CN104925818B - High-purity quartz powder producing technology and device utilizing quartz mill tailings - Google Patents
High-purity quartz powder producing technology and device utilizing quartz mill tailings Download PDFInfo
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- CN104925818B CN104925818B CN201510407863.5A CN201510407863A CN104925818B CN 104925818 B CN104925818 B CN 104925818B CN 201510407863 A CN201510407863 A CN 201510407863A CN 104925818 B CN104925818 B CN 104925818B
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Abstract
The invention provides a high-quality quartz powder producing technology utilizing quartz mill tailings. The high-quality quartz powder producing method comprises the steps that firstly the content of impurity in the quartz mill tailings is tested, and acid picking treatment is conducted according to the content of Al203 in the quartz mill tailings; the materials after being picked with acid are placed into a reaction still, and acid picking is conducted through mixed acid liquor of nitric acid and fluosilicic acid to dissolve the iron in the materials; the quartz mill tailings getting rid of iron is washed to neutral, then dehydration is conducted, the materials are placed into the reaction still through concentrated hydrochloric acid to conduct acid picking, the materials are washed to be neutral, then dehydration is conducted, the quartz powder of 120-200 meshes or 200-400 meshes in the materials is isolated, and then the high-quality quartz powder is acquired. According to the method, the quartz mill tailings can be used effectively, the quartz mill tailings is produced into high-quality quartz powder, and the purpose of changing waste into valuable is realized. The invention further provides a device used in the above technology.
Description
Technical field
The present invention relates to a kind of utilization quartz tail sand produces the method for high-purity ground quartz and special device, belong to nonmetallic
Ore deposit deep processing and environmental technology field.
Background technology
Quartz tail sand: as the term suggests, it is that most end is short during quartz sand processing or the emery dust of caudal end, is also secondary
Product.The mesh number of the tailings that quartz sand processing enterprise of current China is produced is mostly in 120 mesh sieves with the area down to more than 400 mesh sieves
Between scope, produce quartz tail sand per year in terms of ten million ton, main distribution again Area, Fengyang County, Anhui, Heyuan, Shandong Linyi, Hebei Shahe and
Lei Zhuan etc..Quartz tail sand is for finished product quartz sand (24 mesh sieves down to 120 mesh sieves on): not only its particle diameter is little, specific surface
Long-pending big, surface energy is big, the time length of precipitation, contained moisture are high, impurity is many, difficult processing, drying are more difficult to, and the market demand
Have a small amount of use factory as construction ceramic, cement industry and aerated bricks industry for building etc., its price per ton regarding different, the stone-like pulse of its quality
Tailings that English ore deposit is produced per ton about dozens of yuan；The quartz tail sand of other sedimentary rocks per ton at 10～15 yuan.Therefore, stone
English tailings not only becomes " chicken ribs " that each produces quartz sand enterprise, but also must be special, larger cement court carries out
Storage, stacking.More make one headache: rainy day, quartz tail sand trickles everywhere with rainwater, seriously pollute water resource environment；
Fine day, when blowing, dust waves with the wind, seriously contaminated air quality environment etc..So, the general enterprise producing quartz sand is all
Quartz tail sand is processed as rubbish.
With scientific and technological level developing rapidly and society continuous progress, the living standard of people and self diathesis continuous
Improve, people's environmental consciousness also more and more strong.After on January 1st, 2015 new revision, " environmental law " comes into effect, and makes the ring of people
Consciousness of protecting has risen to a new height again.Integrated treatment with regard to quartz tail sand and Utilizing question get more and more and cause and be subject to
Very big concern to quartz sand processing enterprise and the whole society.Therefore, how scientifically, reasonably, fully, effectively utilize me
State is existing, abundant, cheap quartz tail sand resource, develops market in urgent need and has high technology content and high added value stone
English tailings product, and accomplish no pollution in production process, the advanced technology of zero-emission and technique and device, it is that pendulum is each at us
One in face of individual silicon materials research and development technology personnel brand-new, be rich in epochal character and challenging problem.Inquiry is related specially
Profit and documents and materials, do not retrieve with regard to producing high-purity ground quartz patent literature using quartz tail sand.
