CN109665528A - Method containing corundum type quartzite preparation use for electronic products high purity quartz emery dust - Google Patents
Method containing corundum type quartzite preparation use for electronic products high purity quartz emery dust Download PDFInfo
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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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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of methods containing corundum type quartzite preparation use for electronic products high purity quartz emery dust, first raw ore carry out it is artificial it is selected after, then quartz particles are carried out sand processed, the sand produced, except corundum, irony isodensity are greater than the impurity of quartz, separates feldspar particle using the method for flotation again later using the method for heavy-fluid separation；The feldspar that flotation is not isolated again go by hydroflouric acid washout；Quartz sand is eluted pure, reduction roasting by calcining, water quenching, high-temperature acid again, the method for high-temp chlorination removes impurity to bottom line, so that it is guaranteed that the product after purification meets or exceeds the quality technology requirement of rower " use for electronic products glass sand ", to meet the needs of domestic user.
Description
Technical field
The invention belongs to non-metal ore advanced processing technical areas, in particular to a kind of corundum type quartzite that contains to prepare electronics
The method of product high purity quartz emery dust.
Background technique
It is provided according to National Standard of the People's Republic of China SJ3228.1-2016 " use for electronic products glass sand ": electricity
Sub- product glass sand product is for manufacturing the devices such as pipe, stick, block, plate, piece and the crucible of semiconductor quartz member.Its
Technical requirements provide: use for electronic products glass sand appearance should be the white particle with certain transparency, should be without heterochromatic, meat
The visible impurity of eye.Partial size should be greater than or equal to 90% in the mass accumulation score of 70um-350um range；Partial size is less than 100um
Or the mass accumulation score greater than 300um should be less than 1%；Dioxide-containing silica:
Primes should greatly >=99.9991%；Seconds >=99.9990%；Three-level product >=99.9980%；
Impurity element total content see the table below
2 impurity content of table
Unit is every gram of microgram
Currently, the use for electronic products glass sand raw material that China uses is mostly from the import of Unimin Corp. (US), the U.S..And I
The manufacturer of the domestic use for electronic products glass sand of state mostly uses domestic or import igneous rock vein quartz for raw material production
Use for electronic products glass sand, although certain technical indicators in the product of production meet or exceed Unimin Corp. (US), the U.S.
Product, but the unstable quality of product, can not large batch of industrialized production, main cause includes: 1, the raw material selected
A quality technology standard is not formulated；2, production technology and equipments are still not perfect；3, crucial purification technique do not grasp also and
It breaks through；4, none full-time R&D team；5, the dynamics of the support of government department is inadequate.
In order to solve the problems, such as preparation use for electronic products glass sand raw material, we must make full use of China existing
Silicon ore resources advantage, strengthens research and development capabilities, and develops a kind of extensive use for electronic products high purity quartz of novel and raw material sources
The purification technique and process route of sand preparation, make it industrialized production on a large scale, import substitutes, to meet China
The growing demand of use for electronic products high purity quartz product industry.China has many good type Quartz sand resources, just
Beautiful type Quartz sand is quartz and corundum and feldspar chiasma type association type mineral, and major impurity is corundum, and feldspar color is shallow
It is red.Through chemical analysis: corundum (Al2O3) accounts for 2-5%；Feldspar is with potassium feldspar (K2O·Al2O3·6SiO(2)For 1% hereinafter, also
0..5% or so is accounted for altogether containing a small amount of albite and anorthite；With the quartz components in magnifying glass viewing rock mine, quartz crystal
In pelletized form, transparency is good, but there is pore shape object in inside.The rock mine oil in place is big, is easy to exploit, but quartzy in use process
It is kept completely separate with corundum and feldspar and the black impurity in quartz particles is removed difficulty is larger, temporarily not mature separation
Technique, and utilize related literatures and report containing corundum type quartzite preparation use for electronic products high purity quartz emery dust.
