CN106517798A - Method for preparing glass-ceramic by use of medium-low titanium type blast furnace slag - Google Patents
Method for preparing glass-ceramic by use of medium-low titanium type blast furnace slag Download PDFInfo
- Publication number
- CN106517798A CN106517798A CN201610920833.9A CN201610920833A CN106517798A CN 106517798 A CN106517798 A CN 106517798A CN 201610920833 A CN201610920833 A CN 201610920833A CN 106517798 A CN106517798 A CN 106517798A
- Authority
- CN
- China
- Prior art keywords
- blast furnace
- furnace slag
- glass
- devitrified glass
- low titanium
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
- C03C10/0009—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 silica as main constituent
Abstract
The invention belongs to the preparation field of the glass-ceramic, and in particular relates to a method for preparing glass-ceramic by use of medium-low titanium type blast furnace slag. The method comprises the following steps: by taking medium-low titanium type blast furnace slag as basic raw materials, adding a titanium ferrochromium three-phase composite nucleation agent, Cr2O3, TiO2 and Fe2O3, and preparing the glass-ceramic with high strength, high hardness, acid-base resistance, corrosion resistance and other good performances by use of a specific melting process and a thermal treatment mode. The invention provides specific melting and thermal treatment process parameters so as to solve the problem that the glass-ceramic is poor in physical performance since the glass-ceramic prepared by use of the high titanium type blast furnace slag is unstable in crystal phase and various in crystal phase in the prior art is solved; and the blank in the comprehensive utilization and research aspect of the medium-low titanium type blast furnace slag in the prior art is filled.
Description
Technical field
The invention belongs to the preparation field of devitrified glass, and in particular to it is a kind of utilize in, low titanium blast furnace slag prepare crystallite
The method of glass.
Background technology
By TiO in slag2Blast furnace slag can be divided into three types by content:Low titanium blast furnace slag (TiO2<10%), middle titanium-type is high
Slag (TiO210-20%) with high-titanium blast furnace slag (TiO2>20%).In prior art, the comprehensive utilization ratio of titanium-containing blast furnace slag
Low, only part high-titanium blast furnace slag is integrated into utilizing, and remainder is in the state of storing up, while its Land use systems is also only
It is for producing the low value-added product such as cement.
In the at present research done to titanium-containing blast furnace slag devitrified glass by researcher, only to adding Cr2O3With other Nucleating Agent systems
Devitrified glass is studied, and is mixed with the situation of devitrified glass without studying various Nucleating Agents, therefore obtained micro-
Crystal glass crystalline phase is more, and has uncertainty, and the performance of devitrified glass can have been affected.The researcher also having in addition is with height
Titanium blast furnace slag is prepared in devitrified glass, but no solution, low titanium blast furnace slag, such as holds the Utilizing question of steel blast furnace slag, and
The Composite Nucleation Agents for adding under study for action promote the overall crystallize of parent glass, but there are coarse grains, arrange and disperse not advise
Then, the larger problem of crystallize difference of ability, causes that finished product devitrified glass is more crisp, and physical property is poor.
Therefore, existing research can not effectively improve the comprehensive utilization ratio of titanium-containing blast furnace slag, while obtained crystallite glass
Glass physical and chemical performance is poor, it is impossible to is further used as product and applies to building industry field, causes the wasting of resources.Additionally, existing
Have in terms of technology centering, the comprehensive utilizating research of low titanium blast furnace slag still in blank.
The content of the invention
For solving the above problems, the present invention is provided in a kind of utilization, the method that low titanium blast furnace slag prepares devitrified glass, institute
State method with, low titanium blast furnace slag as base stock, by add ferrochrome titanium three-phase composite Nucleating Agent, improve devitrified glass
Growth index, promote the carrying out of Crystallization Process, effectively improve crystallize effect, promote the overall crystallize of sample, and will not
There is the defects such as the incomplete, shrinkage cavity of coarse grains, crystallize.
