CN103896285B - A kind of method preparing high pure and ultra-fine silica flour with waste and old quartz crucible - Google Patents
A kind of method preparing high pure and ultra-fine silica flour with waste and old quartz crucible Download PDFInfo
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- CN103896285B CN103896285B CN201410161419.5A CN201410161419A CN103896285B CN 103896285 B CN103896285 B CN 103896285B CN 201410161419 A CN201410161419 A CN 201410161419A CN 103896285 B CN103896285 B CN 103896285B
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Abstract
The invention discloses a kind of preparation method preparing high pure and ultra-fine silica flour with waste and old quartz crucible, including crushing, pickling, wash, dry, grind, the step such as classification and collection.Due to used in the present invention be waste and old quartz crucible, SiO in raw material2Very high purity, processing by waste and old quartz crucible further being purified remove impurity and grinding superfineization, obtaining SiO2Content is not less than 99.95%; particle size distribution is 1～100 μm; amorphous rate is the high pure and ultra-fine silica flour of 98%～100%; the high pure and ultra-fine silica flour that the new high-tech industries such as optical fiber industry, electronics industry, microelectronics industry use can be met; such that it is able to quartz raw ore is depended on unduly by notable alleviation; realize recycling of quartz sand; be conducive to the protection to land resources; it is substantially reduced the manufacturing cost of quartz crucible, the production simultaneously also solving quartz crucible and the pollution of the solid waste using enterprise and emission problem.
Description
Technical field
The present invention relates to the preparation method of high pure and ultra-fine quartz material, particularly to one with waste and old quartz crucible
The method preparing high pure and ultra-fine silica flour for raw material.
Background technology
High pure and ultra-fine silica flour possesses excellent chemico-physical properties, and fusing point is at 1715 DEG C, and the structure of alpha-beta turns
Changing temperature is 573 DEG C, without cleavage, has fabulous chemical stability, high insulation voltage endurance capability, punctures
Voltage 32-34KV/mm, low-thermal-expansion, it is applied to integrated circuit, microelectronics product as high-quality inserts
Product, capsulation material etc..
Along with the new high-tech industries such as optical fiber industry, electronics industry, microelectronics industry develop rapidly, to height
The requirement of pure ultrafine quartz powder is more and more higher, and demand is the most increasing.The making of quartz micropowder is former at present
Material mostly be high-quality natural quartz mineral aggregate, its technological process is: raw material → coarse crushing → in broken → pickling → washing
→ it is dried → dry method superfine grinding → classification → product.But the quartzy head grade of all parts of the country differs,
Impurity content difference is very big, and the purity of the high pure and ultra-fine silica flour that employing traditional handicraft prepares is difficult to ensure.
And along with the exhaustion of high-grade quartz ore resource, raw-material price can be more and more higher, produces into
This also can be more and more higher.
Quartz crucible is to utilize glass sand to form through founding, and quartz crucible actually has become as SiO2Contain
Measure high, Fe2O3Deng the amorphous Si O that impurity content is extremely low2, have that thermal coefficient of expansion is little, heat resistanceheat resistant is shaken surely
Qualitative strong, transparency advantages of higher.The most often produce 1 ton of quartz crucible and to have 0.25 ton useless
Quartz crucible.Therefore, comprehensively utilize these quartz crucible waste materials prepare high value-added product be possible not only to solve
An enterprise pollution difficult problem, and higher economic worth can be created.
Summary of the invention
The present invention is directed to the problem that prior art exists, it is proposed that one is prepared high-purity super with waste and old quartz crucible
The method of fine quartz powder, to realize the purpose of the recycling of quartz crucible waste material.
The technical problem to be solved is achieved through the following technical solutions.The present invention proposes
A kind of method preparing high pure and ultra-fine silica flour with waste and old quartz crucible, it is characterised in that step is as follows:
(1) broken: using waste and old quartz crucible is raw material, obtain the block that particle diameter is 1～30mm after pulverizing；
(2) pickling: utilize the acid dip pickle adding supersonic generator that block is carried out pickling impurity removal, ultrasonic
Wave frequency is 35～50Hz, and ultrasonic power is 600～700W, uses the two end number mixing acid of oxalic acid and hydrochloric acid
Or Fluohydric acid., oxalic acid and the ternary mixed acid of nitric acid；Two end number mixing acid mesoxalic acid with the proportion of hydrochloric acid is
1: 1～3, in ternary mixed acid, Fluohydric acid., oxalic acid are 1: 1～5: 1 with the proportion of nitric acid；Block with mix
The weight ratio of acid is 1: 1～5；Detailed process is: at room temperature, utilizes mixed acid solution to soak block
10～100h, intermediate agitation 3～5 times, in ultrasonic field, then process 50～100min, flow away surface solution；
(3) washing: use pure water that the block after pickling carries out ultrasonic cleaning 3～5 times, supersonic frequency
Being 10～20Hz, ultrasonic power is 100～200W, and washing is to neutral；
(4) dry: carry out drying to wet weight than ＜ 1% by the block baking oven after washing；
(5) grind: use high thin ball mill to be ground, use different size in the 4 of 10～40mm
Ball-milling medium, charge ratio of media is between 28%～35%；
(6) classification, collection: the silica flour after ball milling is carried out air current classifying, collection, i.e. obtains high-purity
Ultrafine quartz powder, SiO in this silica flour2Content be not less than 99.95%, particle size distribution is 1～100 μm,
Amorphous rate is 98%～100%.
