CN103896285A - Method for preparing high-purity superfine quartz powder through waste quartz crucible - Google Patents
Method for preparing high-purity superfine quartz powder through waste quartz crucible Download PDFInfo
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- CN103896285A CN103896285A CN201410161419.5A CN201410161419A CN103896285A CN 103896285 A CN103896285 A CN 103896285A CN 201410161419 A CN201410161419 A CN 201410161419A CN 103896285 A CN103896285 A CN 103896285A
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Abstract
The invention discloses a method for preparing high-purity superfine quartz powder through a waste quartz crucible. The method comprises steps of crushing, acid pickling, water washing, drying, grinding, grading, collecting and the like. Due to the use of the waste quartz crucible, the purity of SiO2 in the raw material is very high, through further purification and impurity removal and ultrafine grinding of the waste quartz crucible, high-purity superfine quartz powder with not less than 99.95% of SiO2, size distribution of 1-100mu m and amorphous rate of 98%-100% is obtained, which is applicable to high and new technology industries like optical fiber industry, electronic industry, microelectronics industry and the like, so that the method can remarkably relieve excessive dependency on quartz raw ore, recycles quartz sand, is beneficial to protecting land resources, greatly lowers the manufacture cost of the quartz crucible, and also solves the problems of pollution and emission of solid waste of the enterprises producing and using the quartz crucible.
Description
Technical field
The present invention relates to the preparation method of high pure and ultra-fine quartz material, particularly a kind of method of preparing high pure and ultra-fine silica powder take waste and old quartz crucible as raw material.
Background technology
High pure and ultra-fine silica powder possesses good chemico-physical properties, fusing point is at 1715 ℃, the Structure Conversion temperature of alpha-beta is 573 ℃, without cleavage, there is fabulous chemical stability, high dielectric voltage withstand ability, voltage breakdown 32-34KV/mm, low-thermal-expansion, is applied to unicircuit, microelectronic product, capsulation material etc. as high-quality stopping composition.
Along with the new high-tech industries such as optical fiber industry, electronic industry, microelectronics industry develop rapidly, more and more higher to the requirement of high pure and ultra-fine silica powder, demand is also increasing.At present the making raw material of quartz micropowder mostly is high-quality natural quartz mineral aggregate, and its technical process is: raw material → coarse crushing → in broken → pickling → washing → be dried → dry method superfine grinding → classification → product.But quartzy head grade in all parts of the country differs, and foreign matter content difference is very large, the purity of the high pure and ultra-fine silica powder that employing traditional technology makes is difficult for guaranteeing.And along with the exhaustion of high-grade quartzy ore resource, raw-material price can be more and more higher, production cost also can be more and more higher.
Quartz crucible is to utilize glass sand to form through founding, and quartz crucible has in fact become SiO
2content is high, Fe
2o
3deng the extremely low amorphous Si O of foreign matter content
2, stability is strong, transparency advantages of higher to have that thermal expansivity is little, heat resistanceheat resistant is shaken.1 ton of quartz crucible of every production will have the useless quartz crucible of 0.25 ton in process of production.Therefore, fully utilize these quartz crucible waste materials and prepare high value-added product and not only can solve an enterprise pollution difficult problem, and can create higher economic worth.
Summary of the invention
The present invention is directed to the problem that prior art exists, proposed a kind of method of preparing high pure and ultra-fine silica powder with waste and old quartz crucible, to realize the object of recycling of quartz crucible waste material.
