CN106892430A - A kind of preparation method of ultrapure quartz sand - Google Patents
A kind of preparation method of ultrapure quartz sand Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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Abstract
A kind of preparation method of ultrapure quartz sand, belongs to mineral purification, mining industry deep processing and field of comprehensive utilization.Including producing for a coarse sands：Ore reduction, pick, water sieve roughing, broken classification, sand processed, roller classification, color sorting, magnetic separation, pickling, drip washing, ultrasonic washing, electrodialysis, drying oven drying, roaster roasting, acid are quenched, pickling, ultra-pure water washing, flotation, ultra-pure water washing, ultrasound washing, electrodialysis, it is ultrasonic wash, drying oven is dried, collection；The purification of b quartz sands：High intensity magnetic separation, color sorting, microwave drying, packaging.SiO2Purity is up to more than 99.999%.The present invention is not in that the environmental problem in industrial processes and the accessory substance in course of reaction can also make full use of without pollutant emission, it is to avoid the waste of resource.
Description
Technical field
The invention belongs to mineral purification, mining industry deep processing and field of comprehensive utilization, and in particular to one kind is with silicon oxide-containing ore deposit
Stone is the method for waste ultrapure quartz sand.
Technical background
China's industry related to silicon product is started late, and technical merit falls behind, and not yet recognizes high-quality silicon resource
Immense value, as raw silicon product maximum exported country.With economic development, as the important material that current high and new technology develops
Material basis, to hyperpure silicon, this non-renewable resources increases protective policy for country：In March, 2006 country Department of Commerce, General Administration of Customs
List silica sand and other natural silica Sands in goods forbidden to be exported catalogue, and plan to be implemented from May 1st, 2006.Afterwards because of sandstone
Association and the reflection of sea sand exploitatiom enterprise are difficult to adjust management direction in a short time, are the sufficient time to set up new operation to enterprise
Channel, country determines the execution time determined before postponing.On March 1st, 2007, national Department of Commerce, General Administration of Customs's joint issue
Bulletin, has formally recovered to forbid natural ore particle export control measure, and in addition to metallic mineral ore, silica sand and other natural ore particles forbid
Mouthful.This protection in policy China not abundant non-renewable silicon resource in itself, is also HIGH-PURITY SILICON sand raw material supply from now on
Policy foundation is established.
In 2011 national " development plans of silica glass industry 12 ", even more the research and development of high-purity silica sand technology of preparing are made
It is " the first big task " in the big specific tasks of 12 period of industry seven, is explicitly pointed out in planning：" silica glass industry maximum
Bottleneck problem is raw material problem, does not have silica best in quality to be impossible to the optoelectronic information industry of fast development ",
As the basic material of new energy, it is also not possible to there is the New Energy Industry of independent intellectual.In the upper and lower pay attention to day by day section of current government
Under the background of energy emission reduction, as photovoltaic, the important materials of electronic applications, the representative products of low-carbon economy --- the high-purity new material of silicon
Increasingly paid close attention to by each side, undoubtedly, this is national industrial policies inclination, a Chaoyang industry for continued support.
The present invention proposes the multistage purification technique for producing ultrapure sand, for the industrialized production of ultrapure quartz sand provides guarantor
Barrier.
The content of the invention
It is an object of the invention to provide a kind of method for producing ultrapure sand.
A kind of preparation method of ultrapure quartz sand, it is characterised in that with the ore of silicon oxide-containing be the ultrapure sand of waste,
The main purification produced with quartz sand including coarse sand；Comprise the following steps that：
A coarse sands are produced including following several steps：
(1) ore reduction, pick:The ore of silica be will be enriched in by crusher in crushing into bulk, size be 40-50 in the least
Rice；
(2) water sieve roughing：The soil on the massive ore raw material surface that will have been crushed is cleaned up, removal tcrude ore epidermis
Mud and humus；
(3) jaw crusher classification:The ore of wash clean enters jaw crusher by ore reduction into 10-20 millimeters of stone
Son carries out the treatment of next step sand；
(4) sand processed：Sand processed in the ore feeding sand making machine that classification is obtained will be passed through in step (3)；
It is preferred that sand making machine used is tumbling ball mill (inner liner of bowl mill corundum or zirconium oxide), abrading-ball is zirconium oxide/oxygen
Change aluminium/agate, sphere diameter proportioning is 30mm, 20mm, 10mm, 5mm=2/5/5/8, and ratio of grinding media to material is (2~4)/1, Ball-milling Time 1-2
Hour, it is made the ore in sand form of 100-200 mesh；
(5) roller is classified：The ore in sand form that step (4) processing is obtained by mesh number be classified and picks out the ore in sand form for meeting mesh number
It is 100-200 mesh, the ore in sand form for not meeting size continues step (4)；
(6) color sorting：It is using detecting technique that the heterochromatic particle in ore in sand form is for example black according to the difference of ore in sand form optical characteristics
The defects inspectings such as point, brown point are simultaneously sorted out；
(7) magnetic separation：Select and remove the magnetisable material and iron content particle contained in ore in sand form；
(8) pickling：Ore in sand form after magnetic separation stirs mixed processing in being immersed in the pickling tank for fill acid solution, in removal ore in sand form
The foreign particle of acid can be dissolved in；
It is preferred that acid solution used be hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid in one or several.Pickling temperature is 70-
95 DEG C, pickling time is 0.5-3 hours, is stood after pickling, and the time is 0.5-1 hours；Stirring container liner is ceramic or poly-
Tetrafluoroethene, it is to avoid contacting metal in whipping process.
