CN112777600B - Ultra-pure quartz and preparation method thereof - Google Patents
Ultra-pure quartz and preparation method thereof Download PDFInfo
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- CN112777600B CN112777600B CN202110267642.8A CN202110267642A CN112777600B CN 112777600 B CN112777600 B CN 112777600B CN 202110267642 A CN202110267642 A CN 202110267642A CN 112777600 B CN112777600 B CN 112777600B
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Abstract
The invention relates to ultra-pure quartz and a preparation method thereof. The preparation method comprises the steps of quartz pretreatment, surface impurity cleaning, surface defect increasing, diffusion segregation of quartz crystal lattice metal impurities and surface impurity segregation region denudation which are sequentially carried out; the diffusion segregation step of the quartz crystal lattice metal impurities adopts roasting for treatment, and the surface impurity segregation region denudation step adopts sodium hydroxide for treatment. The preparation method does not use substances such as hydrofluoric acid, chlorine, hydrogen fluoride gas and the like which are not friendly to the environment or have high danger, and is environment-friendly; and the waste liquid generated in the hydrochloric acid leaching step and the sodium hydroxide leaching step can be mutually neutralized, so that the treatment cost of the quartz industrial wastewater can be greatly reduced.
Description
Technical Field
The invention relates to the technical field of quartz sand production, in particular to ultra-pure quartz and a preparation method thereof.
Background
The ultra-pure quartz sand is generally SiO2The quartz sand with the content higher than 99.99 percent has excellent chemical stability, high insulation and pressure resistance and extremely low volume expansion coefficient. Is an important basic material indispensable to high and new technology industries such as electronic core guide parts, optical-guide communication materials, solar cells and the like. The high-grade product is widely applied to industries such as large-scale integrated circuits, solar cells, optical fibers, lasers, aerospace, military and the like. The purity of the quartz sand and the types and contents of impurity elements directly influence the quality of products.
The prior purification process of quartz sand mainly comprises the following steps: the method comprises the following steps of manual ore dressing, water washing, coarse crushing, fine crushing, screening, magnetic separation, acid washing, flotation, deionized water washing, drying and quartz sand quality detection. The purification process is complex in flow, and can not effectively remove the wrapping impurities and surface impurities in the quartz sand, and new impurities can be introduced in the production process. In the prior art, alkali washing is reported, for example, the publication number is CN102674376A, the invention name is 'a production method for purifying quartz tailings', an alkali washing process is introduced, but impurity metal elements which are gathered inside quartz sand are difficult to remove effectively.
Disclosure of Invention
In view of the above, there is a need for a method for preparing ultra-pure quartz, which can effectively remove the metallic impurity elements segregated inside the quartz sand.
The invention provides a method for preparing ultra-pure quartz, which comprises the steps of quartz pretreatment, surface impurity cleaning, surface defect increasing, diffusion segregation of quartz crystal lattice metal impurities and surface impurity segregation region denudation which are sequentially carried out; the step of increasing the surface defects adopts sodium hydroxide for treatment, the step of diffusing and partially polymerizing the quartz crystal lattice metal impurities adopts roasting for treatment, and the step of denudating the surface impurity partially polymerized area adopts sodium hydroxide for treatment.
Specifically, the quartz pretreatment step comprises the steps of crushing, magnetic separation and screening of quartz.
Specifically, in the step of cleaning the surface impurities, 1-4 mol/L hydrochloric acid solution is adopted for hot-pressing leaching and cleaning, the liquid-solid ratio of the hydrochloric acid solution to the quartz particles is (6-10) mL:1g, the leaching temperature is 150-250 ℃, and the leaching time is 1-8 h.
Specifically, in the step of increasing the surface defects, 0.2-2 mol/L of sodium hydroxide solution is adopted to erode the quartz particles, the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is (6-10) mL:1g, the leaching temperature is 150-200 ℃, and the leaching time is 1-8 h.
Preferably, in the step of increasing the surface defects, the concentration of the sodium hydroxide solution is 0.6667mol/L, and the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is 6mL:1 g.
