CN104961325A - Production method of quartz powder for TFT-LCD substrate glass - Google Patents
Production method of quartz powder for TFT-LCD substrate glass Download PDFInfo
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Abstract
The invention provides a production method of quartz powder for TFT-LCD substrate glass. White vein quartz ore is selected as a raw material, and foreign ore in the white vein quartz ore is removed so that the white vein quartz ore can be used later; the ore is crushed by a crusher, variegated foreign particles in the ore are removed through a color selector, the ore particles are fed to a pickling tank to be leached at the room temperature, and the ore particles subjected to acid pickling is fully washed through water to be neutral and then are aired to be used later; the aired ore particles are calcinated and subjected to water quenching, impurities are removed after water quenching is conducted, and the ore particles are used later; the ore particles are fed into an edge runner to be subjected to wet milling to obtain mortar, the mortar is subjected to magnetic separation and then is classified, semi-finished products are collected and dewatered for use later; the dewatered sand powder is dried, and the dried sand powder is subjected to magnetic separation, and then the quartz powder for TFT-LCD substrate glass can be obtained. The method overcomes the defects in the prior art, the technology is simple, and the prepared quartz powder is high in quality.
Description
Technical field
The invention provides a kind of production method of silica powder, particularly relate to the production method of the special high quality silica powder of a kind of FT-LCD base plate glass.
Background technology
Along with the develop rapidly of global Flat Panel Display Industry, also achieve significant achievement with China's flat pannel display industry that the enterprises such as photoelectricity in CaiHong Group, Dong Xu group, Chengdu are representative.The flat-panel display device being representative with TFT-LCD, PDP, OLED becomes the core component of the terminal demonstration such as flat panel TV, panel computer, mobile phone, under the driving of the continuous progressive and innovation of technique of display of new generation, has driven the fast development of photoelectronic industry.
Glass substrate is one of basic element of character for liquid crystal display device, is also one of key and basic parts in flat pannel display industry.Along with glass substrate is more and more to the future development such as ultra-thin, high resolving power, high pixel, high transmission rate, high strength, lightweight and alkali-free, this proposes higher specification of quality just to the raw material of glass substrate and manufacturing process.Silica powder accounts for the ratio of about 60% as the siliceous raw material of the key of base plate glass in base plate glass, and therefore the height of this silica powder quality directly has influence on the quality of glass substrate.
At present, China be used as glass substrate silica powder quality due to the raw material of each enterprise and its quality of difference of production technique uneven, this also serious fast development that have impact on China's the sector, glass substrate also needs to solve by import with high-quality special silica powder.For this reason, developing the production technique of the special silica powder of a kind of glass substrate and relevant device, is the task of top priority promoting China's glass substrate industry rapid and healthy.
Summary of the invention
The invention provides a kind of production method of TFT-LCD base plate glass silica powder, solve the deficiency in background technology, the method technique is simple, and prepared TFT-LCD base plate glass silica powder quality is high, wherein SiO
2content can reach more than 99.7%.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of production method of TFT-LCD base plate glass silica powder, comprise the following steps: (1), the white vein quartz ore selecting aluminium sesquioxide content≤0.1% are raw material, clean laggard row artificial hand selection, for subsequent use after rejecting wherein contained impurity ore;
(2) after, the ore crusher in crushing after removing impurity in step (1) being become the ore particles of particle diameter≤25 millimeter, with color selector removing variegated impurity particle wherein, then ore particles is sent in pickling tank, with the chlorohydric acid pickling of mass concentration 28 ~ 31%, after at room temperature dynamically leaching 18 ~ 24 hours, bleed off the hydrochloric acid in pickling tank, then with water the ore particles after pickling fully wash dry to neutrality for subsequent use;
(3) after, the ore particles after drying being sent into and is calcined 45 ~ 60 minutes in quartzy calcining furnace under the temperature calcination of 900 ~ 950 DEG C, ore particles is put into the watch-quench tank water of 0 ~ 10 DEG C and carry out shrend, after shrend, ore particles is pulled out, then except for subsequent use after impurity elimination;
(4), wet milling mortar is carried out by ore particles obtained in step (3) feeding wheel roller, the muller of described wheel roller and mill disc all adopt quartz to make, the liner of the cylindrical shell of milling of wheel roller is quartzite slate, and in whole sand powder process processed of milling, material does not contact with irony;
(5) after the magnetic separator being 5000 ~ 7500 Gausses by mortar Surface field intensity obtained in upper step carries out three grades of magnetic separation, then carry out classification, collection cut size be 150 ~ 300 object sand powder as work in-process, with for subsequent use after centrifuge dewatering;
(6), by the sand powder after dehydration carry out drying, after dried sand powder carries out magnetic separation with permanent magnetic separators more than 7500 Gausses again, can obtain TFT-LCD base plate glass silica powder, wherein the massfraction of each component is as follows: SiO
2:>=99.7%, Fe
2o
3:≤0.01%, Al
2o
3:≤0.1%, K
2o+Na
2o :≤0.02%, grain size intervals: 150 ~ 400 orders, wherein 200 order ~ 300 order>=65%, below 400 orders≤5%, 150 orders more than be zero, chlorine ion concentration :≤8ppm.