Content of the invention
The invention provides a kind of employing quartz tail sand produces the process of high-purity ground quartz, solve in background technology
Deficiency, the method effectively can utilize quartz tail sand, be produced into the high-purity ground quartz of high added value, realize change give up into
Precious purpose.
The technical scheme that realizing above-mentioned purpose of the present invention is provided is:
(1) a kind of utilization quartz tail sand produces the technique of high-purity ground quartz, comprises the following steps: (1), test quartz tail sand
In impurity content, impurity includes al2o3、fe2o3, judge al in quartz tail sand2o3Content whether be more than 2%；
(2), for al2o3Content >=2% quartz tail sand, quartz tail sand is put in reactor, adds in reactor
Hydrogenation fluoric acid, opens stirring and carries out pickling to quartz tail sand, and acid solution is removed after finishing and reclaims by pickling, then to the stone after pickling
English tailings carries out flotation, after flotation washs quartz tail sand to neutrality, standby after centrifuge dehydration；
For al2o3Content ＜ 2% quartz tail sand, quartz tail sand is put in reactor, in reactor add hydrogen
Fluoric acid, opens stirring and carries out pickling, stir the al to quartz tail sand2o3Content ＜ 0.1%, then acid solution is removed and returns
Receive；Quartz tail sand after pickling is washed to neutrality, standby after centrifuge dehydration；
(3), the material after processing in step (2) is put in reactor, the mix acid liquor using nitric acid and hexafluosilicic acid enters
Row pickling, pickling 3～6 hours under conditions of 70～90 degree, with molten except the irony in material, finally material is cooled to room
Temperature, removing acid solution simultaneously reclaims；
(4) it is washed with water to dehydration after neutrality by removing the quartz tail sand after irony in upper step, then material is put into instead
Answer in kettle and carry out pickling with concentrated hydrochloric acid, pickling 3～6 hours under conditions of 60～90 degree, remove acid solution recovery；
(5), the quartz tail sand after removing hydrochloric acid in upper step is washed with water to dehydration after neutrality, first isolates therein
Deionized water or electronic grade ultrapure water wash to quartz sand powder the quartz sand powder of 120～200 mesh and 200～400 mesh again
Dehydrate after the total content ＜ 0.001% of chloride ion, nitrate ion and fluorion；Or first deionized water or electronics
Level milli-Q water is to the total content ＜ 0.001% of chloride ion, nitrate ion and fluorion in silica flour and dehydrate
Isolate the quartz sand powder of 120～200 mesh therein and 200～400 mesh afterwards again, that is, high-purity ground quartz is obtained.
Step (1) if in the new output of quartz tail sand quartz tail sand, with clear water rinsing and with centrifuge dewatering to it
Middle moisture is 5～8%, then measures the content of impurity again；If the long-term quartz tail sand stacked, then first pulled an oar,
Again with clear water rinse and with centrifuge dewatering to wherein moisture be 5～8%, then measure the content of impurity again；If water
Divide content to be less than 5% quartz tail sand, then directly measure the content of impurity.
Method for floating in step (2) is specific as follows: with Fluohydric acid. and alkali liquor as regulator, with lauryl amine as trapping agent,
With No. 2 oil as foaming agent, floatingly select dirt under conditions of ph=2.0～3.0.
The concrete concentration of mix acid liquor in step (3) is 20～40% nitric acid and hexafluosilicic acid that concentration is 20～40%
According to the mixed acid solution of the volume ratio of 1:1.
In step (5), after isolating the silica flour of 120～200 mesh, remaining quartz sand powder is sieved again, collects 200
The emery dust of～400 mesh, directly as high-purity ultrafine silicon raw material, it is crushed to 800 with Counter-impact flow pulverizer～
1000 mesh or 1000～2500 mesh or 2500～5000 mesh are high-purity ultrafine silicon.
