CN113735128A - Preparation method of high-purity quartz sand - Google Patents
Preparation method of high-purity quartz sand Download PDFInfo
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- CN113735128A CN113735128A CN202110938039.8A CN202110938039A CN113735128A CN 113735128 A CN113735128 A CN 113735128A CN 202110938039 A CN202110938039 A CN 202110938039A CN 113735128 A CN113735128 A CN 113735128A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010453 quartz Substances 0.000 claims abstract description 104
- 238000005188 flotation Methods 0.000 claims abstract description 91
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 80
- 230000000171 quenching effect Effects 0.000 claims abstract description 65
- 238000010791 quenching Methods 0.000 claims abstract description 62
- 239000012141 concentrate Substances 0.000 claims abstract description 59
- 239000002253 acid Substances 0.000 claims abstract description 39
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 31
- 239000011707 mineral Substances 0.000 claims abstract description 31
- 238000000227 grinding Methods 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000007885 magnetic separation Methods 0.000 claims abstract description 15
- 238000002386 leaching Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 210000003462 vein Anatomy 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 6
- 238000001238 wet grinding Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 29
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 150000001450 anions Chemical class 0.000 claims description 20
- 150000001768 cations Chemical class 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 10
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 10
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 10
- 239000010445 mica Substances 0.000 claims description 9
- 229910052618 mica group Inorganic materials 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000007731 hot pressing Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 239000010433 feldspar Substances 0.000 claims description 6
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 5
- 238000007689 inspection Methods 0.000 claims description 5
- 239000006148 magnetic separator Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 85
- 230000008569 process Effects 0.000 description 15
- 230000008859 change Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 10
- 238000000746 purification Methods 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000011362 coarse particle Substances 0.000 description 5
- 238000010494 dissociation reaction Methods 0.000 description 5
- 230000005593 dissociations Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
A preparation method of high-purity quartz sand comprises the following steps: s1, crushing the low-grade vein quartz ore; s2, carrying out color selection on the crushed sample, and selecting different color particles; s3, carrying out wet grinding and grading on the color selection sample; s4, carrying out magnetic separation on the ore grinding sample, and removing magnetic impurities to obtain quartz rough concentrate; s5, roasting the quartz rough concentrate for 1-3 hours at 400-800 ℃, and performing water quenching treatment on the quartz rough concentrate after roasting; s6, reversely floating the quartz rough concentrate for multiple times to remove gangue minerals to obtain a floating concentrate; s7, placing the flotation concentrate and the mixed acid in a high-pressure acid leaching device for reaction to obtain acid-leached quartz; s8, roasting the acid-leached quartz at 800-1200 ℃ for 1-3 h, performing water quenching treatment on the quartz after roasting, and drying to obtain high-purity quartz; and S9, inspecting the high-purity quartz, and screening to remove fine powder. The design can obviously improve the product quality and the added value.
Description
Technical Field
The invention relates to the technical field of quartz processing, in particular to a preparation method of high-purity quartz sand, which is mainly suitable for improving the product quality and the added value of products.
Background
The gangue quartz is an aggregate of silicon dioxide formed by secretion of underground magma, the chemical components are pure, the content of the silicon dioxide is more than 98 percent, and accompanying minerals comprise aluminosilicate minerals such as mica and feldspar, iron-containing minerals, fluorite and the like. At present, the high-tech fields of semiconductors, photovoltaic power generation, communication, electrics and electronics, national defense and military industry and the like in China develop rapidly, high-purity quartz sand is an indispensable key material, and has an important strategic position in the aspect of high-end manufacturing in China, and the refining, upgrading and lean refinement of the production technology of quartz raw materials are indispensable to the continuous development of the high-tech industry in China.
The vein quartz is used as a high-quality raw material for producing high-purity quartz, and various scholars have intensively studied and obtained abundant results, but the vein quartz with low quality can not be effectively purified according to the prior art and the method due to the limitation of the quality of quartz resources. In the existing secondary roasting water quenching purification technology, a purification process of crushing, roasting water quenching, ore grinding, magnetic separation, flotation, acid leaching and secondary roasting water quenching is adopted, the primary roasting water quenching temperature is too high, for low-grade gangue quartz ores, the gangue mineral content is higher, the mineral inclusion content is more, the roasting temperature is too high, the mineral inclusion is re-wrapped by softened quartz and gangue minerals, internal cracks generated by water quenching permeate into impurities in subsequent processing processes of ore grinding, acid leaching and the like, and the impurities are not easy to clean; and the expansion rate of the quartz with too high temperature is reduced, so that the phase change of the quartz sand in the secondary roasting process is inhibited to a certain extent, and the secondary roasting water quenching effect is influenced. And the roasting temperature is too low, so that cracks are insufficient, and therefore, a purification method beneficial to removing gangue minerals is designed, and the quality and the additional value of quartz products are improved.
