal isolation cover 6 and the waveguide cavity 5a are both kept at a distance of 3-20 mm from the outer wall of the reactor body 1.

[0068] like Figure 1 As shown, during implementation, the ore turning mechanism is a rotary drive mechanism of the reactor body 1, including a rotary drive motor 10, a transmission belt 12, and a driven disk 12 fixed at the tail of the reactor body 1; the rotary drive motor 10 rotates at a constant speed and drives the reactor body 1 to rotate at a constant speed through the transmission belt 12 and the driven disk 12, thereby driving the ore processed in the reactor body 1 to turn over.

[0069] like Figure 1 As shown, during implementation, a regulating mechanism 8 for regulating the air pressure in the reaction kettle cavity, a liquid inlet mechanism 9 for inputting acid and water, a sensor unit 7 and an inlet and outlet water mechanism 11 are also provided; the inner cavity of the reaction kettle body 1 is connected with the air pressure regulating mechanism 8, the liquid inlet mechanism 9 and the inlet and outlet water mechanism 11 through pipelines with valves respectively; the inner cavity of the reaction kettle body 1 is also connected with the sensor unit 7 through pipelines, and the sensor unit 7 is provided with a safety valve, a pressure gauge and a pressure sensor.

[0070] like Figure 1As shown, it is preferred that a PLC for monitoring and controlling is also provided during implementation. The PLC also controls the microwave catalytic device 5, the ultrasonic catalytic device 4 and the ore turning mechanism to work synchronously.

[0071] In one embodiment, the reactor has a volume of 15L, a pressure of 3 MPa, a power supply of 220v±10v, a power of 5000WV, a frequency of 2450+50Hz, and a microwave leakage control of <5mW / cm. The rotary drive motor 10 is a stepper motor, which is controlled by PLC. The reaction temperature in the reactor body is 100°C-200°C, and the wavelengths of ultrasound and microwave need to pass through quartz sand.

[0072] The mixed acid of the present invention is combined with the equipment of the present invention:

[0073] (3) Experimental process, raw ore SiO 2 The content is 99.8%. After roasting, it is sequentially quenched with water, ground, classified, and iron removed with high gradient. Then, it is placed in the equipment for high-purity quartz impurity removal of the present invention, and microwave and ultrasonic waves are synchronously catalyzed and pressurized to 3 Pa. After the reagent is heated and reacted for 48 hours, it is sequentially washed, floated, dried, color sorted, and chlorinated for impurity removal. The finished product is tested for SiO 2 The content is 99.994%. It can be seen that the impurity removal effect of the mixed acid of the present invention combined with the equipment of the present invention is better than that of the traditional formula and equipment.

[0074] A process for removing impurities from high-purity quartz, using the mixed acid for removing impurities from high-purity quartz as described above; in the acid leaching impurity removal process, microwaves and ultrasound are used to simultaneously catalyze and pressurize, the temperature is controlled at 60-80 degrees Celsius, the process is carried out in a closed cavity, and the ore is kept rolling, and the pressure in the cavity is controlled at 1-5 Pa in the middle of the acid leaching; the power ratio of microwave heating and ultrasound is maintained at 1:3 to 5:1 (whether it is accurate). In the acid leaching impurity removal process, microwaves and ultrasound are used to simultaneously catalyze and pressurize, so that the agent can fully play its role, the ultrasound further opens the remaining fine inclusions, and the impurities between the crystals can be better penetrated by the agent under the action of microwaves and ultrasound, achieving a better reaction removal effect. Compared with the traditional process, the present invention can further reduce the reaction time, significantly reduce energy consumption, and improve the impurity removal effect.

[0075] Preferably, at the beginning of the acid leaching impurity removal process, the quartz ore material is first placed in a closed cavity, and then the ore is kept in a rolling state, and then the components of the mixed acid for high-purity quartz impurity removal are sequentially injected into the closed cavity. On the basis of ensuring the impurity removal effect, the operability of the process and the efficiency and convenience of mixed acid preparation are improved.

[0076] During implementation, preferably, the quartz ore material is a powder with a particle size of 40-160 mesh; in the acid leaching and impurity removal process, the pressure in the chamber is controlled at 3 Pa.

[0077] During implementation, preferably, after the acid leaching and impurity removal process is completed, the finished product needs to be washed (flotation can be added), dried, color sorted, and chlorinated to remove impurities in sequence, and then the finished product is obtained.

