CN106064819A - A kind of quartz deposit prepares the method for glass sand - Google Patents
A kind of quartz deposit prepares the method for glass sand Download PDFInfo
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- CN106064819A CN106064819A CN201610382435.6A CN201610382435A CN106064819A CN 106064819 A CN106064819 A CN 106064819A CN 201610382435 A CN201610382435 A CN 201610382435A CN 106064819 A CN106064819 A CN 106064819A
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- C—CHEMISTRY; METALLURGY
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
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Abstract
The invention discloses a kind of method that quartz deposit prepares glass sand, after comprising the steps: to roughly select quartz deposit, pulverize, shrend, grind and obtain the ultra-fine quartz mine that particle diameter is 5 50 μm；And in High gradient high intensity magnetic separator, ultra-fine quartz mine is carried out twice magnetic separation in weak magnetic separator successively, and thickening obtains quartz concentrate；By quartz concentrate roasting, shrend, pickling, sucking filtration, washing, dry and obtain quartz sand；Quartz sand is sized mixing, adds FLOTATION SEPARATION after modified starch, activator and composite collector, washing, air-dry, be dried to obtain quartz washed ore；By quartz washed ore pickling post-heating, under the conditions of ultrasound field, carry out acidleach for the first time, sucking filtration, washing；Reheating carries out second time acidleach, sucking filtration, washing, dries and obtains glass sand.High purity quartz SiO prepared by the present invention2Content reaches 99.99 99.995%, total impurities content ＜ 100ppm.
Description
Technical field
The present invention relates to high purity quartz preparing technical field, particularly relate to a kind of quartz deposit and prepare the side of glass sand
Method.
Background technology
Quartz is that a kind of physics, chemical property are sufficiently stable, and purposes mineral resources widely, common quartz sand is applied
In fields such as glass, pottery, rubber, castings, and highly purified quartz sand SiO2Content is more than 99.995% or higher, main
Apply in new high-tech industry such as Aero-Space, biological engineering, altofrequency technology, electronic technology, fiber optic communication and military project etc.
Field.Owing to these Relationships are to the long term growth of country, therefore the strategic position of glass sand is extremely important.High-purity stone
Sand is in all many-sides such as Aeronautics and Astronautics, electronics, IT, atomic energy, optical telecommunications cable material and science and techniques of defence tip device
Occupy very important effect.The quartz sand being applied to these fields has strict requirements to quality, wherein the content of impurity,
The especially content of the metallic element such as ferrum, aluminum is limited in the lowest scope.
In nature, only aconteta (one-level, two grades of crystals) can meet requirement at present, but reserves own are limited, and
Natural high-purity crystal material is the most exhausted.As far back as 20 century 70s, the most just have started to substitute high-purity stone of crystal material
The processing of English, China starts late in the research of the purification processing of siliceous raw material, and owing to the common quartz mineral products of China exist
During Diagenesis And Mineralization, association plurality of impurities mineral, such as Anhydrite, Muscovitum, clay pit etc., thus purity is the highest, thus gives removing of Ore
Miscellaneous separation brings bigger difficulty.The most common quartzy purification technique or complex process, energy consumption are high, seriously polluted, or quartz
Purity is the highest, it is difficult to meet high-technology industry to quartz purity requirement.Therefore, the means that the various sorting of Appropriate application purifies are from stone
English ore resources is isolated the research emphasis that highly purified quartz sand becomes current.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes a kind of quartz deposit and prepares the side of glass sand
Method, the high purity quartz SiO of preparation2Content reaches 99.99-99.995%, total impurities content ＜ 100ppm, meets quartz glass earthenware
Crucible, high-precision electronics, the microelectronic product requirement to high purity quartz material.
The method that a kind of quartz deposit that the present invention proposes prepares glass sand, comprises the steps:
S1, pulverizing: after being roughly selected by quartz deposit, be crushed to particle diameter≤20mm, immerses 10-20min in 0-10 DEG C of water, takes out
Rear grinding obtains the ultra-fine quartz mine that particle diameter is 5-50 μm；
S2, magnetic separation: the ultra-fine quartz mine obtained by S1 is successively in the weak magnetic separator of magnetic field intensity 0.1-0.5T and magnetic field
The High gradient high intensity magnetic separator of intensity 1.0-1.4T carries out magnetic separation and obtains concentrate serosity, during twice magnetic separation, control feed ore concentration
For 20-30wt%, thickening obtains quartz concentrate；
S3, roasting: the quartz concentrate obtained by S2 roasting 120-200min under conditions of 600-1000 DEG C, be subsequently placed in
Shrend 10-20min in 10-20 DEG C of water, immerses 30-60min in hydrochloric acid-oxalic acid Compound-acid immersion, sucking filtration, washing, dries after taking-up
Dry obtain quartz sand；
S4, flotation: the quartz sand obtained by S3 adds water to modulate and obtains the ore pulp that concentration is 40-50wt%, according to ore deposit per ton
The modified starch of slurry addition 20-30g is as inhibitor, and after stirring 1-3min, acid adding regulation pH values of pulp is 4-5, according still further to per ton
Ore pulp stirs 3-5min, FLOTATION SEPARATION 3-5min, water after adding the activator of 400-500g and the composite collector of 700-800g
Wash, air-dry, be dried 60-80min at 100-200 DEG C and obtain quartz washed ore；
S5, acidleach: the quartzy washed ore obtained by S4 immerses in the first pickle liquor, solid-liquid weight ratio controls to be 0.8-1:1, adds
Heat is to 30-40 DEG C, and acidleach 60-100min under the conditions of the ultrasound field of power 400-800W, sucking filtration is removed the first pickle liquor, used
The deionized water wash of 70-80 DEG C to filtrate is neutrality；Immersing in the second pickle liquor again, solid-liquid weight ratio controls to be 1:2-5, adds
Heat is to 60-80 DEG C, and acidleach 20-40min under stirring condition, sucking filtration removes the second pickle liquor, with the deionized water wash of 70-80 DEG C
It is neutrality to filtrate, dries and obtain glass sand.
