CN109399643A - A method of industrial silicon is prepared using diamond wire sliced crystal scrap silicon - Google Patents
A method of industrial silicon is prepared using diamond wire sliced crystal scrap silicon Download PDFInfo
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- CN109399643A CN109399643A CN201811155543.5A CN201811155543A CN109399643A CN 109399643 A CN109399643 A CN 109399643A CN 201811155543 A CN201811155543 A CN 201811155543A CN 109399643 A CN109399643 A CN 109399643A
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- silicon
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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
- C01B33/02—Silicon
- C01B33/037—Purification
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Abstract
The present invention provides a kind of methods for preparing industrial silicon using diamond wire sliced crystal scrap silicon, its step includes: by mass percentage, by modified water glass 5-10wt%, pretreated crystalline silicon cutting waste material 50-65wt%, water 30-40wt% carries out mixing, is then pressed into the wet bulb that diameter is 1-50mm；Low temperature dewatering is carried out under the conditions of 60-90 DEG C, until wet bulb weight no longer changes, obtains dry bulb；Organic matter is removed to dry bulb, and the organic matter of abjection is decomposed, decomposition product is discharged into atmosphere after spray column absorbs；The dry bulb for removing organic matter is sintered in closed container；It in liner is to carry out melting in graphite crucible and the intermediate induction furnace for being equipped with graphite rod by sintered dry bulb；The casting of skimming of product after melting is obtained into alloy, and detects alloying component.A kind of method preparing industrial silicon using diamond wire sliced crystal scrap silicon provided by the invention, with short production cycle, wet and dry bulb fall intensity and compression strength well and safety and environmental protection.
Description
Technical field
The present invention relates to metallurgical technology field, in particular to a kind of utilization diamond wire sliced crystal scrap silicon prepares industrial
The method of silicon.
Background technique
Buddha's warrior attendant wire cutting at present has become the major way of silicon ingot cutting, cuts the waste material silicone content of generation generally 85%
More than, there is very high recovery value.It is industrially to be mixed in a certain proportion with silica and coke, is heated in electric furnace
1600-1800 DEG C and the thick silicon that purity is 95%-99% is made, for the purity for further increasing thick silicon, then method washed using acidleach
To thick silicon purify, technical process is: by thick silicon powder it is broken after, successively use hydrochloric acid, chloroazotic acid, HF+H2SO4Mixed acid is to the thick of crushing
Silicon carries out sour processing, is finally washed to neutrality with distillation again, and the industrial silicon that purity is 99.9% can be obtained after drying.This silicon side processed
Method is relatively high to temperature requirement is produced, and energy consumption is bigger, and thick silicon purification process needs to carry out to carry out acid repeatedly and with different acid
It washes, acid consumption is bigger, causes certain difficulty to the processing of later period waste water.
It is using the process that diamond wire cutting waste material prepares crystalline silicon: firstly, carrying out pickling impurity removal, gained to cutting waste material
Slurry filtration is washed to obtain powder.Then, cuber compound stalk forming is used after powder being incorporated suitable water and binder mixing, then
Drying obtains dry block.Finally, carrying out ingot casting, both ends are cut, remaining middle section is satisfactory crystalline silicon.It should
Method is not reasonably purified and is recycled to the waste water of washing, and is easy to produce hydrogen not in pelletizing dehydration
Conducive to safety in production, meanwhile, the organic matter of removing is not handled well, is easy pollution environment, and the week smelted
Phase is relatively long, takes time and effort, and economic benefit is low.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of with short production cycle, wet and dry bulbs to fall intensity and compression strength
Well and the method for preparing industrial silicon using diamond wire sliced crystal scrap silicon of safety and environmental protection.