(9) drip washing：By ore in sand form ultra-pure water (resistivity the is 18.1-18.3 megaohms) drip washing after pickling, ore in sand form is washed till
Neutral or close neutrality；Neutralisation treatment is carried out in acid solution barrel of the feeding equipped with alkali lye after cleaning, it is to avoid the discharge of acid solution,
Product after neutralization can be processed further as subsequent product, be effectively utilized accessory substance；
(10) ultrasound washing：Ore in sand form after drip washing carries out ultrasonic washing with ultra-pure water (resistivity is 18.1-18.3 megaohms),
The process utilizes impact of the ultrasonic wave cavitation, acceleration effect in a liquid to quartz sand and dirt, makes crud layer quilt
Disperse, emulsify, peel off and reach cleaning purpose；
(11) electrodialysis：Electrodialysis process is carried out by the ore in sand form after ultrasound washing, under the driving of applying direct current electric field,
Using the selective penetrated property of amberplex, (i.e. cation can pass through cation-exchange membrane, and anion can pass through anion
Exchange membrane), anions and canons are respectively to anode and movable cathode.Using ultra-pure water as electrodialysis liquid during being somebody's turn to do, ultra-pure water
Resistivity is 18.1-18.3 megaohms；Settled from top to bottom during electrodialysis, from top to bottom in infall process, will by electric field
The zwitterion that quartz sand surface is washed out is cleared respectively, and electric-field intensity is more than 50V, best more than 500V, can be by surface
Ion (Na+,K+,Ca2+,NH4 +,Mg2+,Fe3+,Cl-,SO4 2-,CO3 2-,F-) remove, clearance rate is up to more than 99.9%；
(12) repeat step (10)；
(13) drying oven drying：Step (12) cleaned ore in sand form is into carrying out dewater treatment, temperature in drying oven
It it is 300-400 DEG C, process time is 1-2 hours；
(14) roaster roasting：Ore in sand form feeding roaster high temperature after dehydration is calcined, 900-1000 DEG C of sintering temperature,
Roasting time is 2-5 hours；
(15) acid is quenched：Quartz sand after roasting to be put into rapidly and carry out acid in the mixing drum for fill acid solution and quench at high temperature
Treatment, because the thermal coefficient of expansion of ore in sand form inside to ore in sand form surface is different or lowers the temperature uneven so that ore grain bursts, ore deposit
Magnetic and metal impurities inside sand etc. are fully exposed, and foreign particle will be partially soluble in acid solution, realize ore in sand form i.e. quartz sand
Further purification；Acid used in the process of this in hydrofluoric acid, sulfuric acid, hydrochloric acid and nitric acid one or several and with filling
The sealed plastic barrel for having alkali lye is collected due to the acid mist that high temperature is produced, and effectively avoids environmental pollution.During being equally somebody's turn to do
Neutralized reaction product can also carry out next step processing as a kind of product.
(16) pickling：Repeat step (8)；
(17) ultra-pure water washing：Quartz sand after step (16) acidity is cleaned with ultra-pure water, until in cleaning to
Property or close to neutrality；Resistivity of ultra-pure water is 18.1-18.3 megaohms during this；
(18) flotation：In quartz sand feeding flotation device after step (17) is washed, using quartz sand and contaminant surface
The removal of impurity is gone in physical chemical differences, flotation；
(19) ultra-pure water washing：Repeat step (17)；
(20) ultrasound washing：Repeat step (10)；
(21) electrodialysis：Repeat step (11)；
(22) ultrasound washing：Repeat step (10)；
(23) drying oven drying：Repeat step (13)；
(23) collect：High quartz sand after drying and dewatering is dropped into room temperature and collecting packing just can obtain thick quartz
Sand.