[0078] Based on the mixed acid of the present invention, the quartz purification method can adopt the following complete process steps: raw ore → crushing → classification → dry iron removal → roasting → water quenching → grinding → classification → flotation (can be omitted) → high gradient iron removal → composite superconducting band complex reaction (i.e., the impurity removal process of the present invention) → cleaning (thereafter, one flotation can be added) → drying → color sorting → chlorination impurity removal → cooling and packaging. Of course, appropriate adjustments can also be made based on the traditional process. And the obvious front-end process (raw ore → crushing → classification → dry iron removal) and the back-end process (cleaning → drying → color sorting → chlorination impurity removal → cooling and packaging) can be adjusted very flexibly, for example, a flotation effect will be better after cleaning and before drying; the intermediate process (water quenching → grinding → classification → flotation → high gradient iron removal) is obvious, and it can also be appropriately adjusted or process processing can be added as needed, or part of the process can be replaced and / or repeated with the front-end / back-end process.

[0079] Through the mixed acid and the above process of the present invention, combined with suitable domestic quartz ore, and better mixed acid ratio and parameter control, the production of high-purity quartz up to 99.99% can be achieved (combined with supporting equipment and process, the production of high-purity quartz up to 99.998% can be achieved), and it is efficient, low energy consumption, low carbon and environmentally friendly. The patented formula greatly reduces the amount of hydrofluoric acid used, solves the national environmental protection requirements, and avoids the restrictions of environmental protection on the industry, and realizes the production of high-purity quartz.

Claims

1. A mixed acid for removing impurities from high-purity quartz, used in an acid leaching and impurity removal process, comprising: water, oxalic acid, aminosulfonic acid, a penetrant, citric acid and / or hydrochloric acid.

2. The mixed acid for removing impurities from high-purity quartz as claimed in claim 1, characterized in that: The concentration of the mixed acid is 25-35%, and the penetrant is silicate or sodium oleate.

3. The mixed acid for removing impurities from high-purity quartz as claimed in claim 1 or 2, characterized in that: Its ingredients also include: one or more of sulfuric acid, nitric acid, tartaric acid, fulvic acid, silicic acid, perchloric acid, and benzoic acid.

4. The mixed acid for removing impurities from high-purity quartz as claimed in claim 1 or 2, characterized in that: The molar ratio of each component in the mixed acid is: 1-7 of oxalic acid, 3-10 of aminosulfonic acid, 1-5 of penetrant, and 1-5 of citric acid or hydrochloric acid.

5. The mixed acid for removing impurities from high-purity quartz as claimed in claim 3, characterized in that: The molar ratio of each component in the mixed acid is: 1-7 of oxalic acid, 3-10 of aminosulfonic acid, 1-5 of penetrant, 1-5 of citric acid or hydrochloric acid, and 2-8 of other acids.

6. The mixed acid for removing impurities from high-purity quartz as claimed in claim 4, characterized in that The molar ratio of the components of the mixed acid is: 1-2 of oxalic acid, 1 of aminosulfonic acid, 1-5 of penetrant, and 1 of citric acid or hydrochloric acid.

7. A device for removing impurities from high-purity quartz, characterized in that: A mixed acid for removing impurities from high-purity quartz as described in claims 1-6 is used; the equipment comprises an acid leaching chamber with a closed cover, on which a microwave catalytic device and an ultrasonic catalytic device operating simultaneously, an air pressure regulating mechanism and an ore disturbance mechanism are arranged; the inner wall of the acid leaching chamber and the inner wall of the closed cover are made of polyetheretherketone, polyimide or polytetrafluoroethylene.

8. A process for removing impurities from high-purity quartz, characterized in that: Using the mixed acid for high-purity quartz impurity removal as described in claims 1-6; in the acid leaching impurity removal process, microwave and ultrasonic waves are used for simultaneous catalysis and pressurization, the temperature is controlled at 60-80 degrees Celsius, the process is carried out in a closed cavity, and the ore is kept rolling, The middle stage of acid leaching The pressure in the cavity is controlled at 1-5 Pa; the power ratio of microwave heating and ultrasonic wave is maintained at 1:3 to 5:1 (whether it is accurate).

9. The process for removing impurities from high-purity quartz according to claim 8, characterized in that: At the beginning of the acid leaching and impurity removal process, the quartz ore material is first placed in a closed cavity, and then the ore is kept in a rolling state, and then the components of the mixed acid for high-purity quartz impurity removal are sequentially injected into the closed cavity.

10. The process for removing impurities from high-purity quartz according to claim 9, characterized in that: The quartz ore material is a powder with a particle size of 40-160 meshes; in the acid leaching and impurity removal process, the pressure in the chamber is controlled at 3 Pa.