CN105036545B - The process of gas liquid inclusion in a kind of rejecting glass sand - Google Patents
The process of gas liquid inclusion in a kind of rejecting glass sand Download PDFInfo
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- CN105036545B CN105036545B CN201510371544.3A CN201510371544A CN105036545B CN 105036545 B CN105036545 B CN 105036545B CN 201510371544 A CN201510371544 A CN 201510371544A CN 105036545 B CN105036545 B CN 105036545B
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Abstract
The present invention relates to glass sand purification technique field, discloses a kind of process for rejecting gas liquid inclusion in glass sand.It is that the power of the microwave is 1000~4000w, and the radiation treatment time is 1~10h, and glass sand single treatment amount is 100~600g through microwave radiation processing by glass sand.Operation is simple for the process of gas liquid inclusion in present invention rejecting glass sand, Environmental Safety, it is good to reject effect, not only make it possible that common quartz mine replaces the mineral crystal of resource exhaustion, and can also produce and reduced more than an order of magnitude than gas liquid inclusion content in mineral crystal；The inventive method makes major contribution for the raw material replacement upgrading of quartz glass.
Description
Technical field
The present invention relates to the purification technique field of glass sand, is rejected more particularly, to one kind in glass sand
The process of gas liquid inclusion.
Background technology
Quartz glass is one-component SiO2Extraordinary high-grade glass, have fabulous chemical stability, infrared spectrum saturating
Cross that rate is high, impact resistance is strong, high temperature resistant（More than 1800 degree Celsius）Indeformable, resistance to X-ray radiation, the special excellent thing of electric insulation
Reason, chemical property.It is extensively production of polysilicon, photoelectric source, electronics industry, optical communication, medical instrument, SiO2It is thin-film material, big
Scale integrated circuit, laser, Aero-Space, military industry etc. provide tip materials, are indispensable in high-tech.
Last century mid-term, people are raw material production quartz glass with mineral crystal, can be with its extensive application, and crystal ore deposit is
Close to exhaustion, it can not meet the fast development of modern high technology industry already.In decades, people, which have to explore, substitutes crystal
Quartz glass produce new dispensing.
Relative to crystal, quartz mine contains more impurity.Its impurity can be divided into structure composition impurity and non-structural
Property impurity.Unstructuredness impurity is the impurity outside quartz mine crystal, such as surface adhesion thing, associated mineral.Impurity is removed at present
Technology, such as:Water quenching, flotation, pickling, magnetic separation, high-temperature vacuum processing, chlorination, superconduction choosing, electric separation, ultrasonication, doping purification
It can meet quartz glass requirement substantially etc. serial means.Structural impurity refers to the impurity formed in quartz mine crystal growth,
Also referred to as microdefect, such as gas liquid inclusion, gas liquid inclusion be mainly made up of at room temperature liquid phase and a minute bubbles two
Phase inclusion enclave, by H when this is accompanied by mineral growth2、O2、N2、CO、CH4、CO2 、H2O etc. is wrapped in what is formed in quartz crystal
Structural impurity, existing process technology are difficult to eliminate such defect at all, and it is also the weight for influenceing quartz glass purity and performance
Want factor.
Generally contain fluid inclusion in quartz mine, current existing technique is difficult to remove.Countries in the world are in 20th century 80
Age, China, the U.S., Japan, Russia, France, Germany etc. are all realized with common quartzy silicon ore deposit by using hydrofluoric acid dips
After clean, high-temperature calcination, water quenching, electric separation, flotation, magnetic separation, even high temperature is floating boils, at high-temperature vacuum for " chloroazotic acid " immersion for a long time
The selected processing purification of the means such as reason, chlorination, superconduction choosing, ultrasonic wave, doping purification, has picked its acrobatics in addition to gas liquid inclusion
Except crystal can be replaced completely.But for the rejecting to greatest extent of the gas liquid inclusion in the tiny crystals in glass sand
It is still helpless.Even if the U.S. You Niming currently called oneself with " world standard purity "（Unimin）The product of company, also also has
Micro 50PPM or so is present.Studied according to Hou Qinglin etc., the quartz mine self-carry on the ground such as import Angola of China, Madagascar
Gas liquid inclusion in pure so-called glass sand is still in more than 120PPM.Although it also can remove most of gas-liquid by beating to stick together
Inclusion enclave, but still there is structural gas liquid inclusion to become scattered about during quartz glass sticks together so that produce quartz glass with quartz sand
Purposes is greatly limited to.