The purification of b quartz sands includes following several steps：
(1) high intensity magnetic separation：High intensity magnetic separation treatment will be carried out in the rubble sand feeding magnetic separator of collection, magnetic field intensity is at least
3T, further removes the magnetisable material in quartz sand and the ferrous contaminants not eliminated；
(2) color sorting：The variegated particle in quartz sand is separated using the difference of color；
(3) microwave drying：Quartz sand after color sorting is sent in microwave dryer, carries out further dewater treatment, is dried
Temperature is 100-200 DEG C, and drying time is 1-2 hours；The method rate of drying is fast, uniform drying, energy-conservation, moisture content control essence
Really, improve the quality of product.
(4) pack：Dried quartz sand is naturally cooled into room temperature, bag is packaged into finally by packing machine, just can be with
Obtain purity quartz sand product very high.
Invention advantage
1. the ore resource of China is made full use of, and having invented can be with the multistage progressively purification technique, SiO of industrialized production2
Purity is up to more than 99.999%.
2. the present invention is without pollutant emission, in being not in the environmental problem and course of reaction in industrial processes
Accessory substance can also make full use of, it is to avoid the waste of resource.
Brief description of the drawings
Fig. 1：The step of producing ultrapure quartz sand flow chart.
Specific embodiment
With reference to embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1
The step of quartz sand is produced in this example is as shown in figure 1, technique mainly includes producing for coarse sand and proposing for quartz sand
It is pure, it is specific as follows:
Coarse sand is produced：
(1) ore reduction/pick:Ore was broken into block size about 4cm x 4cm x 4cm originally.
(2) water sieve roughing：The soil on the raw material surface that will have been crushed with light water is cleaned up, the soil that removal is mixed into
With the impurity foreign matter of mineral surface.
(3) jaw crusher classification:The stone that cleaned block ore is broken into 10 millimeters is carried out
The sand processed treatment of next step.
(4) sand processed：The ore of step (3) is sent into sand making machine aggregate reclaiming.This grade of ball mill is tumbling ball mill (ball
Mill liner corundum or zirconium oxide), abrading-ball is zirconium oxide/aluminum oxide/agate, and sphere diameter proportioning is：30mm/20mm/10mm/5mm
=2/5/5/8, ratio of grinding media to material is 2/1, Ball-milling Time 2 hours, is made the ore in sand form of 180-200 mesh
(5) roller is classified：By step (4) processing obtain ore in sand form is carried out being classified the ore deposit of picking out 200 mesh or so by mesh number
Sand is standby.
(6) color sorting：The ore in sand form feeding color selector of 200 mesh that will be singled out, the removal heterochromatic particle big with white difference, such as
Sand with impurity such as stain, brown points.
(7) magnetic separation：Quartz sand after color sorting enters magnetic separator, and magnetic separation strength is 2T herein.
(8) pickling：Quartz sand after magnetic separation is sent to the descaling bath of the mixed acid solution for filling hydrofluoric acid, nitric acid and hydrochloric acid
Middle stir process, temperature is that 90 DEG C of process times are 1.5 hours.Stopping is stirred and stands 0.5 hour.
(9) drip washing：Quartz sand after pickling is sent into supersonic cleaning machine by crawler belt, is 18.1 megaohms super with resistivity
Pure water is cleaned by the quartz sand of crawler belt, and quartz sand is washed till close to neutrality.Acid solution after cleaning enters the barrel equipped with alkali lye
In carry out neutralisation treatment.Byproduct after neutralization is otherwise processed into product.
(10) ultrasound washing：Quartz sand after drip washing enters supersonic cleaning machine, with the ultra-pure water that resistivity is 18.1 megaohms
Ultrasonic washing is carried out, the time is 2 hours.
(11) electrodialysis：Electrodialysis process is carried out by the quartz sand after ultrasound washing.Ultra-pure water resistivity is 18.1 million
Europe.Electric-field intensity 100V, the time is 30 minutes.
(12) repeat step (10).
(13) drying oven drying：Cleaned quartz sand is into carrying out dewater treatment in drying oven.Treatment temperature is
400 DEG C, the time is 2 hours.
(14) roaster roasting：By the quartz sand feeding roaster high temperature roasting after dehydration, 950 DEG C of sintering temperature, roasting
The burning time is 4 hours.
