CN109280742A - A method of Antaciron is prepared using diamond wire sliced crystal scrap silicon - Google Patents

A method of Antaciron is prepared using diamond wire sliced crystal scrap silicon Download PDF

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Publication number
CN109280742A
CN109280742A CN201811155542.0A CN201811155542A CN109280742A CN 109280742 A CN109280742 A CN 109280742A CN 201811155542 A CN201811155542 A CN 201811155542A CN 109280742 A CN109280742 A CN 109280742A
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pellet
organic matter
antaciron
diamond wire
preparing
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CN201811155542.0A
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CN109280742B (en
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刘奎仁
邢延慧
李斌川
韩庆
陈建设
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Northeastern University China
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Northeastern University China
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21CPROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04Removing impurities by adding a treating agent
    • C21C7/06Deoxidising, e.g. killing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/14Agglomerating; Briquetting; Binding; Granulating
    • C22B1/16Sintering; Agglomerating
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00Preliminary treatment of ores or scrap
    • C22B1/14Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24Binding; Briquetting ; Granulating
    • C22B1/242Binding; Briquetting ; Granulating with binders
    • C22B1/243Binding; Briquetting ; Granulating with binders inorganic
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention provides a kind of methods for preparing Antaciron using diamond wire sliced crystal scrap silicon, its step includes: by mass percentage, by the crystalline silicon cutting waste material of 21-63wt%, the sodium bentonite of 1-3wt%, the modified water glass of 3-6wt%, the iron powder of 3-20wt% and the water mixing of 30-40wt%, are then pressed into pellet;Pellet is dehydrated under the conditions of 60-90 DEG C, until pellet weight is no longer changed;The pellet of dehydration is removed into organic matter, and the organic matter of abjection is decomposed, decomposition product is discharged into atmosphere after spray column absorbs;The pellet for removing organic matter is sintered in closed container;Sintered pellet is subjected to melting;The casting of skimming of product after melting is obtained into alloy, detects alloying component.A kind of method preparing Antaciron using diamond wire sliced crystal scrap silicon provided by the invention, production safety environmental protection, and pellet falls intensity and compression strength is good.