Summary of the invention
In view of the deficiencies of the prior art, electronics is prepared using containing corundum type quartzite the object of the present invention is to provide a kind of
The method of product high purity quartz emery dust.
To achieve the above object, provided by the invention to prepare use for electronic products high purity quartz using containing corundum type quartzite
The method of emery dust, which comprises the steps of:
(1) pretreatment of ore and sand processed: the soil impurity on ore first is cleaned with clean water, then through artificial just blanking
Visible foreign is removed, carries out dry or wet sand, first magnetic separation with sand making machine, rear gravity treatment regathers 30-150 mesh grain size intervals
Particulate matter, the material of wet process are spare after must drying；It is spare after dry-method sand manufacturing screening；
(2) material in the step (1) is sent into equipped in heavy-fluid reaction kettle；The step of by stirring-standing-separation
The substance for making density be greater than quartz then sinks to heavy-fluid bottom, so that quartz particles be made to separate with corundum, irony substance；The separation
Step repeats 1-3 times, so that corundum, irony and other impurities are separated from quartz particles；
(3) the quartz particles material ethanol washing separated in the step (2) is clean, recycling heavy-fluid recycling
It uses；
(4) the quartz particles material that washing obtains in the step (3) is sent into the calcining that pure quartz glass is material
After carrying out calcining in furnace 1-2 hours, water quenching is carried out rapidly, and the material after water quenching carries out being dehydrated again spare, obtains quartz sand particle；
(5) quartz sand particle in the step (4) is subjected to flotation, to separate the spectra impurity that do not remove, it
The hydrofluoric acid solution with mass percent concentration not less than 20% carries out heating dynamic pickling afterwards, to remove the feldspar not floatingly selected
Mineral；Again with originally water washing quartz sand particle until the liquid shows neutral being washed out, then with pure water quartz sand particle
It is spare after dehydrating afterwards three times；
(6) step (5) quartz sand spare after dry is sent into the calcining furnace that pure quartz glass is material
After 550-600 DEG C of temperature carries out reduction roasting 1-2 hours, water quenching is carried out rapidly, the material after water quenching carries out being dehydrated again spare；
(7) at room temperature using the hydrofluoric acid of mass percentage concentration >=20% to spare material after dehydration in step (6) into
Row fluidisation state washing, is passed through ClO to acid solution bottom while washing2After gas oxidation purification 45-60 minutes, then stop being passed through
ClO2Gas is warming up to 90 DEG C, and after insulation reaction 3 hours, the aluminium in sampling analysis material, and with the mass percentage of aluminium
≤ 5.0ppm is pickling terminal；Acid solution is removed, with clean tap water washing material until after the liquid shows neutral being washed out,
It is washing terminal that with electron level pure water, into the liquid being washed out, fluorine ion and chlorine ion concentration, which are respectively less than 10ppm, again,
Quartz sand particle that is dry afterwards, screening out 30-150 mesh grain size intervals is spare；
(8) quartz sand particle in the step (7) after dry screening is sent into high-temperature chlorination device, 1250~
Cooling after being carried out high-temp chlorination 1-2 hours using hydrogen chloride gas as chlorinating agent at a temperature of 1300 DEG C, packaging can be obtained electronics and produce
Product high purity quartz emery dust finished product.
As a preferred embodiment, the heavy-fluid in the step (2) are as follows: tried by bromoform or tetrabromoethane to be main
Agent is the organic heavy liquid that density that auxiliary reagent is made into is 2.9-3.0 by ether or ethyl alcohol；Or by silico-tungstic acid cerium, metatungstic acid iron,
Metatungstic acid sodium, ammonium metatungstate, it is any in silico-tungstic acid be main agents, by any in water, ethyl alcohol, dichlroroethanol, ethylene glycol, glycerol
The heavy-fluid for being 2.9-3.0 for the density that auxiliary reagent is made into.