Disclosure of Invention
The invention aims to overcome the defects and problems of poor product quality and low product added value in the prior art, and provides a preparation method of high-purity quartz sand with good product quality and high product added value.
In order to achieve the above purpose, the technical solution of the invention is as follows: a preparation method of high-purity quartz sand comprises the following steps:
s1, crushing the low-grade vein quartz ore to obtain a crushed sample;
s2, carrying out color sorting on the crushed sample, and selecting different color particles to obtain a color sorting sample;
s3, carrying out wet grinding and grading on the color sorting sample to obtain a grinding sample;
s4, carrying out magnetic separation on the ground ore sample by using a magnetic separator, and removing magnetic impurities to obtain quartz rough concentrate;
s5, placing the quartz rough concentrate into a high-temperature furnace, roasting at low temperature in air atmosphere, wherein the roasting temperature is 400-800 ℃, the roasting time is 1-3 h, and after roasting, taking the quartz rough concentrate out of the high-temperature furnace and directly pouring the quartz rough concentrate into room-temperature deionized water to finish water quenching;
s6, carrying out reverse flotation on the roasted and water-quenched quartz rough concentrate for multiple times to remove gangue minerals, and obtaining flotation concentrate;
s7, placing the flotation concentrate and the mixed acid in a high-pressure acid leaching device for hot-pressing reaction, repeatedly washing the flotation concentrate and the mixed acid until the solution is neutral, filtering and dehydrating the flotation concentrate and the mixed acid, and drying the flotation concentrate and the mixed acid to obtain acid-leached quartz;
s8, firstly, placing the acid-leached quartz into a high-temperature furnace, roasting at the high temperature of 800-1200 ℃ for 1-3 h in the air atmosphere, taking out the quartz from the high-temperature furnace after roasting, directly pouring the quartz into room-temperature deionized water to finish water quenching, washing for many times, and drying at the temperature of 40-110 ℃ to obtain high-purity quartz;
s9, carrying out inspection and screening on the high-purity quartz to remove fine powder with a size fraction less than 0.106 mm.
In step S1, the particle size of the crushed sample is 20mm or less.
In step S3, the grain size of the ore grinding sample is-0.18 mm +0.106 mm.
In the step S4, the magnetic separation intensity of the magnetic separation is 1-1.6T, and the pulse frequency is 100-200 r/min.
In the step S6, 1-2 mol/L sulfuric acid is used as a pH regulator, dodecylamine, octadecylamine, cocoamine or mixed amine is used as a collecting agent, mica is removed through reverse flotation for multiple times under the condition that the pH is 2-3, and then feldspar impurities are removed through reverse flotation for multiple times under the condition that the pH is 1.5-2 by using 1-2 mol/L sulfuric acid as a pH regulator and utilizing a cation and anion mixed collecting agent.
In the step S6, the total usage amount of the collecting agent for removing mica is 100-200 g/t, wherein the usage amount ratio of the collecting agent in the first stage reverse flotation, the second stage reverse flotation, the third stage reverse flotation, the fourth stage reverse flotation, … … and the nth stage reverse flotation is 4:3:2:1: … …: 1.
In step S6, the anion and cation mixed collector includes propylenediamine + sodium dodecylsulfonate, sodium oleate + dodecylamine, octadecylamine + sodium dodecylsulfonate, propylenediamine + sodium petroleum sulfonate, wherein a ratio of the anion collector to the cation collector is 3:1 to 7: 1.
In the step S6, the total using amount of the anion and cation mixed collector is 800-1800 g/t, wherein the using amount ratio of the collector in the first stage reverse flotation, the second stage reverse flotation, the third stage reverse flotation, the fourth stage reverse flotation, … … and the nth stage reverse flotation is 5:5:2:1: … …: 1.