Specifically, in the step of diffusion and segregation of the quartz crystal lattice metal impurities, the roasting temperature is 600-1400 ℃, and the roasting time is 5-70 h.
Preferably, in the step of diffusion segregation of the quartz crystal lattice metal impurities, the roasting temperature is 1000 ℃.
Specifically, in the step of denudation of the surface impurity segregation region, the concentration of a sodium hydroxide solution used is 0.1-0.5 mol/L, the liquid-solid ratio of the sodium hydroxide solution to quartz particles is (2-10) mL:1g, the leaching temperature is 150-200 ℃, and the leaching time is 1-8 h.
Preferably, in the step of denudating the surface impurity segregation region, the concentration of the sodium hydroxide solution is 0.3799mol/L, and the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is 6mL:1 g.
The invention also provides the ultra-pure quartz prepared by the method.
Has the advantages that:
1. the preparation method does not use substances such as hydrofluoric acid, chlorine, hydrogen fluoride gas and the like which are not friendly to the environment or have high danger, and is environment-friendly; and the waste liquid generated in the hydrochloric acid leaching step and the sodium hydroxide leaching step can be mutually neutralized, so that the treatment cost of the quartz industrial wastewater can be greatly reduced.
2. After the treatment of the preparation method, the Al element content in the quartz is reduced from 56.5 mu g/g to 7.8 mu g/g, the requirements of the IOTA 6 series on the Al content of 8 mu g/g are met, the total content of impurity elements is reduced to 38.2 mu g/g, which is far lower than 50 mu g/g required by the high-purity quartz standard.
Drawings
FIG. 1 is a flow chart of a method for preparing ultra-high purity quartz according to an embodiment of the present invention.
Fig. 2 is a surface topography diagram of a raw quartz ore provided by an embodiment of the present invention.
Fig. 3 is a surface topography diagram of a quartz raw ore leached by hydrochloric acid according to an embodiment of the present invention.
Fig. 4 is a surface topography diagram of a quartz raw ore leached by hydrochloric acid + sodium chloride according to an embodiment of the present invention.
Fig. 5 is a surface topography diagram of a quartz raw ore leached by hydrochloric acid + hydrofluoric acid according to an embodiment of the present invention.
Fig. 6 is a surface topography diagram of a raw quartz ore leached by sodium hydroxide according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
An embodiment of the present invention provides a method for preparing ultra-high purity quartz, as shown in fig. 1, including steps of quartz pretreatment, surface impurity cleaning, surface defect increasing, diffusion segregation of quartz lattice metal impurities, and surface impurity segregation region denudation, which are performed in sequence. The step of increasing the surface defects adopts sodium hydroxide for treatment, the step of diffusing and partially polymerizing the quartz crystal lattice metal impurities adopts roasting for treatment, and the step of denudating the surface impurity partially polymerized area adopts sodium hydroxide for treatment.
When the quartz particles are treated by using the denudating agent, and the quartz particles are gradually denuded and dissolved from the surface to the inner part of the particles, the content C of certain impurity elements in the quartz after leaching and purification can be expressed as follows:
in the above formula (1), C0Is the initial average content of the element, n0Δ C is the average content of the element in the dissolved part of the quartz, and Δ n is the amount of the substance in which the quartz is dissolved, as the initial amount of the substance of the quartz.
During the process of denudation and dissolution of the quartz, if the average content of the element in the dissolved part is greater than the initial average content of the quartz, the average content of the element in the quartz after denudation is reduced; if the average content of the dissolved fraction is less than the initial average content of quartz, the average content of the quartz increases after the erosion.
Therefore, in the step of denudation of the surface impurity segregation region, when a certain impurity element in the quartz particles is segregated, but the element is not present on the surface of the quartz particles or the element on the surface of the quartz particles is completely removed, the initial average content of the element in the quartz particles is the content of the element in the matrix of the quartz particles, the content of the segregation region is higher than that of the matrix, and the content of the depletion region is lower than that of the matrix. According to the formula (1), when the surface impurity segregation region is corroded, the concentration of the element in the residual quartz is reduced, the element reaches the lowest value when the segregation region is corroded, when the corrosion is continued to reach a loss region, the concentration of the element in the residual part is increased, when the loss region is completely corroded and dissolved, the concentration of the element in the residual part is the same as that in the matrix again, the quartz is continuously corroded, and the concentration of the element is basically not changed.