As a preferred embodiment, the temperature of step (4) calcining is 880-950 DEG C.
As another preferred embodiment, the method for floating in the step (5) is as follows: being adjustment with hydrofluoric acid and lye
Agent, using No. 2 oil as foaming agent, floatingly selects spectra impurity under conditions of pH=2.0~3.0 using lauryl amine as capturing agent.
As another preferred embodiment, the spectra impurity separated in the step (5) carries out physics again and changes
Learn the feldspar emery dust finished product refined after deep processing processing.
As another preferred embodiment, pickling is carried out to material using fluidization pickling purifying plant in the step (7)
Purification, ClO2Gas is passed through in pickling solution from fluidization pickling purifying plant bottom；ClO used2Gas air or nitrogen or its
It is 10% or less that his inert gas, which is diluted to volume ratio,.
Technical solution of the present invention first raw ore carry out it is artificial it is selected after, quartz particles are carried out sand processed, are produced
Sand (need to first drying for wet production) is first isolated corundum and irony element from quartz sand using the method for heavy-fluid separation
Come；The feldspar particle in quartz sand is separated using the method for flotation again；Hydroflouric acid removes the feldspar that flotation is not isolated again
Go, then the quartz sand after purification by calcining, water quenching, high-temperature acid elute pure, reduction roasting, high-temp chlorination method miscellaneous
Matter is removed to bottom line, so that it is guaranteed that the product after purification meets or exceeds the quality of rower " use for electronic products glass sand "
Technical requirements, to meet the needs of domestic user.
The invention has the following advantages: having captured corundum type Quartz sand in the prior art, can not to prepare purity big
Technical barrier in 99.99% quartz sand purifying, whole process are served as theme with the separation of quartz and corundum and feldspar；Not
It is kept completely separate before feldspar, quartz is not calcined, in case feldspar causes to expect after melting at high temperature to subsequent purification
Less than difficulty；After separating feldspar, takes and first calcine water quenching+preliminary removal of impurities of pickling purification；Then oxidizing roasting+acid is being carried out
Remove miscellaneous, during pickling impurity removal, the present invention provides a kind of hydrofluoric acid+chlorine dioxides as in pickling purification process
Preferred reagent: the mix reagent has played a kind of good synergistic effect effect: particularly hydrofluoric acid in purification process
Open the lattice of silicon dioxide molecules crystal；And the metal impurities in chlorine dioxide rapid oxidation lattice, to reach quick
The purpose of removal of impurities；And ClO2Gas is a kind of feature of environmental protection gas, is diluted in air and not can cause environmental pollution in water.Its
Impurity-eliminating effect is obvious, after impurity is reduced within the scope of intermediate control, is finally cleaned with the method for high-temp chlorination, it is ensured that most
Product afterwards meets or exceeds requirements of the national standard.China's glass sand raw material use scope is opened up.
Specific embodiment
Detailed specific description done to the present invention combined with specific embodiments below, but protection scope of the present invention not office
It is limited in following embodiment.