Preferably, in S1, after being roughly selected by quartz deposit, being crushed to particle diameter is 1-6mm, immerses 12-in 0-5 DEG C of water
18min, grinds the ultra-fine quartz mine obtaining particle diameter 5-30 μm after taking-up.
Preferably, in S2, described weak magnetic separator is cartridge type weak magnetic separator；Described High gradient high intensity magnetic separator is vertical ring pulsation
High gradient high intensity magnetic separator.
Preferably, in S3, in described hydrochloric acid-oxalic acid Compound-acid immersion, the content of HCl is 10-15wt, H2C2O4Contain
Amount is 6-8g/L.
Preferably, in S4, described modified starch is polyphosphoric acids modified starch, prepares described polyphosphoric acids modified starch
Including: starch is added in ethanol water, with sodium hydroxide quaternization 20-30min at 60-80 DEG C, add poly
Phosphoric acid, reacts 90-150min at 120-140 DEG C, obtains described polyphosphoric acids modified starch, wherein starch, sodium hydroxide, many
The weight proportion of polyphosphoric acid is 1:0.1-0.3:0.6-0.8.
Preferably, in S4, described activator is at least one in calcium ion and magnesium ion；Described composite collector by
The 18-amine. hydrochlorate of quality proportioning 1:2-4 and dodecylbenzene sodium sulfonate composition.
Preferably, in S5, described first pickle liquor is hydrochloric acid-nitric acid Compound-acid immersion, the second pickle liquor be Fluohydric acid .-
Hydrochloric acid Compound-acid immersion；Preferably, described hydrochloric acid-nitric acid Compound-acid immersion is joined by hydrochloric acid and salpeter solution in mass ratio 8-10: 1
System forms, and in described hydrochloric acid, HCl content is 31-37wt%, HNO in described salpeter solution3Content is 60-63wt%；Preferably,
Described Fluohydric acid .-hydrochloric acid Compound-acid immersion is formulated by hydrofluoric acid solution and hydrochloric acid in mass ratio 4-6: 1, and described Fluohydric acid. is molten
In liquid, the content of HF is 30-45wt%, and in described hydrochloric acid, the content of HCl is 31-37wt%.
Preferably, in S5, the frequency of ultrasound field is 1-10KHz.
Heretofore described quartz deposit prepares the method for glass sand, first during smashing, by quartz
Raw ore is roughly selected, and impurity obvious in quartz raw ore and foreign body is removed, then through primary fragmentation can effectively make associated mineral and
Quartz separates, and by the separating effect that shrend is mutual with quartz particles to strengthen impure mineral, more once grinds, to enter
Ore deposit foreign body within particle diameter in raw ore is effectively removed by one step；Secondly, during magnetic separation, feeble field-high field is used to combine
Magnetic separation mode, first remove the mechanical ferrum entered in the strongly magnetic mineral in quartz sand and the course of processing, then remove quartz sand
In biotite, Fe2O3、TiO2Deng weak magnetic mineral, can be by the magnetic in quartz sand by the way of low intensity magnetic separation and high intensity magnetic separation combination
Property mineral and the high intergrowth quartz of iron-holder carry out repeated screening, are removed to the full extent, thus improve stone
The purity of sand；Again in roasting process, by quartz mine is used calcining-water quenching technology, on the one hand utilize quartz in difference
At a temperature of volume and crystal form change, chilling after calcining, quartz volume can produce fusion, rupture along crystallize layer, and crystallize
Often in the local appearance containing impurity, thus the impurity of the intracell of not easy-clear is come out；On the other hand
By the quartz mineral after roasting is immersed in acid, the impurity exposed in removing quartz mine and the steam bubble of inside, water wave and bag
Wrap up in internal impurity；In floatation process, by controlling inhibitor and the addition of collecting agent, can effectively remove Muscovitum and various contain
Iron mineral and dark colour mineral, for ensureing product quality, improve product whiteness and serve critical effect, wherein to change
Property starch as inhibitor, to improving collecting agent effect, improve floatation process selectivity and efficiently separate various mineral tool
Having extremely important meaning, the zwitterion of the 18-amine. hydrochlorate of specific proportioning and dodecylbenzene sodium sulfonate composition is compound catches
Receiving agent, on the one hand cation-collecting agent can be in Anhydrite surface A l3+Microcell Formation and characteristics adsorbs, on the other hand anions and canons collecting
Agent itself is incorporated into hydrophobic molecule micelle, forms hydrophobic adsorption at hydrophobic interface, is finally formed on Anhydrite surface
