Low-acid-consumption 5N-grade quartz sand under regulation and control of compound field as well as preparation method and application of low-acid-consumption 5N-grade quartz sand

Abstract

The invention relates to the technical field of mineral purification, in particular to low-acid-consumption 5N-grade quartz sand under compound field regulation and control and a preparation method and application thereof.The preparation method comprises the steps that quartz sand raw materials are pretreated, under compound field synergistic strengthening treatment, a mixed acid solution is added for leaching treatment, and the low-acid-consumption 5N-grade quartz sand under compound field regulation and control is obtained; the composite field synergistic strengthening treatment comprises a magnetic field, a microwave field, an ultrasonic field and a thermal field, through the synergistic effect of the composite field, single-step completion of quartz sand strengthening treatment is achieved, ultra-high-purity quartz sand with the purity stably reaching the 5N level is prepared, acid consumption is remarkably reduced, environmental pollution is reduced, the technological process is simplified, and production efficiency is improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of mineral purification, in particular to a 5N-grade quartz sand with low acid consumption under the regulation of a composite field and a preparation method and application thereof. BACKGROUND

[0002] Quartz sand (main component is SiO2) is an inorganic non-metallic material, which does not react with other acids except hydrofluoric acid, has a melting point of about 1670℃ (quartz) ~ 1710℃ (cristobalite), and a Mohs hardness of 7. The quartz sand will present different colors due to internal impurities, and the high-purity quartz sand is usually milky white or colorless.

[0003] Ultra-high-purity quartz sand refers to quartz sand with a purity of >99.999%, which is an important basic material in the semiconductor field and an important raw material for preparing quartz crucibles and other products, and is widely used in the semiconductor industry.

[0004] The existing quartz sand purification process mainly includes multiple steps such as mechanical crushing, scrubbing and desliming, magnetic separation, flotation, acid leaching, and calcination. These processes often accompany high process costs while improving the purity of quartz sand, and the multi-step purification process also increases the operation complexity and time cost. Some technologies attempt to introduce single physical field assisted purification, such as selective heating of microwaves, which can cause thermal stress differences between impurities and quartz matrix, promoting crack propagation. However, the purity of quartz sand prepared by single physical field assisted purification process is difficult to stabilize at 5N level, which cannot meet the strict requirements of the semiconductor industry for ultra-high-purity quartz sand. SUMMARY

[0005] In view of the above deficiencies of the prior art, the present application aims to provide a 5N-grade quartz sand with low acid consumption under the regulation of a composite field and a preparation method and application thereof. Through the synergistic effect of magnetic field, microwave field, ultrasonic field, and temperature field, the single-step completion of quartz sand strengthening treatment is realized, the process flow is simplified while the acid consumption is greatly reduced, and ultra-high-purity quartz sand with stable purity of 5N level is prepared.

[0006] To solve the above technical problems, the present application adopts the following technical solutions: A preparation method of a 5N-grade quartz sand with low acid consumption under the regulation of a composite field, comprising the following steps: Pretreat the quartz sand raw material, and perform synchronous strengthening treatment in a composite field of four-field coupling of magnetic field, microwave field, ultrasonic field, and thermal field, then add a mixed acid solution for leaching treatment to obtain a 5N-grade quartz sand with low acid consumption under the regulation of a composite field.

[0007] In the preferred embodiment of the present application, in the composite field, the magnetic field parameter is 0.5T-2T; the microwave field parameter is 500MHz-1500MHz; the thermal field temperature parameter is 200℃-950℃, the heating rate is 5℃ / min-10℃ / min; the ultrasonic field parameter is 20kHz-80kHz, and the synchronous strengthening treatment time in the composite field is 30min-120min.

[0008] In the preferred embodiment of the present application, the mixed acid solution is a mixed solution of hydrofluoric acid, nitric acid and hydrochloric acid, and the volume ratio of hydrofluoric acid, nitric acid and hydrochloric acid is 2-6:1-3:1.

[0009] In the preferred embodiment of the present application, the particle size of the quartz sand raw material after pretreatment is 100-150 mesh.

[0010] In the preferred embodiment of the present application, the ball milling speed of the pretreatment is 80r / min-120r / min, the ball-to-material ratio of the pretreatment is 1:0.3-1, the ball milling time of the pretreatment is 30min-60min, the washing times of the pretreatment are 2-3 times, and the washing liquid is ultrapure water.

[0011] In the preferred embodiment of the present application, the use amount of the quartz sand raw material is 100±0.005g per part.

[0012] In the preferred embodiment of the present application, the leaching treatment time is 1h-9h.

[0013] In the preferred embodiment of the present application, the leaching treatment time is 4.5h.