In step S7, the mixed acid includes 1.5-4.5 mol/L hydrochloric acid, 0.5-1.5 mol/L nitric acid, and 0.5-1.5 mol/L hydrofluoric acid.
In the step S7, the flotation concentrate in the ratio of 1: 1-1: 8 and the mixed acid are subjected to hot-pressing reaction for 3-6 hours at the temperature of 150-300 ℃, then deionized water is used for repeatedly washing for 5-10 times until the solution is neutral, then filtration and dehydration are carried out, and finally drying is carried out at the temperature of 40-110 ℃ to obtain acid-leached quartz.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation method of the high-purity quartz sand, the first roasting-water quenching is carried out after ore grinding, because the roasting-water quenching effect of the coarse particles is inferior to that of the roasting-water quenching after the ore grinding, and because the roasting-water quenching of the coarse particles is limited by thermal reaction power, the dissociation of mineral interfaces in the coarse particles is insufficient, and the roasting-water quenching effect cannot be fully exerted; roasting-water quenching is carried out after ore grinding, the particle size is reduced, roasting-water quenching dissociation effects are more sufficient, gangue minerals in particles are exposed due to cracks generated by roasting-water quenching, the floatation action of the gangue minerals and intergrowth is directly influenced, and meanwhile, mineral inclusion in quartz is communicated with the outside, so that subsequent acid leaching removal is facilitated.
2. In the preparation method of the high-purity quartz sand, the first roasting-water quenching adopts low-temperature roasting, part of inclusion can be reserved by controlling the temperature, the vacancy defect of the inclusion cannot be generated, and fine impurities and ionic impurities cannot be adsorbed into the internal vacancy in the subsequent processing process and are not beneficial to washing and removing; meanwhile, the low-temperature roasting with accurate control can generate enough mineral interface cracks to dissociate or expose the gangue minerals, thereby being beneficial to subsequent removal; in addition, the phase change influence process of the precisely controlled low-temperature roasting on the second roasting process of the quartz is very small, so that the secondary roasting-water quenching can fully play a role.
3. In the preparation method of the high-purity quartz sand, the acid leaching is carried out on the flotation concentrate by adopting the mixed acid solution in the acid leaching process, so that gangue minerals can be effectively removed; the second roasting-water quenching adopts high-temperature roasting, so that a large amount of inclusion can be removed, the impurity content is reduced, the purity is improved, the additional value is increased, and more heat required in the secondary roasting process can be met. Therefore, the invention improves the product quality and the added value of the product.
Drawings
FIG. 1 is a flow chart of a method for preparing high purity silica sand according to the present invention.
In FIG. 1, +0.18mm means that particles having a size fraction of 0.18mm or more were returned to the mill and reground, particles having a size fraction of-0.18 mm +0.106mm were the test samples, and particles having a size fraction of-0.106 mm were undersized as by-products.
FIG. 2 is a TG-DSC graph of a vein quartz sample.
Detailed Description
The present invention will be described in further detail with reference to the following description and embodiments in conjunction with the accompanying drawings.
Referring to fig. 1, a method for preparing high-purity quartz sand includes the following steps:
s1, crushing the low-grade vein quartz ore to obtain a crushed sample;
s2, carrying out color sorting on the crushed sample, and selecting different color particles to obtain a color sorting sample;
s3, carrying out wet grinding and grading on the color sorting sample to obtain a grinding sample;
s4, carrying out magnetic separation on the ground ore sample by using a magnetic separator, and removing magnetic impurities to obtain quartz rough concentrate;
s5, placing the quartz rough concentrate into a high-temperature furnace, roasting at low temperature in air atmosphere, wherein the roasting temperature is 400-800 ℃, the roasting time is 1-3 h, and after roasting, taking the quartz rough concentrate out of the high-temperature furnace and directly pouring the quartz rough concentrate into room-temperature deionized water to finish water quenching;
s6, carrying out reverse flotation on the roasted and water-quenched quartz rough concentrate for multiple times to remove gangue minerals, and obtaining flotation concentrate;
s7, placing the flotation concentrate and the mixed acid in a high-pressure acid leaching device for hot-pressing reaction, repeatedly washing the flotation concentrate and the mixed acid until the solution is neutral, filtering and dehydrating the flotation concentrate and the mixed acid, and drying the flotation concentrate and the mixed acid to obtain acid-leached quartz;
s8, firstly, placing the acid-leached quartz into a high-temperature furnace, roasting at the high temperature of 800-1200 ℃ for 1-3 h in the air atmosphere, taking out the quartz from the high-temperature furnace after roasting, directly pouring the quartz into room-temperature deionized water to finish water quenching, washing for many times, and drying at the temperature of 40-110 ℃ to obtain high-purity quartz;
s9, carrying out inspection and screening on the high-purity quartz to remove fine powder with a size fraction less than 0.106 mm.