In order to solve the above technical problems, the present invention provides it is a kind of using diamond wire sliced crystal scrap silicon prepare it is industrial
The method of silicon, includes the following steps:
By mass percentage, by modified water glass 5-10wt%, pretreated crystalline silicon cutting waste material 50-
65wt%, water 30-40wt% carry out mixing, are then pressed into the wet bulb that diameter is 1-50mm；
Low temperature dewatering is carried out under the conditions of 60-90 DEG C, until wet bulb weight no longer changes, obtains dry bulb；
Organic matter is removed to dry bulb, and the organic matter of abjection is decomposed, decomposition product is discharged into atmosphere after spray column absorbs；
The dry bulb for removing organic matter is sintered in closed container；
It in liner is to carry out melting in graphite crucible and the intermediate induction furnace for being equipped with graphite rod by sintered dry bulb；
The casting of skimming of product after melting is obtained into alloy, and detects alloying component.
Further, the pretreatment of the crystalline silicon cutting waste material includes filtering to crystalline silicon cutting waste material pickling except iron,
Washing, dry, break process process.
Further, the pickling to crystalline silicon cutting waste material is except iron is to remove iron with sulfuric acid washing, pickling time 1-3h,
40-80 DEG C of temperature, sulfuric acid concentration 1-1.5mol/L, liquid-solid ratio 2:1-5:1.
Further, it after the washing to crystalline silicon cutting waste material, with organic matter in activated carbon adsorption water lotion, and recycles
Utilize purified water.
Further, described to crystalline silicon cutting waste material break process, it is to have broken crystalline silicon cutting waste material
90% or more grain graininess is less than 100 μm.
Further, the dewatering time of the wet bulb is 5-20h.
Further, the dry bulb removing organic matter is to remove organic matter under the conditions of 200-400 DEG C, removes organic matter
Time is 1-5h.
Further, the organic matter decomposition of the abjection is that organic matter enters in incinerator and decomposes.
Further, the temperature that the dry bulb is sintered in closed container is 350-950 DEG C, sintering time 5-15h.
Further, the dry bulb melting is that melting is carried out under vacuum or inert gas shielding, and smelting temperature is
1450-1650 DEG C, soaking time 0.5-2h.
A kind of method preparing industrial silicon using diamond wire sliced crystal scrap silicon provided by the invention, will be sintered
Dry bulb carries out melting in induction furnace, the liner of induction furnace be graphite crucible and it is intermediate be equipped with graphite rod, induction furnace when melting
Silicon heat source is refined from graphite crucible, the diffusion of heat ecto-entad, furnace centralised temperature is lower, heats by intermediate graphite rod, heat
Amount is spread from inside to outside, and the heating means that such graphite crucible is combined with intermediate graphite rod improve heating effect, Ke Yi great
It is big to shorten melting cycle.Also, the present invention uses modified water glass in pellet ingredient and makees binder, due to modified water glass
Property with low viscosity, so that the wet bulb of compression moulding falls intensity and compression strength with good.Again due to
Modified water glass colloidal particle forms stable space net structure with Si-O-Si bond conjunction and securely ties particle in sintering process
It is combined, so that the dry bulb that wet bulb obtains after drying also has and good falls intensity and compression strength.In addition,
The present invention is dehydrated when being dehydrated to wet bulb using low-temperature zone, and the generation of hydrogen is avoided or be greatly reduced, convenient for safety
Production.Meanwhile the present invention carries out the organic matter that dry bulb is deviate to burn spray column adsorption treatment, avoids used in crystalline silicon cutting
Water-base cutting fluid remain in the elements such as N, P, S in sliced crystal scrap silicon, production sintering in generate pernicious gas be discharged to
Air is polluted in air, reduces the pollution to environment, it is environmentally protective.
Detailed description of the invention
Fig. 1 is the work of the method provided in an embodiment of the present invention that industrial silicon is prepared using diamond wire sliced crystal scrap silicon
Skill flow chart.