Slightly solubility hydrophobic film, thus by the feldspar associated minerals diffeential floatation in mineral out, removes containing alumina matter and nonmetal miscellaneous
Matter；During acidleach, the ultrasound wave first with power 400-800W produces higher-order of oscillation effect, ultrasound wave to the first pickle liquor
High-frequency energy when acting on the first pickle liquor makes pickle liquor suffer strength to tear moment and forms cavity, and cavity is again due to acid around
The high vibration of immersion and constantly move, grow up and vanish suddenly, when vanishing around pickling liquid pour suddenly in cavity
Produce instantaneous high-temperature, high pressure and shock wave phenomena, the most also can produce electric charge because of internal friction, cause the first pickle liquor reaction system to live
Property change, produce the high energy center of acid liquid reaction of being adequate to bring about, be therefore effectively guaranteed quartz mine the most suitable
Profit carries out acid-leaching reaction, and the consumption of pickle liquor also reduces because of volatilization, reacts abundant and significantly reduce；Second pickle liquor utilizes
The mixed solution of HF, HCl carries out acidification reaction purification, and the HF in mixed acid solution preferentially removes at quartz surfaces and interface thereof
Impurity metal oxide, directly acts on metal oxide surface for HCl and creates favorable conditions, and then realizes quartz sterling
Purify further, obtain described glass sand.
The method of purification technique that the present invention provides is simple, easily operates；The cost of raw material is low, it is easy to obtain, resource utilization
High；Impurity removing technology efficiency is high, and targetedly, technique is easily controllable；The SiO of the ultralow metallic element high purity quartz prepared2
Content can reach 99.99-99.995%, impurity metallic elements total amount ＜ 100ppm, can meet some special-purposes of quartz such as
Prepare silica crucible, crystalline silicon, electronic material, optical glass, high temp glass, vitreous silica, aerospace vehicle sight glass, height
The requirement to quartz raw material such as level trombone slide glass.
Accompanying drawing explanation
Fig. 1 is the method flow diagram that a kind of quartz deposit that the present invention proposes prepares glass sand.
Detailed description of the invention
As it is shown in figure 1, a kind of quartz deposit that Fig. 1 is the present invention to be proposed prepares the method flow diagram of glass sand.
With reference to Fig. 1, the method that a kind of quartz deposit that the present invention proposes prepares glass sand, comprise the steps:
S1, pulverizing: after being roughly selected by quartz deposit, be crushed to particle diameter≤20mm, immerses 10-20min in 0-10 DEG C of water, takes out
Rear grinding obtains the ultra-fine quartz mine of particle diameter 5-50 μm；
S2, magnetic separation: the ultra-fine quartz mine obtained by S1 is successively in the weak magnetic separator of magnetic field intensity 0.1-0.5T and magnetic field
The High gradient high intensity magnetic separator of intensity 1.0-1.4T carries out magnetic separation and obtains concentrate serosity, during twice magnetic separation, control feed ore concentration
For 20-30wt%, thickening obtains quartz concentrate；
S3, roasting: the quartz concentrate obtained by S2 roasting 120-200min under conditions of 600-1000 DEG C, be subsequently placed in
Shrend 10-20min in 10-20 DEG C of water, immerses 30-60min in hydrochloric acid-oxalic acid Compound-acid immersion, sucking filtration, washing, dries after taking-up
Dry obtain quartz sand；
S4, flotation: the quartz sand obtained by S3 adds water to modulate and obtains the ore pulp that concentration is 40-50wt%, according to ore deposit per ton
The modified starch of slurry addition 20-30g is as inhibitor, and after stirring 1-3min, acid adding regulation pH values of pulp is 4-5, according still further to per ton
Ore pulp stirs 3-5min, FLOTATION SEPARATION 3-5min, water after adding the activator of 400-500g and the composite collector of 700-800g
Wash, air-dry, be dried 60-80min at 100-200 DEG C and obtain quartz washed ore；
S5, acidleach: the quartzy washed ore obtained by S4 immerses in the first pickle liquor, and solid-liquid weight ratio is 0.8-1:1, is heated to
30-40 DEG C, acidleach 60-100min under the conditions of the ultrasound field of power 400-800W, sucking filtration is removed the first pickle liquor, is used 70-
The deionized water wash of 80 DEG C to filtrate is neutrality；Immersing in the second pickle liquor again, solid-liquid weight ratio is 1:2-5, is heated to 60-
80 DEG C, acidleach 20-40min under stirring condition, sucking filtration removes the second pickle liquor, with the deionized water wash of 70-80 DEG C to filtrate
In neutrality, sucking filtration, dry and obtain glass sand.