In step S1, the particle size of the crushed sample is 20mm or less.
In step S3, the grain size of the ore grinding sample is-0.18 mm +0.106 mm.
In the step S4, the magnetic separation intensity of the magnetic separation is 1-1.6T, and the pulse frequency is 100-200 r/min.
In the step S6, 1-2 mol/L sulfuric acid is used as a pH regulator, dodecylamine, octadecylamine, cocoamine or mixed amine is used as a collecting agent, mica is removed through reverse flotation for multiple times under the condition that the pH is 2-3, and then feldspar impurities are removed through reverse flotation for multiple times under the condition that the pH is 1.5-2 by using 1-2 mol/L sulfuric acid as a pH regulator and utilizing a cation and anion mixed collecting agent.
In the step S6, the total usage amount of the collecting agent for removing mica is 100-200 g/t, wherein the usage amount ratio of the collecting agent in the first stage reverse flotation, the second stage reverse flotation, the third stage reverse flotation, the fourth stage reverse flotation, … … and the nth stage reverse flotation is 4:3:2:1: … …: 1.
In step S6, the anion and cation mixed collector includes propylenediamine + sodium dodecylsulfonate, sodium oleate + dodecylamine, octadecylamine + sodium dodecylsulfonate, propylenediamine + sodium petroleum sulfonate, wherein a ratio of the anion collector to the cation collector is 3:1 to 7: 1.
In the step S6, the total using amount of the anion and cation mixed collector is 800-1800 g/t, wherein the using amount ratio of the collector in the first stage reverse flotation, the second stage reverse flotation, the third stage reverse flotation, the fourth stage reverse flotation, … … and the nth stage reverse flotation is 5:5:2:1: … …: 1.
In step S7, the mixed acid includes 1.5-4.5 mol/L hydrochloric acid, 0.5-1.5 mol/L nitric acid, and 0.5-1.5 mol/L hydrofluoric acid.
In the step S7, the flotation concentrate in the ratio of 1: 1-1: 8 and the mixed acid are subjected to hot-pressing reaction for 3-6 hours at the temperature of 150-300 ℃, then deionized water is used for repeatedly washing for 5-10 times until the solution is neutral, then filtration and dehydration are carried out, and finally drying is carried out at the temperature of 40-110 ℃ to obtain acid-leached quartz.
The principle of the invention is illustrated as follows:
in the process of quartz purification, roasting-water quenching utilizes the difference of phase change and expansion rate of quartz and gangue minerals in the heating-cooling process, so that cracks are generated between interfaces of the quartz and the gangue minerals. In the prior art, gas-liquid inclusions can be removed by high-temperature roasting and water quenching before impurity removal, and generated inclusion vacancies are soaked and adsorbed with fine particles and ionic impurities in the subsequent processing process, so that the inclusions are not easy to remove by washing, and the product quality is low. In addition, the prior art does not consider that when the first firing temperature is too high, the quartz may be overheated to soften and re-encapsulate the internal gangue minerals and inclusions.