Technical problem to be solved by this invention is achieved through the following technical solutions.The present invention proposes a kind of method of preparing high pure and ultra-fine silica powder with waste and old quartz crucible, it is characterized in that, step is as follows:
(1) fragmentation: adopting waste and old quartz crucible is raw material, obtains the piece material that particle diameter is 1~30mm after pulverizing;
(2) pickling: utilize the pickler that adds ultrasonic generator to carry out pickling impurity removal to piece material, ultrasonic frequency is 35~50Hz, ultrasonic power is 600~700W, adopts oxalic acid and the binary mixing acid of hydrochloric acid or the ternary mixing acid of hydrofluoric acid, oxalic acid and nitric acid; The proportion of binary mixing acid mesoxalic acid and hydrochloric acid is 1: 1~3, and in ternary mixing acid, the proportion of hydrofluoric acid, oxalic acid and nitric acid is 1: 1~5: 1; The weight ratio of piece material and mixing acid is 1: 1~5; Detailed process is: at room temperature, utilize mixed acid solution to soak piece material 10~100h, middle stirring 3~5 times then processed 50~100min in ultrasonic field, and surface solution flows away;
(3) washing: adopt pure water that the piece material after pickling is carried out to ultrasonic cleaning 3~5 times, ultrasonic frequency is 10~20Hz, and ultrasonic power is 100~200W, washing is to neutral;
(4) dry: the piece material after washing is dried to weight in wet base than < 1% with baking oven;
(5) grind: adopt high thin ball mill to grind, adopt 10~40mm 4 in the ball-milling medium of different size, charge ratio of media is between 28%~35%;
(6) classification, collection: the silica powder after ball milling is carried out to air classification, collection, obtain high pure and ultra-fine silica powder, SiO in this silica powder
2content be not less than 99.95%, size-grade distribution is 1~100 μ m, amorphous rate is 98%~100%.
Another technical problem that will solve of the present invention can also be come further to realize by the following technical programs, a kind of above-described method of preparing high pure and ultra-fine silica powder with waste and old quartz crucible, be characterized in, in step (1), waste and old quartz crucible be quartz crucible manufacturing concern defective scrap and/or use after quartz crucible.
Another technical problem that will solve of the present invention can also be come further to realize by the following technical programs, a kind of above-described method of preparing high pure and ultra-fine silica powder with waste and old quartz crucible, be characterized in, in step (5), the rotating speed of ball mill is 100~300r/min, and Ball-milling Time is 40~70min.
A kind of method of preparing high pure and ultra-fine silica powder with waste and old quartz crucible of the present invention; to quartz crucible waste material purify removal of impurities and grinding superfine processing; can be met the high pure and ultra-fine silica powder that the new high-tech industries such as optical fiber industry, electronic industry, microelectronics industry are used; thereby can significantly alleviate depending on unduly quartzy raw ore; realize the recycle of quartz sand; be conducive to the protection to land resources; greatly reduce the manufacturing cost of quartz crucible, also solved pollution and the emission problem of the production of quartz crucible and the solid waste of use enterprise simultaneously.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art further understands the present invention.
Embodiment 1:
(1) fragmentation: adopting waste and old quartz crucible is raw material, obtains the piece material that particle diameter is 1mm after pulverizing;
(2) pickling: utilize the pickler that adds ultrasonic generator to carry out pickling impurity removal to piece material, ultrasonic frequency is 35Hz, and ultrasonic power is 600W, adopts oxalic acid and the binary mixing acid of hydrochloric acid or the ternary mixing acid of hydrofluoric acid, oxalic acid and nitric acid; The proportion of binary mixing acid mesoxalic acid and hydrochloric acid is 1: 3, and in ternary mixing acid, the proportion of hydrofluoric acid, oxalic acid and nitric acid is 1: 5: 1; The weight ratio of piece material and mixing acid is 1: 5; Detailed process is: at room temperature, utilize mixed acid solution to soak piece material 10h, middle stirring 3 times then processed 100min in ultrasonic field, and surface solution flows away;
(3) washing: adopt pure water that the piece material after pickling is carried out to ultrasonic cleaning 5 times, ultrasonic frequency is 20Hz, and ultrasonic power is 100W, washing is to neutral;
(4) dry: the piece material after washing is dried to weight in wet base than < 1% with baking oven;
(5) grind: adopt high thin ball mill to grind, adopt 10~40mm 4 in the ball-milling medium of different size, charge ratio of media is between 28%;
(6) classification, collection: the silica powder after ball milling is carried out to air classification, collection, obtain high pure and ultra-fine silica powder, SiO in this silica powder
2content be 99.95%, size-grade distribution is 1~20 μ m, amorphous rate is 98%.