By utilizing the phenomenon and the principle and combining the processes of leaching, roasting and denudation (namely the steps of increasing the surface concentration of defects, diffusing and partially aggregating metal impurities in quartz crystal lattices and denudating a surface impurity partially aggregated region), the embodiment of the invention provides a method for preparing ultra-pure quartz.
According to the method, quartz is treated by leaching, surface defects are increased (the defects refer to an incomplete area of a certain crystal face, microscopically refer to missing atoms or crystal cells, macroscopically form states such as corrosion pits, corrosion seams and the like, such as the circled part in figure 6), and the crystal face with the increased surface defects can facilitate roasting to promote impurity elements to diffuse and segregate metal impurities in the quartz crystal lattice. Specifically, as shown in fig. 2 to 6, in order to deeply research the characteristics of reaction with quartz in the leaching process of hydrochloric acid, sodium chloride, hydrofluoric acid and sodium hydroxide, surface morphology analysis of a quartz raw ore and quartz subjected to hydrochloric acid leaching, quartz subjected to hydrochloric acid + sodium chloride leaching, quartz subjected to hydrochloric acid + hydrofluoric acid leaching and quartz subjected to sodium hydroxide leaching and then hydrochloric acid leaching sample is carried out by using a scanning electron microscope, and it is found that after sodium hydroxide leaching, a plurality of pits and erosion seams are formed on quartz particles, compared with hydrofluoric acid, the corrosion pit and the corrosion seam formed by the sodium hydroxide have round shapes, and the inner walls of the corrosion pit and the corrosion seam are more round as can be seen from the local detail image, which shows that the dissolution amount of the sodium hydroxide to quartz on the inner walls of the corrosion pit and the corrosion seam is more than that of the hydrofluoric acid, it can be concluded that sodium hydroxide leaches impurities and inclusions less selectively than hydrofluoric acid, and that leaching in the leaching test is less effective than hydrofluoric acid. That is, leaching with sodium hydroxide can produce an effect of increasing surface defects.
Then, impurity metal elements such as Al element and the like in the quartz are diffused and are partially gathered in the range of several micrometers in the surface of the quartz to form a local partial gathering area through roasting. Finally, the local segregation areas are accurately dissolved by using a stripping agent capable of dissolving quartz, so that the content of each impurity metal element in the quartz is rapidly and remarkably reduced.
The method can extend and diffuse the removal range of impurity metal elements, particularly Al elements, from the surface and a plurality of atomic layers near the surface of the general method to a region which is more than ten microns to more than dozens of microns inside the surface of quartz, namely, the inner boundary of a loss region is reached, so that the content of the impurity metal elements such as Al in the purified quartz is greatly reduced (as shown in figures 2 to 6).
Specifically, the quartz pretreatment step comprises crushing, magnetic separation and screening of quartz.
Specifically, the step of cleaning the surface impurities mainly adopts 1-4 mol/L hydrochloric acid solution to carry out hot-pressing leaching and cleaning on the pretreated quartz. In hot-pressing leaching, the liquid-solid ratio of the hydrochloric acid solution to the quartz particles is (6-10) mL:1g, the leaching temperature is 150-250 ℃, and the leaching time is 1-8 h.
Specifically, the increase in surface defects means an increase in the proportion of an incomplete region of one crystal plane. Wherein, the defect refers to an incomplete area of a certain crystal face, microscopically refers to a missing atom or unit cell, macroscopically forms a state of etching pits, erosion seams and the like. The specific step of increasing the surface defects is to erode quartz particles by adopting 0.2-2 mol/L sodium hydroxide solution, wherein the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is (6-10) mL:1g, the leaching temperature is 150-200 ℃, and the leaching time is 1-8 h. Preferably, in the step, the concentration of the sodium hydroxide solution is 0.6667mol/L, and the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is 6mL:1 g.