Reuse after laggard for the HCl recovery in pickling tank row relax in step (2), when washing the ore particles after pickling, first with clear water ore particles washing to neutral, then use deionized water wash 3 times.
In step (5), collection cut size is that 150 ~ 300 object sand powder are as after work in-process, mortar more than 150 orders again Returning wheel mill repeats to make sand powder, with being pumped into pressure filter press filtration after mortar inflow thickener precipitation below 300 orders, namely filter cake obtains silicon powder after drying, and the clear water after precipitation recycles with pumped back workshop again.
When carrying out classification in step (5), the hydroclassifier made by non-metallic material, or carry out classification with the flexible sizing screen of multiple 150 order that non-metallic material make.
Mill in the wheel roller used in step (5) both sides of cylindrical shell are two pillar stiffeners, the drive unit of the wheel rollers such as the motor in supporting-point roller mill, step-down gear; It is 120 object discharging screen clothes that the other both sides of wheel roller are provided with order number.
Compared with prior art, the present invention has the following advantages: 1, process stabilizing of the present invention, and prepared TFT-LCD base plate glass silica powder moderate purity is high, and wherein the massfraction of each component is as follows: SiO
2:>=99.7%, Fe
2o
3:≤0.01%, Al
2o
3:≤0.1%, K
2o+Na
2o :≤0.02%.2, epigranular in silica powder, grain size intervals concentrates between 150 ~ 400 orders substantially, wherein 200 order ~ 300 order >=65%, below 400 orders≤5%, 150 orders more than be zero.3, in production technique provided by the invention, muller and the mill disc of the wheel roller described in when adopting wet method defibrination all adopt quartz to make, the liner of the cylindrical shell of milling of wheel roller is quartzite slate, in whole sand powder process processed of milling, material does not contact with irony, therefore, it is possible to avoid mixing of iron substance.4, the waste water in this technique after pickling carries out recovery, has namely saved resource, can not work the mischief again to environment.
Embodiment
Below in conjunction with specific embodiment, detailed specific description is done to the present invention, but protection scope of the present invention is not limited to following examples.
Embodiment 1
1, select the white quartz deposit in Xin County, Xinyang City, Henan Province to be raw material, the white vein quartz ore of aluminium sesquioxide content≤0.01% is raw material, and it is used clear water wash clean mouth, carry out artificial hand selection, reject containing for subsequent use after the impurity ores such as mica, feldspar, mountain stone.
2, the ore in 1 with after crusher in crushing to particle diameter≤25 mm granules, with color selector removing containing after variegated impurity particle, send in pickling tank, with the hydrochloric acid of concentration 28%, after room temperature dynamically leaches 24 hours, bleed off acid solution recovery, again with clear water ore washing to neutrality, more for subsequent use with drying after deionized water wash 3 times.
3, the material after drying in 2 is sent in quartzy calcining furnace and after 1 hour at the temperature calcination of 900 degree, puts into watch-quench tank 0-10 degree cold water and carry out shrend, after shrend, pull out, then artificial hand selection is except for subsequent use after impurity elimination.
4, wet milling sand powder is carried out in the muller that material feeding high purity quartz in 3 is made and the wheel roller of mill disc, the surrounding high purity quartz stone slab of wheel roller is liner, form circle to mill cylindrical shell, the both sides of cylindrical shell are two pillar stiffeners, the drive unit of the wheel rollers such as the motor in supporting-point roller mill, step-down gear; The other both sides of wheel roller are then installation order numbers is 120 object discharging screen clothes, is beneficial to mortar and overflows.The mortar Surface field intensity of overflowing is after the magnetic separator of 7500 Gausses carries out three grades of magnetic separation, classification is carried out again with the hydroclassifier that plastic material makes, collect the sand powder of more than below 150 orders 300 order as work in-process, with for subsequent use after centrifuge dewatering, silica powder more than 150 orders again Returning wheel grinds Machine-made Sand powder, with being pumped into pressure filter after mortar inflow thickener precipitation below 300 orders, namely filter cake is silicon powder after drying, and the clear water after precipitation recycles with pumped back workshop again.
