CN108640524A - A kind of method that high carbon chromium scum prepares devitrified glass - Google Patents
A kind of method that high carbon chromium scum prepares devitrified glass Download PDFInfo
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- CN108640524A CN108640524A CN201810856407.2A CN201810856407A CN108640524A CN 108640524 A CN108640524 A CN 108640524A CN 201810856407 A CN201810856407 A CN 201810856407A CN 108640524 A CN108640524 A CN 108640524A
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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
- C03C10/0063—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 waste materials, e.g. slags
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
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Abstract
The invention discloses a kind of methods preparing devitrified glass using high carbon chromium scum, and using high carbon chromium scum as base stock, fluxing agent, fining agent and KOH is added, by batch mixing, heating melting, moulding by casting, annealing, Crystallizing treatment and etc. be prepared.Devitrified glass produced by the present invention has preferable wearability, corrosion resistance and shock resistance, and solves the problems such as environmental pollution of existing ferrochrome tailing, safety problem.
Description
Technical field
The present invention relates to microcrystal glass material technical fields, and in particular to a kind of high carbon chromium scum prepares the side of devitrified glass
Method.
Background technology
Devitrified glass is also known as microcrystalline jade or glass-ceramic, is comprehensive glass, and it is novel to be that a kind of foreign country has just developed
Construction material, its scientific name are called glass quartz.Devitrified glass and our common glass seem to differ widely.It has glass
The double grading of glass and ceramics, the atomic arrangement inside simple glass be do not have the reason of well-regulated, this is also Glass breadks easily it
One, and devitrified glass is made of, that is to say, that its atomic arrangement is regular as ceramics crystal.So crystallite
Glass is higher than the brightness of ceramics, stronger than glass toughness, and composition includes silicate.
Tailing is one of the product of separation operation in ore dressing, and in the product of this operation, the content of useful component is minimum,
It is the mine that should not be further sorted under current condition of technology and economy.Most composition is silicic acid in general tailing
Salt, it is much like with cast stone and the required ingredient of devitrified glass, thus be possible to add part chemical industry as raw material using tailing
Raw material and prepare high abrasion, acid and alkali-resistance corrode, impact-resistant devitrified glass replace cast stone.It is domestic to use rare earth tail through having
Mine, flyash, iron tailings etc. prepare the report of devitrified glass.
As CN101024554A is disclosed, a kind of rich rare earth, niobium, fluorite is dilute selects tailing microcrystal glass and manufacturing method, belongs to
In the comprehensive utilization of trade waste.Feature is:The raw material for preparing of the devitrified glass selects tailing, quartz sand, chemical group to be dilute
At being by weight percentage:SiO2 30-70%, CaO 5-20%, Al2O35-15%, CaF2 3-15%, ReO 3-15%, Nb2O5
0-5%, TiO2 0-10%。
And a kind of microcrystalline glass prepared from desulphurized and preparation method thereof is disclosed in CN102167516A, it is to use desulfurized powder
Coal ash (30-65wt%), through dispensing, mixing, be melted, molding, annealing, nucleus crystallization, be cold worked.Product main component
For:SiO2(50-60%), Fe2O3(1-2.5%), Al2O3(3-10%), CaO (20-30%), MgO (1-9%), Na2O(5-
10%).
And devitrified glass is prepared using the tailing of scum containing high carbon chromium and is not yet reported that.And high carbon chromium scum belongs to weight toxicity
Waste does not only take up a large amount of soils, and causes seriously to pollute.Therefore devitrified glass tool is prepared by using high carbon chromium scum
There is important meaning.
Invention content
The present invention provides a kind of method that high carbon chromium scum prepares devitrified glass, devitrified glass obtained has preferable
Wearability, corrosion resistance and shock resistance, and environmental pollution, the safety problem etc. that solve existing ferrochrome tailing are asked
Topic.