Present invention also offers a kind of for the device in above-mentioned technique, at least include reactor, vacuum deacidification system, true
Empty multi-level water tourie, the liner material of described reactor is stereotype, politef or silicon carbide ceramics, in reactor
The double-deck sieve plate of politef material is installed, upper and lower two layer screen in double-deck sieve plate at the 50～150mm of its inner distance bottom
The shape of plate is identical, and is provided with one block of filter cloth or screen cloth between upper and lower two-layer sieve plate, and a diameter of the 5 of sieve aperture in double-deck sieve plate～
20mm, the hole heart between two sieve apertures of arbitrary neighborhood, away from for 40～60mm, is provided with for supporting between double-deck sieve plate and bottom
The support column of double-deck sieve plate, double-deck sieve plate be provided centrally with a discharging opening with the cylindrical shape of ft connection, described discharging
Mouth is connected with outlet valve by ring flange, and the bottom of reactor is provided with an acid solution pipe for acid solution turnover, acid solution pipe
On outer end, tee T is connected with by flange, one end of tee T connects acid inlet tube by valve, and the other end of tee T passes through
Valve is connected with vacuum deacidification system；Chuck for steam heating or water-cooled and and chuck are provided with the kettle wall of reactor
Corresponding valve；The condenser of one lead matter is provided with the top kettle cover of reactor, the top of described condenser is provided with one
Pipeline, and being connected with vacuum multi-stage water tourie by pipeline, the end of vacuum multi-stage water tourie and acid fog absorption tower system
System is connected, and the end of acid fog absorption tower system connects air-introduced machine；Visor, thermometer, agitator are also equipped with described kettle cover
And manhole.
Compared with prior art, provide a kind of side that discarded quartz tail sand is carried out reworking process in the present invention
Method, and it is used for first preparation production high-purity ground quartz, at produced waste gas, waste water all recovery in whole production process
Manage and recycle, be energy-saving and environmental protection, the process line of green.
Brief description
The overall structure diagram of the device that Fig. 1 provides for the present invention；
Fig. 2 is the structural representation of reactor；
In figure: 1- reactor, 2- vacuum deacidification system, 3- vacuum multi-stage water tourie, 4- condenser, 5- acid fog absorption tower
System, 6- air-introduced machine, 7- bilayer sieve plate, 8- filter cloth, 9- discharging opening, 10- outlet valve, 11- acid solution pipe, 12- acid inlet tube, 13- presss from both sides
Set, 14- agitator, 15- thermometer.
Specific embodiment
With reference to specific embodiment, detailed specific description is done to the present invention, but protection scope of the present invention not office
It is limited in following examples.
In the following examples of the present invention, the overall structure of the device being adopted as shown in figure 1, at least include reactor 1,
Vacuum deacidification system 2, vacuum multi-stage water tourie 3.The structure of reactor 1 is as shown in Fig. 2 the liner material of described reactor
For stereotype, politef or silicon nitride ceramics, in reactor, at the 100mm of its inner distance bottom, politef is installed
The double-deck sieve plate 7 of material, in double-deck sieve plate 7, the shape of upper and lower two-layer sieve plate is identical, and is provided with one between upper and lower two-layer sieve plate
Block filter cloth 8 or screen cloth, a diameter of 5-20mm of sieve aperture in double-deck sieve plate 7, the hole heart between two sieve apertures of arbitrary neighborhood is away from for 40
～60mm, is provided with the support column for supporting double-deck sieve plate between double-deck sieve plate and bottom, being provided centrally with of double-deck sieve plate
One discharging opening 9 with the cylindrical shape of ft connection, described discharging opening 9 is connected with outlet valve 10 by ring flange, reactor
Bottom is provided with an acid solution pipe 11 for acid solution turnover, and the outer end of acid solution pipe 11 is connected with tee T by flange, and three
One end of siphunculus connects acid inlet tube 12 by valve, and the other end of tee T is connected with vacuum deacidification system 2 by valve；Reaction
Chuck 13 for steam heating or water-cooled and valve corresponding with chuck 13 are provided with the kettle wall of kettle；The top of reactor
The condenser 4 of one lead matter is provided with kettle cover, the top of described condenser 4 is provided with a pipeline, and passes through pipeline and vacuum
Multi-level water tourie 3 is connected, and the end of vacuum multi-stage water tourie 3 is connected with acid fog absorption tower system 5, acid fog absorption tower system
The end of system 5 connects air-introduced machine 6；Visor, thermometer 15, agitator 14 and manhole are also equipped with described kettle cover.