5, the material in 4 is sent in drying machine and carries out drying, after dried material carries out magnetic separation with the permanent magnetic separator of more than 7500 Gausses again, the special quartz sand powder of high quality TFT-LCD base plate glass can be obtained.After testing: SiO
2: 99.8%, Fe
2o
3: 0.006%, Al
2o
3: 0.037%, K
2o+Na
2o:0.016%, grain size intervals: 150-400 order, wherein 200 order ~ 300 order>=70%, below 400 orders≤5%, 150 orders more than be zero, chlorion≤6ppm.
Embodiment 2
1, select the white quartz deposit of Taihu County, Anqing, Anhui Province to be raw material, the white vein quartz ore of aluminium sesquioxide content≤0.09% is raw material, and it is used clear water wash clean mouth, carry out artificial hand selection, reject containing for subsequent use after the impurity ores such as mica, feldspar, mountain stone.
2, the ore in 1 with after crusher in crushing to particle diameter≤25 mm granules, with color selector removing containing after variegated impurity particle, send in pickling tank, with the hydrochloric acid of concentration 29.5%, after room temperature dynamically leaches 20 hours, bleed off acid solution recovery, again with clear water ore washing to neutrality, more for subsequent use with drying after deionized water wash 3 times.
3, the material after drying in 2 is sent in quartzy calcining furnace and after 53 minutes at the temperature calcination of 925 degree, puts into watch-quench tank 0-10 degree cold water and carry out shrend, after shrend, pull out, then artificial hand selection is except for subsequent use after impurity elimination.
4, wet milling sand powder is carried out in the muller that material feeding high purity quartz in 3 is made and the wheel roller of mill disc, the surrounding high purity quartz stone slab of wheel roller is liner, form circle to mill cylindrical shell, the both sides of cylindrical shell are two pillar stiffeners, the drive unit of the wheel rollers such as the motor in supporting-point roller mill, step-down gear; The other both sides of wheel roller are then installation order numbers is 120 object discharging screen clothes, is beneficial to mortar and overflows.The mortar Surface field intensity of overflowing is after the magnetic separator of 5000 Gausses carries out three grades of magnetic separation, classification is carried out again with the flexible sizing screen of multiple 150 order that glass-reinforced plastic material makes, collect the sand powder of more than below 150 orders 300 order as work in-process, with for subsequent use after centrifuge dewatering, silica powder more than 150 orders again Returning wheel grinds Machine-made Sand powder, with being pumped into pressure filter after mortar inflow thickener precipitation below 300 orders, namely filter cake is silicon powder after drying, and the clear water after precipitation recycles with pumped back workshop again.
5, the material in 4 is sent in drying machine and carries out drying, after dried material carries out magnetic separation with permanent magnetic separators more than 7500 Gausses again, the special quartz sand powder of high quality TFT-LCD base plate glass can be obtained.After testing: SiO
2:>=99.7%, Fe
2o
3: 0.008%, Al
2o
3: 0.086%, K
2o+Na
2o:0.017%, grain size intervals: 150 ~ 400 orders, wherein 200 order ~ 300 order>=68%, below 400 orders≤5%, 150 orders more than be zero, chlorine ion concentration :≤5ppm.
Embodiment 3
1, select the white quartz deposit of Qinglong County, Qinhuangdao, Hebei province to be raw material, aluminium sesquioxide content: the white vein quartz ore of 0.09% is raw material, it is used clear water wash clean mouth, carry out artificial hand selection, reject containing for subsequent use after the impurity ores such as mica, feldspar, mountain stone.
2, the ore in 1 with after crusher in crushing to particle diameter≤25 mm granules, with color selector removing containing after variegated impurity particle, send in pickling tank, with the hydrochloric acid of concentration 31%, after room temperature dynamically leaches 18 hours, bleed off acid solution recovery, again with clear water ore washing to neutrality, more for subsequent use with drying after deionized water wash 3 times.
