CN108101357A - A kind of quartz sand oxalic acid remove iron after saliferous give up oxalic acid water processing and reuse method - Google Patents
A kind of quartz sand oxalic acid remove iron after saliferous give up oxalic acid water processing and reuse method Download PDFInfo
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- CN108101357A CN108101357A CN201711395697.7A CN201711395697A CN108101357A CN 108101357 A CN108101357 A CN 108101357A CN 201711395697 A CN201711395697 A CN 201711395697A CN 108101357 A CN108101357 A CN 108101357A
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- oxalic acid
- quartz sand
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- saliferous
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/022—Purification of silica sand or other minerals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
Abstract
The present invention propose a kind of quartz sand oxalic acid except after iron saliferous give up oxalic acid water processing and reuse method, including pickling process, recovery of oxalic acid process and tail mud treatment process, this technology utilization absorption resin to predetermined substance characterization of adsorption, target ferro element in oxalic acid cleaning solution is effectively removed, reuses the oxalic acid liquid of pollution;Former technique is changed to use in lime and discharge, and the way that substantial amounts of oxalic acid is caused to be lost in.This method only removes objectionable impurities, and oxalic acid and water overwhelming majority return system are reused, the consumption of oxalic acid and lime is greatly reduced, while reduces the discharge capacity of the three wastes;The processing cost of glass sand is significantly reduced, while bringing good economic benefit to enterprise, also meets demand of the society to low price glass sand;Three-protection design is thorough, process water cycling and reutilization, reduces the consumption and discharge capacity of water, becomes the good raw material in cement plant after the heat treatment of tail mud.
Description
Technical field
The present invention relates to quartz sand manufacture field more particularly to quartz sand oxalic acid except after iron saliferous give up oxalic acid water processing and
The method of reuse.
Background technology
Photovoltaic glass and quartz glass are more demanding to required raw material quartz sand, the iron-holder of quartz sand needed for photovoltaic glass
It is less than 80PPM, quartz glass requires higher to the iron content of quartz sand.Natural quartz ore is by broken, washing, high intensity magnetic separation
Afterwards, the iron-holder still containing more than 100PPM, the quartz sand iron-holder higher after Quartz sand processing, it is necessary to add to its depth
Work.The effective ways for reducing the iron content in quartz sand at present are using pickling, and most commonly used is oxalic acid heating acid cleaning process.
Since ferro element is reacted into the complex compounds such as ferrous oxalate in acid cleaning process, solubility in water it is very low (ferrous oxalate it is molten
There was only 0.022g/100g under solution degree room temperature, other complex compounds are slightly higher), pickling number cannot be too many, and otherwise, the oxalic acid of generation is sub-
The complex compounds such as iron can be crystallized out from water, be attached to using quartz sand particle on the particle surface of nucleus, quartz sand to be caused to produce
Product are unqualified, it is therefore desirable to be continuously updated pickle.Therefore the oxalic acid only a small part in pickle is utilized, big portion
Oxalic acid is divided to be discharged to be neutralized with lime, causes oxalic acid waste, while consumes substantial amounts of lime, bigger is brought to environment
Pollution.Oxalic acid calcium salt after neutralization is high organic matter salt, and COD is very high, and the fixed-end forces center that can only spend is burned
It can solve the problems, such as partial contamination.
The defects of technique, is that the utilization rate of oxalic acid is low, and three-protection design amount is big, of high cost.It is brought to manufacturing enterprise huge
Financial burden, processing factory's cost remains high.
In existing patent application, as Patent publication No is:The patent of invention of 105692629 A of CN, discloses a kind of acid
The method for washing quartz sand Rapid Cleaning is to send the quartz sand after pickling into water washing device, is buried into quartz sand more
A absorbent packet, the absorbent packet are activated carbon fibre material, and the grain size that 1~5g is housed inside the absorbent packet is 0.2~0.5mm
Green stone, adsorb quartz sand in residual acid, by multiple clear water washing finally obtain pure quartz sand, devise acid solution
Retracting device first passes through sour ingredient volatile in heating recovery acid solution, and acid is converted into precipitation discharge by pH is overregulated, is added
Entering lye to discharge the iron tramp in acid solution, this kind of mode is that calcium carbonate is reacted with oxalic acid using green stone, is to consume oxalic acid,
Rather than oxalic acid is recycled, oxalic acid utilization rate is not high.