After device provided by the present invention, after bottom enters in kettle, in the presence of buoyancy, material is sour for acid solution
After liquid floats, open stirring, motor just can start under very low electric current.When running into midway power failure, quartz sand just deposits
In bottom portion, if using common reactor, motor now can not be started, otherwise motor must burn, and more makes one
Headache, according to common response kettle, it is necessary to again material be risen out after material is deposited on bottom portion, puts into again again
Go, otherwise cannot be carried out normally producing, this multiple authentication aborning.And adopt this reactor, it is not afraid of midway and repeatedly stop
The situation of electricity occurs, and substantially increases production efficiency；
Additionally, being easy to remove acid solution using this reactor, material discharging is convenient.If do not adopted this kettle, then discharging is acid solution
Enter centrifuge deacidification together with mortar, its working environment is very severe, after this kettle, first remove acid solution, then use clear water again
Material is delivered to centrifuge dewatering, then during feeding, acid solution greatly dilutes, have very big changing for its production environment
Become.
Embodiment 1
The quartz deposit that raw material in the present embodiment is produced by Tangshan gold Xin Shidagui industry company limited produces quartz sand mistake
White tailings in journey, specific production technology is as follows:
1st, first quartz tail sand centrifuge dehydration after clear water rinsing, detect impurity therein: al2o3: 0.16%, fe2o3:
0.053%th, moisture: 5.6%
2nd, surface clean and remove impurity
Quartz tail sand in step 1 is put in reactor, first opens acid fog absorption tower system, make whole response system
Assume micro-vacuum state, after being then turned on chuck cooling water and the condenser cooling water of kettle, be then turned on sour pump, with Frequency Converter Control to
Send into the amount of Fluohydric acid. in kettle, the concentration of Fluohydric acid. is 10% (specifically depending on the circumstances), when the quartz tail sand in kettle present by
Acid solution is flooded and sand granule is in the state stirred up and down, opens the stirring on kettle, during normal operation to be mixed, stops sending acid
Liquid.And in this stirring reaction 3h, sample analysis aluminium sesquioxide content, al2o3: 0.04%.Removing acid solution recovery, thing
Material clear water washs to neutrality, sends in step 3 after dehydration.
3, pickling removes ferrum
According to the analysis result of step 2, the al of this material2o3Content conform to quality requirements, remaining main task
It is except irony.Material after dehydration is sent in reactor, is pumped into the body by 1:1 with 20% nitric acid and 30% hexafluosilicic acid with acid
Long-pending than the acid solution that mixed in reactor, flooded by acid solution and sand granule is stirring up and down when the quartz tail sand in kettle presents
State when, open the stirring on kettle, during normal operation to be mixed, stop sending acid solution, and after this stirring reaction 3h, sampling point
Analysis: fe2o3: 0.0018%, with vacuum removal acid solution recovery；Again material is sent into the washing step in step 4 with water.
4, the material in step 3 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then material is put
Enter in reactor, be passed through steam and with being pumped into 25% hydrochloric acid in reactor to kettle chuck, when the quartz tail sand in kettle is in
Now flooded by acid solution and sand granule is in the state stirred up and down, open the stirring on kettle, during normal operation to be mixed, stop sending
Acid solution, continues to be heated to 60 degree and at this temperature after stirring reaction 6h, sample analysis: fe2o3: 0.0006%, use vacuum removal
Acid solution recovery, then material is sent into the washing step in step 5 with clear water.
5, the material in step 4 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then divided with wet method
Level, collects 120 mesh～200 mesh, the emery dust of 200 mesh～400 mesh respectively；After being dehydrated respectively；Be washed with deionized respectively again to
Chloride ion or nitrate ion, less than after 10ppm, are dehydrated respectively and dry；120 mesh～200 mesh are high-purity ground quartz；200 mesh
～400 mesh are high-purity ultrafine silicon raw material, collect the emery dust of 200～400 mesh, are crushed to Counter-impact flow pulverizer
800～1000 mesh or 1000～2500 mesh or 2500～5000 mesh, that is, be obtained high-purity ultrafine silicon.