The present invention to solve the technical problem that another can also come by the following technical programs to realize further,
A kind of above-described method preparing high pure and ultra-fine silica flour with waste and old quartz crucible, is characterized in, in step
Suddenly in (1), waste and old quartz crucible be quartz crucible manufacturing enterprise defective scrap and/or use after stone
English crucible.
The present invention to solve the technical problem that another can also come by the following technical programs to realize further,
A kind of above-described method preparing high pure and ultra-fine silica flour with waste and old quartz crucible, is characterized in, in step
Suddenly in (5), the rotating speed of ball mill is 100～300r/min, and Ball-milling Time is 40～70min.
A kind of method preparing high pure and ultra-fine silica flour with waste and old quartz crucible of the present invention, to quartz crucible waste material
Carry out purifying remove impurity and grinding superfineization processes, optical fiber industry, electronics industry, micro-electricity can be met
The high pure and ultra-fine silica flour that the new high-tech industries such as son industry use, such that it is able to notable alleviation is former to quartz
Depending on unduly of ore deposit, it is achieved recycling of quartz sand, is conducive to the protection to land resources, significantly drops
The manufacturing cost of low quartz crucible, also solves the production of quartz crucible simultaneously and uses the solid waste of enterprise
Pollution and emission problem.
Detailed description of the invention
The concrete technical scheme of the present invention described further below, in order to those skilled in the art enters one
Step understands the present invention.
Embodiment 1:
(1) broken: using waste and old quartz crucible is raw material, obtaining particle diameter after pulverizing is the block of 1mm；
(2) pickling: utilize the acid dip pickle adding supersonic generator that block is carried out pickling impurity removal, ultrasonic
Wave frequency is 35Hz, and ultrasonic power is 600W, uses oxalic acid sour with the two end number mixing of hydrochloric acid or hydrogen
Fluoric acid, oxalic acid and the ternary mixed acid of nitric acid；Two end number mixing acid mesoxalic acid is 1: 3, three with the proportion of hydrochloric acid
In unit's mixed acid, Fluohydric acid., oxalic acid are 1: 5: 1 with the proportion of nitric acid；Block and the weight ratio of mixed acid
It is 1: 5；Detailed process is: at room temperature, utilizes mixed acid solution to soak block 10h, intermediate agitation 3
Secondary, in ultrasonic field, then process 100min, flow away surface solution；
(3) washing: using pure water that the block after pickling is carried out ultrasonic cleaning 5 times, supersonic frequency is
20Hz, ultrasonic power is 100W, and washing is to neutral；
(4) dry: carry out drying to wet weight than ＜ 1% by the block baking oven after washing；
(5) grind: use high thin ball mill to be ground, use different size in the 4 of 10～40mm
Ball-milling medium, charge ratio of media is between 28%；
(6) classification, collection: the silica flour after ball milling is carried out air current classifying, collection, i.e. obtains high-purity
Ultrafine quartz powder, SiO in this silica flour2Content be 99.95%, particle size distribution is 1～20 μm, amorphous
Rate is 98%.
Embodiment 2:
(1) broken: using waste and old quartz crucible is raw material, obtaining particle diameter after pulverizing is the block of 5mm；
(2) pickling: utilize the acid dip pickle adding supersonic generator that block is carried out pickling impurity removal, ultrasonic
Wave frequency is 40Hz, and ultrasonic power is 650W, uses oxalic acid sour with the two end number mixing of hydrochloric acid or hydrogen
Fluoric acid, oxalic acid and the ternary mixed acid of nitric acid；Two end number mixing acid mesoxalic acid is 1: 2, three with the proportion of hydrochloric acid
In unit's mixed acid, Fluohydric acid., oxalic acid are 1: 4: 1 with the proportion of nitric acid；Block and the weight ratio of mixed acid
It is 1: 4；Detailed process is: at room temperature, utilizes mixed acid solution to soak block 20h, intermediate agitation 3
Secondary, in ultrasonic field, then process 80min, flow away surface solution；
(3) washing: using pure water that the block after pickling is carried out ultrasonic cleaning 4 times, supersonic frequency is
15Hz, ultrasonic power is 150W, and washing is to neutral；
(4) dry: carry out drying to wet weight than ＜ 1% by the block baking oven after washing；
(5) grind: use high thin ball mill to be ground, use different size in the 4 of 10～40mm
Ball-milling medium, charge ratio of media is between 30%；
(6) classification, collection: the silica flour after ball milling is carried out air current classifying, collection, i.e. obtains high-purity
Ultrafine quartz powder, SiO in this silica flour2Content be 99.96%, particle size distribution is 1～30 μm, amorphous
Rate is 99%.
