CN105884184B - A kind of blast furnace cinder prepares the controlled micro crystallization method of devitrified glass - Google Patents
A kind of blast furnace cinder prepares the controlled micro crystallization method of devitrified glass Download PDFInfo
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- CN105884184B CN105884184B CN201610458722.0A CN201610458722A CN105884184B CN 105884184 B CN105884184 B CN 105884184B CN 201610458722 A CN201610458722 A CN 201610458722A CN 105884184 B CN105884184 B CN 105884184B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/16—Halogen containing crystalline phase
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Abstract
The present invention relates to a kind of controlled micro crystallization methods that blast furnace cinder prepares devitrified glass, it is characterised in that mainly including following three step：1. the glass blank after sizing to be cooled to the transition temperature of blast furnace cinder parent glass, and stop 58 minutes, make temperature uniform；1. 2. the temperature of glass blank after process, is risen to the nucleation temperature of glass and keeps the temperature 40 90 minutes, carry out nucleating course by step；3. after nucleating course, continue the temperature of glass blank rising to the controlled micro crystallization temperature of glass and keep the temperature 40 90 minutes, crystallization process is carried out, so as to the devitrified glass before being annealed.The present invention is before hot glass blank carries out coring, crystallization, its temperature must be reduced to the transition temperature of corresponding blast furnace cinder parent glass, to ensure the science and harmony of glass coring, crystallization process sequence, so as to ensure that prepared devitrified glass intensity is high, density is big；The glass blank is in the state of heat simultaneously, and mass energy can be saved by being begun to warm up by Tg temperature.
Description
Technical field
The present invention relates to a kind of controlled micro crystallization methods that blast furnace cinder prepares devitrified glass, and this method is particularly useful for making height
The material for carving on it field of performance.
Background technology
The waste discharged from blast furnace when blast furnace cinder is manUfaCtUre of pig iron, when furnace temperature reaches 1400-1600 DEG C, furnace charge melts
Melt, the ash content in gangue, coke and fluxing agent and other impurity that cannot enter in the pig iron in ore formed with silicate and
The slag above molten iron is floated on based on aluminate.Main component is CaO, SiO in blast furnace cinder2、Al2O3.A kind of industry of blast furnace slag
Solid waste often refines the slag that 1 ton of iron discharges 0.3 ton or so, and the grade of ore is lower, and bed drain purge is bigger.The height of China's cinder field accumulation
About 100,000,000 tons of clinker, if be not added with recycling treatment, the still significant wastage of available resources, does not accumulate over a long period and is bound to cause
A series of serious problems such as field, pollution environment are invaded in occupation of land.
Devitrified glass is a kind of existing glass properties, and has the composite material of ceramic performance, for its microstructure
Refer to the composite material containing micron or nanocrystal using glass as matrix, be a kind of homogeneous polycrystalline material of near ideal.
Devitrified glass shows excellent performance in all various aspects such as mechanical strength, case hardness, coefficient of thermal expansion, chemical stability.