(15) acid is quenched：Quartz sand after roasting to be put into rapidly and carry out acid in the mixing drum for fill acid solution and quench at high temperature
Treatment, should used in the process of acid for the mixed acid in hydrofluoric acid, hydrochloric acid and nitric acid and with the sealed plastic barrel that alkali lye is housed
Collect due to a large amount of acid mists that high temperature is produced, the neutralized reaction product during being somebody's turn to do also serves as a kind of product carries out next step processing.
(16) pickling：Repeat step (8).
(17) ultra-pure water washing：Quartz sand is cleaned with ultra-pure water, until cleaning to neutral or close neutrality.It is used
Ultra-pure water resistivity is 18.1 megaohms.
(18) flotation：Quartz sand after washing is sent into flotation device, using quartz sand and the physical chemistry of contaminant surface
The removal of impurity is gone in nature difference, flotation.
(19) wash：Repeat step (17).
(20) ultrasound washing：Repeat step (10).
(21) electrodialysis：Repeat step (11).
(22) ultrasound washing：Repeat step (10)
(23) drying oven drying：Repeat step (13).
(24) collect：Quartz sand product is collected.
The purification of quartz sand includes following several steps：
(1) high intensity magnetic separation：The quartz sand of collection is carried out into high intensity magnetic separation treatment, magnetic field intensity is 3T.
(2) color sorting：The variegated particle in quartz sand is separated using the difference of color.
(3) microwave drying：Quartz sand carries out further dewater treatment.200 DEG C of drying temperature, the time is 2 hours.
(4) pack：Dried quartz sand is naturally cooled into room temperature, final quartz sand is collected finally by packing machine
Product.
The purity of quartz sand can be widely applied to industrial production more than 99.999% in the example.
Embodiment 2
This example is essentially identical with the technique of example 1, and difference is to remove electrodialysis process.Final quartz sand testing result
As shown in table 1.TA60-1B samples SiO by elements2Purity is 99.9974%, TA60-3 samples SiO by elements2Purity is
99.9953%.
Table 1：Testing result in example 2
Claims (6)
1. a kind of preparation method of ultrapure quartz sand, it is characterised in that with the ore of silicon oxide-containing be the ultrapure sand of waste, it is main
To include the purification produced with quartz sand of coarse sand；Comprise the following steps that：
A coarse sands are produced including following several steps：
(1) ore reduction, pick:The ore of silica be will be enriched in by crusher in crushing into bulk, size is 40-50 millimeters；
(2) water sieve roughing：The soil on the massive ore raw material surface that will have been crushed is cleaned up, remove tcrude ore epidermis mud and
Humus；
(3) jaw crusher classification:Stone of the ore of wash clean into jaw crusher by ore reduction into 10-20 millimeters enters
The treatment of row next step sand；
(4) sand processed：Sand processed in the ore feeding sand making machine that classification is obtained will be passed through in step (3)；
(5) roller is classified：Step (4) ore in sand form that obtains of processing by mesh number be classified and is picked out the ore in sand form for meeting mesh number and is
100-200 mesh, the ore in sand form for not meeting size continues step (4)；
(6) color sorting：According to the difference of ore in sand form optical characteristics, using detecting technique by the heterochromatic particle such as stain in ore in sand form,
The defects inspectings such as brown point are simultaneously sorted out；
(7) magnetic separation：Select and remove the magnetisable material and iron content particle contained in ore in sand form；
(8) pickling：Ore in sand form after magnetic separation stirs mixed processing in being immersed in the pickling tank for fill acid solution, can be molten in removal ore in sand form
In the foreign particle of acid；
(9) drip washing：By the ultrapure water wash of the ore in sand form after pickling, ore in sand form is washed till neutral or close neutrality；Acid after cleaning
Neutralisation treatment is carried out in liquid barrel of the feeding equipped with alkali lye, it is to avoid the discharge of acid solution, the product after neutralization can be processed further
As subsequent product, it is effectively utilized accessory substance；
(10) ultrasound washing：Ore in sand form after drip washing carries out ultrasonic washing with ultra-pure water, the process using ultrasonic wave in a liquid
The impact of cavitation, acceleration effect to quartz sand and dirt, makes crud layer be disperseed, emulsified, peeled off and reach cleaning mesh
's；
(11) electrodialysis：Electrodialysis process is carried out by the ore in sand form after ultrasound washing, under the driving of applying direct current electric field, is utilized