Embodiment 2:
(1) fragmentation: adopting waste and old quartz crucible is raw material, obtains the piece material that particle diameter is 5mm after pulverizing;
(2) pickling: utilize the pickler that adds ultrasonic generator to carry out pickling impurity removal to piece material, ultrasonic frequency is 40Hz, and ultrasonic power is 650W, adopts oxalic acid and the binary mixing acid of hydrochloric acid or the ternary mixing acid of hydrofluoric acid, oxalic acid and nitric acid; The proportion of binary mixing acid mesoxalic acid and hydrochloric acid is 1: 2, and in ternary mixing acid, the proportion of hydrofluoric acid, oxalic acid and nitric acid is 1: 4: 1; The weight ratio of piece material and mixing acid is 1: 4; Detailed process is: at room temperature, utilize mixed acid solution to soak piece material 20h, middle stirring 3 times then processed 80min in ultrasonic field, and surface solution flows away;
(3) washing: adopt pure water that the piece material after pickling is carried out to ultrasonic cleaning 4 times, ultrasonic frequency is 15Hz, and ultrasonic power is 150W, washing is to neutral;
(4) dry: the piece material after washing is dried to weight in wet base than < 1% with baking oven;
(5) grind: adopt high thin ball mill to grind, adopt 10~40mm 4 in the ball-milling medium of different size, charge ratio of media is between 30%;
(6) classification, collection: the silica powder after ball milling is carried out to air classification, collection, obtain high pure and ultra-fine silica powder, SiO in this silica powder
2content be 99.96%, size-grade distribution is 1~30 μ m, amorphous rate is 99%.
Embodiment 3:
(1) fragmentation: adopting waste and old quartz crucible is raw material, obtains the piece material that particle diameter is 10mm after pulverizing;
(2) pickling: utilize the pickler that adds ultrasonic generator to carry out pickling impurity removal to piece material, ultrasonic frequency is 45Hz, and ultrasonic power is 700W, adopts oxalic acid and the binary mixing acid of hydrochloric acid or the ternary mixing acid of hydrofluoric acid, oxalic acid and nitric acid; The proportion of binary mixing acid mesoxalic acid and hydrochloric acid is 1: 1, and in ternary mixing acid, the proportion of hydrofluoric acid, oxalic acid and nitric acid is 1: 3: 1; The weight ratio of piece material and mixing acid is 1: 3; Detailed process is: at room temperature, utilize mixed acid solution to soak piece material 50h, middle stirring 4 times then processed 60min in ultrasonic field, and surface solution flows away;
(3) washing: adopt pure water that the piece material after pickling is carried out to ultrasonic cleaning 5 times, ultrasonic frequency is 20Hz, and ultrasonic power is 200W, washing is to neutral;
(4) dry: the piece material after washing is dried to weight in wet base than < 1% with baking oven;
(5) grind: adopt high thin ball mill to grind, adopt 10~40mm 4 in the ball-milling medium of different size, charge ratio of media is between 32%;
(6) classification, collection: the silica powder after ball milling is carried out to air classification, collection, obtain high pure and ultra-fine silica powder, SiO in this silica powder
2content be 99.97%, size-grade distribution is 1~50 μ m, amorphous rate is 99.5%.