Patent CN104313211A discloses a kind of method that molten blast furnace slag directly produces building material brick, is related to Ferrous Metallurgy
In waste residue utilization, the method that specifically a kind of molten blast furnace slag directly produces building material brick.Its technical process is：By slag iron point
From being heated up up to 1400 DEG C to 1500 DEG C molten blast furnace slags into slag runner temperature, being homogenized or quenched in liquid storage tank, subsequently into confession
Liquid pool and work department, work department outlet temperature are 1330 DEG C to 1450 DEG C；The slag liquid come out from work department enters calender molding,
The plank for the surface cure that surface temperature is 950 DEG C to 1200 DEG C is cooled by calendering；Calendering plate enters crystallization furnace progress
Crystallization, crystallization temperature are 950 DEG C to 1200 DEG C；Plank after crystallization enters anneal and eliminates stress, and cool to 70 DEG C
Go out annealing furnace, the plank for going out annealing furnace forms finished bricks through Length-fixing cutting, polishing, cutting and treating selvedge.This method takes full advantage of
The sensible heat of blast furnace cinder and solids resource.Patent CN105417957A is related to a kind of preparation of energy-saving type blast furnace slag microcrystalline glass
Method, by molten state blast-furnace cement sensible heat for the melting process of other auxiliary materials needed for devitrified glass preparation, the dosage of blast furnace slag
In 45-65%, the target component (wt.%) of high slag microcrystallite glass is：CaO 10-30%, SiO235-60%, Al2O3 10-
15%, MgO 8-12%, Na2O 3-6%, K2O 1-2%, Zn O 3-4%, TiO23-6%；All materials complete melting simultaneously
After full and uniformization, being poured into one in the constant temperature mold of flexible control, can complete the forming of female glass in mold, treat
After glass matrix molding, the heat treatment of devitrified glass is carried out directly in 700 DEG C to 1250 DEG C temperature ranges.The shape of devitrified glass
Core and crystal grow up, are cooled to room temperature, without stove is needed to change, optimize devitrified glass and prepare blast furnace slag dosage in raw material, technique
Rational Parameters save energy consumption and manufacturing cycle, solve existing devitrified glass preparation process complex process, energy consumption it is big,
The problems such as of high cost.
Although more than patent application is for the utilization of blast furnace cinder, it is proposed for preparing in building material brick and microcrystal glass plate etc.
Hold；Furthermore, it is believed that glass metal slightly cools down after high-temperature molding, and respectively at 900 DEG C to 1200 DEG C, 700 DEG C to 1250 DEG C temperature
It spends range and carries out controlled micro crystallization, it is intended that there is higher temperature using glass matrix after molding, controlled micro crystallization is carried out using this point
Can again be heated up from room temperature heating by glass matrix after molding to avoid traditional crystallization, carry out coring, controlled micro crystallization heat at
Reason mode, reaching reduces energy consumption, energy saving purpose.But there are in the problems in reality, with operating process for above method
Limitation, after glass metal is molded and does slightly cooling, just corresponding controlled micro crystallization, there are microcrystal glass material systems for this mode
Defective workmanship during standby can cause temperature excessively high and without necessary nucleation stage, the crystallization of prepared devitrified glass
Measure limited, the intensity of material is generally relatively low.
Invention content
The technical problems to be solved by the invention are to provide a kind of blast furnace in view of the deficiency of the prior art and melt
Slag prepares the controlled micro crystallization method of devitrified glass, and prepared devitrified glass has the advantages that density height and intensity are big.
The present invention is solves the problems, such as that used technical solution set forth above is：
A kind of blast furnace cinder prepares the controlled micro crystallization method of devitrified glass, mainly including following three step：1. by the glass after sizing
Glass blank is cooled to the transition temperature of blast furnace cinder parent glass, and stops 5-8 minutes, makes glass temperature uniform；2. step is 1.
After process, the temperature of glass blank is risen into the nucleation temperature of glass and keeps the temperature 40-90 minutes, carry out nucleating course；③
After nucleating course, continue the temperature of glass blank rising to the controlled micro crystallization temperature of glass and keep the temperature 40-90 minutes, carry out brilliant
Change process, so as to the devitrified glass before being annealed.
By said program, the glass transformation temperature, i.e. Tg are 440-480 DEG C, and nucleation temperature is 760-800 DEG C, crystallite
It is 1040-1180 DEG C to change temperature.Wherein, in temperature-rise period, heating rate is preferably 2-4 DEG C/min.
By said program, the preparation method of the glass blank after the sizing is：Using blast furnace cinder as primary raw material, and match
It closes auxiliary material and is prepared into batch；It is glass blank by the cast molding of gained glass metal, after to be formed after being melted to batch
Glass blank sizing after to get to the glass blank after sizing.