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
A kind of quartz deposit prepares the method for glass sand, comprises the steps:
S1, pulverizing: after being roughly selected by quartz deposit, being crushed to particle diameter is 1-6mm, is placed in shrend 10min in 10 DEG C of water, takes out
Rear grinding obtains the ultra-fine quartz mine that particle diameter is 5-30 μm；
S2, magnetic separation: the ultra-fine quartz mine obtained by S1 is successively in the cartridge type weak magnetic separator that magnetic field intensity is 0.1T and magnetic
Field intensity be 1.4T vertical ring pulsating high gradient intensity magnetic separator in carry out magnetic separation and obtain concentrate serosity, control during twice magnetic separation
Feed ore concentration is 20wt%, and thickening obtains quartz concentrate；
S3, roasting: the quartz concentrate obtained by S2 is roasting 120min under conditions of 1000 DEG C, be subsequently placed in 20 DEG C of water
Shrend 10min, immerses 60min in hydrochloric acid-oxalic acid Compound-acid immersion, sucking filtration, washing, dries and obtain quartz sand after taking-up, described
In hydrochloric acid-oxalic acid Compound-acid immersion, the content of HCl is 10wt%, H2C2O4Content be 8g/L；
S4, flotation: the quartz sand obtained by S3 adds water to modulate and obtains the ore pulp that concentration is 40wt%, adds according to ore pulp per ton
Entering the polyphosphoric acids modified starch of 30g as inhibitor, after stirring 1min, acid adding regulation pH values of pulp is 4-5, according still further to ore deposit per ton
Calcium ion activator and the 700g of slurry addition 500g are 1:4 18-amine. hydrochlorate and dodecylbenzene sodium sulfonate group by quality proportioning
Stir 3min, FLOTATION SEPARATION 5min, washing after the composite collector become, air-dry, be dried 80min at 100 DEG C and obtain quartz washed ore,
Prepare described polyphosphoric acids modified starch to include: added by starch in ethanol water, alkalize at 60 DEG C instead with sodium hydroxide
Answer 30min, add polyphosphoric acids, at 120 DEG C, react 150min, obtain described polyphosphoric acids modified starch, wherein starch,
Sodium hydroxide, the weight proportion of polyphosphoric acids are 1:0.1:0.8；
S5, acidleach: the quartzy washed ore obtained by S4 immerses in the first pickle liquor, solid-liquid weight ratio controls as 0.8:1, heating
To 40 DEG C, acidleach 60min under the conditions of the ultrasound field that power is 800W, sucking filtration removes the first pickle liquor, with 80 DEG C go from
The washing of sub-water is neutrality to filtrate, and described first pickle liquor is hydrochloric acid-nitric acid Compound-acid immersion, described hydrochloric acid-nitric acid Compound-acid
Immersion is formulated by hydrochloric acid solution and salpeter solution in mass ratio 8: 1, and in described hydrochloric acid solution, HCl content is 37wt%, institute
State HNO in salpeter solution3Content is 60wt%；Immersing in the second pickle liquor again, solid-liquid weight ratio controls to be 1:5, is heated to 60
DEG C, acidleach 40min under stirring condition, sucking filtration is removed the second pickle liquor, is neutrality with the deionized water wash of 70 DEG C to filtrate, takes out
Filter, dries and obtains glass sand, and the second pickle liquor is Fluohydric acid .-hydrochloric acid Compound-acid immersion, described Fluohydric acid .-hydrochloric acid Compound-acid
Immersion is mixed by hydrofluoric acid solution and hydrochloric acid solution in mass ratio 6: 1, and in described hydrofluoric acid solution, the content of HF is
30wt%, in described hydrochloric acid solution, the content of HCl is 37wt%.