The present invention is adopted the following technical scheme that：
With reference to composition in slag, with, low titanium blast furnace slag as base stock, add ferrochrome titanium three-phase composite Nucleating Agent, adopt
With the good devitrified glass of following steps processability.
Step 1. is melted：By raw material mix homogeneously, in being put into resistance furnace, raw material is made to melt completely；Meanwhile, with another electricity
Resistance stove is preheated to mould with standby；
It is prepared by step 2. parent glass：After the completion of founding, sample is taken out from resistance furnace；Taking a little sample carries out chilled water (chw)
Quench, the water quenching sample for obtaining is carried out into DSC detections, and result is analyzed and is calculated, determine nucleation temperature and crystallization temperature；
Remaining sample is cast in preheated mould, and the sample cast is put back in resistance furnace rapidly, is made annealing treatment, system
Into parent glass；
Step 3. heat treatment：According to DSC testing results, heat treatment is carried out to parent glass；
It is prepared by step 4. devitrified glass：Sample after heat treatment is taken out after cooling to room temperature with the furnace, obtains devitrified glass.
Further, ferrochrome titanium three-phase composite Nucleating Agent is Cr2O3、TiO2And Fe2O3；
Further, in described, low titanium blast furnace slag mass percent in the feed be 32.70%-38.47%, institute
State Cr in ferrochrome titanium three-phase composite Nucleating Agent2O3、TiO2And Fe2O3Mass percent in the feed is respectively 0.96%-
2.88%, 3.85%-9.62%, 0-0.96%, other compositions are assorted with pure material oxide according to parent glass formula；
Further, the technological parameter of the melting is：Melt temperature is 1460-1530 DEG C, and settling time is 2.5-4h,
During resistance furnace is warming up to melt temperature, when less than 920 DEG C, heating rate is 5-8 DEG C/min, and more than 920 DEG C heating rates are
2-4℃/min；
Further, the water quenching sample be dried, grind, cross 200 mesh sieves after carry out DSC detections；
Further, the heat treatment is specially：Sample is put into into resistance furnace, through coring, Crystallizing treatment process；Wherein
Nucleation temperature reduces 15-25 DEG C than the corresponding detected values of differential scanning calorimetry DSC, and crystallization temperature is than differential scanning calorimetry DSC
Corresponding detected value raises 15-25 DEG C, nucleation time 1-1.5h, crystallization time 2-2.5h；
Further, the devitrified glass principal crystalline phase is diopside crystalline phase；
Further, the resistance furnace is chamber type electric resistance furnace；
Further, mould is preheated in step 1 500-800 DEG C it is standby.
Present invention beneficial effect compared with the prior art：
1)Cr2O3、TiO2And Fe2O3Three-phase composite Nucleating Agent improves nucleus quantity, and the growth that improve devitrified glass refers to
Number, promotes the carrying out of Crystallization Process, effectively improves crystallize effect, promote the overall crystallize of sample, and be not in crystal grain
The defects such as thick, crystallize is incomplete, shrinkage cavity；
2) present invention solves the problems, such as that devitrified glass crystalline phase is unstable and various crystalline phases occurs, promotes crystalline phase unification,
The devitrified glass prepared using technical solution of the present invention only has 2-3 kind crystalline phases, or even only a kind crystalline phase, and principal crystalline phase is very
Clearly, be diopside crystalline phase, while crystal is in " staged " layered distribution, rule and it is fine and close, structure neatly, compare by this crystalline phase
For the common crystalline phase of the CMAS microcrystalline glass in series such as wollastonite and cacoclasite, with high intensity, high rigidity, acid and alkali-resistance and
The superperformance such as corrosion-resistant；
3) devitrified glass obtained in the present invention has good physical and chemical performance, and bending strength is up to 114.74MPa, body
Product density is 2.770g/cm3, water absorption rate is 0, and acid-alkali-resistant degree is 0.085%, far superior to Expectation of Glass-Ceramics Used as Decorated Materials and work
Industry devitrified glass concerned countries standard, is worth with commercial introduction.