Preferably, the blast furnace cinder chemical composition range that is suitable for the invention is：SiO230wt%-35wt%,
Al2O313wt%-17wt%, CaO 35wt%-40wt%, MgO 7wt%-10wt%, Fe2O31wt%-5wt%, TiO2
0wt%-3wt%, MnO20wt%-3wt%.
Preferably, the basicity of the blast furnace cinder is higher, frit is partially short, add a certain amount of auxiliary material carry out basicity with
The adjustment of material property, 55wt%-72wt% of the blast furnace cinder incorporation for the two gross mass；The auxiliary material mainly include quartz sand,
Aluminium mountain flour, zinc white, stibium trioxide, pyrolusite, soda ash, barium carbonate, cryolite and titanium oxide etc., the specific additive amount of auxiliary material need to ensure to melt
The chemical composition of glass metal after melting is in following ranges：SiO260wt%-70wt%, Al2O35wt%-8wt%, CaO
15wt%-20wt%, MgO 2wt%-3wt%, BaO 3wt%-8wt%, Na2O 3wt%-6wt%, K2O 1wt%-
2wt%, ZnO 1wt%-3wt%, Sb2O30wt%-3wt%, Fe2O30.2wt%-2wt%, TiO20wt%-3wt%,
MnO20wt%-3wt%, F 1wt%-3wt%, the specific additive amount of auxiliary material can refer to the composition of blast furnace cinder in actual production and
Adjustment.
By said program, devitrified glass before the annealing is after annealing to get to devitrified glass.It is also wrapped after the annealing
Include cooling, cutting and etc..
On this basis, it is with blast furnace cinder the present invention also provides a kind of method that blast furnace cinder prepares devitrified glass
For primary raw material, and auxiliary material is coordinated to be prepared into batch；It is glass by the cast molding of gained glass metal after being melted to batch
Glass blank, it is to be formed after glass blank sizing after, controlled micro crystallization and annealing are carried out to it, obtain high-performance devitrified glass.Wherein,
The method of controlled micro crystallization, mainly including following three step：1. the glass blank after sizing is cooled to turning for blast furnace cinder parent glass
Temperature, and stop 5-8 minutes, make glass temperature uniform；1. 2. the temperature of glass blank after process, is risen to glass by step
The nucleation temperature of glass simultaneously keeps the temperature 40-90 minutes, carries out nucleating course；3. after nucleating course, continue the temperature of glass blank
Degree rises to the controlled micro crystallization temperature of glass and keeps the temperature 40-90 minute, progress crystallization process, so as to the devitrified glass before being annealed.
By said program, the method for the annealing is as follows：Devitrified glass before annealing is cooled to annealing temperature, in annealing
It is 640-700 DEG C to limit temperature range, ranging from 400-440 DEG C of lower limit temperature of annealing.Preferably, it is cooled to the rate of annealing temperature
It is 2-5 DEG C/min；The rate of temperature fall annealed between ceiling temperature and lower limit temperature need to be less than 0.8 DEG C/min.
By said program, the fusing, by total-oxygen combustor, supplements melting furnaces certain heat using pure oxygen combustion technology
Amount, to ensure the stability of fusing system, fusion temperature is maintained at 1420-1480 DEG C, keeps the temperature 8-12 hours.
By said program, the cast molding is that glass metal is continuously shaped using the method progress of direct casting.Wherein,
The temperature of shaping casting mouth is 1280-1360 DEG C.
Devitrified glass prepared by the present invention has the characteristics that density is big and intensity is high, density 2.8-3.0g/cm3, anti-folding
Intensity is up to 140-180MPa.