Specifically, in the step of diffusion and segregation of the quartz crystal lattice metal impurities, the roasting temperature is 600-1400 ℃, the roasting time is 5-70 hours, and the preferred roasting temperature is 1000 ℃.
Specifically, in the step of denudation of the surface impurity segregation zone, the concentration of a sodium hydroxide solution used is 0.1-0.5 mol/L, the liquid-solid ratio of the sodium hydroxide solution to quartz particles is (2-10) mL:1g, the leaching temperature is 150-200 ℃, and the leaching time is 1-8 h. Preferably, the concentration of the sodium hydroxide solution is 0.3799mol/L, and the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is 6mL:1 g.
For the purpose of describing specific examples of the method for preparing ultra-high purity quartz according to the present invention, specific preparation parameters are shown in Table 1 below, in order to evaluate the influence of each parameter on the final result.
TABLE 1 summary of conditions for the preparation of ultra-pure quartz
In order to evaluate the impurity removal process and the impurity removal effect of the above examples, the removal effect is shown in table 2.
And measuring the concentrations of impurity elements in the original quartz ore and the treated quartz sample by an ICP-MS test method. Weighing 2g of quartz sample, adding 10ml of hydrofluoric acid, fixing the volume to 100ml, dissolving the quartz sample, heating the quartz sample to 200 ℃ by adopting a flat plate, evaporating the redundant hydrofluoric acid until no white smoke is emitted, and measuring the concentration of impurity elements in the quartz. In the raw quartz ore, the aluminum (Al) content was 56.5. mu.g/g, the lithium (Li) content was 12.3. mu.g/g, the sodium (Na) content was 48.1. mu.g/g, the potassium (K) content was 22.9. mu.g/g, the magnesium (Mg) content was 0.52. mu.g/g, the beryllium (Be) content was 0.02. mu.g/g, the calcium (Ca) content was 68.87. mu.g/g, the iron (Fe) content was 26.3. mu.g/g, the titanium (Ti) content was 15.2. mu.g/g, the manganese (Mn) content was 9.62. mu.g/g, the chromium (Cr) content was 0.16. mu.g/g, the nickel (Ni) content was 0.35. mu.g/g and the copper (Cu) content was 5.2. mu.g/g.
The data in Table 2 are the concentrations of the respective impurities after the diffusion-segregation step of the metal impurities of the quartz crystal lattice and after the denudation step of the segregation region of the surface impurities, while the data in comparative example 8 are the final concentrations of the respective impurities in the particles. As can be seen from Table 2:
1. the quartz crystal lattice substituted impurity is one of the most difficult impurities to separate, and the conventional separation method has no effect on removing impurity elements such as Al and the like in the crystal lattice substituted impurity. By adopting the method provided by the invention, through the steps of increasing surface defects, diffusing and partially concentrating metal impurities in quartz crystal lattices and denudating a surface impurity partially-concentrated region, good removing capability is generated on Al and other metal elements of the quartz crystal lattices (for example, examples 1-14 are compared with comparative example 8).
2. Example 6 is compared with examples 3 and 4, its diffusion segregation time is lengthened, degrade the surface impurity segregation area after the diffusion segregation step of the metal impurity of quartz crystal lattice, its impurity content removed reaches 10.1 microgram/g, higher than examples 3 and 4, demonstrate that the diffusion segregation time of metal impurity of quartz crystal lattice in example 6 lengthens, can further strengthen the diffusion segregation effect of metal impurity of quartz crystal lattice, thus facilitate the leaching degradation of subsequent impurity, make finally can greatly remove impurity.
3. Compared with the embodiment, the roasting temperature and the roasting time of the comparative examples 1-2 are unreasonable, so that the impurity diffusion segregation effect is poor, the removal effect of the denudation of the surface impurity segregation region is influenced through the diffusion segregation step of the quartz crystal lattice metal impurities, and the effect is obviously inferior to that of the embodiment. This shows that the impurity diffusion segregation method provided by the invention needs to accurately control the roasting time and the roasting temperature.