Embodiment 2
The silicilyte that raw material in the present embodiment is produced by Linyi Yishui silica sand company limited produces quartz sand mistake
Yellow tailings in journey, specific production technology is as follows:
1st, because this tailings is the long-term tailings stacked, it is centrifuged with after clear water rinsing after therefore first quartz tail sand being pulled an oar again
Dehydration, detects impurity therein: al2o3: 0.94%, fe2o3: 0.15%；Moisture: 6.3%
2nd, surface clean and remove impurity
Quartz tail sand in step 1 is put in reactor, first opens acid fog absorption tower system, make whole response system
Assume micro-vacuum state, after being then turned on chuck cooling water and the condenser cooling water of kettle, be then turned on sour pump, with Frequency Converter Control to
Send into the amount of Fluohydric acid. in kettle, the concentration of Fluohydric acid. is 20% (specifically depending on the circumstances), when the quartz tail sand in kettle present by
Acid solution is flooded and sand granule is in the state stirred up and down, opens the stirring on kettle, during normal operation to be mixed, stops sending acid
Liquid.And in this stirring reaction 6h, sample analysis aluminium sesquioxide content, al2o3: 0.02%.Removing acid solution recovery, thing
Material clear water washs to neutrality, sends in step 3 after dehydration.
3, pickling removes ferrum
According to the analysis result of step 2, the al of this material2o3Content conform to quality requirements, remaining main task
It is except irony.Material after dehydration is sent in reactor, is pumped into the body by 1:1 with 30% hexafluosilicic acid+30% nitric acid with acid
Long-pending than the acid solution that mixed in reactor, flooded by acid solution and sand granule is stirring up and down when the quartz tail sand in kettle presents
State when, open the stirring on kettle, during normal operation to be mixed, stop sending acid solution, and after this stirring reaction 3h, sampling point
Analysis: fe2o3: 0.0027%.With vacuum removal acid solution recovery；Again material is sent into the washing step in step 4 with water.
4, the material in step 3 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then material is put
Enter in reactor, be passed through steam and with being pumped into 30% hydrochloric acid in reactor to kettle chuck, when the quartz tail sand in kettle is in
Now flooded by acid solution and sand granule is in the state stirred up and down, open the stirring on kettle, during normal operation to be mixed, stop sending
Acid solution, continues to be heated to 80 degree and at this temperature after stirring reaction 5h, sample analysis: fe2o3: 0.0008%, use vacuum removal
Acid solution recovery, then material is sent into the washing step in step 5 with clear water.
5, the material in step 4 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then divided with wet method
Level, collects 120 mesh～200 mesh, the emery dust of 200 mesh～400 mesh respectively；After being dehydrated respectively；Be washed with deionized respectively again to
Chloride ion or nitrate ion, less than after 10ppm, are dehydrated respectively and dry；120 mesh～200 mesh are high-purity ground quartz；200 mesh
～400 mesh are high-purity ultrafine silicon raw material.
Embodiment 3
The silicilyte that raw material in the present embodiment is produced by Area, Fengyang County, Anhui silica sand Science and Technology Ltd. produces quartz
Shallow white tailings during sand, specific production technology is as follows:
1st, because this emery dust is that emery dust, therefore direct detection therein impurity: al are dried2o3: 2.44%, fe2o3:
0.058%；Moisture: 4.3%.
2nd, surface clean and remove impurity
Quartz tail sand in step 1 is put in reactor, first opens acid fog absorption tower system, make whole response system
Assume micro-vacuum state, after being then turned on chuck cooling water and the condenser cooling water of kettle, be then turned on sour pump, with Frequency Converter Control to
Send hydrogen to enter the amount of fluoric acid in kettle, the concentration of Fluohydric acid. is 30% (specifically depending on the circumstances), when the quartz tail sand in kettle present by
Acid solution is flooded and sand granule is in the state stirred up and down, opens the stirring on kettle, during normal operation to be mixed, stops sending acid
Liquid.And in this stirring reaction 5h, acid solution is removed after finishing and reclaims by pickling, then carries out flotation to the quartz tail sand after pickling,
After flotation, quartz tail sand is washed to neutrality, standby after centrifuge dehydration；Method for floating is specific as follows: with Fluohydric acid. and alkali liquor for adjusting
Whole dose, with lauryl amine as trapping agent, with No. 2 oil as foaming agent, floatingly select dirt under conditions of ph=2.0～3.0.Floating
Sample analysis aluminium sesquioxide content, al after choosing2o3: 0.026%.
