CN113182051A - Preparation method of pomegranate seed-shaped high-purity quartz grinding medium for high-purity silicon micropowder mill - Google Patents
Preparation method of pomegranate seed-shaped high-purity quartz grinding medium for high-purity silicon micropowder mill Download PDFInfo
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- CN113182051A CN113182051A CN202110446089.4A CN202110446089A CN113182051A CN 113182051 A CN113182051 A CN 113182051A CN 202110446089 A CN202110446089 A CN 202110446089A CN 113182051 A CN113182051 A CN 113182051A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C21/00—Disintegrating plant with or without drying of the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
- B02C23/10—Separating or sorting of material, associated with crushing or disintegrating with separator arranged in discharge path of crushing or disintegrating zone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
- B02C23/14—Separating or sorting of material, associated with crushing or disintegrating with more than one separator
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Abstract
The invention relates to a preparation method of a pomegranate seed-shaped high-purity quartz grinding medium for a high-purity silicon micropowder mill, which is characterized by comprising the following steps of: (1) the vein quartz ore with a compact block structure is selected as a raw material, and the chemical composition requirements are as follows: SiO 22≥99.80%，Al2O3≤0.010%，Fe2O3Less than or equal to 0.0020 percent; the maximum block size is controlled to be 350 mm; (2) three-stage crushing is adopted, firstly, a jaw crusher is adopted, and the ore discharge opening is controlled to be 70 mm; secondly, a cone crusher is adopted, and the ore discharge port is controlled to be 25 mm; finally, a cone crusher is adopted, and the ore discharge port is controlled to be 10 mm; (3) screening the crushed material in the second stage to obtain 20-30 mm and 10-20 mm grain-size grinding media; screening the material crushed in the third section to prepare 5-10 mm and 3-5 mm grain size grinding media; (4) shaping with wet stirring mill while controlling the pictographic coefficient to be not less than 06; (5) and screening fine crushed aggregates and removing foreign matters by using a vibrating screen. Has the advantages that: the pomegranate seeds have the shape, the bulk density is more than or equal to 2.0, and the ore grinding efficiency is high; the grinding medium has high purity: SiO 22≥99.95%，Al2O3≤0.0050%，Fe2O3Less than or equal to 0.0010 percent, and can solve the pollution problem caused by ore grinding.
Description
Technical Field
The invention belongs to the field of deep processing of nonmetallic minerals, and relates to a preparation method of a pomegranate seed-shaped high-purity quartz grinding medium for a high-purity silicon micropowder mill.
Background
With the rapid development of the electronic industry, especially the strict requirements of 5G communication chips, the development of electronic devices is moving to high frequency, high speed, high power density and light weight, and a large amount of packaging materials are required for the corresponding IC/EMC (epoxy film plastic) plastic package, CCL (copper clad laminate) manufacturing and the like. Because of its excellent insulating property, chemical resistance and high adhesive strength, the resin is widely used in the above-mentioned electronic insulating materials, but its pure resin has high price, large thermal expansion coefficient, poor mechanical strength and poor single use effect. The inorganic filler is added to improve the mechanical strength and the thermal stability of the resin insulation composite material, and the reduction of the dielectric constant, the dielectric loss and the cost is the inevitable choice. The high-purity superfine silica powder filler is a preferred solution meeting the requirements, and the high purity refers to the chemical components of the silica powder filler: SiO 22≥99.90%，Al2O3≤0.0030%（30ppm），Fe2O3Less than or equal to 0.0010 percent (10 ppm); superfine refers to the grain size composition: d50≤5μm，D100≤20μm。
In order to meet the fineness requirement of high-purity silicon micropowder and achieve certain large-scale production, wet stirring milling or ball milling classification technology is generally adopted for production, and because quartz has high hardness (Mohs hardness of 7), at present, powder processing enterprises generally select zirconia or alumina as a milling medium, but in the long-time ore milling process, the milling medium is abraded to bring doping pollution to materials.
In order to solve the problem, the conventional scheme improves the quality of the zirconia grinding medium as much as possible and reduces the abrasion in unit time; on the other hand, the fineness of the grinding materials is reduced as much as possible, and the total pollution is reduced by a method of reducing the ore grinding time. However, in the actual production of ultrafine silicon powder, grinding for obtaining ultrafine silicon powder causes contamination of the silicon powder by the grinding medium, which affects the purity of the silicon powder, and results in defective products. Such as zirconia grinding medium (phi 3-phi 5mm, ZrO)2Not less than 95%) in the ore grinding process for 3h, considering the weight ratio of ore medium as 1: 7, SiO2The reduction from 99.94% to 99.62%, the increase in Zr from 1ppm to 0.21%, and the average abrasion of 0.012%/h resulted in the final silicon powder having unsatisfactory chemical quality.