Specific embodiment
It is provided in an embodiment of the present invention a kind of to prepare industrial silicon using diamond wire sliced crystal scrap silicon referring to Fig. 1
Method includes the following steps:
Step 1: crystalline silicon cutting waste material being subjected to pickling impurity removal iron, iron, pickling time 1-3h, temperature are removed using sulfuric acid
40-80 DEG C, sulfuric acid concentration 1-1.5mol/L, liquid-solid ratio 2:1-5:1, the iron content in crystalline silicon cutting waste material can be down to
0.5% or less.Then it is filtered and the crystalline silicon cutting waste material filtered out is washed, while with activated carbon adsorption water lotion
Middle organic matter, recycles water resource, has saved resource.
Step 2: break process will be carried out after the drying of above-mentioned crystalline silicon cutting waste material, the granularity of 90% or more particle after being crushed
Less than 100 μm.By percentage to the quality, modified water glass 5-10wt%, crystalline silicon cutting waste material 50-65wt%, water 30- are taken
40wt% matches according to this and carries out mixing, then ingredient is pressed into the wet bulb of diameter 1-50mm with high pressure roller press.
Step 3: wet bulb is subjected to low temperature dewatering, dewatering time 5-20h, until the weight of wet bulb under the conditions of 60-90 DEG C
It is no longer changed, obtains dry bulb.
Step 4: dry bulb being removed into organic matter under the conditions of 200-400 DEG C, takes off organic matter time 1-5h, the organic matter of abjection
It burns and decomposes into incinerator, the flue gas of generation is most discharged into atmosphere after spray column elutes afterwards.By elements such as N, P, S in sintering
It generates pernicious gas to sponge, avoids it from being discharged in air and pollute air, reduce the pollution to environment, it is environmentally protective.
Step 5: the dry bulb for having taken off organic matter being packed into closed vessel, is sintered under the conditions of 350-950 DEG C, sintering time 5-
15h。
Step 6: sintered silicon ball being packed into induction furnace, is smelted under vacuum or inert gas conditions, temperature
1450-1650 DEG C, soaking time 0.5-2h.The liner of induction furnace is graphite crucible, intermediate graphite rod, it can be achieved that dual-heated,
Heating effect is improved, melting cycle is substantially shorter.
Step 7: industrial silicon being obtained to the casting that skim of the product after melting, and detects its silicone content.
Below by specific embodiment to provided by the invention a kind of industrial using the preparation of diamond wire sliced crystal scrap silicon
It is illustrated with the method for silicon.
Embodiment 1
A method of industrial silicon being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to pickling impurity removal iron, iron, time 1h, 80 DEG C of acid concentrations of temperature is removed using sulfuric acid
Then 1.5mol/L, liquid-solid ratio 2:1 are filtered washing, be 0.36% through detection iron content.
(2) above-mentioned crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μ after being crushed
m.It 1 kilogram of modified water glass dosage, 5 kilograms of crystalline silicon cutting waste material, 4 kilograms of water, is matched according to this and carries out mixing, with high pressure pair
Roll squeezer is pressed into the ball of diameter 25mm.
(3) low temperature dewatering, dewatering time 12h are carried out under the conditions of 70 DEG C, until the weight of wet bulb is no longer changed.
(4) organic matter being removed under the conditions of 300 DEG C, takes off organic matter time 1h, the organic matter of abjection enters incinerator decomposition,
Flue gas is most discharged into atmosphere after spray column elutes afterwards.
(5) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 500 DEG C, sintering time 9h.
(6) silicon ball after molding is packed into induction furnace, is smelted under vacuum conditions, 1450 DEG C of temperature, soaking time
2h。
(7) casting that carries out skimming obtains industrial silicon, and detection silicone content is 98.54%, and impurity summation < 2% meets second level silicon
National standard.
Embodiment 2
A method of industrial silicon being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to pickling impurity removal iron, iron is removed using sulfuric acid, time 1.5h, temperature 70 C acid is dense
1mol/L is spent, then liquid-solid ratio 3:1 is filtered washing, be 0.31% through detection iron content.