It is of the existing technology in order to solve the problems, such as, it adopts the following technical scheme that:
A kind of method that high carbon chromium scum prepares devitrified glass, by mass percentage, which becomes:High carbon ferro-chrome
Slag 88-92wt%, fluxing agent 5-7wt%, fining agent 2.2-4.4wt%, KOH 0.5-1.5wt%;
Wherein, the high carbon ferro-chrome slag ingredient is by mass percentage:0.5%MoO3, 0.7%NiO, 1.5%TiO2, 4.5%
Na2O, 1.2%Cr2O3, 5.3%ZnO, 6.8%Fe2O3, 6.5%Al2O3, 19.0%CaO, 12.3%MgO, 41.7%SiO2;
And it is prepared using following methods:
(1)The desired amount of ferrochrome slag, fluxing agent and fining agent are crushed, and ferrochrome slag, fluxing agent and fining agent after sieving are thrown
Enter batch mixer to be sufficiently mixed, obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 30-40min at 650 DEG C, is added in high temperature furnace and is melted
Change, fusion temperature is 1300-1400 DEG C, keeps the temperature 40-60min, and KOH is then added, is first warming up to 1500 with the speed of 5 DEG C/min
DEG C, 30-50min is kept the temperature, is then cooled to 1350 DEG C again with the speed of 8 DEG C/min, 20-30min is kept the temperature, waits for that melt is uniform, clear
Qualified glass metal is formed after clear;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:In 520-650 DEG C of stove
Inside holding 1-2h;Then it is warming up to 740-780 DEG C with≤5 DEG C/min, keeps the temperature 2-4h;Then 820- is warming up to≤5 DEG C/min
850 DEG C, keep the temperature 1-2h;Then it is warming up to 930-950 DEG C with 10-14 DEG C/min, keeps the temperature 0.5-1h;Then with 15-20 DEG C/min
It is cooled to 520-650 DEG C, keeps the temperature 1-2h;Then 100 DEG C or less are cooled to 10-14 DEG C/min to come out of the stove, devitrified glass hair is made
Blanket;
(5)Thickness, corase grinding, fine polishing, cutting, chamfered edge are determined to the devitrified glass blank flat of preparation, obtain devitrified glass.
Preferably, by mass percentage, which becomes:High carbon chromium scum 90wt%, fluxing agent
6wt%, fining agent 3wt%, KOH 1wt%.
Preferably, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight between them
Than being 15:8:3:1.
Preferably, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Preferably, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh
Sieve.
Preferably, the step(3)In, the temperature of mold preheating is 800 DEG C.
Preferably, the step(3)Middle annealing condition:80- is made annealing treatment in 650 DEG C of Muffle furnace
100min。
Preferably, the step(4)In, the technical process of crystallization is as follows:In 540 DEG C of stove inside holding 1.5h;So
760 DEG C are warming up to≤5 DEG C/min afterwards, keeps the temperature 3h;Then 835 DEG C are warming up to≤5 DEG C/min, keep the temperature 1.5h;Then with 12
DEG C/min is warming up to 940 DEG C, keep the temperature 0.8h;Then 535 DEG C are cooled to 18 DEG C/min, keep the temperature 1.5h;Then with 12 DEG C/min
It is cooled to 100 DEG C or less to come out of the stove, devitrified glass blank flat is made.
Compared with prior art, the present invention it has the advantages that:
(1)The present invention uses high carbon chromium scum, and by adding fluxing agent, fining agent, KOH, prepares with preferable wearability
Energy, corrosion resistance and impact-resistant devitrified glass, while also solving the environmental pollution of ferrochrome tailing, security problems.
(2)Not only contain the main chemical compositions prepared needed for devitrified glass in the high carbon chromium scum of the present invention, contains simultaneously
There is the Cr of regulation and control devitrified glass institutional framework2O3、TiO2、NiO、MoO3Etc. micro constitutents, to make the more refinement of crystal development
Small, crystal eduction rate is high, and then improves wearability, acid-alkali-corrosive-resisting and the excellent shock resistance of devitrified glass.
(3)Invent addition fluxing agent can the fusion temperature of system reduce, while the crystallization of devitrified glass can be effectively improved
Rate and principal crystalline phase percentage;And the addition of fining agent can eliminate the bubble in glass metal, improve devitrified glass quality;And
KOH can be used as the oxidant and activator that high carbon chromium scum prepares the method for devitrified glass, can not only be oxidized at high temperature
K2O, have the function of it is fluxing, meanwhile, KOH activity becomes strong, the Cr in adsorbable high carbon chromium scum under high temperature, to fix Cr
In devitrified glass, its dissolution pollution environment is prevented.