The content of the invention
In order to solve the above technical problems, the present invention propose a kind of quartz sand oxalic acid except after iron saliferous give up the processing of oxalic acid water
And the method for reuse, including pickling process, recovery of oxalic acid process and tail mud treatment process;
The pickling process comprises the following steps:
S1:It by dissolving oxalic acid in hot water, and is put into the pond for installing quartz sand, sour water is higher by quartz sand 100mm, constantly
Circulating-heating acid solution between reaching pond temperature and maintaining 40 DEG C -80 DEG C, maintains a few hours;
S2:Sour water is bled off, is gone over low temperature sour water from hot quartz sand pond, to recycle thermal energy;And it is taken out with vacuum equipment
Dry acid water, quartz sand are produced from Sha Chizhong, into cleaning process;
S3:It is cleaned in suspension backwash equipment with the limewash that pH value is 8.5, is finally rinsed with deionized water, examined
Test packaging and storage;
The recovery of oxalic acid process comprises the following steps:
A1:Sand filtration;The useless oxalic acid aqueous solution filtered in above-mentioned S2 is taken, carries out sand filtration, the useless oxalic acid water after sand filtration, which is put in, to be treated
In process container;
A2:Resin adsorption:Pending useless oxalic acid water is conveyed by flowmeter with infusion pump, and adsorption resin column is sent into from top
Tank body, volume flow rate are controlled between 2-4, and the oxalic acid water after absorption is flowed out from the bottom of adsorption column tank body, by Line glass
It is spare that visor is sent into clear acid solution storage tank;
A3:With quartz sand acid washing lotion:The clear acid solution dispensing in A2 is taken, powdery oxalic acid is added to reach required concentration of oxalic acid, again
Carry out pickling process.
Preferably, in the recovery of oxalic acid process, adsorption resin column tank body sets multiple, single resin column tube body saturation
Afterwards, adsorption column charging is terminated immediately, and material inlet valve is switched in another spare adsorption resin column and is adsorbed.
Preferably, absorption resin regeneration process is further included, including adding in regenerative elution liquid, absorption into absorption resin container body
It is spare after resin regeneration.
Preferably, in S3, the clear water after sedimentation basin precipitates after sand filter filters, is back to containing the clear of sour quartz sand again
It washes, recycles.
Preferably, the tail mud treatment process is:The glar in S3 is taken to be calcined after pressure-filteration drying, generation metal oxidation
After object, the stable silicates with silica generation.
Quartz sand oxalic acid proposed by the present invention remove iron after saliferous give up oxalic acid water processing and reuse method have it is following beneficial
Effect:1st, using adsorb resin to predetermined substance characterization of adsorption, the target ferro element in oxalic acid cleaning solution is carried out effective
It removes, reuses the oxalic acid liquid of pollution.
2nd, former technique is changed to use in lime and discharge, and the way that substantial amounts of oxalic acid is caused to be lost in.This method is only moved
Go out objectionable impurities, oxalic acid and water overwhelming majority return system are reused, greatly reduce the consumption of oxalic acid and lime, together
When reduce the discharge capacitys of the three wastes;The processing cost of glass sand is significantly reduced, economic effect well is brought to enterprise
While beneficial, demand of the society to low price glass sand is also met.
3rd, three-protection design is thorough, process water cycling and reutilization, reduces the consumption and discharge capacity of water, after the heat treatment of tail mud
Become the good raw material in cement plant.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described.
Fig. 1 is the process flow chart of the present invention;
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes.