The present invention using blast furnace cinder using as primary raw material and will coordinate certain auxiliary material to be prepared into batch, to matching
Close material melted after, by glass metal cast molding be glass blank, it is to be formed after glass blank sizing after, utilize roller kilns
Crystallizing treatment is carried out to it, makes the fluorcanasite that the principal crystalline phase being wherein precipitated is stratiform, to replace a part of lithotome.Its
In, controlled micro crystallization is very crucial process, particularly before glass blank carries out coring, crystallization, it is necessary to which its temperature is reduced
To Tg temperature, to ensure that glass coring, crystallization harmony, while the glass blank are in the state of heat, add by Tg temperature
Heat can save mass energy.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, the present invention proposes the controlled micro crystallization new method for preparing blast furnace cinder devitrified glass, and parent glass after molding is cold
But to the transition temperature of glass, glass also has 450 DEG C or more of temperature at this time, on this condition, heats up to it and carries out coring, crystalline substance
Change can save certain energy, and prepared devitrified glass has the advantages that density height and intensity are big.
2nd, the present invention is directed to the design in terms of the composition characteristic of blast furnace cinder, progress component and preparation process, blast furnace cinder
Incorporation accounts for the 55wt%-72wt% of batch gross mass, and a large amount of blast furnace cinder is utilized, and is saved in terms of glass melting big
Measure the energy.
3rd, the devitrified glass for preparing of the present invention has bigger excellent in raw material, the more existing devitrified glass of energy saving aspect
Gesture greatly reduces production cost, and in addition the market price of devitrified glass product is high, and added value is higher；It has saved simultaneously a large amount of
The energy.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention is not
It is limited only to the following examples.
Embodiment 1
A kind of method that blast furnace cinder prepares devitrified glass using blast furnace cinder as primary raw material, and coordinates auxiliary material to be prepared into
Batch；After being melted to batch, by the cast molding of gained glass metal be Glass body, it is to be formed after Glass body determine
After type, controlled micro crystallization and annealing are carried out to it, high-performance devitrified glass is obtained, is as follows：
(1) blast furnace cinder selected, chemical composition are：SiO230wt%, Al2O317wt%, CaO 40wt%, MgO
7wt%, Fe2O32wt%, TiO23wt%, MnO21wt%, the auxiliary material of addition is quartz sand, aluminium mountain flour, zinc white, stibium trioxide, soft
Manganese ore, soda ash, barium carbonate, cryolite and titanium oxide；
Wherein, in terms of the gross mass of blast furnace cinder and auxiliary material, blast furnace cinder incorporation is 55wt%, and the incorporation of auxiliary material is
45wt%, the chemical composition of gained glass metal is as follows after fusing：SiO260wt%, Al2O35wt%, CaO 18wt%, MgO
2wt%, BaO 4wt%, Na2O 4wt%, K2O 1wt%, ZnO 3wt%, Sb2O30.5wt%, Fe2O31wt%, TiO2
0.5wt%, MnO20wt%, F 1wt%；
(2) blast furnace cinder in high-temperature liquid state is transported by blast furnace cinder transfer cask to the preceding mistake of blast furnace cinder melting furnaces
Pond is crossed, and the refractory material guide groove for passing through its lower end is thrown into glass furnace mouth；The auxiliary material of basic ingredient modulation is carried out through stirring
Auxiliary material transition is put into adding in storehouse after mixing mixing, is thrown by the guide groove of its lower end into glass furnace mouth；
Blast furnace cinder and auxiliary material make to enter melting end by wrapping up in material formula batch charger；Glass melter uses pure oxygen combustion technology, melts
Change temperature and be maintained at 1420 DEG C, keep the temperature 8 hours, obtain glass metal；Then gained glass metal is carried out using mechanical agitation clear feelings,
Homogenizing；
(3) method that the glass metal melted obtained by step 2) is used direct casting, carries out in heat resisting steel forming tank
Continuously shaped, glassware section after molding is rectangular continuous glass blank, and wherein the temperature of shaping casting mouth is 1280
℃；
(4) hot glass blank after molding enters roller kilns and carries out controlled micro crystallization and anneal.Specifically method is：1. hot glass
Blank requires cool to the Tg temperature spots (440 DEG C) of glass, and stops 5 minutes；2. after the constant temperature of Tg temperature spots, with 2 DEG C/
The temperature of hot glass blank is risen to the nucleation temperature (800 DEG C) of glass and keeps the temperature 40 minutes by the heating rate of minute, carries out core
Change process；3. after nucleating course, the temperature of hot glass blank is risen to the crystallite of glass with 4 DEG C/min of heating rate
Change temperature (1040 DEG C) and keep the temperature 90 minutes, carry out glass-ceramic process；4. after glass-ceramic process, with 5 DEG C/min of cooling
Speed to annealing region, annealing ceiling temperature is 640 DEG C, and the annealing lower limit temperature of glass is 400 DEG C, bound temperature of annealing
In the range of rate of temperature fall be less than 0.8 DEG C/min, be subsequently cooled to 100 DEG C hereinafter, obtaining using blast furnace cinder as primary raw material
Devitrified glass green body；5. the method using cutting+chilling is needed to cut devitrified glass green body by product, crystallite is obtained
Glass.