Mainly there is the minimizing technology of gas liquid inclusion in existing quartz sand：Soda acid difference of corrosion method, cold heat decrepitation method,
Chlorination degassing method, microwave radiation-acid-hatching of young eggs etc., it removes the effect or not satisfactory of gas liquid inclusion, or excessively complicated, behaviour
Made into potential safety hazard be present, production technology is not environmentally.
The existing research in this area thinks that only relying on microwave treatment can not be completely severed gas liquid inclusion or wrap up gas-liquid
Impurity after body rupture is peeled off, so the quality requirement of one-level crystal can not be reached, therefore it is necessary on the basis of microwave treatment
With reference to other various processing means, including plus load（Such as ball milling）, acid etching etc..The applicant is devoted for years in microwave treatment
The research of glass sand, formerly research in sum up using microwave treatment glass sand do not reach mineral crystal quality will
Ask, it is unsatisfactory with reference to other plus loads and/effect that the processing means of acid etching are obtained, and also the processing means such as acid etching are not
Environmental protection, it is important to can still bring the impurity such as hydrone into processing procedure.
The content of the invention
The technical problem to be solved in the present invention is to overcome the removal technology of gas liquid inclusion in existing glass sand not
A kind of foot, there is provided process for rejecting gas liquid inclusion in glass sand.
Another technical problem to be solved by the present invention is that provide the gas liquid inclusion being prepared using the elimination method
Content reaches the glass sand of even above one-level crystalline quality requirement.
The purpose of the present invention is achieved by the following technical programs：
A kind of process for rejecting gas liquid inclusion in glass sand is provided, is through microwave radiation by glass sand
Processing, the power of the microwave are 1000~4000w, and the radiation treatment time is 1~10h, glass sand single treatment
Measure as 100~600g.
For some gas liquid inclusions, can be burst before reaching homogenization temperature, the inclusion enclave of 5~10 microns of sizes in quartz
（0.1~300）Burst in the range of Mpa, and for the bursting stress required for smaller gas liquid inclusion up to 500
Mpa.The present invention summarizes to obtain through scientific research with reference to long-term many experiments, can rationally utilize SiO in quartz mine2The dielectric of molecule
Constant is for 3~5, and the main component H in gas liquid inclusion2O dielectric constant reaches as high as 88, so when suitable power
After the microwave treatment reasonable time hydrone can absorb and produce vibration, persistently risen sharply from phase friction temperature between molecule, due to it
" space " is restricted, then causes the increase of " inside " pressure, when reach certain " limit " then avulsion crystal " gushing " and go out.
The present invention, which breaks prior art, must combine the limitation of plus load and/or acid etching, and summary obtains microwave treatment science essence
True technique, realize the micro gas liquid inclusion realized and rejected in quartz sand only with the technological means of microwave treatment.
Preferably, the power of the microwave is 1500~2500w, and the radiation treatment time is 1~6h, glass sand
Single treatment amount is 200g.
It is further preferred that the power of the microwave is 1600w, the radiation treatment time is 80min.
Preferably, the high purity quartz ore deposit is Madagascar's quartz mine.
Preferably, the Task-size Controlling of the glass sand is in 0.178~1.43mm.
Present invention simultaneously provides the glass sand being prepared using the process.
The glass sand is to be obtained quartz sand through thick broken, sorting, calcining, screening using existing traditional handicraft.Institute
It is the gas liquid inclusion quartz mine rich in water to state quartz mine, i.e., liquid component is mainly the quartz of water in described gas liquid inclusion
Ore deposit.
Beneficial effects of the present invention：
Prior art is that glass sand is first passed through into microwave treatment to produce micro-crack, then passes through acid etching again
Impurity in the inclusion enclave of micro-crack is produced to discharge.Accurate process conditions of the invention by adjusting microwave treatment so that at this
Obtained glass sand is handled under the conditions of invention microwave processes, its gas liquid inclusion content is very low, and amount is also seldom,
Acid etching step is successfully abandoned, avoids the severe of environmental pollution and operating condition.