3, pickling removes ferrum
According to the analysis result of step 2, the al of this material2o3Content conform to quality requirements, remaining main task
It is except irony.Material after dehydration is sent in reactor, is pumped into the body by 1:1 with 20% hexafluosilicic acid+30% nitric acid with acid
Long-pending than the acid solution that mixed in reactor, flooded by acid solution and sand granule is stirring up and down when the quartz tail sand in kettle presents
State when, open the stirring on kettle, during normal operation to be mixed, stop sending acid solution, and after this stirring reaction 3h, sampling point
Analysis: fe2o3: 0.0023%.With vacuum removal acid solution recovery；Again material is sent into the washing step in step 4 with water.
4, the material in step 3 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then material is put
Enter in reactor, be passed through steam and with being pumped into 30% hydrochloric acid in reactor to kettle chuck, when the quartz tail sand in kettle is in
Now flooded by acid solution and sand granule is in the state stirred up and down, open the stirring on kettle, during normal operation to be mixed, stop sending
Acid solution, continues to be heated to 80 degree and at this temperature after stirring reaction 5h, sample analysis: fe2o3: 0.0010%, use vacuum removal
Acid solution recovery, then material is sent into the washing step in step 5 with clear water.
5, the material in step 4 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then divided with wet method
Level, collects 120 mesh～200 mesh, the emery dust of 200 mesh～400 mesh respectively；After being dehydrated respectively；Be washed with deionized respectively again to
Chloride ion or nitrate ion, less than after 10ppm, are dehydrated respectively and dry；120 mesh～200 mesh are high-purity ground quartz；200 mesh
～400 mesh are high-purity ultrafine silicon raw material.
Embodiment 4
The deposition quartzy sandstone that raw material in the present embodiment is produced by Heyuan quartz sand company limited produces quartz
Shallow white tailings during sand, specific production technology is as follows:
1st, because this emery dust is that emery dust, therefore direct detection therein impurity: al are dried2o3: 3.5%, fe2o3:
0.78%th,；Moisture: 4.3%.
2nd, surface clean and remove impurity
Quartz tail sand in step 1 is put in reactor, first opens acid fog absorption tower system, make whole response system
Assume micro-vacuum state, after being then turned on chuck cooling water and the condenser cooling water of kettle, be then turned on sour pump, with Frequency Converter Control to
Send into the amount of Fluohydric acid. in kettle, the concentration of Fluohydric acid. is 40% (specifically depending on the circumstances), when the quartz tail sand in kettle present by
Acid solution is flooded and sand granule is in the state stirred up and down, opens the stirring on kettle, during normal operation to be mixed, stops sending acid
Liquid.And in this stirring reaction 5h, acid solution is removed after finishing and reclaims by pickling, then carries out flotation to the quartz tail sand after pickling,
After flotation, quartz tail sand is washed to neutrality, standby after centrifuge dehydration；Method for floating is specific as follows: with Fluohydric acid. and alkali liquor for adjusting
Whole dose, with lauryl amine as trapping agent, with No. 2 oil as foaming agent, floatingly select dirt under conditions of ph=2.0～3.0.Floating
Sample analysis aluminium sesquioxide content, al after choosing2o3: 0.03%.
3, pickling removes ferrum
According to the analysis result of step 2, the al of this material2o3Content conform to quality requirements, remaining main task
It is except irony.Material after dehydration is sent in reactor, is pumped into the body by 1:1 with 20% hexafluosilicic acid+20% nitric acid with acid
Long-pending than the acid solution that mixed in reactor, flooded by acid solution and sand granule is stirring up and down when the quartz tail sand in kettle presents
State when, open the stirring on kettle, during normal operation to be mixed, stop sending acid solution, and after this stirring reaction 3h, sampling point
Analysis: fe2o3: 0.0028%.With vacuum removal acid solution recovery；Again material is sent into the washing step in step 4 with water.