Embodiment 3:
(1) broken: using waste and old quartz crucible is raw material, obtaining particle diameter after pulverizing is the block of 10mm；
(2) pickling: utilize the acid dip pickle adding supersonic generator that block is carried out pickling impurity removal, ultrasonic
Wave frequency is 45Hz, and ultrasonic power is 700W, uses oxalic acid sour with the two end number mixing of hydrochloric acid or hydrogen
Fluoric acid, oxalic acid and the ternary mixed acid of nitric acid；Two end number mixing acid mesoxalic acid is 1: 1, three with the proportion of hydrochloric acid
In unit's mixed acid, Fluohydric acid., oxalic acid are 1: 3: 1 with the proportion of nitric acid；Block and the weight ratio of mixed acid
It is 1: 3；Detailed process is: at room temperature, utilizes mixed acid solution to soak block 50h, intermediate agitation 4
Secondary, in ultrasonic field, then process 60min, flow away surface solution；
(3) washing: using pure water that the block after pickling is carried out ultrasonic cleaning 5 times, supersonic frequency is
20Hz, ultrasonic power is 200W, and washing is to neutral；
(4) dry: carry out drying to wet weight than ＜ 1% by the block baking oven after washing；
(5) grind: use high thin ball mill to be ground, use different size in the 4 of 10～40mm
Ball-milling medium, charge ratio of media is between 32%；
(6) classification, collection: the silica flour after ball milling is carried out air current classifying, collection, i.e. obtains high-purity
Ultrafine quartz powder, SiO in this silica flour2Content be 99.97%, particle size distribution is 1～50 μm, amorphous
Rate is 99.5%.
Embodiment 4:
(1) broken: using waste and old quartz crucible is raw material, obtaining particle diameter after pulverizing is the block of 30mm；
(2) pickling: utilize the acid dip pickle adding supersonic generator that block is carried out pickling impurity removal, ultrasonic
Wave frequency is 50Hz, and ultrasonic power is 700W, uses oxalic acid sour with the two end number mixing of hydrochloric acid or hydrogen
Fluoric acid, oxalic acid and the ternary mixed acid of nitric acid；Two end number mixing acid mesoxalic acid is 1: 1, three with the proportion of hydrochloric acid
In unit's mixed acid, Fluohydric acid., oxalic acid are 1: 1: 1 with the proportion of nitric acid；Block and the weight ratio of mixed acid
It is 1: 1；Detailed process is: at room temperature, utilizes mixed acid solution to soak block 100h, intermediate agitation 5
Secondary, in ultrasonic field, then process 100min, flow away surface solution；
(3) washing: using pure water that the block after pickling is carried out ultrasonic cleaning 5 times, supersonic frequency is
15Hz, ultrasonic power is 150W, and washing is to neutral；
(4) dry: carry out drying to wet weight than ＜ 1% by the block baking oven after washing；
(5) grind: use high thin ball mill to be ground, use different size in the 4 of 10～40mm
Ball-milling medium, charge ratio of media is between 35%；
(6) classification, collection: the silica flour after ball milling is carried out air current classifying, collection, i.e. obtains high-purity
Ultrafine quartz powder, SiO in this silica flour2Content be 99.99%, particle size distribution is 1～100 μm, non-
Brilliant rate is 100%.
Although embodiment of the present invention are disclosed as above, but it is not restricted to description and embodiment party
Listed utilization in formula, it can be applied to various applicable the field of the invention completely, for being familiar with ability
For the personnel in territory, be easily achieved other amendment, therefore without departing substantially from claim and etc. homotype
Enclosing under limited general concept, the present invention is not limited to specific details and shown here as the reality with description
Example.