Embodiment 2
A kind of quartz deposit prepares the method for glass sand, comprises the steps:
S1, pulverizing: after being roughly selected by quartz deposit, be crushed to particle diameter≤10mm, is placed in shrend 20min in 0 DEG C of water, after taking-up
Grind and obtain the ultra-fine quartz mine that particle diameter is 5-40 μm；
S2, magnetic separation: the ultra-fine quartz mine obtained by S1 is successively in the cartridge type weak magnetic separator that magnetic field intensity is 0.5T and magnetic
Field intensity be 1.0T vertical ring pulsating high gradient intensity magnetic separator in carry out twice magnetic separation and obtain concentrate serosity, control during magnetic separation
Feed ore concentration is 30wt%, and thickening obtains quartz concentrate；
S3, roasting: the quartz concentrate obtained by S2 is roasting 200min under conditions of 600 DEG C, be subsequently placed in 10 DEG C of water
Shrend 20min, immerses 30min in hydrochloric acid-oxalic acid Compound-acid immersion, sucking filtration, washing, dries and obtain quartz sand after taking-up, described
In hydrochloric acid-oxalic acid Compound-acid immersion, the content of HCl is 15wt%, H2C2O4Content be 6g/L；
S4, flotation: the quartz sand obtained by S3 adds water to modulate and obtains the ore pulp that concentration is 50wt%, adds according to ore pulp per ton
Entering the polyphosphoric acids modified starch of 20g as inhibitor, after stirring 3min, acid adding regulation pH values of pulp is 4-5, according still further to ore deposit per ton
Calcium ion activator and the 800g of slurry addition 400g are 1:2 18-amine. hydrochlorate and dodecylbenzene sodium sulfonate group by quality proportioning
Stir 5min, FLOTATION SEPARATION 3min, washing after the composite collector become, air-dry, be dried 60min at 200 DEG C and obtain quartz washed ore,
Prepare described polyphosphoric acids modified starch to include: added by starch in ethanol water, alkalize at 80 DEG C instead with sodium hydroxide
Answer 20min, add polyphosphoric acids, at 140 DEG C, react 90min, obtain described polyphosphoric acids modified starch, wherein starch,
Sodium hydroxide, the weight proportion of polyphosphoric acids are 1:0.3:0.6；
S5, acidleach: the quartzy washed ore obtained by S4 immerses in the first pickle liquor, solid-liquid weight ratio controls to be 1:1, is heated to
30 DEG C, acidleach 100min under the conditions of the ultrasound field that power is 400W, sucking filtration removes the first pickle liquor, with the deionization of 70 DEG C
Water washing is neutrality to filtrate, and described first pickle liquor is hydrochloric acid-nitric acid Compound-acid immersion, and described hydrochloric acid-nitric acid is combined acidleach
Liquid is formulated by hydrochloric acid solution and salpeter solution in mass ratio 10: 1, and in described hydrochloric acid solution, HCl content is 31wt%, described
HNO in salpeter solution3Content is 63wt%；Immersing in the second pickle liquor again, solid-liquid weight ratio controls to be 1:2, is heated to 80 DEG C,
Acidleach 20min under stirring condition, sucking filtration removes the second pickle liquor, is neutrality with the deionized water wash of 80 DEG C to filtrate, sucking filtration,
Drying obtains glass sand, and the second pickle liquor is Fluohydric acid .-hydrochloric acid Compound-acid immersion, and described Fluohydric acid .-hydrochloric acid is combined acidleach
Liquid is mixed by hydrofluoric acid solution and hydrochloric acid solution in mass ratio 4: 1, and in described hydrofluoric acid solution, the content of HF is 45wt%,
In described hydrochloric acid solution, the content of HCl is 31wt%.
Embodiment 3
A kind of quartz deposit prepares the method for glass sand, comprises the steps:
S1, pulverizing: after being roughly selected by quartz deposit, be crushed to particle diameter≤6mm, is placed in shrend 15min in 5 DEG C of water, after taking-up
Grind and obtain the ultra-fine quartz mine that particle diameter is 5-25 μm；
S2, magnetic separation: the ultra-fine quartz mine obtained by S1 is successively in the cartridge type weak magnetic separator that magnetic field intensity is 0.3T and magnetic
Field intensity be 1.2T vertical ring pulsating high gradient intensity magnetic separator in carry out twice magnetic separation and obtain concentrate serosity, control during magnetic separation
Feed ore concentration is 25wt%, and thickening obtains quartz concentrate；
S3, roasting: the quartz concentrate obtained by S2 is roasting 160min under conditions of 800 DEG C, be subsequently placed in 15 DEG C of water
Shrend 15min, immerses 45min in hydrochloric acid-oxalic acid Compound-acid immersion, sucking filtration, washing, dries and obtain quartz sand after taking-up, described
In hydrochloric acid-oxalic acid Compound-acid immersion, the content of HCl is 12wt%, H2C2O4Content be 7g/L；
S4, flotation: the quartz sand obtained by S3 adds water to modulate and obtains the ore pulp that concentration is 45wt%, adds according to ore pulp per ton
Entering the polyphosphoric acids modified starch of 25g as inhibitor, after stirring 2min, acid adding regulation pH values of pulp is 4-5, according still further to ore deposit per ton
Calcium ion activator and the 750g of slurry addition 450g are 1:3 18-amine. hydrochlorate and dodecylbenzene sodium sulfonate group by quality proportioning
Stir 4min, FLOTATION SEPARATION 4min, washing after the composite collector become, air-dry, be dried 70min at 150 DEG C and obtain quartz washed ore,