3, the material after drying in 2 is sent in quartzy calcining furnace and after 45 minutes at the temperature calcination of 950 degree, puts into watch-quench tank 0-10 degree cold water and carry out shrend, after shrend, pull out, then artificial hand selection is except for subsequent use after impurity elimination.
4, wet milling sand powder is carried out in the muller that material feeding high purity quartz in 3 is made and the wheel roller of mill disc, the surrounding high purity quartz stone slab of wheel roller is liner, form circle to mill cylindrical shell, the both sides of cylindrical shell are two pillar stiffeners, the drive unit of the wheel rollers such as the motor in supporting-point roller mill, step-down gear; The other both sides of wheel roller are then installation order numbers is 120 object discharging screen clothes, is beneficial to mortar and overflows.The mortar Surface field intensity of overflowing is after the magnetic separator of 7500 Gausses carries out three grades of magnetic separation, then carries out classification with the hydroclassifier that plastic material makes.Collect the sand powder of more than below 150 orders 300 order as work in-process, with for subsequent use after centrifuge dewatering, silica powder more than 150 orders again Returning wheel grinds Machine-made Sand powder, with being pumped into pressure filter after mortar inflow thickener precipitation below 300 orders, namely filter cake is silicon powder after drying, and the clear water after precipitation recycles with pumped back workshop again.
5, the material in 4 is sent in drying machine and carries out drying, after dried material carries out magnetic separation with permanent magnetic separators more than 7500 Gausses again, the special quartz sand powder of high quality TFT-LCD base plate glass can be obtained.After testing: SiO
2: 99.72%, Fe
2o
3: 0.008%, Al
2o
3:≤0.08%, K
2o+Na
2o :≤0.015%, grain size intervals: 150 ~ 400 orders, wherein 200 order ~ 300 order>=72%, below 400 orders≤5%, 150 orders more than be zero, chlorine ion concentration :≤4ppm.
Claims (5)
1. the production method of a TFT-LCD base plate glass silica powder, it is characterized in that comprising the following steps: (1), the white vein quartz ore selecting aluminium sesquioxide content≤0.1% are raw material, clean laggard row artificial hand selection, for subsequent use after rejecting wherein contained impurity ore;
(2) after, the ore crusher in crushing after removing impurity in step (1) being become the ore particles of particle diameter≤25 millimeter, with color selector removing variegated impurity particle wherein, then ore particles is sent in pickling tank, with the chlorohydric acid pickling of mass concentration 28 ~ 31%, after at room temperature dynamically leaching 18 ~ 24 hours, bleed off the hydrochloric acid in pickling tank, then with water the ore particles after pickling fully wash dry to neutrality for subsequent use;
(3) after, the ore particles after drying being sent into and is calcined 45 ~ 60 minutes in quartzy calcining furnace under the temperature calcination of 900 ~ 950 DEG C, ore particles is put into the watch-quench tank water of 0 ~ 10 DEG C and carry out shrend, after shrend, ore particles is pulled out, then except for subsequent use after impurity elimination;
(4), wet milling mortar is carried out by ore particles obtained in step (3) feeding wheel roller, the muller of described wheel roller and mill disc all adopt quartz to make, the liner of the cylindrical shell of milling of wheel roller is quartzite slate, and in whole sand powder process processed of milling, material does not contact with irony;
(5) after the magnetic separator being 5000 ~ 7500 Gausses by mortar Surface field intensity obtained in upper step carries out three grades of magnetic separation, then carry out classification, collection cut size be 150 ~ 300 object sand powder as work in-process, with for subsequent use after centrifuge dewatering;
(6), by the sand powder after dehydration carry out drying, after dried sand powder carries out magnetic separation with permanent magnetic separators more than 7500 Gausses again, can obtain TFT-LCD base plate glass silica powder, wherein the massfraction of each component is as follows: SiO
2:>=99.7%, Fe
2o
3:≤0.01%, Al
2o
3:≤0.1%, K
2o+Na
2o :≤0.02%, grain size intervals: 150 ~ 400 orders, wherein 200 order ~ 300 order>=65%, below 400 orders≤5%, 150 orders more than be zero, chlorine ion concentration :≤8ppm.
2. production method according to claim 1, it is characterized in that: reuse after laggard for the HCl recovery in pickling tank row relax in step (2), when washing the ore particles after pickling, first with clear water ore particles washing to neutral, then use deionized water wash 3 times.