[0014] Another object of the present application is the composite field regulated low-acid-consumption 5N grade quartz sand prepared by the preparation method of the composite field regulated low-acid-consumption 5N grade quartz sand according to any one of the present application.

[0015] The application of the composite field regulated low-acid-consumption 5N grade quartz sand according to the present application in the field of semiconductors.

[0016] Compared with the prior art, the present application has the beneficial effects that: 1、The preparation method of the composite field regulated low-acid-consumption 5N grade quartz sand according to the present application pretreats the quartz sand raw material, and performs synchronous strengthening treatment in a composite field coupled by a magnetic field, a microwave field, an ultrasonic field and a thermal field, then adds a mixed acid solution for leaching treatment, to obtain the composite field regulated low-acid-consumption 5N grade quartz sand, so that the purity of the ultra-high-purity quartz sand reaches 5N grade through the synchronous strengthening effect of the composite field coupled by the four fields, the process flow is simplified, the production efficiency is improved, the cost is significantly reduced, and the environmental pollution is reduced.

[0017] 2, the present application is through the four field coupling of magnetic field, microwave field, ultrasonic field and thermal field in the composite field of synchronous reinforcement processing, the microwave field can make the impurities and quartz matrix produce thermal stress difference, promote crack propagation;Ultrasonic field can produce high temperature and high pressure microjet in local, impact the quartz surface;Magnetic field uses the magnetic susceptibility difference of impurities, selectively removes the element impurities;The additional thermal field makes the quartz crystal phase change with the volume change, thereby producing cracks, it is convenient for subsequent acid immersion reagent depth immersion quartz sand, the purpose is that the surface of quartz sand produces extension crack, part of impurity elements in quartz sand precipitate, so that the impurity removal rate is high, the removal effect is good, increases the purification efficiency of 5N grade quartz sand;The preparation method of low acid consumption 5N grade quartz sand under the regulation of the composite field described in the application is a green, saving and sustainable quartz sand purification method;The quartz sand prepared by the application has a final purity of 5N, and the impurity content is very low, meeting the requirements of semiconductor grade quartz sand. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 SEM image of the sample of example 3 of the present application. DETAILED DESCRIPTION

[0019] The technical solutions in the embodiments of the present application will be described clearly and completely in combination with the preferred embodiments and the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0020] It should be noted that all the professional terms used in the present application are only for the purpose of describing the specific embodiments, and are not intended to limit the protection scope of the present application. Unless otherwise specified, all the materials, reagents, instruments and equipment used in the following embodiments of the present application can be purchased from the market or prepared by the existing method.

[0021] A preparation method of low acid consumption 5N grade quartz sand under the regulation of the composite field, comprising the following steps: The quartz sand raw material is pretreated and subjected to synchronous reinforcement processing in the composite field of the coupling of magnetic field, microwave field, ultrasonic field and thermal field, and then mixed acid solution is added for leaching treatment, to obtain low acid consumption 5N grade quartz sand under the regulation of the composite field.

[0022] In the preferred embodiment of the present application, in the composite field, the magnetic field parameter is 0.5T~2T;The microwave field parameter is 500MHz~1500MHz;The thermal field temperature parameter is 200℃~950℃, and the heating rate is 5℃ / min~10℃ / min;The ultrasonic field parameter is 20kHz~80kHz, and the synchronous reinforcement processing time in the composite field is 30min~120min.

[0023] In a preferred embodiment of the present application, the mixed acid solution is a mixed solution of hydrofluoric acid, nitric acid and hydrochloric acid, and the volume ratio of hydrofluoric acid, nitric acid and hydrochloric acid is 2-6:1-3:1.

[0024] In a preferred embodiment of the present application, the particle size of the quartz sand raw material after pretreatment is 100-150 mesh.

[0025] In a preferred embodiment of the present application, the rotation speed of the ball mill during pretreatment is 80-120 r / min, the ball-to-material ratio during pretreatment is 1:0.3-1, the pretreatment time is 30-60 min, the washing times during pretreatment are 2-3 times, and the washing liquid is ultrapure water.

[0026] In a preferred embodiment of the present application, the amount of the quartz sand raw material used is 100±0.005 g per portion.

[0027] In a preferred embodiment of the present application, the leaching treatment time is 1-9 h.

[0028] In a preferred embodiment of the present application, the leaching treatment time is 4.5 h.

[0029] Another object of the present application is the composite field regulated low-acid-consumption 5N grade quartz sand prepared by the method for preparing composite field regulated low-acid-consumption 5N grade quartz sand according to any one of the preceding items.

[0030] Example 1 A method for preparing composite field regulated low-acid-consumption 5N grade quartz sand, comprising the following steps: (1) Ball milling of high-purity quartz sand, ball mill rotation speed 110 r / min, ball-to-material ratio 1:0.3, ball milling time 30 min, and 100-150 mesh quartz sand powder is obtained due to the fact that the ball milling cannot reach a uniform particle size, and the ball-milled quartz sand powder is washed 3 times and then dried at 110°C for 8 h.