(2) above-mentioned crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μ after being crushed
m.It 0.8 kilogram of modified water glass dosage, 5.2 kilograms of crystalline silicon cutting waste material, 4 kilograms of water, is matched according to this and carries out mixing, with height
Pressure is pressed into the ball of diameter 20mm to roll squeezer.
(3) low temperature dewatering, dewatering time 12h are carried out under the conditions of 70 DEG C, until the weight of wet bulb is no longer changed.
(4) organic matter is removed under the conditions of 250 DEG C, takes off organic matter time 1.5h, the organic matter of abjection enters incinerator point
Solution, flue gas are most discharged into atmosphere after spray column elutes afterwards.
(5) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 450 DEG C, sintering time 7h.
(6) silicon ball after molding is packed into induction furnace, is smelted under vacuum conditions, 1500 DEG C of temperature, soaking time
1.5h。
(7) casting that carries out skimming obtains industrial silicon, and detection silicone content is 98.11%, and impurity summation < 2% meets second level silicon
National standard.
Embodiment 3
A method of industrial silicon being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to pickling impurity removal iron, iron is removed using sulfuric acid, time 1.5h, temperature 60 C acid is dense
1mol/L is spent, then liquid-solid ratio 5:1 is filtered washing, be 0.16% through detection iron content.
(2) above-mentioned crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μ after being crushed
m.It 0.6 kilogram of modified water glass dosage, 5.6 kilograms of crystalline silicon cutting waste material, 3.8 kilograms of water, is matched according to this and carries out mixing, used
High pressure roller press is pressed into the grain of diameter 2mm.
(3) low temperature dewatering, dewatering time 10h are carried out under the conditions of 80 DEG C, until the weight of wet bulb is no longer changed.
(4) organic matter is removed under the conditions of 350 DEG C, takes off organic matter time 0.5h, the organic matter of abjection enters incinerator point
Solution, flue gas are most discharged into atmosphere after spray column elutes afterwards.
(5) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 500 DEG C, sintering time 7h.
(6) silicon ball after molding is packed into induction furnace, is smelted under vacuum conditions, 1550 DEG C of temperature, soaking time
1h。
(7) casting that carries out skimming obtains industrial silicon, and detection silicone content is 99.08, and impurity summation < 1% meets level-one silicon state
Family standard %.
Embodiment 4
A method of industrial silicon being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to pickling impurity removal iron, iron, time 12h, temperature 70 C acid concentration is removed using sulfuric acid
Then 1.5mol/L, liquid-solid ratio 4:1 are filtered washing, be 0.27% through detection iron content.
(2) above-mentioned crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μ after being crushed
m.It 0.8 kilogram of modified water glass dosage, 5.4 kilograms of crystalline silicon cutting waste material, 3.8 kilograms of water, is matched according to this and carries out mixing, used
High pressure roller press is pressed into the ball of diameter 40mm.
(3) low temperature dewatering, dewatering time 8h are carried out under the conditions of 70 DEG C, until the weight of wet bulb is no longer changed.
(4) organic matter is removed under the conditions of 350 DEG C, takes off organic matter time 0.5h, the organic matter of abjection enters incinerator point
Solution, flue gas are most discharged into atmosphere after spray column elutes afterwards.
(5) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 600 DEG C, sintering time 5h.
(6) by silicon ball after molding be packed into induction furnace, argon atmosphere protection under under smelted, 1550 DEG C of temperature, protect
Warm time 2h.
(7) casting that carries out skimming obtains industrial silicon, and detection silicone content is 98.32%, and impurity summation < 2% meets second level silicon
National standard.
It should be noted last that the above specific embodiment is only used to illustrate the technical scheme of the present invention and not to limit it,
Although being described the invention in detail referring to example, those skilled in the art should understand that, it can be to the present invention
Technical solution be modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention, should all cover
In the scope of the claims of the present invention.