(4)For the present invention by constantly regulating and controlling fusing, molding and crystallization process parameter, it is principal crystalline phase that can obtain as diopside
Devitrified glass and crystal content can arrive 70-76%, and to be the devitrified glass of principal crystalline phase using diopside have excellent mechanical property
Energy, wearability and corrosion resistance, to make devitrified glass obtained that there is preferable wearability, corrosion resistance and impact resistance
Energy.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, technical scheme of the present invention will be carried out below
Clear, complete description.Obviously, described embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.
Based on the embodiments of the present invention, those of ordinary skill in the art obtained institute without making creative work
There are other embodiments, belongs to the range that the present invention is protected.
Embodiment 1
The method that the high carbon chromium scum of the present embodiment prepares devitrified glass, by mass percentage, the glass raw material group become:It is high
Carbon ferrochrome slag 88%, fluxing agent 6.5wt%, fining agent 4.4wt%, KOH 1.1wt%.
It is prepared according to following preparation method:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 30min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1300 DEG C, keeps the temperature 40min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 30min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 20min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 520 DEG C of stoves
Warm 1h;Then 740 DEG C are warming up to≤5 DEG C/min, keep the temperature 2h;Then 820 DEG C are warming up to≤5 DEG C/min, keep the temperature 1h;So
930 DEG C are warming up to 10 DEG C/min afterwards, keeps the temperature 0.5h;Then 520 DEG C are cooled to 15 DEG C/min, keep the temperature 1h;Then with 10
DEG C/min is cooled to 100 DEG C or less and comes out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:80min is made annealing treatment in 650 DEG C of Muffle furnace.
Embodiment 2
The method that the high carbon chromium scum of the present embodiment prepares devitrified glass, by mass percentage, the glass raw material group become:It is high
Carbon ferrochrome slag 90wt%, fluxing agent 5.5wt%, fining agent 3.3wt%, KOH 1.2wt%.
It is prepared as follows method and is prepared:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 40min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1400 DEG C, keeps the temperature 60min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 50min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 30min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 650 DEG C of stoves
Warm 2h;Then 780 DEG C are warming up to≤5 DEG C/min, keep the temperature 4h;Then 850 DEG C are warming up to≤5 DEG C/min, keep the temperature 2h;Then
950 DEG C are warming up to 14 DEG C/min, keeps the temperature 1h;Then 650 DEG C are cooled to 20 DEG C/min, keep the temperature 2h;Then with 14 DEG C/min
It is cooled to 100 DEG C or less to come out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:100min is made annealing treatment in 650 DEG C of Muffle furnace.
Embodiment 3
The method that the high carbon chromium scum of the present embodiment prepares devitrified glass, by mass percentage, the glass raw material group become:It is high
Carbon ferrochrome slag 90wt%, fluxing agent 6wt%, fining agent 3wt%, KOH 1wt%.
It is prepared as follows method and is prepared:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 35min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1350 DEG C, keeps the temperature 50min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 40min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 25min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 540 DEG C of stoves
Warm 1.5h;Then 760 DEG C are warming up to≤5 DEG C/min, keep the temperature 3h;Then 835 DEG C are warming up to≤5 DEG C/min, heat preservation
1.5h;Then 940 DEG C are warming up to 12 DEG C/min, keep the temperature 0.8h;Then 535 DEG C are cooled to 18 DEG C/min, keep the temperature 1.5h;
Then 100 DEG C or less are cooled to 12 DEG C/min to come out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:90min is made annealing treatment in 650 DEG C of Muffle furnace.
Embodiment 4
The method that the high carbon chromium scum of the present embodiment prepares devitrified glass, by mass percentage, the glass raw material group become:It is high
Carbon ferrochrome slag 89wt%, fluxing agent 7wt%, fining agent 3.6wt%, KOH 0.8wt%.
It is prepared as follows method and is prepared:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 32min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1330 DEG C, keeps the temperature 45min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 35min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 22min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 560 DEG C of stoves
Warm 1.3h;Then 750 DEG C are warming up to≤5 DEG C/min, keep the temperature 2.5h;Then 830 DEG C are warming up to≤5 DEG C/min, heat preservation
1.2h;Then 940 DEG C are warming up to 11 DEG C/min, keep the temperature 0.6h;Then 530 DEG C are cooled to 16 DEG C/min, keep the temperature 1.3h;
Then 100 DEG C or less are cooled to 12 DEG C/min to come out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:85min is made annealing treatment in 650 DEG C of Muffle furnace.