Embodiment one:
Illustrate technical process of the invention as raw material using the produced Quartz sand containing corundum type in Inner Mongol Chifeng:
(1) pretreatment of ore and sand processed: the soil impurity on ore first is cleaned with clean water, then through artificial just blanking
Remove solid impurity, carry out dry or wet sand with sand making machine, after magnetic separation and gravity treatment, collect 30-120 mesh or 40-140 mesh or
The particulate matter of 60-150 mesh or grain size intervals as needed, the material of wet process are spare after must drying；After dry-method sand manufacturing screening
It is spare；
(2) material in step (1) is sent into equipped with bromoform is main agents, chloroform is that auxiliary reagent is made into
D25Density is the heavy-fluid of 2.9-3.0g/ml and opens in stirred autoclave；30 minutes are stood-separation by stirring 30 minutes-
15 minutes the step of make corundum, irony isodensity be greater than quartz substance then sink to heavy-fluid bottom, thus make quartz particles and just
Beautiful, irony substance separation；It is separated 1-3 times again depending on quartz sand particle size and isolated effect, makes the impurity such as corundum, irony from stone
It is separated in English particle；
(3) the quartz particles material ethanol washing separated in step (2) is completely spare, recycling heavy-fluid recycling
It uses；
(4) quartz sand particle in step (3) flotation is carried out to isolate to separate the spectra in quartz sand
The spectra come is purified again；The quartz sand separated with originally water washing it is neutral after again with pure water three times, take off
It is spare after water is dry；
(5) the at a temperature of high-temperature calcination that feeding pure quartz glass in step (4) is in the calcining furnace of material at 950 DEG C
After 1-2 hours, water quenching is carried out rapidly, and the material after water quenching carries out being dehydrated again spare；
(6) hydrofluoric acid solution the quartz sand particle in step (5) with mass percent concentration not less than 20% carries out
Dynamic pickling is heated, to remove the spectra not floatingly selected；Later with originally water washing to neutrality, then three times with pure water
It is spare after dehydrating afterwards；
(7) the quartz sand in step (6), to be sent into pure quartz glass be in the calcining furnace of material with CO gas is fuel,
600 DEG C Celsius at a temperature of reduction roasting 1 hour after, carry out water quenching rapidly, the material after water quenching carries out being dehydrated again spare；
(8) fluidisation state is carried out to the material in step (6) using the hydrofluoric acid of mass percentage concentration >=20% at room temperature
Washing is passed through ClO to acid solution bottom while washing2Gas oxidation purification 60 minutes；Stopping is passed through ClO2Gas；It is warming up to 90
DEG C, and after insulation reaction 3 hours, sampling analysis aluminium therein, and using mass percentage≤5.0ppm of aluminium as pickling terminal；
Acid solution is removed, after clean originally water washing to neutrality, then it is equal with electron level pure water to fluorine ion and chlorine ion concentration
It is drying after washing terminal less than 10ppm, screens out 30-120 mesh or 40-140 mesh or 60-150 mesh or required grain size intervals
Sand particle it is spare；
9) step (8) resulting material send into high-temperature chlorination device 1300 DEG C Celsius or so at a temperature of with chlorination
Hydrogen is that use for electronic products glass sand product can be obtained in cooling, packaging after chlorinating agent carries out high-temp chlorination 1 hour.
It is as follows with the impurity content in ICP-MS test quartz sand: unit (ug/g)
Al:4,8；Ca:0.40；Fe:0.10；Na:0.05；K:0.06；Li:0.11；Mg:0.02；Cr0.01；Ni:0.01；
B:0.03；Mn:0.01；Cu:0.01.
Its all technical indicator meets or exceeds rower use for electronic products glass sand quality technology standard requirements.