Disclosure of Invention
The invention aims to solve the problem that the purity of the silicon micropowder is seriously influenced by pollution caused by grinding by adopting grinding media such as zirconia and the like in the existing production of the high-purity silicon micropowder, and provides a preparation method of pomegranate seed-shaped high-purity quartz grinding media for high-purity silicon micropowder grinding. The invention adopts vein quartz ore to control the granularity composition through crushing and screening, adopts reshaping and impurity removal to control the shape and purity of the vein quartz ore, prepares the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill, and can effectively solve the pollution problem caused by grinding by adopting grinding media such as zirconia and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of pomegranate seed-shaped high-purity quartz grinding media for high-purity silicon micropowder mill is characterized by comprising the following steps:
(1) selecting raw materials: selecting vein quartz ore with a compact block structure as a raw material, and controlling the quality standard as follows: transformingChemical components: SiO 22≥99.80%，Al2O3≤0.010%，Fe2O3Less than or equal to 0.0020 percent; the maximum block size is controlled to be 350 mm;
(2) crushing: a three-section crushing process is adopted, a jaw crusher is adopted in the first section, and the ore discharge opening (e 1) is controlled to be 70 mm; the second section adopts a cone crusher, and the ore discharge opening (e 2) is controlled to be 25 mm; the third section adopts a cone crusher, and the ore discharge port (e 3) is controlled by 10 mm; ensuring that the crushed quartz blocks are polygonal by using the crushing motion track of the cone crusher;
(3) screening and grading: screening and grading (can be carried out according to needs) in the material crushed in the second stage to prepare 20-30 mm and 10-20 mm grain-size grinding media; the crushed material in the third stage is screened and classified to prepare grinding media with particle sizes of 5-10 mm and 3-5 mm (the classification particle size in actual production can be adjusted according to needs);
(4) and shaping: shaping by a wet stirring mill, and grinding off false particles such as sharp corners and intergrowths of the particles to enable the vein quartz particles to be in a pomegranate seed shape, wherein the pictographic coefficient is more than or equal to 0.6;
(5) removing impurities: the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill is prepared by screening fine crushed materials by using a vibrating screen and removing impurities and foreign matters (dark, black and wampee-dyed impurity minerals) and the like in the grinding medium.
Further, the step (4) is shaped into a step of autogenous grinding for 16-26h in a stirring mill, and the weight ratio of materials to water is 1: 1.
Further, impurity minerals in the grinding medium are removed by adopting an acid pickling or color sorting process in the impurity removal step (5), so that the quality of the grinding medium is improved.
Further, the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill comprises the following quality standards: chemical components: SiO 22≥99.95%，Al2O3≤0.0050%，Fe2O3Less than or equal to 0.0010 percent; the pictographic coefficient is more than or equal to 0.6, and the bulk density is more than or equal to 2.0 (see figure 2).
Furthermore, the crushed material with the particle size of minus 3mm generated in the process is used as a raw material for preparing high-purity quartz sand or silicon micropowder, so that comprehensive utilization is realized.
The invention achieves the goal by controlling the following three aspects: (1) selecting compact blocky vein quartz ore with quality meeting the requirement; (2) controlling the shape of grinding medium particles into a polygon through the combined crushing of a jaw crusher and two sections of cone crushers; (3) stirring, grinding and self-grinding for shaping to form the shape of pomegranate seeds and close packing, and finally obtaining the final product through screening, grading and impurity removal processes.
The invention has the beneficial effects that: the grinding medium prepared by the invention has pomegranate seed shape, higher bulk density (more than or equal to 2.0) and high purity (SiO)2≥99.95%，Al2O3≤0.0050%，Fe2O3Less than or equal to 0.0010 percent), and the ore grinding efficiency is higher; replaces the prior zirconia or alumina grinding media, solves the pollution problem in the superfine silicon powder grinding process by high-purity autogenous grinding, and plays a key role in ensuring the product quality.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a pomegranate seed-shaped high-purity quartz grinding medium for a high-purity silicon micropowder mill;
FIG. 2 is a diagram of a process for preparing a quartz grinding medium according to the present invention.