Embodiment 5
The method that the high carbon chromium scum of the present embodiment of the present embodiment prepares devitrified glass, by mass percentage, the glass are former
Material group becomes:High carbon chromium scum 91wt%, fluxing agent 6wt%, fining agent 2.5wt%, KOH 0.5wt%.
It is prepared as follows method and is prepared:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 38min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1380 DEG C, keeps the temperature 55min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 45min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 28min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 620 DEG C of stoves
Warm 1.8h;Then 770 DEG C are warming up to≤5 DEG C/min, keep the temperature 3.5h;Then 840 DEG C are warming up to≤5 DEG C/min, heat preservation
1.8h;Then 945 DEG C are warming up to 13 DEG C/min, keep the temperature 0.8h;Then 620 DEG C are cooled to 18 DEG C/min, keep the temperature 1.8h;
Then 100 DEG C or less are cooled to 13 DEG C/min to come out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:95min is made annealing treatment in 650 DEG C of Muffle furnace.
Embodiment 6
The method that the high carbon chromium scum of the present embodiment prepares devitrified glass, by mass percentage, the glass raw material group become:It is high
Carbon ferrochrome slag 88.5wt%, fluxing agent 5.6wt%, fining agent 4.4wt%, KOH 1.5wt%.
It is prepared as follows method and is prepared:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 35min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1300 DEG C, keeps the temperature 55min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 45min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 25min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 560 DEG C of stoves
Warm 1.5h;Then 760 DEG C are warming up to≤5 DEG C/min, keep the temperature 3.5h;Then 840 DEG C are warming up to≤5 DEG C/min, heat preservation
1.5h;Then 940 DEG C are warming up to 12 DEG C/min, keep the temperature 0.8h;Then 600 DEG C are cooled to 16 DEG C/min, keep the temperature 1.2h;
Then 100 DEG C or less are cooled to 12 DEG C/min to come out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:85min is made annealing treatment in 650 DEG C of Muffle furnace.
Embodiment 7
The method that the high carbon chromium scum of the present embodiment prepares devitrified glass, by mass percentage, the glass raw material group become:It is high
Carbon ferrochrome slag 90.5wt%, fluxing agent 5.5wt%, fining agent 2.7wt%, KOH 1.3wt%.
It is prepared as follows method and is prepared:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 38min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1330 DEG C, keeps the temperature 45min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 35min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 25min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 550 DEG C of stoves
Warm 1.8h;Then 750 DEG C are warming up to≤5 DEG C/min, keep the temperature 2.5h;Then 830 DEG C are warming up to≤5 DEG C/min, heat preservation
1.2h;Then 935 DEG C are warming up to 12 DEG C/min, keep the temperature 0.6h;Then 580 DEG C are cooled to 18 DEG C/min, keep the temperature 1.8h;
Then 100 DEG C or less are cooled to 12 DEG C/min to come out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:95min is made annealing treatment in 650 DEG C of Muffle furnace.
Embodiment 8
The method that the high carbon chromium scum of the present embodiment prepares devitrified glass, by mass percentage, the glass raw material group become:It is high
Carbon ferrochrome slag 91.5wt%, fluxing agent 5.5wt%, fining agent 2.2wt%, KOH 0.8wt%.
It is prepared as follows method and is prepared:
(1)By the desired amount of high carbon chromium scum, fluxing agent and fining agent crush, and will sieving after high carbon chromium scum, fluxing agent and
Fining agent input batch mixer is sufficiently mixed, and obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 33min at 650 DEG C, is added in high temperature furnace and is melted,
Fusion temperature is 1350 DEG C, keeps the temperature 55min, and KOH is then added, and is first warming up to 1500 DEG C with the speed of 5 DEG C/min, heat preservation
Then 35min is cooled to 1350 DEG C with the speed of 8 DEG C/min again, keep the temperature 22min, and qualification is formed after, clarification uniform after melt
Glass metal;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:It is protected in 550 DEG C of stoves
Warm 1.8h;Then 770 DEG C are warming up to≤5 DEG C/min, keep the temperature 3.5h;Then 845 DEG C are warming up to≤5 DEG C/min, heat preservation
1.8h;Then 945 DEG C are warming up to 12 DEG C/min, keep the temperature 0.8h;Then 580 DEG C are cooled to 18 DEG C/min, keep the temperature 1.5h;
Then 100 DEG C or less are cooled to 12 DEG C/min to come out of the stove, devitrified glass blank flat is made;
(5)The method blank flat that devitrified glass is prepared to the high carbon chromium scum of preparation determines thickness, corase grinding, fine polishing, cutting, chamfered edge, obtains
To devitrified glass.