[0031] (2) Intensifying treatment of the quartz sand in a composite field device of magnetic field, microwave field, ultrasonic field and temperature field, the magnetic field is set to 1.5 T, the microwave field is set to 915 MHz, the temperature is 450°C, and the time is 30 min, and the ultrasonic parameter is set to 20 and the time is 30 min.

[0032] (3) Leaching of the intensified quartz sand in a mixed acid solution of hydrofluoric acid, nitric acid and hydrochloric acid in a volume ratio of 6:3:1, and drying.

[0033] Example 2 A method for preparing composite field regulated low-acid-consumption 5N grade quartz sand, comprising the following steps: (1) Ball milling of high-purity quartz sand, ball milling speed 110 r / min, ball-to-material ratio 1:0.3, ball milling time 30 min, 100-150 mesh quartz sand powder is obtained due to the uneven particle size after ball milling; the quartz sand powder after ball milling is washed for 3 times, and then dried at 110°C for 8 h.

[0034] (2) The quartz sand is subjected to strengthening treatment in a composite field device of magnetic field, microwave field, ultrasonic field and temperature field, the magnetic field is set to 1.6T; the microwave field is set to 915MHz, the temperature is 550°C, and the time is 30 min; the ultrasonic parameters are set to 40kHz, and the time is 30 min.

[0035] (3) The strengthened quartz sand is immersed in a mixed acid solution of hydrofluoric acid, nitric acid and hydrochloric acid in a volume ratio of 5:2:1, and then dried.

[0036] Example 3 A preparation method of low-acid-consumption 5N-grade quartz sand under the regulation of a composite field, comprising the following steps: (1) Ball milling of high-purity quartz sand, ball milling speed 110 r / min, ball-to-material ratio 1:0.3, ball milling time 30 min, 100-150 mesh quartz sand powder is obtained due to the uneven particle size after ball milling; the quartz sand powder after ball milling is washed for 3 times, and then dried at 110°C for 8 h.

[0037] (2) The quartz sand is subjected to strengthening treatment in a composite field device of magnetic field, microwave field, ultrasonic field and temperature field, the magnetic field is set to 1.8T; the microwave field is set to 915MHz, the temperature is 650°C, and the time is 30 min; the ultrasonic parameters are set to 80kHz, and the time is 30 min.

[0038] (3) The strengthened quartz sand is immersed in a mixed acid solution of hydrofluoric acid, nitric acid and hydrochloric acid in a volume ratio of 2:1:1, and then dried.

[0039] Comparative Example 1 (1) Crushing: the particle size of quartz sand is required to be 100-150 mesh.

[0040] (2) Magnetic separation: the above quartz sand is subjected to magnetic separation under a magnetic field strength of 1.0T.

[0041] (3) Acid leaching: solid-to-liquid ratio 1Kg:18L of organic acid, solid-to-liquid ratio 1Kg:0.2L of hydrofluoric acid with a concentration of 0.5mol / L.

[0042] (4) First ultrasonic treatment: the above acid leaching mixture is treated by ultrasonic waves with a frequency of 25kHz and a power of 200W.

[0043] (5) Second ultrasonic: using ultrasonic with frequency of 40 kHz and power of 250 W for secondary treatment, and drying.

[0044] Comparative Example 2 The same process as Comparative Example 1 was adopted, except that the first ultrasonic was not used, and only the second ultrasonic was used.

[0045] Result analysis Figure 1 The SEM image of the sample of Example 3 of the application is shown in the figure, and it can be seen from the figure that cracks of different degrees appear on the surface of the quartz sand particles, providing a path for subsequent acid leaching.

[0046] The chemical composition of the quartz sand products in Examples 1-3 above was analyzed by inductively coupled plasma emission spectrometer, and Table 1 was obtained.

[0047] Table 1: Impurity element content and purity calculation results of samples in Examples 1-3 by ICP-MS The chemical composition of the quartz sand products in Examples 1-3 and Comparative Examples 1-2 above was analyzed by inductively coupled plasma emission spectrometer, and the results are shown in Table 2.

[0048] Table 2: Quartz sand element content results As can be seen from Tables 1 and 2, multi-field synergy can reduce the impurity content in quartz sand, but the process is often complicated, the acid consumption is high, and the purity of the obtained quartz sand is not high. However, by using the purification method of the application, only one step of composite field is required to meet the requirements of magnetic separation, microwave, and ultrasonic, and the acid consumption can be reduced to obtain quartz sand with a purity of 5N.