Detailed description of the preferred embodiments
Referring to fig. 1, the invention is described in detail, and a method for preparing a pomegranate seed-shaped high-purity quartz grinding medium for high-purity silicon micropowder mill comprises the following specific implementation steps:
example 1
1. Raw materials: selecting compact (no dissociation, no micro-crack, compact structure) blocky vein quartz ore (SiO)2 99.85%，Al2O3 0.0087%，Fe2O30.0015%), white overall, greasy gloss on the cross section, maximum lumpiness: dmax =350mm, and a small amount (less than or equal to 5%) of wampee and iron dip-dyed materials are arranged on the surface;
2. crushing: the ore feeding amount is 40t/h, and the operation is 6.5h every day; the first stage of crushing is performed by adopting a JC0850 jaw crusher of Nanchang mining machinery Limited, and the ore discharge opening e1 is controlled to be 70 mm; the secondary crushing adopts a Sandvik CS420 single-cylinder hydraulic cone crusher, and the ore discharge opening e2 is controlled to be 25 mm; the three-section crushing adopts a Sandvik CH420 hydraulic cone crusher, and the ore discharge opening e3 is controlled to be 10 mm;
3. screening and grading: screening and grading 40% of the two-stage crushed material, wherein a vibrating screen is a 2ZKR1437H double-layer screen (screen hole 20/10 mm) of Nanchang mine machinery limited company, and 20-30 mm and 10-20 mm grain-size grinding media are prepared; sieving and grading the three-section crushed materials by a 2ZKR1645H double-layer sieve (sieve holes 5/3 mm) to prepare 5-10 mm and 3-5 mm grade grinding media;
4. shaping: stirring and grinding by adopting a 2000L wet method (1200 kg of grinding medium with the diameter of 5-10 mm and 1200L of water), wherein the self-grinding and shaping time is 24h, and grinding off false particles such as particle sharp corners, intergrowth and the like to enable vein quartz particles to be in a pomegranate seed shape, wherein the pictographic coefficient is more than or equal to 0.65;
5. removing impurities: 2ZKR1022 double-layer vibrating screen (5/3 mm screen hole) is adopted to separate crushed ore and the like in the shaping process; respectively obtaining 5-10 mm and 3-5 mm grinding media; -3mm crushed ore is comprehensively utilized;
6. color selection: the method comprises the steps of removing individual heterochromatic impurity minerals in grinding media of 5-10 mm and 3-5 mm by adopting an LKD1920-1K ore color sorter of Zhongke photoelectric color sorting machinery, Inc., and obtaining the high-purity quartz grinding media.
Example 2
1. Raw materials: selecting compact lump vein quartz ore (SiO)2 99.90%，Al2O3 0.0067%，Fe2O30.0010%), white overall, greasy gloss on the cross section, maximum lumpiness: dmax =380mm, and a small amount (less than or equal to 5%) of wampee and iron dip-dyed materials are arranged on the surface;
2. crushing: the ore feeding amount is 40t/h, and the operation is 6.5h every day; the first stage of crushing is performed by adopting a JC0850 jaw crusher of Nanchang mining machinery Limited, and the ore discharge opening e1 is controlled to be 75 mm; the secondary crushing adopts a Sandvik CS420 single-cylinder hydraulic cone crusher, and the ore discharge opening e2 is controlled to be 25 mm; the three-section crushing adopts a Sandvik CH420 hydraulic cone crusher, and the ore discharge opening e3 is controlled to be 10 mm;
3. screening and grading: screening and grading 60% of the two-stage crushed material, wherein a vibrating screen is a 2ZKR1437H double-layer screen (screen hole 20/10 mm) of Nanchang mine machinery limited company, and 20-30 mm and 10-20 mm grain-size grinding media are prepared; sieving and grading the three-section crushed materials by a 2ZKR1645H double-layer sieve (sieve holes 5/3 mm) to prepare 5-10 mm and 3-5 mm grade grinding media;
4. shaping: stirring and grinding by adopting a 5000L wet method (3000 kg of grinding medium with the diameter of 20-30 mm and 3000L of water), wherein the self-grinding and shaping time is 18h, and grinding off false particles such as particle sharp corners, intergrowth and the like to enable vein quartz particles to be in a pomegranate seed shape, wherein the pictographic coefficient is more than or equal to 0.63;
5. removing impurities: 2ZKR1022 double-layer vibrating screen (10/20 mm screen hole) is adopted to separate crushed ore and the like in the shaping process; respectively obtaining grinding media of 20-30 mm and 10-20 mm;
6. color selection: the method comprises the steps of removing individual heterochromatic impurity minerals in grinding media of 20-30 mm and 10-20 mm by adopting an LKD1920-1K ore color sorter of Zhongke photoelectric color sorting machinery, Inc., and obtaining high-purity quartz grinding media of 20-30 mm and 10-20 mm respectively.