The process operation that the present invention rejects gas liquid inclusion in glass sand is upper simple and easy, Environmental Safety, picks
Except effect is good, not only make it possible that common quartz mine replaces the mineral crystal of resource exhaustion, and can also produce than day
Gas liquid inclusion content reduces glass sand more than an order of magnitude in right crystal, is the raw material replacement upgrading of quartz glass
Make major contribution.
Brief description of the drawings
Fluid inclusion in Fig. 1 Madagascar ore deposit quartz mine.
Fluid inclusion in the ore deposit quartz mine of Fig. 2 Henan Dengfeng.
Fluid inclusion in the ore deposit quartz mine of Fig. 3 East Sea.
Fluid inclusion in Fig. 4 Huayuan, Hunan ore deposit quartz mines.
Fluid inclusion in Fig. 5 Macheng, hubei Province ore deposit quartz mines.
Quartz sand infrared spectrum before Fig. 6 microwave radiations.
Quartz sand infrared spectrum after Fig. 7 microwave radiations.
Sample microscope photo before Fig. 8 microwave treatments.
Sample microscope photo after Fig. 9 microwave treatments.
Influence of Figure 10 microwave powers to quartz sand light transmittance.
Influence of Figure 11 microwave treatment times to quartz sand light transmittance.
Embodiment
The present invention is further described with specific embodiment below in conjunction with the accompanying drawings, unless stated otherwise, the present invention uses
Reagent and raw material be this area routinely reagent and raw material purchased in market.
The applicable quartz sand ore raw material optimization experiment of the inventive method of embodiment 1
The present embodiment is with following quartz mine A- Madagascar quartz mines, B- Donghai Area, Jiangsu quartz mines, C- Huayuan, Hunans
Quartz mine, D- Macheng, hubei Province quartz mines, description of test is carried out exemplified by the quartz mine of E- Henan Dengfeng, the quartz mine in other sources is not
Repeat one by one herein.
The impurity content of the quartz mine of different sources is detected, data record is in table 1；Detect the quartz mine of different sources
Gas liquid inclusion component content, data record is in table 2；By the quartz mine of different sources through conventional traditional handicraft, through it is thick it is broken,
Sorting, calcining, screening obtain glass sand, and Task-size Controlling is in 0.178~1.43 mm；
The quartz mine impurity content of table 1（Unit：PPM）
| Sample | Al | Fe | Ca | Mg | B | Li | Na | K | Mn | Ni | Cu | Cr |
| A | 16.82 | 2.25 | 0.63 | 2.5 | <0.05 | 0.14 | 6.14 | 5.41 | 0.25 | <0.05 | 0.21 | <0.05 |
| B | 17.87 | 10.1 | 0.74 | 2.5 | <0.05 | 1.24 | 9.2 | 9.65 | 0.56 | 0.01 | 0.28 | <0.05 |
| C | 19.4 | 2.36 | 0.68 | 1.21 | <0.05 | 2.31 | 11.2 | 11.2 | 0.52 | 0.02 | 0.32 | <0.05 |
| D | 17.14 | 0.84 | 1.41 | 0.32 | <0.05 | 0.45 | 2.24 | 9.35 | 0.04 | <0.05 | 0.26 | <0.05 |
| E | 36.2 | 5.61 | 2.41 | 0.46 | <0.05 | 0.25 | 16.91 | 15.97 | 0.09 | <0.05 | 0.58 | <0.05 |
The quartz mine gas liquid inclusion component content of table 2（Unit：mg/kg）
| Sample | CO2 | H2O | H2 | O2 | N2 | CH4 | CO | Total amount |
| A | 5.41 | 94.58 | 0.08 | 1.30 | 0.80 | 3.65 | 18.25 | 143.93 |
| B | 32.82 | 258.93 | 0.07 | 0.15 | 9.17 | 0.98 | 12.21 | 314.31 |
| C | 38.50 | 118.04 | 0.93 | 0.29 | 10.21 | 1.96 | 13.23 | 182.32 |
| D | 52.45 | 127.10 | 0.05 | 0.21 | 19.81 | 0.96 | 10.78 | 194.63 |
| E | 60.51 | 168.27 | 2.21 | 0.78 | 28.24 | 3.56 | 10.38 | 264.94 |
In Tables 1 and 2, A represents Madagascar's ore deposit, and B represents Donghai Area, Jiangsu ore deposit, and C represents Huayuan, Hunan
Ore deposit, D represent Macheng, hubei Province ore deposit, and E represents Henan Dengfeng ore deposit.