Devitrified glass density prepared by the present invention is 2.85g/cm3, flexural strength is up to 140MPa.
Embodiment 2
A kind of method that blast furnace cinder prepares devitrified glass using blast furnace cinder as primary raw material, and coordinates auxiliary material to be prepared into
Batch；After being melted to batch, by the cast molding of gained glass metal be Glass body, it is to be formed after Glass body determine
After type, controlled micro crystallization and annealing are carried out to it, high-performance devitrified glass is obtained, is as follows：
(1) blast furnace cinder selected, chemical composition are：SiO235wt%, Al2O315wt%, CaO 40wt%, MgO
7wt%, Fe2O31.5wt%, TiO21wt%, MnO20.5wt%, the auxiliary material of addition is quartz sand, aluminium mountain flour, zinc white, antimony
In vain, pyrolusite, soda ash, barium carbonate, cryolite and titanium oxide；
Wherein, in terms of the gross mass of blast furnace cinder and auxiliary material, blast furnace cinder incorporation is 62wt%, and the incorporation of auxiliary material is
38wt%, the chemical composition of gained glass metal is as follows after fusing：SiO266wt%, Al2O35wt%, CaO 15wt%, MgO
2wt%, BaO 4wt%, Na2O 4.5wt%, K2O 1.5wt%, ZnO 1wt%, Sb2O30.5wt%, Fe2O30.2wt%,
TiO20.2wt%, MnO20.1wt%, F 1wt%；
(2) blast furnace cinder in high-temperature liquid state is transported by blast furnace cinder transfer cask to the preceding mistake of blast furnace cinder melting furnaces
Pond is crossed, and the refractory material guide groove for passing through its lower end is thrown into glass furnace mouth；The auxiliary material of basic ingredient modulation is carried out through stirring
Auxiliary material transition is put into adding in storehouse after mixing mixing, is thrown by the guide groove of its lower end into glass furnace mouth；
Blast furnace cinder and auxiliary material make to enter melting end by wrapping up in material formula batch charger；Glass melter uses pure oxygen combustion technology, melts
Change temperature and be maintained at 1460 DEG C, keep the temperature 10 hours, obtain glass metal；Then gained glass metal is carried out using mechanical agitation clear
Feelings, homogenizing；
(3) method that the glass metal melted obtained by step 2) is used direct casting, carries out in heat resisting steel forming tank
Continuously shaped, glassware section after molding is rectangular continuous glass blank, and wherein the temperature of shaping casting mouth is 1320
℃；
(4) hot glass blank after molding enters roller kilns and carries out controlled micro crystallization and anneal.Specifically method is：1. hot glass
Blank requires cool to the Tg temperature spots (460 DEG C) of glass, and stops 6 minutes；2. after the constant temperature of Tg temperature spots, with 3 DEG C/
The temperature of hot glass blank is risen to the nucleation temperature (780 DEG C) of glass and keeps the temperature 60 minutes by the heating rate of minute, carries out core
Change process；3. after nucleating course, the temperature of hot glass blank is risen to the crystallite of glass with 3 DEG C/min of heating rate
Change temperature (1120 DEG C) and keep the temperature 60 minutes, carry out glass-ceramic process；4. after glass-ceramic process, with 4 DEG C/min of cooling
Speed to annealing region, annealing ceiling temperature is 680 DEG C, and the annealing lower limit temperature of glass is 420 DEG C, bound temperature of annealing
In the range of rate of temperature fall be less than 0.7 DEG C/min, be subsequently cooled to 100 DEG C hereinafter, obtaining using blast furnace cinder as primary raw material
Devitrified glass green body；5. the method using cutting+chilling is needed to cut devitrified glass green body by product, crystallite is obtained
Glass.