Prepare described polyphosphoric acids modified starch to include: added by starch in ethanol water, alkalize at 70 DEG C instead with sodium hydroxide
Answer 25min, add polyphosphoric acids, at 130 DEG C, react 120min, obtain described polyphosphoric acids modified starch, wherein starch,
Sodium hydroxide, the weight proportion of polyphosphoric acids are 1:0.2:0.7；
S5, acidleach: the quartzy washed ore obtained by S4 immerses in the first pickle liquor, solid-liquid weight ratio controls as 0.9:1, heating
To 35 DEG C, acidleach 80min under the conditions of the ultrasound field that power is 600W, sucking filtration removes the first pickle liquor, with 75 DEG C go from
The washing of sub-water is neutrality to filtrate, and described first pickle liquor is hydrochloric acid-nitric acid Compound-acid immersion, described hydrochloric acid-nitric acid Compound-acid
Immersion is formulated by hydrochloric acid solution and salpeter solution in mass ratio 9: 1, and in described hydrochloric acid solution, HCl content is 34wt%, institute
State HNO in salpeter solution3Content is 61wt%；Immersing in the second pickle liquor again, solid-liquid weight ratio controls to be 1:3.5, is heated to
70 DEG C, acidleach 30min under stirring condition, sucking filtration removes the second pickle liquor, is neutrality with the deionized water wash of 75 DEG C to filtrate,
Sucking filtration, dries and obtains glass sand, and the second pickle liquor is Fluohydric acid .-hydrochloric acid Compound-acid immersion, and described Fluohydric acid .-hydrochloric acid is combined
Pickle liquor is mixed by hydrofluoric acid solution and hydrochloric acid solution in mass ratio 5: 1, and in described hydrofluoric acid solution, the content of HF is
38wt%, in described hydrochloric acid solution, the content of HCl is 34wt%.
Embodiment 4
A kind of quartz deposit prepares the method for glass sand, comprises the steps:
S1, pulverizing: after being roughly selected by quartz deposit, be crushed to particle diameter≤3mm, is placed in shrend 14min in 6 DEG C of water, after taking-up
Grind and obtain the ultra-fine quartz mine that particle diameter is 5-20 μm；
S2, magnetic separation: the ultra-fine quartz mine obtained by S1 is successively in the cartridge type weak magnetic separator that magnetic field intensity is 0.4T and magnetic
Field intensity be 1.3T vertical ring pulsating high gradient intensity magnetic separator in carry out twice magnetic separation and obtain concentrate serosity, control during magnetic separation
Feed ore concentration is 26wt%, and thickening obtains quartz concentrate；
S3, roasting: the quartz concentrate obtained by S2 is roasting 180min under conditions of 850 DEG C, be subsequently placed in 12 DEG C of water
Shrend 16min, immerses 40min in hydrochloric acid-oxalic acid Compound-acid immersion, sucking filtration, washing, dries and obtain quartz sand after taking-up, described
In hydrochloric acid-oxalic acid Compound-acid immersion, the content of HCl is 13wt%, H2C2O4Content be 7.5g/L；
S4, flotation: the quartz sand obtained by S3 adds water to modulate and obtains the ore pulp that concentration is 43wt%, adds according to ore pulp per ton
Entering the polyphosphoric acids modified starch of 28g as inhibitor, after stirring 2.5min, acid adding regulation pH values of pulp is 4-5, according still further to per ton
Calcium ion activator and the 740g of ore pulp addition 460g are 1:3 18-amine. hydrochlorate and dodecylbenzene sodium sulfonate by quality proportioning
Stir 4.5min, FLOTATION SEPARATION 3.5min, washing after the composite collector of composition, air-dry, be dried 75min at 160 DEG C and obtain stone
English washed ore, prepares described polyphosphoric acids modified starch and includes: added by starch in ethanol water, with sodium hydroxide at 70 DEG C
Quaternization 28min, adds polyphosphoric acids, reacts 116min, obtain described polyphosphoric acids modified starch at 132 DEG C, its
Middle starch, sodium hydroxide, the weight proportion of polyphosphoric acids are 1:0.2:0.7；
S5, acidleach: the quartzy washed ore obtained by S4 immerses in the first pickle liquor, solid-liquid weight ratio controls as 0.9:1, heating
To 36 DEG C, acidleach 75min under the conditions of the ultrasound field that power is 650W, sucking filtration removes the first pickle liquor, with 73 DEG C go from
The washing of sub-water is neutrality to filtrate, and described first pickle liquor is hydrochloric acid-nitric acid Compound-acid immersion, described hydrochloric acid-nitric acid Compound-acid
Immersion is formulated by hydrochloric acid solution and salpeter solution in mass ratio 9: 1, and in described hydrochloric acid solution, HCl content is 35wt%, institute
State HNO in salpeter solution3Content is 61wt%；Immersing in the second pickle liquor again, solid-liquid weight ratio controls to be 1:4, is heated to 75
DEG C, acidleach 25min under stirring condition, sucking filtration is removed the second pickle liquor, is neutrality with the deionized water wash of 78 DEG C to filtrate, takes out
Filter, dries and obtains glass sand, and the second pickle liquor is Fluohydric acid .-hydrochloric acid Compound-acid immersion, described Fluohydric acid .-hydrochloric acid Compound-acid
Immersion is mixed by hydrofluoric acid solution and hydrochloric acid solution in mass ratio 5: 1, and in described hydrofluoric acid solution, the content of HF is
32wt%, in described hydrochloric acid solution, the content of HCl is 33wt%.