It can be seen in table 1 that Al3+ content is 16.82 in the quartz sand in Madagascar mining area, it is less than one-level crystal
In Al3+Content be 17.8, and Li+、K+、Na+、Ca2+、Fe2+Content Deng element is respectively less than East Sea one-level crystal, wherein
Mg2+Content and East Sea one-level crystal in Mg2+Content and its close.Secondly it is the quartz mine in Macheng, hubei Province mining area, and Henan
The impurity content of the quartz mine in Dengfeng mining area is most, and the impurity content close to level Four crystal forms.
As seen from Table 2, in the quartz mine of East China Sea gas liquid inclusion H2O density is up to 0.823, its
Secondary is that Madagascar's quartz sand is 0.657, but Li in the quartz mine of the East Sea+、K+、Na+、Ca2+、Fe2+ 、Al3+Far
Far above one-level crystal.So East China Sea is not suitable as test raw material, and Madagascar area is more suitable.
From Fig. 1 to Fig. 5, in the quartz mine in Madagascar area, the liquid phase volume packing density containing inclusion enclave is most
Greatly, it is secondly East Sea mining area, and the liquid phase volume packing density of gas liquid inclusion is minimum in the quartz mine in Henan Dengfeng mining area.
Embodiment 2
The present embodiment illustrates the technique that the present invention rejects gas liquid inclusion in glass sand with Madagascar's quartz sand
Condition experiment result.
Microwave radiation is tested
Using 1000w microwave powers, quartz specimen 30min is radiated, sample temperature is up to 550 DEG C or so, by microwave radiation
Front and rear quartz sand makees infrared contrast, as a result as shown in Fig. 6 and Fig. 7, shows after 1000w microwave treatments, than without microwave
The infrared absorption peak intensity and area of the sample hydrone of processing are significantly increased, and IRintensity has and largely increased,
Illustrate there is new hydrone generation.Research shows that newly-generated hydrone derives from the hydroxyl water (OH) in lattice-。
As seen from Figure 8, the larger gas liquid inclusion of a number of volume before microwave treatment in sample be present, can by Fig. 9
See, after microwave action, volume that these gas liquid inclusions have reduces, and with new liquid phase inclusion all living creatures into.This is due to micro-
The effect of wave field selection heating, produces very big pressure at gas liquid inclusion interface, promotes these gas liquid inclusions to burst or on boundary
Face produces micro-crack.The generation of new liquid phase inclusion group is due under microwave field action, is produced necessarily inside gas liquid inclusion
Pressure and temperature, promote hydroxyl water (OH)-generation hydrone in lattice, and along the lattice passage of increase or the space of formation
Between form a large amount of new liquid phase inclusions.
By the quartz sand after the microwave radiation processing of different capacity, its light transmission rate is observed using 721 spectrophotometers
Situation, experimental result are as shown in Figure 10.As seen from Figure 10, when the time of microwave treatment is 50min, when power is 1200W, sample
The light transmittance of product significantly increases, and as the increase of microwave power, the light transmittance of sample are presented incremental trend, work as microwave action
Time more than 1600W when, the light transmittance of sample reaches higher value and is not further added by substantially, accordingly, it is determined that best power is
1600w。
As seen from Figure 11, from the experimental data of light transmittance it was found that when power is 1000W, the time of microwave treatment
For 30min when, the light transmittance of sample is significantly increased, and with the increase of microwave action time, the light transmittance of sample, which is presented, to be incremented by
Trend, when the time of microwave action is more than 80min, the light transmittance of sample is not further added by substantially, accordingly, it is determined that microwave is optimal
Time is 80min.During 40min, there is situation about declining in light transmittance, and proves that this is due in test process through analysis of experiments
Photometric error causes.
Table 4 and table 5 sets forth glass sand through microwave condition of the present invention before and after the processing gas liquid inclusion content and
Bubble number experimental result after molten.In table 4 and table 5, sample 1 is glass sand raw material, sample 2 be by sample 1 through microwave at
Glass sand after reason.From table 4, after 1600w, 80min microwave radiation, in quartz sand gas liquid inclusion content from
176.94 quickly fall to 85.39, much smaller than the content 98.74 of gas liquid inclusion in one-level crystal.