The position of roasting water quenching has important influence on the purification of quartz in the purification process of quartz, the influence of the roasting water quenching on ore grinding is mainly considered in the prior art, the influence of the roasting water quenching on ore dressing purification is neglected, and the gain effects of the roasting water quenching and the ore dressing purification are not compared. The roasting water quenching is limited by the thermal reaction power of the coarse particles before ore grinding, the dissociation of mineral interfaces in the coarse particles is insufficient, and the gain effect of the roasting water quenching cannot be fully exerted after the ore grinding. And roasting water quenching is carried out after ore grinding, the particle size is reduced, the roasting water quenching dissociation effect is more sufficient, the gangue minerals inside the particles are exposed due to cracks generated by roasting water quenching, the flotation behavior of the gangue minerals and the intergrowth is directly influenced, and meanwhile, the mineral inclusion inside quartz is communicated with the outside, so that the subsequent acid leaching removal is facilitated, and the requirement of the subsequent process for effective ore dressing purification can be better met. As shown in fig. 2, the quartz is subjected to phase transition at 572.1 ℃ and 862.5 ℃, due to the difference between the phase transition temperature and the expansion rate of the quartz and the gangue minerals, cracks are generated between the quartz and the gangue mineral interface by controlling the temperature, so that the monomer dissociation of the quartz and the gangue minerals is facilitated in the ore grinding process, and the generated cracks are beneficial to enabling mixed acid to enter the quartz through the cracks in the acid leaching process so as to achieve the purpose of removing impurities in the quartz. Therefore, the first roasting-water quenching adopts low temperature to be beneficial to subsequent acid leaching. The energy absorbed by the quartz sand in phase change during heating is larger than the heat released in phase change during cooling, and more energy is needed during the phase change of the roasted quartz sand. The first roasting-water quenching adopts relatively low temperature, and the second roasting-water quenching adopts relatively high temperature, so that the condition that the roasted quartz sand phase change needs more energy can be better met, and the influence of the first roasting-water quenching on the second roasting-water quenching is very small. In addition, the expansion rate of the quartz sand is increased along with the rise of the temperature in the heating process, the expansion rate of the roasted quartz sand is obviously lower than that of new sand, the first roasting adopts relatively low temperature, the temperature of the second phase change of the quartz is not reached, and the influence on the phase change and the expansion rate of the relatively high temperature in the second roasting is very small.
The second roasting adopts relatively high temperature, the change in the crystal is violent, the fluid inclusion can be broken, and the gangue mineral monomer is dissociated; in the process of secondary roasting-water quenching, the primary roasting-water quenching is respectively carried out at 400 ℃, 600 ℃ and 800 ℃, the secondary roasting-water quenching is carried out at 1000 ℃, and the lowest Al and Fe elements are 216.16 mu g/g and 3.73 mu g/g respectively when the primary roasting temperature is 600 ℃, and are lower than the quartz concentrate obtained by purification through the primary roasting-water quenching process flow, so that the additional value of the quartz concentrate is further improved. Because the roasted quartz sand needs more energy, if the same temperature or lower temperature is adopted, the higher energy required by the phase change of the roasted quartz sand is difficult to meet, the second roasting-water quenching adopts relatively high temperature which is far higher than the temperature generated by the phase change of the first relatively low-temperature roasting water quenching and is also higher than the temperature generated by the second phase change of the quartz, and the higher energy required by the phase change of the roasted quartz sand can be met.
Example 1:
referring to fig. 1, a method for preparing high-purity quartz sand includes the following steps:
s1, crushing low-grade vein quartz ore (from some places in Gansu province, wherein the content of silicon dioxide is 98.96 percent) to obtain a crushed sample, wherein the particle size of the crushed sample is less than or equal to 20 mm;
s2, carrying out color sorting on the crushed sample, and selecting different color particles to obtain a color sorting sample;
s3, carrying out wet grinding classification on the color sorting sample to obtain a grinding sample, wherein the grain size of the grinding sample is-0.18 mm +0.106 mm;
s4, performing magnetic separation on the ground ore sample by using a magnetic separator, wherein the magnetic separation strength is 1-1.6T, the pulse frequency is 100-200 r/min, removing magnetic impurities to obtain quartz rough concentrate, and drying at 40-110 ℃ to prepare a sample;