Claims (2)
1. the preparation method preparing high pure and ultra-fine silica flour with waste and old quartz crucible, it is characterised in that with
Waste and old quartz crucible is raw material, and its step is as follows:
(1) broken: using waste and old quartz crucible is raw material, obtain the block that particle diameter is 1～30mm after pulverizing；
(2) pickling: utilize the acid dip pickle adding supersonic generator that block is carried out pickling impurity removal, ultrasonic
Wave frequency is 40～50Hz, and ultrasonic power is 650～700W, uses the two end number mixing acid of oxalic acid and hydrochloric acid
Or Fluohydric acid., oxalic acid and the ternary mixed acid of nitric acid；Two end number mixing acid mesoxalic acid with the proportion of hydrochloric acid is
1:3, in ternary mixed acid, Fluohydric acid., oxalic acid are 1:1～5:1 with the proportion of nitric acid；Block and mixed acid
Weight ratio be 1:1～5；Detailed process is: at room temperature, utilizes mixed acid solution to soak block 10～100h,
Intermediate agitation 3～5 times, then process 50～100min in ultrasonic field, and flow away surface solution；
(3) washing: use pure water that the block after pickling carries out ultrasonic cleaning 3～5 times, supersonic frequency
Rate is 10～20Hz, and ultrasonic power is 100～200W, and washing is to neutral；
(4) dry: carry out drying to wet weight ratio < 1% by the block baking oven after washing；
(5) grind: using high thin ball mill to be ground, the rotating speed of ball mill is 100～300r/min,
Ball-milling Time is 40～70min, uses the ball-milling medium of different size in the 4 of 10～40mm, and medium is filled out
Rate of filling is between 28%～35%；
(6) classification, collection: the silica flour after ball milling is carried out air current classifying, collection, i.e. obtains high-purity
Ultrafine quartz powder, SiO in this silica flour2Content be not less than 99.95%, particle size distribution is 1～100 μm,
Amorphous rate is 98%～100%.
A kind of preparation preparing high pure and ultra-fine silica flour with waste and old quartz crucible
Method, it is characterised in that waste and old quartz crucible is defective scrap and/or the use of quartz crucible manufacturing enterprise
After quartz crucible.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104891971A (en) * | 2015-05-20 | 2015-09-09 | 南通路博石英材料有限公司 | Manufacturing method of high-purity quartz ceramic slurry |
| CN105271633B (en) * | 2015-11-27 | 2017-07-07 | 湖南鑫生矿冶废弃物综合利用科技有限公司 | A kind of preparation method for producing glass silica flour |
| CN105271257B (en) * | 2015-11-27 | 2017-03-29 | 湖南鑫生矿冶废弃物综合利用科技有限公司 | A kind of preparation method for producing glass silica flour |
| CN105883820B (en) * | 2016-04-19 | 2018-11-06 | 赵美玲 | A method of preparing high-purity silicon dioxide ore in sand form |
| CN107244824A (en) * | 2017-06-26 | 2017-10-13 | 安徽安顺硅基玻璃原料有限公司 | A kind of high whiteness sheet material sand production technology |
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| CN103130405A (en) * | 2013-03-15 | 2013-06-05 | 连云港利思特电子材料有限公司 | Preparation method of precision casting fused quartz powder and quartz powder produced by same |
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| US4983370A (en) * | 1990-02-06 | 1991-01-08 | The Feldspar Corporation | Purified quartz and process for purifying quartz |
| CN101503194B (en) * | 2009-03-02 | 2011-03-30 | 申士富 | Preparation of active high purity silica flour |
| CN102145898A (en) * | 2011-05-05 | 2011-08-10 | 张冬玲 | Production method of silicon dioxide ultrafine powder |
| RU2492143C1 (en) * | 2011-12-26 | 2013-09-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Иркутский государственный технический университет" (ФГБОУ ВПО "ИрГТУ") | Method of producing high-quality quartz grit |
| CN202465292U (en) * | 2012-03-16 | 2012-10-03 | 江苏融汇石英材料科技有限公司 | Device for producing molten obtuse quartz sand by taking waste quartz crucible as raw material |
| CN103613103A (en) * | 2013-12-04 | 2014-03-05 | 南京工业大学东海先进硅基材料研究院 | Method for preparing filler-level silicon micropowder by using waste quartz crucibles as raw materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557389A (en) * | 2012-01-06 | 2012-07-11 | 徐州协鑫太阳能材料有限公司 | Method for preparing high-purity fused silica by recovering waste quartz crucible |
| CN103130405A (en) * | 2013-03-15 | 2013-06-05 | 连云港利思特电子材料有限公司 | Preparation method of precision casting fused quartz powder and quartz powder produced by same |
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Address after: 221412 Xinyi City, Xuzhou Province town of Lake Town Industrial Park, No. 18, No. Patentee after: Jiangsu Kaida quartz Limited by Share Ltd Address before: The new city of Xinyi road 221400 Jiangsu city of Xuzhou province No. 10 Patentee before: Jiangsu Kaida Silica Co., Ltd. |
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