4. Compared with the embodiment, the comparative examples 3-7 have the advantages that the surface defect increasing step is not reasonably controlled, the subsequent treatment effects of diffusion segregation of quartz crystal lattice metal impurities and surface impurity segregation region denudation are seriously influenced, the impurity content of quartz particles is still high, the subsequent treatment is not facilitated, and the final impurity removal efficiency is obviously reduced.
In conclusion, the preparation method of the ultra-pure quartz avoids using substances such as hydrofluoric acid, chlorine gas, hydrogen fluoride gas and the like which are not friendly to the environment or have high risk, and is relatively friendly to the environment; and the waste liquid generated in the hydrochloric acid leaching step and the sodium hydroxide leaching step can be mutually neutralized, so that the treatment cost of the quartz industrial wastewater can be greatly reduced. The Al element content in the finally prepared quartz is reduced to 7.8 mu g/g from 56.5 mu g/g, the requirement of IOTA 6 series on the Al content of 8 mu g/g is met, and the total content of impurity elements can be reduced to 38.2 mu g/g which is far higher than the standard requirement of high-purity quartz of 50 mu g/g.
While the invention has been described with reference to specific preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the following claims.
Claims (4)
1. The method for preparing the ultra-pure quartz is characterized by comprising the steps of quartz pretreatment, surface impurity cleaning, surface defect increasing, diffusion segregation of quartz crystal lattice metal impurities and denudation of a surface impurity segregation region which are sequentially carried out;
the method comprises the following steps of performing surface defect increasing, performing diffusion segregation of quartz crystal lattice metal impurities, performing roasting, and performing surface impurity segregation region denudation, wherein the roasting temperature is 600-1400 ℃, and the roasting time is 5-70 h;
in the step of cleaning the surface impurities, 1-4 mol/L hydrochloric acid solution is adopted for hot-pressing leaching and cleaning, the liquid-solid ratio of the hydrochloric acid solution to quartz particles is (6-10) mL:1g, the leaching temperature is 150-250 ℃, and the leaching time is 1-8 h;
in the step of increasing the surface defects, 0.6667mol/L of sodium hydroxide solution is adopted to erode the quartz particles, the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is 6mL:1g, the leaching temperature is 150-200 ℃, and the leaching time is 1-8 h;
in the step of denudation of the surface impurity segregation region, the concentration of a sodium hydroxide solution used is 0.1-0.5 mol/L, the liquid-solid ratio of the sodium hydroxide solution to quartz particles is (2-10) mL:1g, the leaching temperature is 150-200 ℃, and the leaching time is 1-8 h.
2. The method of claim 1, wherein the step of pretreating the quartz comprises crushing, magnetic separation, and sieving the quartz.
3. The method of claim 1, wherein the step of diffusion-biasing the quartz lattice metal impurities comprises firing at 1000 ℃.
4. The method as claimed in claim 1, wherein in the step of denudating the surface impurity segregation region, the concentration of the sodium hydroxide solution is 0.3799mol/L, and the liquid-solid ratio of the sodium hydroxide solution to the quartz particles is 6mL:1 g.
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| JPS62270424A (en) * | 1986-05-15 | 1987-11-24 | Nippon Sekiei Glass Kk | Production of ultra-high purity quartz glass powder |
| CN103539133B (en) * | 2013-11-05 | 2015-07-22 | 武汉理工大学 | Method for preparing ultralow-metallic-element ultrahigh-purity quartz through mixed acid hot-pressing leaching reaction |
| CN105936509A (en) * | 2016-06-01 | 2016-09-14 | 安徽晶晶石英科技有限公司 | Purifying method of ultralow-metal element highly pure quartz |
| CN107827115A (en) * | 2017-09-15 | 2018-03-23 | 江苏闽江矿业有限公司 | A kind of method of purity quartzite |
| CN107626437B (en) * | 2017-09-19 | 2019-11-29 | 江苏凯达石英股份有限公司 | A kind of glass sand preparation method of ultra-low metals content |
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