Description of the drawings
Fig. 1 preparation technology flow charts of the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is below in conjunction with drawings and Examples, right
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
Conversely, the present invention covers any replacement done in the spirit and scope of the present invention being defined by the claims, repaiies
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to the thin of the present invention
It is in section description, detailed to describe some specific detail sections.Part without these details for a person skilled in the art
Description can also understand the present invention completely.
The concrete proportion scheme that the present invention is adopted is as follows：According to parent glass formula, by 36g low titanium blast furnace slag and difference
For the Cr of 3g, 8g and 1g2O3、TiO2And Fe2O3Mix homogeneously, not enough other compositions are assorted with pure material oxide, are specifically contained
Amount is as shown in table 1.Final dispensing gross weight is 109g.
1 embodiment proportion scheme (unit of table：Gram)
The present embodiment selects fusion method, carries out parent glass using 1600 DEG C of high temperature box type resistance furnaces and founds.Specific experiment
Data and operational approach are as follows：The dispensing of mix homogeneously is put into into corundum crucible, and crucible is put into into intensification in chamber type electric resistance furnace,
With the ramp of 5 DEG C/min to 920 DEG C protecting furnace lining, then with the ramp of 3 DEG C/min to 1510 DEG C, in stove inside holding
3.5h, makes raw material melt completely, and allows bubble collapse, while ensureing that vitreous humour will not be acutely sprayed because of the too fast, reaction that heats up
Splash.
Meanwhile, using another 1200 DEG C of chamber type electric resistance furnaces, mould is carried out being preheated to 550 DEG C it is standby, to prevent basis
Glass is burst because of excessive temperature differentials in forming process.
After the completion of founding, sample is taken out from high temperature resistance furnace, be cast in preheated mould.And will cast
Sample is put back in high temperature resistance furnace rapidly, is made annealing treatment, with reduce casting after sample in cooling procedure surface with it is interior
Portion's cooldown rate has big difference and produces larger thermal stress.Annealing is specially：The sample cast is put back to into rapidly electricity
Resistance furnace is warming up to 600 DEG C by resistance stove, is incubated 30min, and rear furnace cooling makes parent glass.Meanwhile, before casting, will be few
Perhaps sample is poured in the crucible for filling cold water, carries out chilling water quenching, and the water quenching sample drying that obtains, grinding, to cross 200 mesh sieves laggard
Row DSC is detected, result is analyzed and is calculated, determine nucleation temperature and crystallization temperature.
According to DSC testing results, heat treatment is carried out to parent glass, wherein, the nucleation temperature of selection is than differential scanning amount
Full-boiled process DSC detected values reduce by 20 DEG C, and crystallization temperature raises 20 DEG C than DSC detected value, nucleation time 1.3h, crystallization time 2.3h,
Sample is put into into resistance furnace, through coring, crystallization process, is taken out after room temperature is cooled to the furnace, be finally obtained of good performance
Devitrified glass.
Claims (10)
1. in utilizing, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that with, low titanium blast furnace slag is as base
This raw material, adds ferrochrome titanium three-phase composite Nucleating Agent, prepares devitrified glass.
2. it is as claimed in claim 1 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that it is concrete
Operating procedure is：
Step 1. is melted：By raw material mix homogeneously, in being put into resistance furnace, raw material is made to melt completely；Meanwhile, use another resistance furnace
Mould is preheated with standby；
It is prepared by step 2. parent glass：After the completion of founding, sample is taken out from resistance furnace；Taking a little sample carries out chilling water quenching,
The water quenching sample for obtaining is carried out into DSC detections, and result is analyzed and is calculated, for determining in subsequent thermal steps
Nucleation temperature and crystallization temperature；Remaining sample is cast in preheated mould, and the sample cast is put back to rapidly resistance
In stove, made annealing treatment, made parent glass；
Step 3. heat treatment：According to DSC testing results, heat treatment is carried out to parent glass；
It is prepared by step 4. devitrified glass：Sample after heat treatment is taken out after cooling to room temperature with the furnace, obtains devitrified glass.