Embodiment two:
Quartz sand containing corundum type, which is produced, using Hubei somewhere illustrates technical process of the invention as raw material:
(1) pretreatment of ore and sand processed: the soil impurity on ore first is cleaned with clean water, then through artificial just blanking
Remove solid impurity, carry out dry or wet sand with sand making machine, after magnetic separation and gravity treatment, collect 30-120 mesh or 40-140 mesh or
The particulate matter of 60-150 mesh or grain size intervals as needed, the material of wet process are spare after must drying；After dry-method sand manufacturing screening
It is spare；
(2) material in step (1) is sent into equipped with silico-tungstic acid cerium is main agents, and ethylene glycol etc. is made into for auxiliary reagent
D25Density is the heavy-fluid of 3.0g/ml and opens in stirred autoclave；30 minutes are stood -15 points of separation by stirring 30 minutes -
The substance that the step of clock makes corundum, irony isodensity be greater than quartz then sinks to heavy-fluid bottom, to make quartz particles and corundum, iron
Metallic substance separation；It is separated 1-3 times again depending on quartz sand particle size and isolated effect, makes the impurity such as corundum, irony from quartz
It is separated in grain；
(3) the quartz particles material ethanol washing separated in step (2) is completely spare, recycling heavy-fluid recycling
It uses；
(4) quartz sand particle in step (3) flotation is carried out to isolate to separate the spectra in quartz sand
The spectra come is purified again；The quartz sand separated with originally water washing it is neutral after again with pure water three times, take off
It is spare after water is dry；
(5) the at a temperature of high-temperature calcination that feeding pure quartz glass in step (4) is in the calcining furnace of material at 880 DEG C
After 1 hour, water quenching is carried out rapidly, and the material after water quenching carries out being dehydrated again spare；
(6) quartz sand particle in step (5) is heated with the hydrofluoric acid solution that mass percent concentration is 20%
Dynamic pickling, to remove the spectra not floatingly selected；It is taken off afterwards three times with originally water washing to neutrality, then with pure water later
It is spare after water is dry；
(7) the quartz sand in step (6), to be sent into pure quartz glass be in the calcining furnace of material with CO gas is fuel,
550 DEG C Celsius at a temperature of reduction roasting 2 hours after, carry out water quenching rapidly, the material after water quenching carries out being dehydrated again spare；
(8) fluidisation state is carried out to the material in step (6) using the hydrofluoric acid of mass percentage concentration 30% at room temperature to wash
It washs, is passed through ClO to acid solution bottom while washing2Gas oxidation purification 45 minutes；Stopping is passed through ClO2Gas；90 degree are warming up to,
And after insulation reaction 3 hours, sampling analysis aluminium therein, and using mass percentage≤5.0ppm of aluminium as pickling terminal；It is de-
Except acid solution, after clean originally water washing to neutrality, then it is small with electron level pure water to fluorine ion and chlorine ion concentration
It dried after 10ppm is washing terminal, screen out 30-120 mesh or 40-140 mesh or 60-150 mesh or required grain size intervals
Sand particle is spare；
9) step (8) resulting material send into high-temperature chlorination device 1250 degree Celsius or so at a temperature of with chlorination
Hydrogen is that use for electronic products glass sand product can be obtained in cooling, packaging after chlorinating agent carries out high-temp chlorination 2 hours.
It is as follows with the impurity content in ICP-MS test quartz sand: unit (ug/g)
Al:4,2.0；Ca:0.26；Fe:0.08；Na:0.06；K:0.05；Li:0.20；Mg:0.03；Cr0.03；Ni:
0.02；B:0.03；Mn:0.02；Cu:0.03.
Its all technical indicator meets or exceeds rower use for electronic products glass sand quality technology standard requirements.
Embodiment three:
Quartz sand containing corundum type, which is produced, using Anhui somewhere illustrates technical process of the invention as raw material:
(1) pretreatment of ore and sand processed: the soil impurity on ore first is cleaned with clean water, then through artificial just blanking
Remove solid impurity, carry out dry or wet sand with sand making machine, after magnetic separation and gravity treatment, collect 30-120 mesh or 40-140 mesh or
The particulate matter of 60-150 mesh or grain size intervals as needed, the material of wet process are spare after must drying；After dry-method sand manufacturing screening
It is spare；
(2) material in step (1) is sent into and is equipped with using tetrabromoethane as main agents main agents, supplemented by second ether etc.