Devitrified glass density prepared by the present invention is 2.90g/cm3, flexural strength is up to 160MPa.
Embodiment 3
A kind of method that blast furnace cinder prepares devitrified glass using blast furnace cinder as primary raw material, and coordinates auxiliary material to be prepared into
Batch；After being melted to batch, by the cast molding of gained glass metal be Glass body, it is to be formed after Glass body determine
After type, controlled micro crystallization and annealing are carried out to it, high-performance devitrified glass is obtained, is as follows：
(1) blast furnace cinder selected, chemical composition are：SiO235wt%, Al2O315wt%, CaO 35wt%, MgO
10wt%, Fe2O32wt%, TiO22.5wt%, MnO20.5wt%, the auxiliary material of addition is quartz sand, aluminium mountain flour, zinc white, antimony
In vain, pyrolusite, soda ash, barium carbonate, cryolite and titanium oxide；
Wherein, in terms of the gross mass of blast furnace cinder and auxiliary material, blast furnace cinder incorporation is 62wt%, and the incorporation of auxiliary material is
38wt%, the chemical composition of gained glass metal is as follows after fusing：SiO268wt%, Al2O35wt%, CaO 15wt%, MgO
2wt%, BaO 3wt%, Na2O 3wt%, K2O 1wt%, ZnO 1wt%, Sb2O30.4wt%, Fe2O30.2wt%, TiO2
0.2wt%, MnO20.2wt%, F 1wt%；
(2) blast furnace cinder in high-temperature liquid state is transported by blast furnace cinder transfer cask to the preceding mistake of blast furnace cinder melting furnaces
Pond is crossed, and the refractory material guide groove for passing through its lower end is thrown into glass furnace mouth；The auxiliary material of basic ingredient modulation is carried out through stirring
Auxiliary material transition is put into adding in storehouse after mixing mixing, is thrown by the guide groove of its lower end into glass furnace mouth；
Blast furnace cinder and auxiliary material make to enter melting end by wrapping up in material formula batch charger；Glass melter uses pure oxygen combustion technology, melts
Change temperature and be maintained at 1480 DEG C, keep the temperature 12 hours, obtain glass metal；Then gained glass metal is carried out using mechanical agitation clear
Feelings, homogenizing；
(3) method that the glass metal melted obtained by step 2) is used direct casting, carries out in heat resisting steel forming tank
Continuously shaped, glassware section after molding is rectangular continuous glass blank, and wherein the temperature of shaping casting mouth is 1360
℃；
(4) hot glass blank after molding enters roller kilns and carries out controlled micro crystallization and anneal.Specifically method is：1. hot glass
Blank requires cool to the Tg temperature spots (480 DEG C) of glass, and stops 8 minutes；2. after the constant temperature of Tg temperature spots, with 4 DEG C/
The temperature of hot glass blank is risen to the nucleation temperature (760 DEG C) of glass and keeps the temperature 90 minutes by the heating rate of minute, carries out core
Change process；3. after nucleating course, the temperature of hot glass blank is risen to the crystallite of glass with 2 DEG C/min of heating rate
Change temperature (1180 DEG C) and keep the temperature 90 minutes, carry out glass-ceramic process；4. after glass-ceramic process, with 5 DEG C/min of cooling
Speed to annealing region, annealing ceiling temperature is 700 DEG C, and the annealing lower limit temperature of glass is 440 DEG C, bound temperature of annealing
In the range of rate of temperature fall be less than 0.6 DEG C/min, be subsequently cooled to 100 DEG C hereinafter, obtaining using blast furnace cinder as primary raw material
Devitrified glass green body；5. the method using cutting+chilling is needed to cut devitrified glass green body by product, crystallite is obtained
Glass.