[0049] The preparation method of low-acid-consumption 5N-grade quartz sand under the regulation of a composite field provided by the application, the quartz sand raw material is pretreated and subjected to synchronous strengthening treatment in a composite field coupled by a magnetic field, a microwave field, an ultrasonic field, and a thermal field, and then a mixed acid solution is added for leaching treatment to obtain low-acid-consumption 5N-grade quartz sand under the regulation of a composite field. Through the synchronous strengthening effect of the four-field coupled composite field, ultra-high-purity quartz sand with a stable purity of 5N is prepared, the process flow is simplified, the production efficiency is improved, the cost is significantly reduced, and environmental pollution is reduced.

[0050] The application carries out synchronous strengthening treatment in a composite field of four-field coupling of a magnetic field, a microwave field, an ultrasonic field and a thermal field, the microwave field can cause thermal stress difference between impurities and the quartz matrix, promote crack propagation, the ultrasonic field can generate high-temperature and high-pressure microjet in local, impact the quartz surface, the magnetic field uses the magnetic susceptibility difference of the impurities, selectively removes the element impurities, the additional thermal field makes the quartz crystal undergo phase transition with volume change, thereby generating cracks, facilitating subsequent acid immersion reagent deep immersion into quartz sand, the purpose is to produce extended cracks on the surface of quartz sand, and part of impurity elements in the quartz sand are precipitated, so that the impurity removal rate is high, the removal effect is good, and the purification efficiency of 5N grade quartz sand is increased; the preparation method of the 5N grade quartz sand with low acid consumption under the regulation of the composite field is a green, saving and sustainable quartz sand purification method; the quartz sand prepared by the application has a final purity of 5N, and the impurity content is very low, meeting the requirements of semiconductor grade quartz sand.

[0051] It should be noted that when the numerical range is involved in the application, both endpoints of each numerical range and any number between the two endpoints can be selected, since the same steps and examples are adopted, in order to prevent repetition, the preferred embodiments are described in the application. Although the preferred embodiments of the application have been described, those skilled in the art can make further changes and modifications to the embodiments once they know the basic creative concept. Therefore, the appended claims are intended to include the preferred embodiments and all changes and modifications falling within the scope of the application.

[0052] Obviously, those skilled in the art can make various modifications and variations to the application without departing from the spirit and scope of the application. Thus, if these modifications and variations of the application fall within the scope of the claims of the application and their equivalent technologies, the application also intends to include these modifications and variations.

Claims

1. A method for preparing low-acid-consumption 5N grade quartz sand under composite field control, characterized in that, Includes the following steps: Quartz sand raw materials are pretreated and simultaneously enhanced in a composite field coupled with magnetic field, microwave field, ultrasonic field and thermal field. Then, a mixed acid solution is added for leaching treatment to obtain low acid consumption 5N grade quartz sand under composite field control.

2. The method for preparing low-acid-consumption 5N-grade quartz sand under composite field control according to claim 1, characterized in that, In the composite field, the magnetic field parameters are 0.5T~2T; the microwave field parameters are 500MHz~1500MHz; the thermal field temperature parameters are 200℃~950℃, and the heating rate is 5℃ / min~10℃ / min; the ultrasonic field parameters are 20kHz~80kHz, and the synchronous strengthening treatment time in the composite field is 30min~120min.

3. The method for preparing low-acid-consumption 5N grade quartz sand under composite field control according to claim 1, characterized in that, The mixed acid solution is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, with a volume ratio of hydrofluoric acid:nitric acid:hydrochloric acid of 2~6:1~3:

1.

4. The method for preparing low-acid-consumption 5N grade quartz sand under composite field control according to claim 1, characterized in that, The particle size of the pretreated quartz sand raw material is 100-150 mesh.

5. The method for preparing low-acid-consumption 5N grade quartz sand under composite field control according to claim 1, characterized in that, The ball milling speed for pretreatment is 80 r / min to 120 r / min, the ball-to-material ratio for pretreatment is 1:0.3 to 1, the ball milling time for pretreatment is 30 min to 60 min, the number of washing cycles for pretreatment is 2 to 3, and the washing solution is ultrapure water.

6. The method for preparing low-acid-consumption 5N grade quartz sand under composite field control according to claim 1, characterized in that, The amount of quartz sand raw material used is 100±0.005g per part.

7. The method for preparing low-acid-consumption 5N grade quartz sand under composite field control according to claim 1, characterized in that, The leaching treatment time is 1 hour to 9 hours.

8. The low acid consumption 5N grade quartz sand under composite field control prepared by the method of preparing low acid consumption 5N grade quartz sand under composite field control according to any one of claims 1-7.

9. The application of low acid consumption 5N grade quartz sand under composite field control as described in claim 8 in the semiconductor field.

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