If can solve the problems, such as that the oxalic acid in discarded pickle returns to pickling process and is continuing with, the utilization rate of oxalic acid obtains
To increasing substantially, the treating capacity and discharge capacity of the three wastes are reduced simultaneously, and above-mentioned defective workmanship just solves.This problem is solved,
First have to solve the problems, such as that iron content is stepped up in oxalic acid pickle, as long as the complex compounds such as ferrous oxalate generated in pickling
Concentration is no more than crystalline temperature concentration at the operational, and pickling effect would not be had an impact.Due to iron content in quartz sand
Content 300PPM of relatively low di-iron trioxide before pickling or so is measured, the amount containing di-iron trioxide is no more than in quartz sand per ton
300 grams, so iron content in pickle and not bery high, is calculated, the iron handled daily by daily 1000 tons of quartz sands of processing
No more than 300 kilograms, in the level less from treating capacity for remove ferro element be feasible and most economical.Draw therefore
Enter the fine resin isolation technics of comparison, separate the complex compound to tap a blast furnace.The present invention be directed to be produced in oxalic acid acid-washed quartz sand technique
Raw useless oxalic acid liquid, is adsorbed by adsorption resin column, removes the ferro element being harmful in pickle acid, except the pickle after iron returns
The method that pickling process reuses.Solution oxalic acid utilization rate is low, and three-protection design amount is big, of high cost three big drawback of three-protection design.
Tail mud after lime neutralizes mainly contains calcium oxalate etc., it is organic salt, and directly landfill can cause environment secondary
Pollution, therefore, need to carry out harmless treatment to it.Because calcium oxalate is at 500 degree or more, CO and H2O are resolved into completely, it is carried out
High temperature oxidation process generates harmless CO2 and H2O, and residue is the oxides such as calcium, iron, can intentionally add in a little silicon in calcining
Sand allows metal oxide to react with it the stable silicates of generation, thoroughly solves the problems, such as the secondary pollution of tail mud.
Specifically:The present invention propose a kind of quartz sand oxalic acid except after iron saliferous give up oxalic acid water processing and reuse side
Method, including pickling process, recovery of oxalic acid process and tail mud treatment process;
As shown in Figure 1, the pickling process comprises the following steps:
S1:It by dissolving oxalic acid in hot water, and is put into the pond for installing quartz sand, sour water is higher by quartz sand 100mm, constantly
Circulating-heating acid solution between reaching pond temperature and maintaining 40 DEG C -80 DEG C, maintains a few hours;
S2:Sour water is bled off, is gone over low temperature sour water from hot quartz sand pond, to recycle thermal energy;And it is taken out with vacuum equipment
Dry acid water, quartz sand are produced from Sha Chizhong, into cleaning process;
S3:It is cleaned in suspension backwash equipment with the limewash that pH value is 8.5, is finally rinsed with deionized water, examined
Test packaging and storage;
The isolation technics for adsorbing resin is introduced into the acid cleaning process of quartz sand subtractive process so that the purification of pickle
Processing becomes simpler, and not only processing cost is very low, but also acid pickle has obtained fully recovering, reduces oxalic acid consumption, section
About processing cost.
The recovery of oxalic acid process comprises the following steps:
A1:Sand filtration;The useless oxalic acid aqueous solution filtered in above-mentioned S2 is taken, carries out sand filtration, the useless oxalic acid water after sand filtration, which is put in, to be treated
In process container;
A2:Resin adsorption:Pending useless oxalic acid water is conveyed by flowmeter with infusion pump, and adsorption resin column is sent into from top
Tank body, volume flow rate are controlled between 2-4, and the oxalic acid water after absorption is flowed out from the bottom of adsorption column tank body, by Line glass
It is spare that visor is sent into clear acid solution storage tank;
A3:With quartz sand acid washing lotion:The clear acid solution dispensing in A2 is taken, powdery oxalic acid is added to reach required concentration of oxalic acid, again
Carry out pickling process.