3. it is as claimed in claim 1 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that ferrochrome
Titanium three-phase composite Nucleating Agent is Cr2O3、TiO2And Fe2O3。
4. it is as claimed in claim 3 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that it is described
In, low titanium blast furnace slag mass percent in the feed be 32.70%-38.47%, the ferrochrome titanium three-phase composite Nucleating Agent
Middle Cr2O3、TiO2And Fe2O3Mass percent in the feed is respectively 0.96%-2.88%, 3.85%-9.62%, 0-
0.96%.
5. it is as claimed in claim 2 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that step 1
In, the technological parameter of the melting is：Melt temperature is 1460-1530 DEG C, and settling time is 2.5-4h, and resistance furnace is warming up to molten
Melt in temperature course, when less than 920 DEG C, heating rate is 5-8 DEG C/min, and more than 920 DEG C heating rates are 2-4 DEG C/min.
6. it is as claimed in claim 2 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that in DSC
Before detection, the water quenching sample is dried, is ground, crossing 200 mesh sieves.
7. it is as claimed in claim 2 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that it is described
Heat treatment is specially：Parent glass is put into into resistance furnace, through coring, Crystallizing treatment process；Wherein nucleation temperature is swept than differential
Retouch the corresponding detected value of calorimetry DSC low 15-25 DEG C, crystallization temperature 15-25 higher than the corresponding detected values of differential scanning calorimetry DSC
DEG C, nucleation time 1-1.5h, crystallization time 2-2.5h.
8. it is as claimed in claim 2 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that it is described
Resistance furnace is chamber type electric resistance furnace.
9. it is as claimed in claim 2 utilize in, the low titanium blast furnace slag method for preparing devitrified glass, it is characterised in that step 1
In mould is preheated to 500-800 DEG C it is standby.
10. a kind of devitrified glass, the devitrified glass are prepared using the arbitrary methods described of claim 1-9, it is characterised in that institute
Devitrified glass principal crystalline phase is stated for diopside crystalline phase.
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| CN201610920833.9A CN106517798B (en) | 2016-10-21 | 2016-10-21 | In utilization, the method that low titanium blast furnace slag prepares devitrified glass |
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| CN201610920833.9A CN106517798B (en) | 2016-10-21 | 2016-10-21 | In utilization, the method that low titanium blast furnace slag prepares devitrified glass |
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| CN106517798B CN106517798B (en) | 2019-05-17 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108947258A (en) * | 2018-09-18 | 2018-12-07 | 西南科技大学 | It is a kind of to mention devitrified glass of the titanium slag as raw material containing chlorine |
| CN109133649A (en) * | 2018-09-18 | 2019-01-04 | 西南科技大学 | It is a kind of to propose the system that titanium slag prepares devitrified glass using containing chlorine |
| CN109133650A (en) * | 2018-09-18 | 2019-01-04 | 西南科技大学 | A method of devitrified glass is prepared using titanium slag is mentioned containing chlorine |
| CN109133651A (en) * | 2018-11-13 | 2019-01-04 | 西南科技大学 | It is a kind of by mentioning the devitrified glass that titanium slag is prepared containing chlorine |
| CN109279782A (en) * | 2018-11-07 | 2019-01-29 | 西南科技大学 | It is a kind of to propose the system that titanium warm sludge prepares devitrified glass using containing chlorine |
| CN109279783A (en) * | 2018-11-13 | 2019-01-29 | 西南科技大学 | A kind of raw material includes the devitrified glass that titanium slag is mentioned containing chlorine |