Wherein, the cosolvent is fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:
3:1。
Wherein, the fining agent is sodium nitrate, sodium carbonate or antimony oxide.
Wherein, the step(1)Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
Wherein, the step(3)In, the temperature of mold preheating is 800 DEG C.
Wherein, the step(3)Middle annealing condition:95min is made annealing treatment in 650 DEG C of Muffle furnace.
Experimental example
To devitrified glass made from above-described embodiment 1-8 according to national standard《GB/T9966-2001》It makes a service test, specifically
The results are shown in Table 1.
Table 1
Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 |
Draw strength(MPa) | 67.87 | 69.86 | 75.34 | 71.15 | 65.87 | 64.59 | 73.23 | 70.28 |
Acid resistance(%) | 0.056 | 0.044 | 0.038 | 0.056 | 0.054 | 0.062 | 0.048 | 0.053 |
Alkali resistance(%) | 0.001 | 0 | 0 | 0.002 | 0 | 0.003 | 0.002 | 0 |
Wearability(g/cm2) | 0.039 | 0.035 | 0.032 | 0.037 | 0.033 | 0.034 | 0.036 | 0.033 |
As shown in Table 1, the method that the high carbon chromium scum that prepared by the present invention prepares devitrified glass has preferable wearability, acid and alkali-resistance
Corrosivity and shock resistance.
To sum up, creativeness of the invention is mainly reflected in the following:
(1)The present invention uses high carbon chromium scum, and by adding fluxing agent, fining agent, KOH, prepares with preferable wearability
Energy, corrosion resistance and impact-resistant devitrified glass, while also solving the environmental pollution of ferrochrome tailing, security problems.
(2)Not only contain the main chemical compositions prepared needed for devitrified glass in the high carbon chromium scum of the present invention, contains simultaneously
There is the Cr of regulation and control devitrified glass institutional framework2O3、TiO2、NiO、MoO3Etc. micro constitutents, to make the more refinement of crystal development
Small, crystal eduction rate is high, and then improves wearability, acid-alkali-corrosive-resisting and the excellent shock resistance of devitrified glass.
(3)Invent addition fluxing agent can the fusion temperature of system reduce, while the crystallization of devitrified glass can be effectively improved
Rate and principal crystalline phase percentage;And the addition of fining agent can eliminate the bubble in glass metal, improve devitrified glass quality;And
KOH can be used as the oxidant and activator that high carbon chromium scum prepares the method for devitrified glass, can not only be oxidized at high temperature
K2O, have the function of it is fluxing, meanwhile, KOH activity becomes strong, the Cr in adsorbable high carbon chromium scum under high temperature, to fix Cr
In devitrified glass, its dissolution pollution environment is prevented.
(4)For the present invention by constantly regulating and controlling fusing, molding and crystallization process parameter, it is principal crystalline phase that can obtain as diopside
Devitrified glass and crystal content can arrive 70-76%, and to be the devitrified glass of principal crystalline phase using diopside have excellent mechanical property
Energy, wearability and corrosion resistance, to make devitrified glass obtained that there is preferable wearability, corrosion resistance and impact resistance
Energy.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (8)
1. a kind of method that high carbon chromium scum prepares devitrified glass, which is characterized in that by mass percentage, the glass raw material group
Become:High carbon chromium scum 88-92wt%, fluxing agent 5-7wt%, fining agent 2.2-4.4wt%, KOH 0.5-1.5wt%;
Wherein, the high carbon ferro-chrome slag ingredient is by mass percentage:0.5%MoO3, 0.7%NiO, 1.5%TiO2, 4.5%
Na2O, 1.2%Cr2O3, 5.3%ZnO, 6.8%Fe2O3, 6.5%Al2O3, 19.0%CaO, 12.3%MgO, 41.7%SiO2;
And it is prepared using following methods:
(1)The desired amount of ferrochrome slag, fluxing agent and fining agent are crushed, and ferrochrome slag, fluxing agent and fining agent after sieving are thrown
Enter batch mixer to be sufficiently mixed, obtains devitrified glass basis batch;
(2)Mixed devitrified glass basis batch is preheated into 30-40min at 650 DEG C, is added in high temperature furnace and is melted