Preferably, in the recovery of oxalic acid process, adsorption resin column tank body sets multiple, single resin column tube body saturation
Afterwards, adsorption column charging is terminated immediately, and material inlet valve is switched in another spare adsorption resin column and is adsorbed.
Preferably, absorption resin regeneration process is further included, including adding in regenerative elution liquid, absorption into absorption resin container body
It is spare after resin regeneration.
Preferably, in S3, the clear water after sedimentation basin precipitates after sand filter filters, is back to containing the clear of sour quartz sand again
It washes, recycles.
Preferably, the tail mud treatment process is:The glar in S3 is taken to be calcined after pressure-filteration drying, generation metal oxidation
After object, the stable silicates with silica generation.Tail mud after lime neutralization carries out the calcination processing of high temperature, and oxalic acid is divided
Solution oxidation ultimately produces carbon dioxide and water discharge, the metal oxide silicates stable with silica generation, for cement
Building materials raw material uses.Eliminate the secondary pollution of oxalic acid and its esters to environment.
Using above-mentioned technique, following embodiment is made, using this process to 1000,500 tons and 100 tons of quartz
Sand is processed and using the technique in the prior art neutralizing oxalic acid, and the amount of the oxalic acid consumed in whole process carries out pair
Than:
Embodiment 1
1000 tons of quartz sands are taken, and are equipped with oxalic acid powder, by dissolving oxalic acid in hot water, and are put into the pond for installing quartz sand
Interior, sour water is higher by quartz sand 100mm, continuous circulating-heating acid solution, between reaching pond temperature and maintaining 40 DEG C -80 DEG C,
Maintain 4 it is small when;
S2:Sour water is bled off, is gone over low temperature sour water from hot quartz sand pond, to recycle thermal energy;And it is taken out with vacuum equipment
Dry acid water, quartz sand are produced from Sha Chizhong, into cleaning process;
S3:It is cleaned in suspension backwash equipment with the limewash that pH value is 8.5, is finally rinsed with deionized water, examined
Test packaging and storage;
A1:Sand filtration;The useless oxalic acid aqueous solution filtered in above-mentioned S2 is taken, carries out sand filtration, the useless oxalic acid water after sand filtration, which is put in, to be treated
In process container;
A2:Resin adsorption:Pending useless oxalic acid water is conveyed by flowmeter with infusion pump, and adsorption resin column is sent into from top
Tank body, volume flow rate are controlled between 2-4, and the oxalic acid water after absorption is flowed out from the bottom of adsorption column tank body, by Line glass
It is spare that visor is sent into clear acid solution storage tank;
A3:With quartz sand acid washing lotion:The clear acid solution dispensing in A2 is taken, powdery oxalic acid is added to reach required concentration of oxalic acid, again
Carry out pickling process.
In whole process, oxalic acid consumption is:2-2.8 ton.
Embodiment 2
100 tons of quartz sands are taken, and are equipped with oxalic acid powder, by dissolving oxalic acid in hot water, and are put into the pond for installing quartz sand,
Sour water is higher by quartz sand 100mm, and continuous circulating-heating acid solution between reaching pond temperature and maintaining 40 DEG C -80 DEG C, maintains
A few hours;
S2:Sour water is bled off, is gone over low temperature sour water from hot quartz sand pond, to recycle thermal energy;And it is taken out with vacuum equipment
Dry acid water, quartz sand are produced from Sha Chizhong, into cleaning process;
S3:It is cleaned in suspension backwash equipment with the limewash that pH value is 8.5, is finally rinsed with deionized water, examined
Test packaging and storage;
A1:Sand filtration;The useless oxalic acid aqueous solution filtered in above-mentioned S2 is taken, carries out sand filtration, the useless oxalic acid water after sand filtration, which is put in, to be treated
In process container;
A2:Resin adsorption:Pending useless oxalic acid water is conveyed by flowmeter with infusion pump, and adsorption resin column is sent into from top
Tank body, volume flow rate are controlled between 2-4, and the oxalic acid water after absorption is flowed out from the bottom of adsorption column tank body, by Line glass
It is spare that visor is sent into clear acid solution storage tank;
A3:With quartz sand acid washing lotion:The clear acid solution dispensing in A2 is taken, powdery oxalic acid is added to reach required concentration of oxalic acid, again
Carry out pickling process.