Embodiment 4:
(1) fragmentation: adopting waste and old quartz crucible is raw material, obtains the piece material that particle diameter is 30mm after pulverizing;
(2) pickling: utilize the pickler that adds ultrasonic generator to carry out pickling impurity removal to piece material, ultrasonic frequency is 50Hz, and ultrasonic power is 700W, adopts oxalic acid and the binary mixing acid of hydrochloric acid or the ternary mixing acid of hydrofluoric acid, oxalic acid and nitric acid; The proportion of binary mixing acid mesoxalic acid and hydrochloric acid is 1: 1, and in ternary mixing acid, the proportion of hydrofluoric acid, oxalic acid and nitric acid is 1: 1: 1; The weight ratio of piece material and mixing acid is 1: 1; Detailed process is: at room temperature, utilize mixed acid solution to soak piece material 100h, middle stirring 5 times then processed 100min in ultrasonic field, and surface solution flows away;
(3) washing: adopt pure water that the piece material after pickling is carried out to ultrasonic cleaning 5 times, ultrasonic frequency is 15Hz, and ultrasonic power is 150W, washing is to neutral;
(4) dry: the piece material after washing is dried to weight in wet base than < 1% with baking oven;
(5) grind: adopt high thin ball mill to grind, adopt 10~40mm 4 in the ball-milling medium of different size, charge ratio of media is between 35%;
(6) classification, collection: the silica powder after ball milling is carried out to air classification, collection, obtain high pure and ultra-fine silica powder, SiO in this silica powder
2content be 99.99%, size-grade distribution is 1~100 μ m, amorphous rate is 100%.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and embodiment, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the example of describing.
Claims (3)
1. a preparation method who prepares high pure and ultra-fine silica powder with waste and old quartz crucible, is characterized in that, take waste and old quartz crucible as raw material, its step is as follows:
(1) fragmentation: adopting waste and old quartz crucible is raw material, obtains the piece material that particle diameter is 1~30mm after pulverizing;
(2) pickling: utilize the pickler that adds ultrasonic generator to carry out pickling impurity removal to piece material, ultrasonic frequency is 35~50Hz, ultrasonic power is 600~700W, adopts oxalic acid and the binary mixing acid of hydrochloric acid or the ternary mixing acid of hydrofluoric acid, oxalic acid and nitric acid; The proportion of binary mixing acid mesoxalic acid and hydrochloric acid is 1: 1~3, and in ternary mixing acid, the proportion of hydrofluoric acid, oxalic acid and nitric acid is 1: 1~5: 1; The weight ratio of piece material and mixing acid is 1: 1~5; Detailed process is: at room temperature, utilize mixed acid solution to soak piece material 10~100h, middle stirring 3~5 times then processed 50~100min in ultrasonic field, and surface solution flows away;
(3) washing: adopt pure water that the piece material after pickling is carried out to ultrasonic cleaning 3~5 times, ultrasonic frequency is 10~20Hz, and ultrasonic power is 100~200W, washing is to neutral;
(4) dry: the piece material after washing is dried to weight in wet base than < 1% with baking oven;
(5) grind: adopt high thin ball mill to grind, adopt 10~40mm 4 in the ball-milling medium of different size, charge ratio of media is between 28%~35%;
(6) classification, collection: the silica powder after ball milling is carried out to air classification, collection, obtain high pure and ultra-fine silica powder, SiO in this silica powder
2content be not less than 99.95%, size-grade distribution is 1~100 μ m, amorphous rate is 98%~100%.
2. a kind of preparation method who prepares high pure and ultra-fine silica powder with waste and old quartz crucible as claimed in claim 1, is characterized in that, waste and old quartz crucible be quartz crucible manufacturing concern defective scrap and/or use after quartz crucible.
3. a kind of preparation method who prepares high pure and ultra-fine silica powder with waste and old quartz crucible as claimed in claim 1, is characterized in that, the rotating speed of ball mill is 100~300r/min, and Ball-milling Time is 40~70min.
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Cited By (5)
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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 |
CN105271257A (en) * | 2015-11-27 | 2016-01-27 | 湖南鑫生矿冶废弃物综合利用科技有限公司 | Preparation method of quartz powder used for producing glass |
CN105271633A (en) * | 2015-11-27 | 2016-01-27 | 湖南鑫生矿冶废弃物综合利用科技有限公司 | Preparation method of quartz powder used for producing glass |
CN105883820A (en) * | 2016-04-19 | 2016-08-24 | 赵美玲 | Method for preparing high-purity SiO2 ore sand |
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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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 |
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Cited By (7)
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 |
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CN105271633A (en) * | 2015-11-27 | 2016-01-27 | 湖南鑫生矿冶废弃物综合利用科技有限公司 | Preparation method of quartz powder used for producing glass |
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 |
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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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