The method of purification technique that the present invention provides is simple, easily operates；The cost of raw material is low, it is easy to obtain, resource utilization
High；Impurity removing technology efficiency is high, and targetedly, technique is easily controllable；The SiO of the ultralow metallic element high purity quartz prepared2
Content can reach 99.99-99.995%, impurity metallic elements total amount ＜ 100ppm, can meet some special-purposes of quartz such as
Prepare silica crucible, crystalline silicon, electronic material, optical glass, high temp glass, vitreous silica, aerospace vehicle sight glass, height
The requirement to quartz raw material such as level trombone slide glass.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (8)
1. the method that a quartz deposit prepares glass sand, it is characterised in that comprise the steps:
S1, pulverizing: after being roughly selected by quartz deposit, be crushed to particle diameter≤20mm, immerses 10-20min in 0-10 DEG C of water, grinds after taking-up
Mill obtains the ultra-fine quartz mine of particle diameter 5-50 μm；
S2, magnetic separation: the ultra-fine quartz mine obtained by S1 is successively in the weak magnetic separator of magnetic field intensity 0.1-0.5T and magnetic field intensity
Carrying out magnetic separation in the High gradient high intensity magnetic separator of 1.0-1.4T and obtain concentrate serosity, controlling feed ore concentration during twice magnetic separation is
20-30wt%, thickening obtains quartz concentrate；
S3, roasting: the quartz concentrate obtained by S2 roasting 120-200min under conditions of 600-1000 DEG C, be subsequently placed in 10-
Shrend 10-20min in 20 DEG C of water, immerses 30-60min in hydrochloric acid-oxalic acid Compound-acid immersion, sucking filtration, washing, dries after taking-up
To quartz sand；
S4, flotation: the quartz sand obtained by S3 adds water to modulate and obtains the ore pulp that concentration is 40-50wt%, adds according to ore pulp per ton
Entering the modified starch of 20-30g as inhibitor, after stirring 1-3min, acid adding regulation pH values of pulp is 4-5, according still further to ore pulp per ton
3-5min, FLOTATION SEPARATION 3-5min, washing, wind is stirred after adding the activator of 400-500g and the composite collector of 700-800g
Dry, it is dried 60-80min at 100-200 DEG C and obtains quartz washed ore；
S5, acidleach: the quartzy washed ore obtained by S4 immerses in the first pickle liquor, and solid-liquid weight ratio is 0.8-1:1, is heated to 30-
40 DEG C, acidleach 60-100min under the conditions of the ultrasound field of power 400-800W, sucking filtration removes the first pickle liquor, with 70-80 DEG C
Deionized water wash to filtrate be neutrality；Immersing in the second pickle liquor again, solid-liquid weight ratio is 1:2-5, is heated to 60-80
DEG C, acidleach 20-40min under stirring condition, sucking filtration removes the second pickle liquor, with the deionized water wash of 70-80 DEG C to filtrate in
Neutrality, sucking filtration, dry and obtain glass sand.
The method that a kind of quartz deposit the most according to claim 1 prepares glass sand, it is characterised in that in S1,
After being roughly selected by quartz deposit, being crushed to particle diameter is 1-6mm, immerses 12-18min in 0-5 DEG C of water, grinds and obtain particle diameter 5-after taking-up
The ultra-fine quartz mine of 30 μm.
Quartz deposit the most according to claim 1 prepares the method for glass sand, it is characterised in that in S2, described
Weak magnetic separator is cartridge type weak magnetic separator；Described High gradient high intensity magnetic separator is vertical ring pulsating high gradient intensity magnetic separator.
Quartz deposit the most according to claim 1 prepares the method for glass sand, it is characterised in that in S3, described
In hydrochloric acid-oxalic acid Compound-acid immersion, the content of HCl is 10-15wt%, H2C2O4Content be 6-8g/L.
Quartz deposit the most according to claim 1 prepares the method for glass sand, it is characterised in that in S4, described
Modified starch is polyphosphoric acids modified starch, prepares described polyphosphoric acids modified starch and includes: starch is added ethanol water
In, with sodium hydroxide quaternization 20-30min at 60-80 DEG C, add polyphosphoric acids, at 120-140 DEG C, react 90-
150min, obtains described polyphosphoric acids modified starch, and wherein starch, sodium hydroxide, the weight proportion of polyphosphoric acids are 1:0.1-
0.3:0.6-0.8。
Quartz deposit the most according to claim 1 prepares the method for glass sand, it is characterised in that in S4, described
Activator is at least one in calcium ion and magnesium ion；Described composite collector is by the 18-amine. hydrochloric acid of quality proportioning 1:2-4
Salt and dodecylbenzene sodium sulfonate composition.