The consumption of the process mesoxalic acid is:0.24-0.32 tons
In above-mentioned two embodiment, oxalic acid solution generally can be recycled 3 times.
Embodiment 3
Difference lies in reduce heating process, processed under normal temperature state the present embodiment with embodiment 2.Specific step
Suddenly it is:
100 tons of quartz sands are taken, and are equipped with oxalic acid powder, by dissolving oxalic acid in hot water, and are put into the pond for installing quartz sand,
Sour water is higher by quartz sand 100mm;
S2:Sour water is bled off, is gone over low temperature sour water from hot quartz sand pond, to recycle thermal energy;And it is taken out with vacuum equipment
Dry acid water, quartz sand are produced from Sha Chizhong, into cleaning process;
S3:It is cleaned in suspension backwash equipment with the limewash that pH value is 8.5, is finally rinsed with deionized water, examined
Test packaging and storage;
A1:Sand filtration;The useless oxalic acid aqueous solution filtered in above-mentioned S2 is taken, carries out sand filtration, the useless oxalic acid water after sand filtration, which is put in, to be treated
In process container;
A2:Resin adsorption:Pending useless oxalic acid water is conveyed by flowmeter with infusion pump, and adsorption resin column is sent into from top
Tank body, volume flow rate are controlled between 2-4, and the oxalic acid water after absorption is flowed out from the bottom of adsorption column tank body, by Line glass
It is spare that visor is sent into clear acid solution storage tank;
A3:With quartz sand acid washing lotion:The clear acid solution dispensing in A2 is taken, powdery oxalic acid is added to reach required concentration of oxalic acid, again
Carry out pickling process.
The consumption of the process mesoxalic acid is:0.5-0.8 tons.
Comparative example 1
It is tapped a blast furnace using conventional method, takes 1000 tons of quartz sands, and be equipped with oxalic acid powder, by dissolving oxalic acid in hot water,
And be put into the pond for installing quartz sand, sour water is higher by quartz sand 100mm, and continuous circulating-heating acid solution makes pond temperature reach simultaneously
Between maintaining 40 DEG C -80 DEG C, a few hours are maintained;
S2:Sour water is bled off, is gone over low temperature sour water from hot quartz sand pond, to recycle thermal energy;And it is taken out with vacuum equipment
Dry acid water, quartz sand are produced from Sha Chizhong, into cleaning process;
S3:It is cleaned in suspension backwash equipment with the limewash that pH value is 8.5, is finally rinsed with deionized water, examined
Test packaging and storage;
Lime stone is added in the sour water in S2, is neutralized.
During being somebody's turn to do, the consumption of oxalic acid is:10-14 tons.
As it can be seen that using in this technique process, oxalic acid solution is recycled, and ferro element is adsorbed, Er Feiyu
Oxalic acid solution reacts, and the consumption for reducing oxalic acid solution is lost in, and greatly improves productivity effect.
And it compares for comparative example 3, in whole process, after heating, the utilization rate higher of oxalic acid.
A variety of modifications of embodiment will be apparent for those skilled in the art, determine herein
The General Principle of justice can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, originally
Invention is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein
Consistent most wide scope.