4, the material in step 3 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then material is put
Enter in reactor, be passed through steam and with being pumped into 30% hydrochloric acid in reactor to kettle chuck, when the quartz tail sand in kettle is in
Now flooded by acid solution and sand granule is in the state stirred up and down, open the stirring on kettle, during normal operation to be mixed, stop sending
Acid solution, continues to be heated to 80 degree and at this temperature after stirring reaction 5h, sample analysis: fe2o3: 0.00010%, taken off with vacuum
Except acid solution recovery, then material is sent into the washing step in step 5 with clear water.
5, the material in step 4 is washed to ph=6～7 with clear water, is first removed after moisture with centrifuge, then divided with wet method
Level, collects 120 mesh～200 mesh, the emery dust of 200 mesh～400 mesh respectively；After being dehydrated respectively；Be washed with deionized respectively again to
Chloride ion or nitrate ion, less than after 10ppm, are dehydrated respectively and dry；120 mesh～200 mesh are high-purity ground quartz；200 mesh
～400 mesh are high-purity ultrafine silicon raw material.
Claims (6)
1. a kind of technique using quartz tail sand production high-purity ground quartz is it is characterised in that comprise the following steps: (1), testing stone
The content of the impurity in English tailings, impurity includes al2o3、fe2o3, judge al in quartz tail sand2o3Content whether be more than 2%；
(2), for al2o3Content >=2% quartz tail sand, quartz tail sand is put in reactor, in reactor add hydrogen
Fluoric acid, opens stirring and carries out pickling to quartz tail sand, and acid solution is removed after finishing and reclaims by pickling, then to the quartzy tail after pickling
Sand carries out flotation, after flotation washs quartz tail sand to neutrality, standby after centrifuge dehydration；
For al2o3Content ＜ 2% quartz tail sand, quartz tail sand is put in reactor, in reactor add hydrogen fluorine
Acid, opens stirring and carries out pickling, stir the al to quartz tail sand2o3Content ＜ 0.1%, then acid solution is removed and reclaims；
Quartz tail sand after pickling is washed to neutrality, standby after centrifuge dehydration；
(3), the material after processing in step (2) is put in reactor, the mix acid liquor using nitric acid and hexafluosilicic acid carries out acid
Wash, pickling 3～6 hours under conditions of 70～90 degree, finally material is cooled to room temperature with molten except the irony in material, take off
Except acid solution and reclaim；
(4), it is washed with water to dehydration after neutrality by removing the quartz tail sand after irony in upper step, then material is put into reactor
Middle concentrated hydrochloric acid carries out pickling, pickling 3～6 hours under conditions of 60～90 degree, removes acid solution recovery；
(5), the quartz tail sand after removing hydrochloric acid in upper step is washed with water to dehydration after neutrality, first isolates therein 120
The quartz sand powder of～200 mesh and 200～400 mesh again deionized water or electronic grade ultrapure water wash to chlorine in quartz sand powder from
Dehydrate after the total content ＜ 0.001% of son, nitrate ion and fluorion；Or first deionized water or electron level surpass
Pure water is to the total content ＜ 0.001% dehydrate of chloride ion, nitrate ion and fluorion in quartz sand powder
Isolate the quartz sand powder of 120～200 mesh therein and 200～400 mesh again, that is, high-purity ground quartz is obtained.
2. utilization quartz tail sand according to claim 1 produce high-purity ground quartz technique it is characterised in that: step (1)
If in the new output of quartz tail sand quartz tail sand, with clear water rinsing and with centrifuge dewatering to wherein moisture be 5～
8%, then measure the content of impurity again；If the long-term quartz tail sand stacked, then first pulled an oar, then rinsed with clear water and be used in combination
Centrifuge dewatering is 5～8% to wherein moisture, then measures the content of impurity again；If moisture is less than 5% stone
English tailings, then directly measure the content of impurity.