Devitrified glass density prepared by the present invention is 3.0g/cm3, flexural strength is up to 180MPa.
The above is only the preferred embodiment of the present invention, it is noted that those of ordinary skill in the art are come
It says, without departing from the concept of the premise of the invention, several modifications and variations can also be made, these belong to the present invention's
Protection domain.
Claims (10)
1. a kind of blast furnace cinder prepares the controlled micro crystallization method of devitrified glass, it is characterised in that mainly including following three step：It 1. will be fixed
Glass blank after type is cooled to the transition temperature of blast furnace cinder parent glass, and stops 5-8 minutes, makes temperature uniform；2. it walks
Suddenly 1. the temperature of glass blank is risen into the nucleation temperature of glass and keeps the temperature 40-90 minutes after process, carry out coring
Journey；3. after nucleating course, continue the temperature of glass blank rising to the controlled micro crystallization temperature of glass and keep the temperature 40-90 minutes,
Crystallization process is carried out, so as to the devitrified glass before being annealed.
2. a kind of blast furnace cinder according to claim 1 prepares the controlled micro crystallization method of devitrified glass, it is characterised in that described
Transition temperature, that is, Tg is 440-480 DEG C, and nucleation temperature is 760-800 DEG C, and controlled micro crystallization temperature is 1040-1180 DEG C.
3. a kind of blast furnace cinder according to claim 1 prepares the controlled micro crystallization method of devitrified glass, it is characterised in that heating
Rate is 2-4 DEG C/min.
4. a kind of blast furnace cinder according to claim 1 prepares the controlled micro crystallization method of devitrified glass, it is characterised in that described
The preparation method of glass blank after sizing is：Using blast furnace cinder as primary raw material, and auxiliary material is coordinated to be prepared into batch；To matching
Close material melted after, by the cast molding of gained glass metal be glass blank, it is to be formed after glass blank sizing after to get to
Glass blank after sizing.
5. a kind of blast furnace cinder according to claim 4 prepares the controlled micro crystallization method of devitrified glass, it is characterised in that described
The chemical composition of glass metal is in following ranges：SiO260wt%-70wt%, Al2O35wt%-8wt%, CaO 15wt%-
20wt%, MgO 2wt%-3wt%, BaO 3wt%-8wt%, Na2O 3wt%-6wt%, K2O 1wt%-2wt%, ZnO
1wt%-3wt%, Sb2O30wt%-3wt%, Fe2O30.2wt%-2wt%, TiO20wt%-3wt%, MnO20wt%-
3wt%, F 1wt%-3wt%.
6. a kind of method that blast furnace cinder prepares devitrified glass, it is characterised in that it is using blast furnace cinder as primary raw material, and is matched
It closes auxiliary material and is prepared into batch；It is glass blank by the cast molding of gained glass metal, after to be formed after being melted to batch
Glass blank sizing after, controlled micro crystallization and annealing are carried out to it, obtain high-performance devitrified glass；
The method of the controlled micro crystallization includes following three step：1. the glass blank after sizing is cooled to blast furnace cinder parent glass
Transition temperature, and stop 5-8 minutes, make temperature uniform；1. 2. the temperature of glass blank after process, is risen to glass by step
Nucleation temperature and keep the temperature 40-90 minutes, carry out nucleating course；3. after nucleating course, continue the temperature of glass blank
It rises to the controlled micro crystallization temperature of glass and keeps the temperature 40-90 minutes, carry out crystallization process, so as to the devitrified glass before being annealed.