Help the d that reagent is made into25Density is the heavy-fluid of 3.0g/ml and opens in stirred autoclave；30 points are stood by stirring 30 minutes-
The substance that clock-separation 15 minutes the step of make corundum, irony isodensity be greater than quartz then sinks to heavy-fluid bottom, to make quartz
Grain is separated with corundum, irony substance；It is separated 1-3 times again depending on quartz sand particle size and isolated effect, keeps corundum, irony etc. miscellaneous
Matter is separated from quartz particles；
(3) the quartz particles material ethanol washing separated in step (2) is completely spare, recycling heavy-fluid recycling
It uses；
(4) quartz sand particle in step (3) flotation is carried out to isolate to separate the spectra in quartz sand
The spectra come is purified again；The quartz sand separated with originally water washing it is neutral after again with pure water three times, take off
It is spare after water is dry；
(5) the at a temperature of high-temperature calcination that feeding pure quartz glass in step (4) is in the calcining furnace of material at 880 DEG C
After 1 hour, water quenching is carried out rapidly, and the material after water quenching carries out being dehydrated again spare；
(6) quartz sand particle in step (5) is heated with the hydrofluoric acid solution that mass percent concentration is 20%
Dynamic pickling, to remove the spectra not floatingly selected；It is taken off afterwards three times with originally water washing to neutrality, then with pure water later
It is spare after water is dry；
(7) the quartz sand in step (6), to be sent into pure quartz glass be in the calcining furnace of material with CO gas is fuel,
550 DEG C Celsius at a temperature of reduction roasting 2 hours after, carry out water quenching rapidly, the material after water quenching carries out being dehydrated again spare；
(8) fluidisation state is carried out to the material in step (6) using the hydrofluoric acid of mass percentage concentration 30% at room temperature to wash
It washs, is passed through ClO to acid solution bottom while washing2Gas oxidation purification 45 minutes；Stopping is passed through ClO2Gas；90 degree are warming up to,
And after insulation reaction 3 hours, sampling analysis aluminium therein, and using mass percentage≤5.0ppm of aluminium as pickling terminal；It is de-
Except acid solution, after clean originally water washing to neutrality, then it is small with electron level pure water to fluorine ion and chlorine ion concentration
It dried after 10ppm is washing terminal, screen out 30-120 mesh or 40-140 mesh or 60-150 mesh or required grain size intervals
Sand particle is spare；
9) step (8) resulting material send into high-temperature chlorination device 1250 degree Celsius or so at a temperature of with chlorination
Hydrogen is that use for electronic products glass sand product can be obtained in cooling, packaging after chlorinating agent carries out high-temp chlorination 2 hours.
It is as follows with the impurity content in ICP-MS test quartz sand: unit (ug/g)
Al:4.8；Ca:0.23；Fe:0.05；Na:0.07；K:0.06；Li:0.20；Mg:0.02；Cr0.03；Ni:0.01；
B:0.03；Mn:0.01；Cu:0.01.
Its all technical indicator meets or exceeds rower use for electronic products glass sand quality technology standard requirements.
Example IV:
Illustrate technical process of the invention as raw material using the produced Quartz sand containing corundum type in Henan:
(1) pretreatment of ore and sand processed: the soil impurity on ore first is cleaned with clean water, then through artificial just blanking
Remove solid impurity, carry out dry or wet sand with sand making machine, after magnetic separation and gravity treatment, collect 30-120 mesh or 40-140 mesh or
The particulate matter of 60-150 mesh or grain size intervals as needed, the material of wet process are spare after must drying；After dry-method sand manufacturing screening
It is spare；
(2) material in step (1) is sent into equipped with metatungstic acid sodium is main agents, ethyl alcohol is d that auxiliary reagent is made into25
Density is the heavy-fluid of 2.9-3.0g/ml and opens in stirred autoclave；30 minutes are stood -15 points of separation by stirring 30 minutes -
The substance that the step of clock makes corundum, irony isodensity be greater than quartz then sinks to heavy-fluid bottom, to make quartz particles and corundum, iron
Metallic substance separation；It is separated 1-3 times again depending on quartz sand particle size and isolated effect, makes the impurity such as corundum, irony from quartz