Quartz deposit the most according to claim 1 prepares the method for glass sand, it is characterised in that in S5, described
First pickle liquor is hydrochloric acid-nitric acid Compound-acid immersion, and the second pickle liquor is Fluohydric acid .-hydrochloric acid Compound-acid immersion；Preferably, described
Hydrochloric acid-nitric acid Compound-acid immersion is formulated by hydrochloric acid and salpeter solution in mass ratio 8-10: 1, and in described hydrochloric acid, HCl content is
31-37wt%, HNO in described salpeter solution3Content is 60-63wt%；Preferably, described Fluohydric acid .-hydrochloric acid Compound-acid immersion
Being mixed by hydrofluoric acid solution and hydrochloric acid in mass ratio 4-6: 1, in described hydrofluoric acid solution, the content of HF is 30-45wt%,
In described hydrochloric acid, the content of HCl is 31-37wt%.
Quartz deposit the most according to claim 1 prepares the method for glass sand, it is characterised in that in S5, ultrasonic
The frequency of wave field is 1-10KHz.
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| CN107185708A (en) * | 2017-07-14 | 2017-09-22 | 长沙有色冶金设计研究院有限公司 | A kind of method that high-purity quartz is prepared with mine tailing |
| CN107473231A (en) * | 2017-09-19 | 2017-12-15 | 江苏凯达石英股份有限公司 | A kind of processing purifying technique to glass sand mine tailing |
| CN107555443A (en) * | 2017-09-30 | 2018-01-09 | 江苏闽江矿业有限公司 | A kind of quartz sand raw ore handling process at initial stage |
| CN107793035A (en) * | 2017-11-09 | 2018-03-13 | 新沂市宏润石英硅微粉有限公司 | A kind of preparation method of fused quartz powder |
| CN108751210A (en) * | 2018-06-23 | 2018-11-06 | 新疆能源（集团）晶拓科技材料有限责任公司 | A kind of method for calcinating of glass sand |
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| CN110963498A (en) * | 2019-12-26 | 2020-04-07 | 湖南工业大学 | Process for purifying quartz sand by iterative hydrothermal method and high-purity quartz sand |
| CN111268684A (en) * | 2020-02-28 | 2020-06-12 | 新沂市引河石英材料有限公司 | Screening and purifying process for high-purity fused quartz |
| CN112357925A (en) * | 2020-11-12 | 2021-02-12 | 徐州融鑫新材料有限公司 | Purification process for quartz sand by using microorganisms |
| CN112744821A (en) * | 2019-10-31 | 2021-05-04 | 青川县云龙麒达石英砂有限责任公司 | Quartz sand acid elution purification process |
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| CN113735128A (en) * | 2021-08-16 | 2021-12-03 | 武汉理工大学 | Preparation method of high-purity quartz sand |
| CN114014540A (en) * | 2021-12-08 | 2022-02-08 | 连云港太平洋半导体材料有限公司 | Preparation process of opal quartz glass |
| CN114378026A (en) * | 2021-12-17 | 2022-04-22 | 中建材蚌埠玻璃工业设计研究院有限公司 | Method for preparing electronic grade high-purity quartz sand |
| CN114671440A (en) * | 2022-03-08 | 2022-06-28 | 北京科技大学 | Superconducting high-gradient magnetic separation high-silicon solid waste low-carbon green preparation of high-purity SiO2Method (2) |
| CN114813275A (en) * | 2022-04-22 | 2022-07-29 | 云南省地质矿产勘查开发局中心实验室（国土资源部昆明矿产资源监督检测中心） | Preparation method of alpha-quartz type free silicon dioxide breathing dust |
| CN115872407A (en) * | 2021-09-26 | 2023-03-31 | 中国地质科学院郑州矿产综合利用研究所 | Preparation method of 4N-grade high-purity quartz sand |
| WO2024036664A1 (en) * | 2022-08-17 | 2024-02-22 | 鞍钢集团矿业有限公司 | Method for low-carbon efficient extraction of high-purity sio2 from high-silicon hematite tailings |
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| CN107473231A (en) * | 2017-09-19 | 2017-12-15 | 江苏凯达石英股份有限公司 | A kind of processing purifying technique to glass sand mine tailing |
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| CN111268684A (en) * | 2020-02-28 | 2020-06-12 | 新沂市引河石英材料有限公司 | Screening and purifying process for high-purity fused quartz |
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| CN114014540B (en) * | 2021-12-08 | 2022-07-29 | 连云港太平洋半导体材料有限公司 | Preparation process of opal quartz glass |
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| CN114671440A (en) * | 2022-03-08 | 2022-06-28 | 北京科技大学 | Superconducting high-gradient magnetic separation high-silicon solid waste low-carbon green preparation of high-purity SiO2Method (2) |
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