s5, placing the quartz rough concentrate into a high-temperature furnace, roasting at low temperature in air atmosphere, wherein the roasting temperature is 400 ℃, the roasting time is 1-3 h, and after the roasting is finished, taking the quartz rough concentrate out of the high-temperature furnace and directly pouring the quartz rough concentrate into room-temperature deionized water to finish water quenching;
s6, carrying out reverse flotation on the roasted and water-quenched quartz rough concentrate for multiple times to remove gangue minerals, and obtaining flotation concentrate;
firstly, 1-2 mol/L sulfuric acid is used as a pH regulator, dodecylamine, octadecylamine, cocoamine or mixed amine is used as a collecting agent, mica is removed by reverse flotation for many times under the condition that the pH is 2-3, and the total using amount of the adopted collecting agent is 100-200 g/t, wherein the using amount ratio of the collecting agent in the first-stage reverse flotation, the second-stage reverse flotation, the third-stage reverse flotation, the fourth-stage reverse flotation, … … and the nth reverse flotation is 4:3:2:1: … …:1 (1 is used after the third stage); then, 1-2 mol/L sulfuric acid is used as a pH regulator, and a cation and anion mixed collector is utilized to remove feldspar impurities through reverse flotation for multiple times under the condition that the pH is 1.5-2, wherein the cation and anion mixed collector comprises propylene diamine + sodium dodecyl sulfate, sodium oleate + dodecylamine, octadecylamine + sodium dodecyl sulfate, propylenediamine + petroleum sodium sulfonate, the ratio of the anion collector to the cation collector is 3: 1-7: 1, the total dosage of the cation and anion mixed collector is 800-1800 g/t, and the dosage ratio of the collector for the first-stage reverse flotation, the second-stage reverse flotation, the third-stage reverse flotation, the fourth-stage reverse flotation, … … and the nth-stage reverse flotation is 5:5:2:1: … …:1 (all the collector after the third stage is 1);
s7, placing the flotation concentrate and the mixed acid in a ratio of 1: 1-1: 8 in a high-pressure acid leaching device, carrying out hot-pressing reaction for 3-6 h at the temperature of 150-300 ℃, repeatedly washing for 5-10 times by using deionized water until the solution is neutral, filtering and dehydrating, and drying at the temperature of 40-110 ℃ to obtain acid-leached quartz; the mixed acid comprises 1.5-4.5 mol/L hydrochloric acid, 0.5-1.5 mol/L nitric acid and 0.5-1.5 mol/L hydrofluoric acid;
s8, firstly, placing the acid-leached quartz into a high-temperature furnace, roasting at the high temperature of 800 ℃ for 1-3 h in the air atmosphere, taking out the quartz from the high-temperature furnace after roasting is finished, directly pouring the quartz into room-temperature deionized water to finish water quenching, washing for many times, and drying at the temperature of 40-110 ℃ to obtain high-purity quartz;
s9, carrying out inspection and screening on the high-purity quartz to remove fine powder with a size fraction less than 0.106 mm.
The purity of the high-purity quartz is more than 99.95 percent by ICP detection.
Example 2:
the basic contents are the same as example 1, except that:
in step S8, the baking temperature was 1000 ℃.
Example 3:
the basic contents are the same as example 1, except that:
in step S8, the baking temperature was 1200 ℃.
Example 4:
the basic contents are the same as example 1, except that:
in step S5, the baking temperature was 600 ℃.
Example 5:
the basic contents are the same as example 1, except that:
in step S5, the roasting temperature is 600 ℃; in step S8, the baking temperature was 1000 ℃.
Example 6:
the basic contents are the same as example 1, except that:
in step S5, the roasting temperature is 600 ℃; in step S8, the baking temperature was 1200 ℃.
Example 7:
the basic contents are the same as example 1, except that:
in step S5, the baking temperature was 800 ℃.
Example 8:
the basic contents are the same as example 1, except that:
in step S5, the roasting temperature is 800 ℃; in step S8, the baking temperature was 1000 ℃.
Example 9:
the basic contents are the same as example 1, except that:
in step S5, the roasting temperature is 800 ℃; in step S8, the baking temperature was 1200 ℃.
The calcination-water quenching in step S5 was carried out at 400 ℃ and 600 ℃ respectively, and the calcination-water quenching in step S8 was carried out at 800 ℃ respectively, the results of which are shown in Table 1.
TABLE 1 Al and Fe contents (μ g/g) of the final concentrate of double roasting-Water quenching
The calcination and water quenching in step S5 were carried out at 400 deg.C, 600 deg.C and 800 deg.C, respectively, and the calcination and water quenching in step S8 were carried out at 1000 deg.C, the results of which are shown in Table 2.
TABLE 2 Al and Fe contents (μ g/g) of the final concentrate of double roasting-Water quenching
The calcination and water quenching in step S5 were carried out at 400 ℃ and 600 ℃ respectively, and the calcination and water quenching in step S8 were carried out at 1200 ℃ respectively, and the results are shown in Table 3.