Claims (10)
1. a kind of method for preparing industrial silicon using diamond wire sliced crystal scrap silicon, which comprises the steps of:
By mass percentage, by modified water glass 5-10wt%, pretreated crystalline silicon cutting waste material 50-65wt%, water
30-40wt% carries out mixing, is then pressed into the wet bulb that diameter is 1-50mm；
Low temperature dewatering is carried out under the conditions of 60-90 DEG C, until wet bulb weight no longer changes, obtains dry bulb；
Organic matter is removed to dry bulb, and the organic matter of abjection is decomposed, decomposition product is discharged into atmosphere after spray column absorbs；
The dry bulb for removing organic matter is sintered in closed container；
It in liner is to carry out melting in graphite crucible and the intermediate induction furnace for being equipped with graphite rod by sintered dry bulb；
The casting of skimming of product after melting is obtained into alloy, and detects alloying component.
2. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: the pretreatment of the crystalline silicon cutting waste material includes filtering to crystalline silicon cutting waste material pickling except iron, is washed, dry, is crushed
Treatment process.
3. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: the pickling to crystalline silicon cutting waste material except iron is to remove iron with sulfuric acid washing, pickling time 1-3h, 40-80 DEG C of temperature, sulphur
Acid concentration 1-1.5mol/L, liquid-solid ratio 2:1-5:1.
4. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: after the washing to crystalline silicon cutting waste material, with organic matter in activated carbon adsorption water lotion, and recycle purified
Water.
5. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: it is described to crystalline silicon cutting waste material break process, it is the particle for making broken crystalline silicon cutting waste material have 90% or more
Degree is less than 100 μm.
6. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: the dewatering time of the wet bulb is 5-20h.
7. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: the dry bulb removing organic matter is to remove organic matter under the conditions of 200-400 DEG C, and the time for removing organic matter is 1-5h.
8. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
It is that organic matter enters in incinerator and decomposes in the organic matter decomposition of: the abjection.
9. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: the temperature that the dry bulb is sintered in closed container is 350-950 DEG C, sintering time 5-15h.
10. the method according to claim 1 for preparing industrial silicon using diamond wire sliced crystal scrap silicon, feature exist
In: the dry bulb melting is that melting is carried out under vacuum or inert gas shielding, and smelting temperature is 1450-1650 DEG C, heat preservation
Time 0.5-2h.
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| CN102746936A (en) * | 2012-08-08 | 2012-10-24 | 铁生年 | Recycling purification method for carborundum powder in silicon slice cutting waste liquid |
| CN105523557A (en) * | 2016-02-14 | 2016-04-27 | 东北大学 | Method for recycling waste slurry produced during diamond wire cutting of crystalline silicon |
| CN107324337A (en) * | 2017-07-05 | 2017-11-07 | 镇江环太硅科技有限公司 | A kind of method that solar energy crystalline silicon cuts waste slurry recycling |
| CN107747119A (en) * | 2017-10-20 | 2018-03-02 | 东北大学 | A kind of method for preparing crystalline silicon with the diamond wire cutting waste material of crystalline silicon |
-
2018
- 2018-09-30 CN CN201811155543.5A patent/CN109399643A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746936A (en) * | 2012-08-08 | 2012-10-24 | 铁生年 | Recycling purification method for carborundum powder in silicon slice cutting waste liquid |
| CN105523557A (en) * | 2016-02-14 | 2016-04-27 | 东北大学 | Method for recycling waste slurry produced during diamond wire cutting of crystalline silicon |
| CN107324337A (en) * | 2017-07-05 | 2017-11-07 | 镇江环太硅科技有限公司 | A kind of method that solar energy crystalline silicon cuts waste slurry recycling |
| CN107747119A (en) * | 2017-10-20 | 2018-03-02 | 东北大学 | A kind of method for preparing crystalline silicon with the diamond wire cutting waste material of crystalline silicon |
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