Claims (5)
1. a kind of quartz sand oxalic acid remove iron after saliferous give up oxalic acid water processing and reuse method, which is characterized in that including pickling
Process, recovery of oxalic acid process and tail mud treatment process;
The pickling process comprises the following steps:
S1:It by dissolving oxalic acid in hot water, and is put into the pond for installing quartz sand, sour water is higher by quartz sand 100mm, constantly cycles
Acid solution is heated, between reaching pond temperature and maintaining 40 DEG C -80 DEG C, maintains a few hours;
S2:Sour water is bled off, is gone over low temperature sour water from hot quartz sand pond, to recycle thermal energy;And drain acid with vacuum equipment
Water, quartz sand are produced from Sha Chizhong, into cleaning process;
S3:It is cleaned in suspension backwash equipment with the limewash that pH value is 8.5, is finally rinsed with deionized water, examine bag
It is packed into storehouse;
The recovery of oxalic acid process comprises the following steps:
A1:Sand filtration;The useless oxalic acid aqueous solution filtered in above-mentioned S2 is taken, carries out sand filtration, the useless oxalic acid water after sand filtration is put in pending
In container;
A2:Resin adsorption:Pending useless oxalic acid water is conveyed by flowmeter with infusion pump, and adsorption resin column tank is sent into from top
Body, volume flow rate are controlled between 2-4, and the oxalic acid water after absorption is flowed out from the bottom of adsorption column tank body, is regarded by Line glass
It is spare that mirror is sent into clear acid solution storage tank;
A3:With quartz sand acid washing lotion:The clear acid solution dispensing in A2 is taken, powdery oxalic acid is added to reach required concentration of oxalic acid, is carried out again
Pickling process.
2. quartz sand oxalic acid according to claim 1 remove saliferous after iron give up oxalic acid water processing and reuse method, it is special
Sign is, in the recovery of oxalic acid process, the setting of adsorption resin column tank body is multiple, after single resin column tube body saturation, immediately eventually
Only adsorption column is fed, and material inlet valve is switched in another spare adsorption resin column and is adsorbed.
3. quartz sand oxalic acid according to claim 1 or 2 remove iron after saliferous give up oxalic acid water processing and reuse method,
It is characterized in that, further includes absorption resin regeneration process, including adding in regenerative elution liquid into absorption resin container body, absorption resin is again
It is spare after life.
4. quartz sand oxalic acid according to claim 1 remove saliferous after iron give up oxalic acid water processing and reuse method, it is special
Sign is, in S3, the clear water after sedimentation basin precipitates after sand filter filters, is back to the cleaning containing sour quartz sand again, Xun Huan
It utilizes.
5. quartz sand oxalic acid according to claim 1 remove saliferous after iron give up oxalic acid water processing and reuse method, it is special
Sign is that the tail mud treatment process is:The glar in S3 is taken to be calcined after pressure-filteration drying, after generating metal oxide, with
The stable silicates of silica generation.
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Cited By (3)
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CN111874912A (en) * | 2020-07-06 | 2020-11-03 | 安徽凤砂矿业集团有限公司 | Quartz sand and purification method thereof |
CN112010316A (en) * | 2020-07-06 | 2020-12-01 | 安徽凤砂矿业集团有限公司 | Quartz sand processing technology |
CN115367994A (en) * | 2022-08-19 | 2022-11-22 | 陕西合兴硅砂有限公司 | Iron removal method for quartz sand for photovoltaic glass |
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CN105197939A (en) * | 2015-09-26 | 2015-12-30 | 田辉明 | Acid pickling and waste acid treatment process for improving purity of powdery quartz sand |
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DD136259A1 (en) * | 1978-01-09 | 1979-06-27 | Siegfried Mueller | METHOD AND DEVICE FOR PRODUCING HIGH-PURITY SIO DEEP 2 |
SU1127845A1 (en) * | 1983-02-21 | 1984-12-07 | Ордена Трудового Красного Знамени Научно-Исследовательский И Проектный Институт Обогащения И Механической Обработки Полезных Ископаемых "Уралмеханобр" | Method for cleaning quartz raw material |
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CN111874912A (en) * | 2020-07-06 | 2020-11-03 | 安徽凤砂矿业集团有限公司 | Quartz sand and purification method thereof |
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CN115367994A (en) * | 2022-08-19 | 2022-11-22 | 陕西合兴硅砂有限公司 | Iron removal method for quartz sand for photovoltaic glass |
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