TABLE 3 Al and Fe contents (μ g/g) of the final concentrate of double roasting-Water quenching
Example 10:
a preparation method of high-purity quartz sand comprises the following steps:
s1, crushing low-grade vein quartz ore (from some places in Gansu province, wherein the content of silicon dioxide is 98.96 percent) to obtain a crushed sample, wherein the particle size of the crushed sample is less than or equal to 20 mm;
s2, carrying out color sorting on the crushed sample, and selecting different color particles to obtain a color sorting sample;
s3, placing the color selection sample into a high-temperature furnace, roasting at low temperature in air atmosphere, wherein the roasting temperature is 600 ℃, the roasting time is 1-3 h, and after the roasting is finished, taking out the quartz rough concentrate from the high-temperature furnace and directly pouring the quartz rough concentrate into room-temperature deionized water to finish water quenching;
s4, carrying out wet grinding classification on the water quenching sample to obtain an ore grinding sample, wherein the grain diameter of the ore grinding sample is-0.18 mm +0.106 mm;
s5, performing magnetic separation on the ground ore sample by using a magnetic separator, wherein the magnetic separation strength is 1-1.6T, the pulse frequency is 100-200 r/min, removing magnetic impurities to obtain quartz rough concentrate, and drying at 40-110 ℃ to prepare a sample;
s6, carrying out reverse flotation on the roasted and water-quenched quartz rough concentrate for multiple times to remove gangue minerals, and obtaining flotation concentrate;
firstly, 1-2 mol/L sulfuric acid is used as a pH regulator, dodecylamine, octadecylamine, cocoamine or mixed amine is used as a collecting agent, mica is removed by reverse flotation for many times under the condition that the pH is 2-3, and the total using amount of the adopted collecting agent is 100-200 g/t, wherein the using amount ratio of the collecting agent in the first-stage reverse flotation, the second-stage reverse flotation, the third-stage reverse flotation, the fourth-stage reverse flotation, … … and the nth reverse flotation is 4:3:2:1: … …:1 (1 is used after the third stage); then, 1-2 mol/L sulfuric acid is used as a pH regulator, and a cation and anion mixed collector is utilized to remove feldspar impurities through reverse flotation for multiple times under the condition that the pH is 1.5-2, wherein the cation and anion mixed collector comprises propylene diamine + sodium dodecyl sulfate, sodium oleate + dodecylamine, octadecylamine + sodium dodecyl sulfate, propylenediamine + petroleum sodium sulfonate, the ratio of the anion collector to the cation collector is 3: 1-7: 1, the total dosage of the cation and anion mixed collector is 800-1800 g/t, and the dosage ratio of the collector for the first-stage reverse flotation, the second-stage reverse flotation, the third-stage reverse flotation, the fourth-stage reverse flotation, … … and the nth-stage reverse flotation is 5:5:2:1: … …:1 (all the collector after the third stage is 1);
s7, placing the flotation concentrate and the mixed acid in a ratio of 1: 1-1: 8 in a high-pressure acid leaching device, carrying out hot-pressing reaction for 3-6 h at the temperature of 150-300 ℃, repeatedly washing for 5-10 times by using deionized water until the solution is neutral, filtering and dehydrating, and drying at the temperature of 40-110 ℃ to obtain acid-leached quartz; the mixed acid comprises 1.5-4.5 mol/L hydrochloric acid, 0.5-1.5 mol/L nitric acid and 0.5-1.5 mol/L hydrofluoric acid;
s8, firstly, placing the acid-leached quartz into a high-temperature furnace, roasting at high temperature in air atmosphere, wherein the roasting temperature is 1000 ℃, the roasting time is 1-3 h, after the roasting is finished, taking out the quartz from the high-temperature furnace, directly pouring the quartz into deionized water at room temperature to finish water quenching, washing for many times, and drying at 40-110 ℃ to obtain high-purity quartz;
s9, carrying out inspection and screening on the high-purity quartz to remove fine powder with a size fraction less than 0.106 mm.
In this example, the first roasting-water quenching was performed before the grinding, and the results are shown in Table 4, where 600 ℃ was used for the first roasting-water quenching and 1000 ℃ was used for the second roasting-water quenching.