| CN109320090A (en) * | 2018-11-07 | 2019-02-12 | 西南科技大学 | A method of devitrified glass is prepared using titanium warm sludge is mentioned containing chlorine |
| CN112340988A (en) * | 2020-11-03 | 2021-02-09 | 重庆大学 | Titanium-containing blast furnace slag-based TiO2Preparation method of microcrystalline glass as nucleating agent |
| CN112408799A (en) * | 2020-11-25 | 2021-02-26 | 茅台学院 | Method for preparing low-water-absorption microcrystalline glass by using blast furnace slag |
| CN112960907A (en) * | 2021-03-18 | 2021-06-15 | 海南海控特玻科技有限公司 | Coffee microcrystalline glass stone prepared from molybdenum tailings and preparation method thereof |
| CN114230184A (en) * | 2021-12-30 | 2022-03-25 | 武汉理工大学 | Microcrystalline glass using liquid titanium slag as main raw material and preparation method thereof |
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Cited By (18)
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| CN108947258B (en) * | 2018-09-18 | 2021-07-02 | 西南科技大学 | Microcrystalline glass using chlorine-containing titanium extraction slag as raw material |
| CN109133649A (en) * | 2018-09-18 | 2019-01-04 | 西南科技大学 | It is a kind of to propose the system that titanium slag prepares devitrified glass using containing chlorine |
| CN109133650A (en) * | 2018-09-18 | 2019-01-04 | 西南科技大学 | A method of devitrified glass is prepared using titanium slag is mentioned containing chlorine |
| CN109133649B (en) * | 2018-09-18 | 2022-03-01 | 西南科技大学 | System for preparing microcrystalline glass by using chlorine-containing titanium extraction slag |
| CN108947258A (en) * | 2018-09-18 | 2018-12-07 | 西南科技大学 | It is a kind of to mention devitrified glass of the titanium slag as raw material containing chlorine |
| CN109133650B (en) * | 2018-09-18 | 2022-02-11 | 西南科技大学 | Method for preparing microcrystalline glass by using chlorine-containing titanium extraction slag |
| CN109279782A (en) * | 2018-11-07 | 2019-01-29 | 西南科技大学 | It is a kind of to propose the system that titanium warm sludge prepares devitrified glass using containing chlorine |
| CN109320090A (en) * | 2018-11-07 | 2019-02-12 | 西南科技大学 | A method of devitrified glass is prepared using titanium warm sludge is mentioned containing chlorine |
| CN109320090B (en) * | 2018-11-07 | 2022-02-11 | 西南科技大学 | Method for preparing microcrystalline glass by using chlorine-containing titanium extraction hot slag |
| CN109279782B (en) * | 2018-11-07 | 2022-03-01 | 西南科技大学 | System for preparing microcrystalline glass by using chlorine-containing titanium extraction hot slag |
| CN109279783B (en) * | 2018-11-13 | 2021-12-10 | 西南科技大学 | Microcrystalline glass with raw materials including chlorine-containing titanium extraction slag |
| CN109279783A (en) * | 2018-11-13 | 2019-01-29 | 西南科技大学 | A kind of raw material includes the devitrified glass that titanium slag is mentioned containing chlorine |
| CN109133651B (en) * | 2018-11-13 | 2022-02-11 | 西南科技大学 | Microcrystalline glass prepared from chlorine-containing titanium extraction slag |
| CN109133651A (en) * | 2018-11-13 | 2019-01-04 | 西南科技大学 | It is a kind of by mentioning the devitrified glass that titanium slag is prepared containing chlorine |
| CN112340988A (en) * | 2020-11-03 | 2021-02-09 | 重庆大学 | Titanium-containing blast furnace slag-based TiO2Preparation method of microcrystalline glass as nucleating agent |
| CN112408799A (en) * | 2020-11-25 | 2021-02-26 | 茅台学院 | Method for preparing low-water-absorption microcrystalline glass by using blast furnace slag |
| CN112960907A (en) * | 2021-03-18 | 2021-06-15 | 海南海控特玻科技有限公司 | Coffee microcrystalline glass stone prepared from molybdenum tailings and preparation method thereof |
| CN114230184A (en) * | 2021-12-30 | 2022-03-25 | 武汉理工大学 | Microcrystalline glass using liquid titanium slag as main raw material and preparation method thereof |
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