Description

A method of Antaciron is prepared using diamond wire sliced crystal scrap silicon
Technical field
It is the present invention relates to metallurgical technology field, in particular to a kind of to prepare ferrosilicon conjunction using diamond wire sliced crystal scrap silicon The method of gold.
Background technique
Crystalline silicon needs to carry out cutting process when being processed into solar battery, by silicon ingot processing at silicon wafer, this It can generate in the process largely containing scrap silicon.Buddha's warrior attendant line cutting technology have compared with diamond dust cutting technique cutting efficiency it is high, The advantages that environmental pollution is low, silicon wafer precision is good, surface damage is small, and saw kerf loss is few, therefore in recent years as sliced crystal silicon Main way.
Crystalline silicon cutting waste material is mainly for the preparation of crystalline silicon, silicon carbide, alusil alloy etc., these needs without exception Be dehydrated de- organic matter except iron to cutting waste material, and prepares Antaciron and be not necessarily to except iron.Antaciron is mainly used for steel-making and produces Industry makees deoxidier.Traditional production method is to melt silica, carbonaceous reducing agent, the steel cuttings electric arc furnaces of ingredient loading by a certain percentage Refining, replaces carbonaceous reducing agent directly can reduce reaction temperature and reaction time with steel cuttings melting with cutting waste material.It is current to utilize Crystalline silicon cutting waste material production alloy general step be " crystalline silicon cutting waste material add certain metal-alloy melting-skim- Casting-alloy ", but pellet strength is bad after most crystalline silicon cutting waste material moldings in this method.
In addition also having method is to be directly added into powder to carry out high melt, and high melt is directly smelted using powder There are problems.First, bed permeability is poor, and it is slow to react insufficient or reaction speed.Second, it is smelted using powder and is easy hair Raw splash and explosion, raw material availability are low.Third is then steel scrap shove charge melting is blown into powder, in this way using powder smelting The production environment that scene can be deteriorated, causes inspirable particle concentration to increase, is detrimental to health.
Also, the wet and dry bulb after forming in these current technologies falls intensity difference, and had ignored in dehydration silicon with Vapor reaction generates hydrogen and easily causes security risk, in addition, 4% or so organic matter, which is directly discharged into atmosphere, is easy pollution ring Border.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of production safety environmental protection and pellet falls intensity and pressure resistance The method for preparing Antaciron using diamond wire sliced crystal scrap silicon spent.
In order to solve the above technical problems, preparing ferrosilicon conjunction using diamond wire sliced crystal scrap silicon the present invention provides a kind of The method of gold, includes the following steps:
By mass percentage, by the crystalline silicon cutting waste material of 21-63wt%, the sodium bentonite of 1-3wt%, 3- The modified water glass of 6wt%, the iron powder of 3-20wt% and the water mixing of 30-40wt%, are then pressed into pellet;
Pellet is dehydrated under the conditions of 60-90 DEG C, until pellet weight is no longer changed;
The pellet of dehydration is removed into organic matter, and the organic matter of abjection is decomposed, decomposition product absorbs heel row through spray column Enter atmosphere;
The pellet for removing organic matter is sintered in closed container;
Sintered pellet is subjected to melting;
The casting of skimming of product after melting is obtained into alloy, detects alloying component.
Further, the dewatering time of the pellet is 5-20h.
Further, the pellet 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 crystalline silicon cutting waste material carries out break process in advance, and broken crystalline silicon cutting waste material has 90% or more grain graininess is less than 100 μm.
Further, the pellet is pressed into the pellet that diameter is 20-50mm.
Further, the granularity of the iron powder is 2-300 mesh.
Further, the organic matter decomposition of the abjection is that organic matter is passed through in incinerating kiln to decompose.
Further, the temperature that the pellet is sintered in closed container is 350-950 DEG C, sintering time 5-15h.
Further, the pellet melting is to carry out melting in induction furnace under vacuum or inert gas shielding, material Ball smelting temperature is 1450-1650 DEG C, soaking time 0.5-3h.
A kind of method preparing Antaciron using diamond wire sliced crystal scrap silicon provided by the invention, in pellet ingredient In use bentonite and add producing modified organic water-glass bonder formula, and aggregate, the pellet of compression moulding are done with varigrained iron powder Intensity and compression strength are fallen with good.Due to forming fibre structure after bentonite water swelling, so that wet feed ball has It is good to fall intensity and compression strength;Modified water glass colloidal particle is bonded to close with Si-O-Si and be formed surely during the sintering process Particle is firmly combined together fixed space net structure, so that siccative ball also has and good falls intensity and pressure resistance Degree;Iron powder is added and does aggregate, can make pellet pelletizing inside is closer to be combined together, further increase falling for dry and wet pellet It falls and compression strength.In addition, the present invention is dehydrated when being dehydrated to wet feed ball using low-temperature zone, avoids or significantly subtract The generation of few hydrogen, convenient for safety in production.Meanwhile the present invention burn at spray column absorption to the organic matter that pellet is deviate from Reason avoids crystalline silicon cutting water-base cutting fluid used and remains in the elements such as N, P, S in sliced crystal scrap silicon, producing Pernicious gas is generated in sintering and is discharged in air and pollutes 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 Antaciron 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 Antaciron using diamond wire sliced crystal scrap silicon referring to Fig. 1 Method includes the following steps:
Step 1: by mass percentage, by the crystalline silicon cutting waste material of 21-63wt%, the sodium bentonite of 1-3wt%, Then the modified water glass of 3-6wt%, the iron powder of 3-20wt% and the water mixing of 30-40wt% use high pressure roller press pressure At the material of diameter 10-50mm;Wherein, the crystalline silicon cutting waste material carries out break process in advance, cuts broken crystalline silicon Cutting has 90% or more grain graininess less than 100 μm in waste material, the granularity of the iron powder is 2-300 mesh.
Step 2: pellet being placed in tunnel oven or mesh belt dryer, is dehydrated under the conditions of 60-90 DEG C, and will dehydration Time controls in 5-20h, until pellet weight is no longer changed.
Step 3: dewatered pellet being placed in tunnel oven, organic matter is removed under conditions of 200-400 DEG C, and will take off Except the time of organic matter controls in 1-5h.The organic matter of abjection is passed through to burn in incinerator and is decomposed, generation then will be decomposed Flue gas is discharged into atmosphere after spray column absorbs again, and organic matter is avoided to burn the pernicious gas pollution air generated.
Step 4: the pellet for removing organic matter being sintered in closed container, sintering temperature controls the sintering at 350-950 DEG C Time control is 5-15h.
Step 5: under vacuum or inert gas shielding, induction furnace smelts 1450-1650 DEG C, and sintered pellet is existed Melting is carried out in induction furnace, smelting temperature control is 1450-1650 DEG C, and soaking time 0.5-3h.
Step 6: the casting that skim of the product after melting being obtained into alloy, finally detects alloying component.
Below by specific embodiment a kind of ferrosilicon is prepared using diamond wire sliced crystal scrap silicon to provided by the invention The method of alloy illustrates.
Embodiment 1
A method of Antaciron being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μm after being crushed.Sodium 0.2 kilogram of base bentonite dosage, 0.5 kilogram of modified water glass dosage, 1 kilogram of the iron powder of 2-300 mesh, crystalline silicon cutting material 4.3 Kilogram, it 4 kilograms of water, is matched according to this and carries out mixing, the ball of diameter 25mm is pressed into high pressure roller press.
(2) it is dehydrated under the conditions of 80 DEG C, dewatering time 10h, until the weight of wet bulb is no longer changed, is not detected It is generated to hydrogen.
(3) organic matter being removed under the conditions of 200 DEG C, takes off organic matter time 5h, the organic matter of abjection enters incinerator decomposition, Flue gas is most discharged into atmosphere after spray column elutes afterwards.
(4) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 350 DEG C, sintering time 8h.
(5) induction furnace is added under the conditions of 1450 DEG C of nitrogen atmospheres to smelt, soaking time 3h.
(6) casting that carries out skimming obtains alloy, and detection alloy silicon content is 60.50%.
Embodiment 2
A method of Antaciron being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μm after being crushed.Sodium 0.2 kilogram of base bentonite dosage, 0.6 kilogram of modified water glass dosage, 0.8 kilogram of the iron powder of 2-300 mesh, crystalline silicon cutting material It 4.6 kilograms, 3.8 kilograms of water, is matched according to this and carries out mixing, the ball of diameter 25mm is pressed into high pressure roller press.
(2) it is dehydrated under the conditions of 70 DEG C, dewatering time 12h, until the weight of wet bulb is no longer changed, is not detected It is generated to hydrogen.
(3) 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.
(4) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 450 DEG C, sintering time 8h.
(5) induction furnace is added under the conditions of 1550 DEG C of nitrogen atmospheres to smelt, soaking time 2h.
(6) casting that carries out skimming obtains alloy, and detection alloy silicon content is 65.74%.
Embodiment 3
A method of Antaciron being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μm after being crushed.Sodium 0.2 kilogram of base bentonite dosage, 0.6 kilogram of modified water glass dosage, 0.6 kilogram of the iron powder of 2-300 mesh, crystalline silicon cutting material 5 Kilogram, it 3.6 kilograms of water, is matched according to this and carries out mixing, the ball of diameter 25mm is pressed into high pressure roller press.
(2) it is dehydrated under the conditions of 70 DEG C, dewatering time 12h, until the weight of wet bulb is no longer changed, is not detected It is generated to hydrogen.
(3) 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.
(4) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 500 DEG C, sintering time 6h.
(5) induction furnace is added under 1550 DEG C of vacuum conditions to smelt, soaking time 2h.
(6) casting that carries out skimming obtains alloy, and detection alloy silicon content is 71.74%.
Embodiment 4
A method of Antaciron being prepared using diamond wire sliced crystal scrap silicon, is included the following steps:
(1) crystalline silicon cutting waste material is subjected to break process, the granularity of 90% or more particle is less than 100 μm after being crushed.Sodium 0.2 kilogram of base bentonite dosage, 0.8 kilogram of modified water glass dosage, 0.6 kilogram of the iron powder of 2-300 mesh, crystalline silicon cutting material It 4.7 kilograms, 3.7 kilograms of water, is matched according to this and carries out mixing, the ball of diameter 25mm is pressed into high pressure roller press.
(2) it is dehydrated under the conditions of 70 DEG C, dewatering time 12h, until the weight of wet bulb is no longer changed, is not detected It is generated to hydrogen.
(3) 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.
(4) ball for having taken off organic matter is packed into closed vessel.It is sintered under the conditions of 550 DEG C, sintering time 9h.
(5) induction furnace is added under the conditions of 1550 DEG C of argon atmospheres to smelt, soaking time 1.5h.
(6) casting that carries out skimming obtains alloy, and detection alloy silicon content is 68.26%.
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 (9)