It is separated in grain；
(3) the quartz particles material ethanol washing separated in step (2) is completely spare, recycling heavy-fluid recycling
It uses；
(4) quartz sand particle in step (3) flotation is carried out to isolate to separate the spectra in quartz sand
The spectra come is purified again；The quartz sand separated with originally water washing it is neutral after again with pure water three times, take off
It is spare after water is dry；
(5) the at a temperature of high-temperature calcination that feeding pure quartz glass in step (4) is in the calcining furnace of material at 950 DEG C
After 1-2 hours, water quenching is carried out rapidly, and the material after water quenching carries out being dehydrated again spare；
(6) hydrofluoric acid solution the quartz sand particle in step (5) with mass percent concentration not less than 20% carries out
Dynamic pickling is heated, to remove the spectra not floatingly selected；Later with originally water washing to neutrality, then three times with pure water
It is spare after dehydrating afterwards；
(7) the quartz sand in step (6), to be sent into pure quartz glass be in the calcining furnace of material with CO gas is fuel,
600 DEG C Celsius at a temperature of reduction roasting 1 hour after, carry out water quenching rapidly, the material after water quenching carries out being dehydrated again spare；
(8) fluidisation state is carried out to the material in step (6) using the hydrofluoric acid of mass percentage concentration >=20% at room temperature
Washing is passed through ClO to acid solution bottom while washing2Gas oxidation purification 60 minutes；Stopping is passed through ClO2Gas；It is warming up to 90
DEG C, and after insulation reaction 3 hours, sampling analysis aluminium therein, and using mass percentage≤5.0ppm of aluminium as pickling terminal；
Acid solution is removed, after clean originally water washing to neutrality, then it is equal with electron level pure water to fluorine ion and chlorine ion concentration
It is drying after washing terminal less than 10ppm, screens out 30-120 mesh or 40-140 mesh or 60-150 mesh or required grain size intervals
Sand particle it is spare；
9) step (8) resulting material send into high-temperature chlorination device 1300 DEG C Celsius or so at a temperature of with chlorination
Hydrogen is that use for electronic products glass sand product can be obtained in cooling, packaging after chlorinating agent carries out high-temp chlorination 1 hour.
It is as follows with the impurity content in ICP-MS test quartz sand: unit (ug/g)
Al:5.0；Ca:0.30；Fe:0.09；Na:0.03；K:0.06；Li:0.09；Mg:0.02；Cr0.02；Ni:0.01；
B:0.03；Mn:0.02；Cu:0.01.
Its all technical indicator meets or exceeds rower use for electronic products glass sand quality technology standard requirements.
The pickling purifying plant applied in the method for the present invention can be found in inventor and authorize patent of invention:
201110121881.9；201110247061.4；201310279400.6.The quartz sand high-temp chlorination applied in the method for the present invention
Device is existing authorization patent of invention technology, and the patent No. 201610640562.1, which has been successfully realized industrialization and has answered
With.
Claims (6)
1. a kind of utilize the method containing corundum type quartzite preparation use for electronic products high purity quartz emery dust, which is characterized in that packet
Include following steps:
(1) pretreatment of ore and sand processed: the soil impurity on ore first is cleaned with clean water, then is removed admittedly through artificial primary election
Body impurity carries out dry or wet sand, first magnetic separation with sand making machine, and rear gravity treatment regathers the particle of 30-150 mesh grain size intervals
Object, the material of wet process are spare after must drying；It is spare after dry-method sand manufacturing screening；
(2) material in the step (1) is sent into equipped in heavy-fluid reaction kettle；Made by the step of stirring-standing-separation close
The substance that degree is greater than quartz sinks to heavy-fluid bottom, so that quartz particles be made to separate with corundum, irony substance；The separating step weight
It is 1-3 times multiple, so that corundum, irony and other impurities are separated from quartz particles；
(3) the quartz particles material ethanol washing separated in the step (2) is clean, recycling heavy-fluid recycling makes
With；
(4) the quartz particles material that washing obtains in the step (3) is sent into the calcining furnace that pure quartz glass is material