The selective penetrated property of amberplex, anions and canons are respectively to anode and movable cathode；Using ultra-pure water as electricity during being somebody's turn to do
Dialysate, the resistivity of ultra-pure water is 18.1-18.3 megaohms；Settled from top to bottom during electrodialysis, settled from top to bottom
Cheng Zhong, is cleared the zwitterion that quartz sand surface is washed out by electric field respectively, and electric-field intensity is more than 50V, by surface
Ion remove, clearance rate is up to more than 99.9%；
(12) repeat step (10)；
(13) drying oven drying：Into dewater treatment is carried out in drying oven, temperature is step (12) cleaned ore in sand form
300-400 DEG C, process time is 1-2 hours；
(14) roaster roasting：By the ore in sand form feeding roaster high temperature roasting after dehydration, 900-1000 DEG C of sintering temperature, roasting
Time is 2-5 hours；
(15) acid is quenched：Quartz sand after roasting is put into rapidly and carry out in the mixing drum for fill acid solution acid and quench place at high temperature
Reason, because the thermal coefficient of expansion of ore in sand form inside to ore in sand form surface is different or lowers the temperature uneven so that ore grain bursts, ore in sand form
Internal magnetic and metal impurities etc. are fully exposed, and foreign particle will be partially soluble in acid solution, realize the i.e. quartz sand of ore in sand form
Further purification；
(16) pickling：Repeat step (8)；
(17) ultra-pure water washing：Quartz sand after step (16) acidity is cleaned with ultra-pure water, until clean to it is neutral or
Close to neutrality；
(18) flotation：In quartz sand feeding flotation device after step (17) is washed, using quartz sand and the physics of contaminant surface
The removal of impurity is gone in chemical property difference, flotation；
(19) ultra-pure water washing：Repeat step (17)；
(20) ultrasound washing：Repeat step (10)；
(21) electrodialysis：Repeat step (11)；
(22) ultrasound washing：Repeat step (10)；
(23) drying oven drying：Repeat step (13)；
(23) collect：High quartz sand after drying and dewatering is dropped into room temperature and collecting packing just can obtain thick quartz sand
.
The purification of b quartz sands includes following several steps：
(1) high intensity magnetic separation：High intensity magnetic separation treatment will be carried out in the rubble sand feeding magnetic separator of collection, magnetic field intensity is at least 3T, enters
One step removes the magnetisable material in quartz sand and the ferrous contaminants not eliminated；
(2) color sorting：The variegated particle in quartz sand is separated using the difference of color；
(3) microwave drying：Quartz sand after color sorting is sent in microwave dryer, carries out further dewater treatment, drying temperature
It it is 100-200 DEG C, drying time is 1-2 hours；
(4) pack：Dried quartz sand is naturally cooled into room temperature, bag is packaged into finally by packing machine.
2. according to a kind of preparation method of the ultrapure quartz sand described in claim 1, it is characterised in that in the producing of a coarse sands
Sand making machine used by step (4) is tumbling ball mill, inner liner of bowl mill corundum or zirconium oxide, and abrading-ball is zirconium oxide/aluminum oxide/agate
Nao, sphere diameter proportioning is 30mm, 20mm, 10mm, 5mm=2/5/5/8, and ratio of grinding media to material is (2~4)/1, Ball-milling Time 1-2 hours, system
Into the ore in sand form of 100-200 mesh.
3. according to a kind of preparation method of the ultrapure quartz sand described in claim 1, it is characterised in that in the producing of a coarse sands
Acid solution used by step (8) is one or several in hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid.Pickling temperature is 70-95 DEG C,
Pickling time is 0.5-3 hours, is stood after pickling, and the time is 0.5-1 hours；Stirring container liner is ceramics or polytetrafluoroethyl-ne
Alkene, it is to avoid contacting metal in whipping process.
4. according to a kind of preparation method of the ultrapure quartz sand described in claim 1, it is characterised in that ultra-pure water resistivity is
18.1-18.3 megaohms.
5. according to a kind of preparation method of the ultrapure quartz sand described in claim 1, it is characterised in that in the producing of a coarse sands
Step (11) electric field is in more than 500V.
6. according to a kind of preparation method of the ultrapure quartz sand described in claim 1, it is characterised in that in the producing of a coarse sands
Acid used in the process of step (13) in hydrofluoric acid, sulfuric acid, hydrochloric acid and nitric acid one or several and with being equipped with alkali lye
Sealed plastic barrel collect due to high temperature produce acid mist.
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