TABLE 4 Al and Fe contents (μ g/g) of the final concentrate of double roasting-Water quenching
Claims (10)
1. The preparation method of the high-purity quartz sand is characterized by comprising the following steps of:
s1, crushing the low-grade vein quartz ore to obtain a crushed sample;
s2, carrying out color sorting on the crushed sample, and selecting different color particles to obtain a color sorting sample;
s3, carrying out wet grinding and grading on the color sorting sample to obtain a grinding sample;
s4, carrying out magnetic separation on the ground ore sample by using a magnetic separator, and removing magnetic impurities to obtain quartz rough concentrate;
s5, placing the quartz rough concentrate into a high-temperature furnace, roasting at low temperature in air atmosphere, wherein the roasting temperature is 400-800 ℃, the roasting time is 1-3 h, and after roasting, taking the quartz rough concentrate out of the high-temperature furnace and directly pouring the quartz rough concentrate into room-temperature deionized water to finish water quenching;
s6, carrying out reverse flotation on the roasted and water-quenched quartz rough concentrate for multiple times to remove gangue minerals, and obtaining flotation concentrate;
s7, placing the flotation concentrate and the mixed acid in a high-pressure acid leaching device for hot-pressing reaction, repeatedly washing the flotation concentrate and the mixed acid until the solution is neutral, filtering and dehydrating the flotation concentrate and the mixed acid, and drying the flotation concentrate and the mixed acid to obtain acid-leached quartz;
s8, firstly, placing the acid-leached quartz into a high-temperature furnace, roasting at the high temperature of 800-1200 ℃ for 1-3 h in the air atmosphere, taking out the quartz from the high-temperature furnace after roasting, directly pouring the quartz into room-temperature deionized water to finish water quenching, washing for many times, and drying at the temperature of 40-110 ℃ to obtain high-purity quartz;
s9, carrying out inspection and screening on the high-purity quartz to remove fine powder with a size fraction less than 0.106 mm.
2. The method for preparing high purity quartz sand according to claim 1, wherein: in step S1, the particle size of the crushed sample is 20mm or less.
3. The method for preparing high purity quartz sand according to claim 1, wherein: in step S3, the grain size of the ore grinding sample is-0.18 mm +0.106 mm.
4. The method for preparing high purity quartz sand according to claim 1, wherein: in the step S4, the magnetic separation intensity of the magnetic separation is 1-1.6T, and the pulse frequency is 100-200 r/min.
5. The method for preparing high purity quartz sand according to claim 1, wherein: in the step S6, 1-2 mol/L sulfuric acid is used as a pH regulator, dodecylamine, octadecylamine, cocoamine or mixed amine is used as a collecting agent, mica is removed through reverse flotation for multiple times under the condition that the pH is 2-3, and then feldspar impurities are removed through reverse flotation for multiple times under the condition that the pH is 1.5-2 by using 1-2 mol/L sulfuric acid as a pH regulator and utilizing a cation and anion mixed collecting agent.
6. The method for preparing high purity quartz sand according to claim 5, wherein: in step S6, the total usage amount of the collecting agent for removing mica is 100-200 g/t, wherein the usage amount ratio of the collecting agent in the first stage reverse flotation, the second stage reverse flotation, the third stage reverse flotation, the fourth stage reverse flotation, and the nth stage reverse flotation is 4:3:2: 1.
7. The method for preparing high purity quartz sand according to claim 5, wherein: in step S6, the anion and cation mixed collector includes propylenediamine + sodium dodecylsulfonate, sodium oleate + dodecylamine, octadecylamine + sodium dodecylsulfonate, propylenediamine + sodium petroleum sulfonate, wherein a ratio of the anion collector to the cation collector is 3:1 to 7: 1.
8. The method for preparing high purity quartz sand according to claim 7, wherein: in step S6, the total usage amount of the anion and cation mixed collector is 800-1800 g/t, wherein the usage amount ratio of the collector in the first stage reverse flotation, the second stage reverse flotation, the third stage reverse flotation, the fourth stage reverse flotation, and the nth stage reverse flotation is 5:5:2: 1.
9. The method for preparing high purity quartz sand according to claim 1, wherein: in step S7, the mixed acid includes 1.5-4.5 mol/L hydrochloric acid, 0.5-1.5 mol/L nitric acid, and 0.5-1.5 mol/L hydrofluoric acid.
10. The method for preparing high purity quartz sand according to claim 9, wherein: in the step S7, the flotation concentrate in the ratio of 1: 1-1: 8 and the mixed acid are subjected to hot-pressing reaction for 3-6 hours at the temperature of 150-300 ℃, then deionized water is used for repeatedly washing for 5-10 times until the solution is neutral, then filtration and dehydration are carried out, and finally drying is carried out at the temperature of 40-110 ℃ to obtain acid-leached quartz.
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