3. utilization quartz tail sand according to claim 1 produce high-purity ground quartz technique it is characterised in that: step (2)
In method for floating specific as follows: with Fluohydric acid. and alkali liquor as regulator, with lauryl amine as trapping agent, with No. 2 oil as foaming agent,
Dirt is floatingly selected under conditions of ph=2.0～3.0.
4. utilization quartz tail sand according to claim 1 produce high-purity ground quartz technique it is characterised in that: step (3)
In mix acid liquor be specially the nitric acid that concentration is 20～40% and hexafluosilicic acid that concentration is 20～40% volume according to 1:1
Than mixed acid solution.
5. utilization quartz tail sand according to claim 1 produce high-purity ground quartz technique it is characterised in that: step (5)
In, after isolating the quartz sand powder of 120～200 mesh, remaining quartz sand powder is sieved again, collects the sand of 200～400 mesh
Powder, directly as high-purity ultrafine silicon raw material, with Counter-impact flow pulverizer be crushed to 800～1000 mesh or 1000～
2500 mesh or 2500～5000 mesh, that is, be obtained high-purity ultrafine silicon.
6. a kind of for the device in technique described in claim 1 it is characterised in that: at least include reactor, vacuum deacidification system
System, vacuum multi-stage water tourie, the liner material of described reactor is stereotype, politef or silicon carbide ceramics, reaction
It is provided with the 50～150mm of its inner distance bottom in kettle and inner liner of reaction kettle material identical bilayer sieve plate, double-deck sieve plate
In upper and lower two-layer sieve plate shape identical, and be provided with one block of filter cloth or screen cloth between upper and lower two-layer sieve plate, sieve in double-deck sieve plate
A diameter of 5～20mm in hole, the hole heart between two sieve apertures of arbitrary neighborhood, away from for 40～60mm, sets between double-deck sieve plate and bottom
Be equipped with the support column for supporting double-deck sieve plate, double-deck sieve plate be provided centrally with a discharging with the cylindrical shape of ft connection
Mouthful, described discharging opening is connected with outlet valve by ring flange, and the bottom of reactor is provided with an acid solution for acid solution turnover
Pipe, the outer end of acid solution pipe is connected with tee T by flange, and one end of tee T connects acid inlet tube by valve, tee T
The other end is connected with vacuum deacidification system by valve；Chuck for steam heating or water-cooled is provided with the kettle wall of reactor
And valve corresponding with chuck；The condenser of one lead matter is provided with the top kettle cover of reactor, described condenser upper
Portion is provided with a pipeline, and is connected with vacuum multi-stage water tourie by pipeline, the end of vacuum multi-stage water tourie with acid
Mist absorption tower system is connected, and the end of acid fog absorption tower system connects air-introduced machine；Visor, temperature are also equipped with described kettle cover
Meter, agitator and manhole.
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| CN105152168A (en) * | 2015-09-30 | 2015-12-16 | 徐州天正活性炭厂 | Device for pickling activated carbon through phosphoric acid method |
| CN106423986A (en) * | 2016-11-03 | 2017-02-22 | 陆植才 | Yellow peel treatment process and yellow peel treatment equipment for quartz mine or alkalifeldspar mine |
| CN107162008A (en) * | 2017-06-20 | 2017-09-15 | 合肥市惠科精密模具有限公司 | A kind of preparation technology of TFT LCD substrates glass quartz sand powder |
| CN107999459B (en) * | 2017-12-12 | 2023-08-15 | 南通星球石墨股份有限公司 | Stone pickling equipment and method |
| CN108455618B (en) * | 2018-01-19 | 2021-08-06 | 徐州市万达石英有限公司 | Process for large-scale circular pickling of quartz sand |
| CN108821294A (en) * | 2018-07-24 | 2018-11-16 | 衢州市鼎盛化工科技有限公司 | The method for preparing ultrapure quartz sand as raw material using common quartz sand |
| CN113321216B (en) * | 2021-06-22 | 2023-09-22 | 中国地质科学院郑州矿产综合利用研究所 | Method for preparing high-purity quartz by using quartz vein type tungsten waste stone |
| CN113680462B (en) * | 2021-10-27 | 2021-12-31 | 苏州锦艺新材料科技有限公司 | Production process of spherical silicon micropowder |
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