Change, fusion temperature is 1300-1400 DEG C, keeps the temperature 40-60min, and KOH is then added, is first warming up to 1500 with the speed of 5 DEG C/min
DEG C, 30-50min is kept the temperature, is then cooled to 1350 DEG C again with the speed of 8 DEG C/min, 20-30min is kept the temperature, waits for that melt is uniform, clear
Qualified glass metal is formed after clear;
(3)Uniform, clear glass metal is poured into preheated mold, after glass metal molding after after be sent into Muffle furnace in anneal
Processing, obtains parent glass plate;
(4)Molding parent glass plate is sent into resistance furnace and carries out crystallization, the technical process of crystallization is as follows:In 520-650 DEG C of stove
Inside holding 1-2h;Then it is warming up to 740-780 DEG C with≤5 DEG C/min, keeps the temperature 2-4h;Then 820- is warming up to≤5 DEG C/min
850 DEG C, keep the temperature 1-2h;Then it is warming up to 930-950 DEG C with 10-14 DEG C/min, keeps the temperature 0.5-1h;Then with 15-20 DEG C/min
It is cooled to 520-650 DEG C, keeps the temperature 1-2h;Then 100 DEG C or less are cooled to 10-14 DEG C/min to come out of the stove, devitrified glass hair is made
Blanket;
(5)Thickness, corase grinding, fine polishing, cutting, chamfered edge are determined to the devitrified glass blank flat of preparation, obtain devitrified glass.
2. the method that high carbon chromium scum according to claim 1 prepares devitrified glass, which is characterized in that by mass percentage
Meter, the glass raw material group become:High carbon chromium scum 90wt%, fluxing agent 6wt%, fining agent 3wt%, KOH 1wt%.
3. the method that high carbon chromium scum according to claim 1 prepares devitrified glass, which is characterized in that the cosolvent is
Fluorite, boron oxide, dolomite and barite, and the weight ratio between them is 15:8:3:1.
4. the method that high carbon chromium scum according to claim 1 prepares devitrified glass, which is characterized in that the fining agent is
Sodium nitrate, sodium carbonate or antimony oxide.
5. the method that high carbon chromium scum according to claim 1 prepares devitrified glass, which is characterized in that the step(1)
Further include that high carbon chromium scum, fluxing agent and the fining agent of crushing are crossed into 50 mesh sieve.
6. the method that high carbon chromium scum according to claim 1 prepares devitrified glass, which is characterized in that the step(3)
In, the temperature of mold preheating is 800 DEG C.
7. the method that high carbon chromium scum according to claim 1 prepares devitrified glass, which is characterized in that the step(3)
Middle annealing condition:80-100min is made annealing treatment in 650 DEG C of Muffle furnace.
8. the method that high carbon chromium scum according to claim 1 prepares devitrified glass, which is characterized in that the step(4)
In, the technical process of crystallization is as follows:In 540 DEG C of stove inside holding 1.5h;Then 760 DEG C are warming up to≤5 DEG C/min, keep the temperature 3h;
Then 835 DEG C are warming up to≤5 DEG C/min, keep the temperature 1.5h;Then 940 DEG C are warming up to 12 DEG C/min, keep the temperature 0.8h;Then
535 DEG C are cooled to 18 DEG C/min, keeps the temperature 1.5h;Then 100 DEG C or less are cooled to 12 DEG C/min to come out of the stove, devitrified glass is made
Blank flat.
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CN105152536A (en) * | 2015-09-21 | 2015-12-16 | 北京科技大学 | Method for compounding microcrystalline glass materials by means of ferrochrome slags |
CN105924013A (en) * | 2016-04-25 | 2016-09-07 | 四川名微晶科技股份有限公司 | Glass ceramic produced by all electric fused rolling process technique using ferrochrome slags as raw materials and production method therefor |
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CN105152536A (en) * | 2015-09-21 | 2015-12-16 | 北京科技大学 | Method for compounding microcrystalline glass materials by means of ferrochrome slags |
CN105924013A (en) * | 2016-04-25 | 2016-09-07 | 四川名微晶科技股份有限公司 | Glass ceramic produced by all electric fused rolling process technique using ferrochrome slags as raw materials and production method therefor |
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