7. the method that a kind of blast furnace cinder according to claim 6 prepares devitrified glass, it is characterised in that the annealing
Method is as follows：Devitrified glass before annealing is cooled to annealing temperature, ranging from 640-700 DEG C of ceiling temperature of annealing, under annealing
It is 400-440 DEG C to limit temperature range.
8. the method that a kind of blast furnace cinder according to claim 7 prepares devitrified glass, it is characterised in that annealing upper limit temperature
Rate of temperature fall between degree and lower limit temperature need to be less than 0.8 DEG C/min.
9. the method that a kind of blast furnace cinder according to claim 6 prepares devitrified glass, it is characterised in that the blast furnace melts
Dreg chemistry compositing range is：SiO230wt%-35wt%, Al2O313wt%-17wt%, CaO 35wt%-40wt%, MgO
7wt%-10wt%, Fe2O31wt%-5wt%, TiO20wt%-3wt%, MnO20wt%-3wt%.
10. the method that a kind of blast furnace cinder according to claim 6 prepares devitrified glass, it is characterised in that with blast furnace cinder
With the gross mass meter of auxiliary material, 55wt%-72wt% of the blast furnace cinder for the two gross mass, surplus is auxiliary material；The auxiliary material
Mainly include quartz sand, aluminium mountain flour, zinc white, stibium trioxide, pyrolusite, soda ash, barium carbonate, cryolite and titanium oxide.
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| CN106587634B (en) * | 2016-12-16 | 2019-08-23 | 武汉理工大学 | A kind of direct speckle devitrified glass and preparation method thereof using molten blast furnace slag |
| CN107265866B (en) * | 2017-05-27 | 2019-11-26 | 武汉理工大学 | It is a kind of using blast furnace cinder as Venus devitrified glass of main material and preparation method thereof |
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| CN108439809A (en) * | 2018-01-30 | 2018-08-24 | 上海荣丰科技发展有限公司 | Foaming micro crystal material based on smelted furnace cinder and its production technology |
| CN108383390A (en) * | 2018-04-11 | 2018-08-10 | 四川名微晶科技股份有限公司 | A method of preparing devitrified glass new material using blast furnace hot slag |
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| CN112437760A (en) | 2018-07-16 | 2021-03-02 | 康宁股份有限公司 | Glass substrates comprising uniform release agent coating and methods of ceramming thereof |
| EP3694813A2 (en) * | 2018-07-16 | 2020-08-19 | Corning Incorporated | Glass-ceramic articles with increased resistance to fracture and methods for making the same |
| WO2020018408A1 (en) | 2018-07-16 | 2020-01-23 | Corning Incorporated | Methods for ceramming glass with nucleation and growth density and viscosity changes |
| KR102356026B1 (en) | 2018-07-16 | 2022-02-08 | 코닝 인코포레이티드 | Glass ceramic article with improved properties and method of making same |
| CN109399941A (en) * | 2018-12-21 | 2019-03-01 | 河北工业大学 | A method of micro-crystalline ceramic is prepared using flyash and waste slag |
| CN112521012B (en) * | 2020-11-11 | 2022-07-05 | 晶研一材料科技(宜兴)有限公司 | Heat-resistant high-hardness high-light-transmittance glass ceramic and preparation method thereof |
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| CN1696072A (en) * | 2004-05-12 | 2005-11-16 | 肖特股份有限公司 | Translucent or opaque colored glass-ceramic article providing a cooking surface and its use |
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| CN102030476A (en) * | 2010-11-03 | 2011-04-27 | 中国科学院上海光学精密机械研究所 | Cobalt-magnesium-aluminum-doped silicon-based nano microcrystalline glass containing lanthanum oxide and preparation method thereof |
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