3. production method according to claim 1, it is characterized in that: in step (5), collection cut size is that 150 ~ 300 object sand powder are as after work in-process, mortar more than 150 orders again Returning wheel mill repeats to make sand powder, with being pumped into pressure filter press filtration after mortar inflow thickener precipitation below 300 orders, namely filter cake obtains silicon powder after drying, and the clear water after precipitation recycles with pumped back workshop again.
4. production method according to claim 1, is characterized in that: when carrying out classification in step (5), the hydroclassifier made by non-metallic material, or carries out classification with the flexible sizing screen of multiple 150 order that non-metallic material make.
5. production method according to claim 1, is characterized in that: the both sides of cylindrical shell of milling in the wheel roller used in step (5) are two pillar stiffeners, the drive unit of the wheel rollers such as the motor in supporting-point roller mill, step-down gear; It is 120 object discharging screen clothes that the other both sides of wheel roller are provided with order number.
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CN106000622A (en) * | 2016-06-06 | 2016-10-12 | 赣州金环磁选设备有限公司 | Color-magnetic separation combined sorting method for high-purity quartz sand produced through quartzite |
CN106892430A (en) * | 2017-04-10 | 2017-06-27 | 南京中燊硅基新材料科技有限公司 | A kind of preparation method of ultrapure quartz sand |
CN107162008A (en) * | 2017-06-20 | 2017-09-15 | 合肥市惠科精密模具有限公司 | A kind of preparation technology of TFT LCD substrates glass quartz sand powder |
CN107324342A (en) * | 2017-05-20 | 2017-11-07 | 合肥市惠科精密模具有限公司 | A kind of production technology of AMOLED base plate glass silica flour |
CN108866348A (en) * | 2018-07-27 | 2018-11-23 | 阳谷祥光铜业有限公司 | A kind of space blowing material preparation technology and stock preparation system of matte |
CN108975679A (en) * | 2018-09-05 | 2018-12-11 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of TFT-LCD glass substrate silicon powder preparation method |
CN109665529A (en) * | 2019-01-22 | 2019-04-23 | 黄冈师范学院 | A kind of production method for the glass sand not generating quartz tail sand |
CN110156028A (en) * | 2019-05-29 | 2019-08-23 | 连云港原舜光伏材料有限公司 | A kind of glass sand processing technology |
CN110510620A (en) * | 2019-09-11 | 2019-11-29 | 江苏凯达石英股份有限公司 | The method of purification of glass sand tailing |
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CN106000622A (en) * | 2016-06-06 | 2016-10-12 | 赣州金环磁选设备有限公司 | Color-magnetic separation combined sorting method for high-purity quartz sand produced through quartzite |
CN106000622B (en) * | 2016-06-06 | 2018-01-09 | 赣州金环磁选设备有限公司 | A kind of color of quartzite production glass sand-magnetic separation joint dressing method |
CN106892430A (en) * | 2017-04-10 | 2017-06-27 | 南京中燊硅基新材料科技有限公司 | A kind of preparation method of ultrapure quartz sand |
CN106892430B (en) * | 2017-04-10 | 2019-07-12 | 天津天兆御华科技有限公司 | A kind of preparation method of ultrapure quartz sand |
CN107324342A (en) * | 2017-05-20 | 2017-11-07 | 合肥市惠科精密模具有限公司 | A kind of production technology of AMOLED base plate glass silica flour |
CN107162008A (en) * | 2017-06-20 | 2017-09-15 | 合肥市惠科精密模具有限公司 | A kind of preparation technology of TFT LCD substrates glass quartz sand powder |
CN108866348A (en) * | 2018-07-27 | 2018-11-23 | 阳谷祥光铜业有限公司 | A kind of space blowing material preparation technology and stock preparation system of matte |
CN108975679A (en) * | 2018-09-05 | 2018-12-11 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of TFT-LCD glass substrate silicon powder preparation method |
CN109665529A (en) * | 2019-01-22 | 2019-04-23 | 黄冈师范学院 | A kind of production method for the glass sand not generating quartz tail sand |
CN110156028A (en) * | 2019-05-29 | 2019-08-23 | 连云港原舜光伏材料有限公司 | A kind of glass sand processing technology |
CN110510620A (en) * | 2019-09-11 | 2019-11-29 | 江苏凯达石英股份有限公司 | The method of purification of glass sand tailing |
CN110510620B (en) * | 2019-09-11 | 2021-08-24 | 江苏凯达石英股份有限公司 | Purification method of high-purity quartz sand tailings |
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