And (3) carrying out effect comparison:
grinding materials: 0.3-0.1 mm high-purity quartz sand, which comprises the following components: SiO 22 99.95%，Fe2O3 0.00025%（2.5ppm）；
Grinding media: the traditional grinding medium is 95 percent ZrO with the diameter of phi 3-5 mm2After the ball milling and the ore milling are carried out for 3 hours, the granularity of the product reaches the standard; the traditional quartz (agate) ball milling medium is phi 5-8 mm, and the granularity of the product reaches the standard after 4.5h of ore milling; according to the invention, a high-purity quartz grinding medium with the diameter of 3-5 mm is adopted, and the granularity of the product reaches the standard after grinding for 4 hours;
and (3) controlling the product quality: chemical components: SiO 22≥99.90%，Fe2O3≤0.0010%（10ppm）；
And (3) controlling the granularity: d50=1.5μm，D100=10μm。
The implementation result shows that after the traditional zirconium oxide grinding medium or quartz (agate) grinding medium is adopted for grinding ore, the product pollution is serious, and SiO is generated2、Fe2O3And exceeding the standard and having unqualified quality. The pomegranate seed-shaped grinding medium thoroughly avoids pollution, and the product quality completely meets the requirements; if the abrasion (16 kg/t) is considered to become a qualified product, the value added value is about 150 yuan, and the comprehensive cost is reduced by more than 90% compared with that of quartz (agate) grinding media and is reduced by more than 60% compared with that of zirconia grinding media.
The above embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and all changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (5)
1. A preparation method of pomegranate seed-shaped high-purity quartz grinding media for high-purity silicon micropowder mill is characterized by comprising the following steps:
(1) selecting raw materials: selecting vein quartz ore with a compact block structure as a raw material, and controlling the quality standard as follows: chemical components: SiO 22≥99.80%，Al2O3≤0.010%，Fe2O3Less than or equal to 0.0020 percent; the maximum block size is controlled to be 350 mm;
(2) crushing: a three-stage crushing process is adopted, a jaw crusher is adopted in the first stage, and the ore discharge opening is controlled to be 70 mm; the second section adopts a cone crusher, and the ore discharge opening is controlled to be 25 mm; the third section adopts a cone crusher, and the ore discharge port is controlled to be 10 mm; ensuring that the crushed quartz blocks are polygonal by using the crushing motion track of the cone crusher;
(3) screening and grading: screening and grading the crushed materials in the second stage to prepare 20-30 mm and 10-20 mm grain-size grinding media; screening and grading the crushed material in the third section to prepare grinding media with the particle size fraction of 5-10 mm and 3-5 mm;
(4) and shaping: shaping by a wet stirring mill, and grinding off false particles such as sharp corners and intergrowths of the particles to enable the vein quartz particles to be in a pomegranate seed shape, wherein the pictographic coefficient is more than or equal to 0.6;
(5) removing impurities: and screening out fine crushed materials by using a vibrating screen and removing impurities and foreign matters in the grinding medium to obtain the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill.
2. The method for preparing the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill according to claim 1, characterized by comprising the following steps: and (4) shaping, namely autogenous grinding is carried out in a stirring mill for 16-26h, wherein the weight ratio of materials to water is 1: 1.
3. The method for preparing the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill according to claim 1, characterized by comprising the following steps: and (5) impurity removal adopts a leaching or color sorting process to remove impurity minerals in the grinding medium, so that the quality of the grinding medium is improved.
4. The method for preparing the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill according to any one of claims 1 to 3, characterized by comprising the following steps: the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill comprises the following quality standards: chemical components: SiO 22≥99.95%，Al2O3≤0.0050%，Fe2O3Less than or equal to 0.0010 percent; the pictographic coefficient is more than or equal to 0.6, and the bulk density is more than or equal to 2.0.
5. The method for preparing the pomegranate seed-shaped high-purity quartz grinding medium for the high-purity silicon micropowder mill according to any one of claims 1 to 3, characterized by comprising the following steps: the crushed material with the particle size of-3 mm generated in the process is used as a raw material for preparing high-purity quartz sand or silicon micropowder.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202823523U (en) * | 2009-02-19 | 2013-03-27 | 阿萨瑞尔-曼德特公司 | Grinding medium |
| CN104194274A (en) * | 2014-09-09 | 2014-12-10 | 江苏联瑞新材料股份有限公司 | Method for preparing silica powder for full-encapsulated epoxy molding compound |
| CN108048035A (en) * | 2017-10-31 | 2018-05-18 | 江西纳朴实业有限公司 | A kind of preparation method of cobble shaped ceramic grinding media |
| CN109824340A (en) * | 2019-02-28 | 2019-05-31 | 宁国慧宏耐磨材料有限公司 | A kind of processing technology of abrasive media |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202823523U (en) * | 2009-02-19 | 2013-03-27 | 阿萨瑞尔-曼德特公司 | Grinding medium |
| CN104194274A (en) * | 2014-09-09 | 2014-12-10 | 江苏联瑞新材料股份有限公司 | Method for preparing silica powder for full-encapsulated epoxy molding compound |
| CN108048035A (en) * | 2017-10-31 | 2018-05-18 | 江西纳朴实业有限公司 | A kind of preparation method of cobble shaped ceramic grinding media |
| CN109824340A (en) * | 2019-02-28 | 2019-05-31 | 宁国慧宏耐磨材料有限公司 | A kind of processing technology of abrasive media |
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