After carrying out calcining 1-2 hours, water quenching is carried out rapidly, and the material after water quenching carries out being dehydrated again spare, obtains quartz sand particle；
(5) quartz sand particle in the step (4) is subjected to flotation, to separate the spectra impurity that do not remove, Zhi Houyong
Hydrofluoric acid solution of the mass percent concentration not less than 20% carries out heating dynamic pickling, to remove the feldspar ore not floatingly selected
Object；Again with originally water washing quartz sand particle until the liquid shows neutral being washed out, then with pure water quartz sand particle three
It is spare after dehydration and drying after secondary；
(6) step (5) quartz sand spare after dry is sent into the calcining furnace that pure quartz glass is material in 550-
After 600 DEG C of temperature carries out reduction roasting 1-2 hours, water quenching is carried out rapidly, the material after water quenching carries out being dehydrated again spare；
(7) spare material after dehydration in step (6) is flowed using the hydrofluoric acid of mass percentage concentration >=20% at room temperature
Change state washing, is passed through ClO to acid solution bottom while washing2After gas oxidation purification 45-60 minutes, then stop being passed through ClO2Gas
Body is warming up to 90 DEG C, and after insulation reaction 3 hours, the aluminium in sampling analysis material, and with the mass percentage of aluminium≤
5.0ppm is pickling terminal；Acid solution is removed, with clean tap water washing material until after the liquid shows neutral being washed out, then
It is washing terminal that with electron level pure water, into the liquid being washed out, fluorine ion and chlorine ion concentration, which are respectively less than 10ppm, after
Quartz sand particle that is dry, screening out 30-150 mesh grain size intervals is spare；
(8) quartz sand particle after screening dry in the step (7) is sent into high-temperature chlorination device, at 1250~1300 DEG C
At a temperature of carried out high-temp chlorination 1-2 hour using hydrogen chloride gas as chlorinating agent after it is cooling, pack use for electronic products height can be obtained
Pure quartz sand powder finished product.
2. according to claim 1 utilize the side containing corundum type quartzite preparation use for electronic products high purity quartz emery dust
Method, it is characterised in that: the heavy-fluid in the step (2) are as follows: by bromoform or tetrabromoethane be main agents, by ether or second
Alcohol is the organic heavy liquid that the density that auxiliary reagent is made into is 2.9-3.0；Or by silico-tungstic acid cerium, metatungstic acid iron, metatungstic acid sodium, inclined tungsten
Any in sour ammonium, silico-tungstic acid is main agents, is matched by any in water, ethyl alcohol, dichlroroethanol, ethylene glycol, glycerol for auxiliary reagent
At density be 2.9-3.0 heavy-fluid.
3. according to claim 1 utilize the side containing corundum type quartzite preparation use for electronic products high purity quartz emery dust
Method, it is characterised in that: the temperature of step (4) calcining is 880-950 DEG C.
4. according to claim 1 utilize the side containing corundum type quartzite preparation use for electronic products high purity quartz emery dust
Method, it is characterised in that: the method for floating in the step (5) is as follows: being to catch with lauryl amine using hydrofluoric acid and lye as regulator
Agent is obtained, using No. 2 oil as foaming agent, floatingly selects spectra impurity under conditions of pH=2.0~3.0.
5. according to claim 1 utilize the side containing corundum type quartzite preparation use for electronic products high purity quartz emery dust
Method, it is characterised in that: after the spectra impurity separated in the step (5) carries out physics and chemical deep processing processing again
The feldspar emery dust finished product refined.
6. according to claim 1 utilize the side containing corundum type quartzite preparation use for electronic products high purity quartz emery dust
Method, it is characterised in that: pickling purification, ClO are carried out to material using fluidization pickling purifying plant in the step (7)2Gas
It is passed through in pickling solution from fluidization pickling purifying plant bottom；ClO used2Gas air or nitrogen or other inert gases are dilute
Releasing to volume ratio is 10% or less.
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