1. a kind of method for preparing Antaciron using diamond wire sliced crystal scrap silicon, which comprises the steps of:
By mass percentage, by the crystalline silicon cutting waste material of 21-63wt%, the sodium bentonite of 1-3wt%, 3-6wt%'s Modified water glass, the iron powder of 3-20wt% and the water mixing of 30-40wt%, are then pressed into pellet;
Pellet is dehydrated under the conditions of 60-90 DEG C, until pellet weight is no longer changed;
The pellet of dehydration is removed into organic matter, and the organic matter of abjection is decomposed, decomposition product is discharged into greatly after spray column absorbs Gas;
The pellet for removing organic matter is sintered in closed container;
Sintered pellet is subjected to melting;
The casting of skimming of product after melting is obtained into alloy, detects alloying component.
2. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the dewatering time of the pellet is 5-20h.
3. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the pellet 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.
4. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the crystalline silicon cutting waste material carries out break process in advance, and broken crystalline silicon cutting waste material has 90% or more particle Granularity is less than 100 μm.
5. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the pellet is pressed into the pellet that diameter is 20-50mm.
6. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the granularity of the iron powder is 2-300 mesh.
7. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the organic matter decomposition of the abjection is that organic matter is passed through in incinerating kiln to decompose.
8. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the temperature that the pellet is sintered in closed container is 350-950 DEG C, sintering time 5-15h.
9. the method according to claim 1 for preparing Antaciron using diamond wire sliced crystal scrap silicon, feature exist In: the pellet melting is to carry out melting in induction furnace under vacuum or inert gas shielding, and pellet smelting temperature is 1450-1650 DEG C, soaking time 0.5-3h.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU417488A2 (en) * 1972-09-15 1974-02-28
SU1285016A1 (en) * 1985-04-12 1987-01-23 Коммунарский Горнометаллургический Институт Slag-forming mixture for refining molten metal
CN104962763A (en) * 2015-05-25 2015-10-07 北京科技大学 Method for producing chromium-based iron alloys through cutting wastes by crystalline silicon
CN105088052A (en) * 2015-09-22 2015-11-25 刘来宝 Method for producing ferrosilicon through cut waste in photovoltaic industry
CN105567968A (en) * 2016-02-01 2016-05-11 四川川投峨眉铁合金(集团)有限责任公司 Production method for smelting ferrosilicon by utilizing crystalline silicon cutting waste powder
CN108529630A (en) * 2018-07-17 2018-09-14 东北大学 A method of silicon carbide is prepared using synthesis by internal resistance electric melting

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU417488A2 (en) * 1972-09-15 1974-02-28
SU1285016A1 (en) * 1985-04-12 1987-01-23 Коммунарский Горнометаллургический Институт Slag-forming mixture for refining molten metal
CN104962763A (en) * 2015-05-25 2015-10-07 北京科技大学 Method for producing chromium-based iron alloys through cutting wastes by crystalline silicon
CN105088052A (en) * 2015-09-22 2015-11-25 刘来宝 Method for producing ferrosilicon through cut waste in photovoltaic industry
CN105567968A (en) * 2016-02-01 2016-05-11 四川川投峨眉铁合金(集团)有限责任公司 Production method for smelting ferrosilicon by utilizing crystalline silicon cutting waste powder
CN108529630A (en) * 2018-07-17 2018-09-14 东北大学 A method of silicon carbide is prepared using synthesis by internal resistance electric melting

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