Front and rear result after the microwave treatment of table 4
| Sample | H2O | CO2 | O2 | N2 | CH4 | CO | ∑ |
| Sample 1 | 163.05 | 9.45 | 0.3 | 0.22 | 2.31 | 2.31 | 176.94 |
| Sample 2 | 72.51 | 9.13 | 0.16 | 0.20 | 2.01 | 1.38 | 85.39 |
| One-level crystal | 84.17 | 9.74 | 0.30 | 0.50 | 2.35 | 1.62 | 98.74 |
The microwave treatment of table 5 is to gas liquid inclusion content in quartz sand and the influence result of molten rear bubble number
| Sample | Gas liquid inclusion ∑（mg/kg） | Bubble number in a diameter of 6mm kens |
| Sample 1 | 176.94 | 30 |
| Sample 2 | 85.39 | 10 |
| One-level crystal | 98.747 | 21 |
From table 5, by present invention determine that microwave condition processing after, the gas liquid inclusion content in sample significantly drops
Low, especially Madagascar's quartz sand, after being melting into quartz glass, air bubble content also significantly reduces, in a diameter of 6mm kens
Bubble number drops to 10 from 30, so that the transparency of quartz glass dramatically increases, it is no longer necessary to using the side of acid etching
Method is further processed, and has broken the custom thinking that prior art uses acid etching, has been reduced on the basis of product quality is ensured
Environmental pollution and the unsafe hidden danger of operation.
Claims (2)
1. a kind of process for rejecting gas liquid inclusion in glass sand, it is characterised in that be through micro- by glass sand
Wave radiation is handled without acid etching, reaches the quality requirements higher than one-level crystal, the glass sand adds for motor
This adds quartz mine, and the power of the microwave is 1600w, and the radiation treatment time is 80min, glass sand single treatment amount
For 200g；The Task-size Controlling of the glass sand is in 0.178~1.43mm.
2. the glass sand that process is prepared according to claim 1.
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| CN105645757A (en) * | 2015-12-31 | 2016-06-08 | 侯清麟 | Process for manufacturing ultra-pure quartz sand |
| CN106000621B (en) * | 2016-06-01 | 2019-04-19 | 安徽晶晶石英科技有限公司 | A kind of method of the compound purifying quartz sand of chlorination-acidleach |
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|---|---|---|---|---|
| JPH0640713A (en) * | 1992-07-21 | 1994-02-15 | Mitsubishi Material Kuootsu Kk | Method for dehydrating quartz powder |
| CN102180584A (en) * | 2011-02-18 | 2011-09-14 | 银锐明 | Method for removing gas-liquid inclusion and impurity during high-purity quartz sand production |
| CN102775065A (en) * | 2012-06-29 | 2012-11-14 | 湖南工业大学 | Process for removing gas-liquid inclusions and hydroxyl water (OH)- in high-purity quartz sand |
-
2015
- 2015-06-30 CN CN201510371544.3A patent/CN105036545B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0640713A (en) * | 1992-07-21 | 1994-02-15 | Mitsubishi Material Kuootsu Kk | Method for dehydrating quartz powder |
| CN102180584A (en) * | 2011-02-18 | 2011-09-14 | 银锐明 | Method for removing gas-liquid inclusion and impurity during high-purity quartz sand production |
| CN102775065A (en) * | 2012-06-29 | 2012-11-14 | 湖南工业大学 | Process for removing gas-liquid inclusions and hydroxyl water (OH)- in high-purity quartz sand |
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| 《微波-酸蚀去除石英砂中气液包裹体优选矿研究》;侯清麟 等;《湖南工业大学学报》;20130131;第27卷(第1期);1-5页 * |
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Inventor after: Hou Yihui Inventor after: Liu Pingle Inventor after: Hou Qinglin Inventor before: Hou Qinglin Inventor before: Hou Yihui |
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Effective date of registration: 20180103 Address after: 411100 west suburb of Xiangtan City, Hunan Applicant after: Xiangtan University Applicant after: Hunan University of Technology Address before: 412000 Taishan Road, Tianyuan District, Hunan, No. 88, No. Applicant before: Hunan University of Technology |
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