CN108373266A - A method of preparing devitrified glass new material using smelting titanium tailings - Google Patents
A method of preparing devitrified glass new material using smelting titanium tailings Download PDFInfo
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- CN108373266A CN108373266A CN201810322207.9A CN201810322207A CN108373266A CN 108373266 A CN108373266 A CN 108373266A CN 201810322207 A CN201810322207 A CN 201810322207A CN 108373266 A CN108373266 A CN 108373266A
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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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B13/00—Rolling molten glass, i.e. where the molten glass is shaped by rolling
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/02—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a kind of methods preparing devitrified glass new material using smelting titanium tailings, include the following steps：Step 1: raw material selects；Step 2: raw material mixes；Step 3: the fusing of mixture；Step 4: calendaring molding；Step 5: annealing；Step 6: crystallization.The present invention prepares devitrified glass using smelting titanium tailings for the first time, and smelting titanium tailings accounts for the 30~41.5% of raw material weight, by the way that outer doping is added, changes smelting titanium tailings activity, makes it that can prepare devitrified glass.The technological difficulties of glass cannot be prepared by solving it.Due to, containing 10% or so titanium dioxide, during preparing devitrified glass, being not required to additional Nucleating Agent in smelting titanium tailings, significantly saving cost of material.
Description
Technical field
The present invention relates to a kind of preparation methods of devitrified glass, and in particular to a kind of to prepare devitrified glass using smelting titanium tailings
The method of new material.
Background technology
Devitrified glass refers to being added or being added without Nucleating Agent in parent glass, under conditions of controllable heat treatment, shape
At a kind of glass phase and crystallite phase existing new material jointly.Therefore, the basic performance of the existing glass of devitrified glass, and have
The polycrystalline feature for having ceramics has concentrated the advantage of glass and ceramics.With its high mechanical strength, hardness is big, wear-resisting property is good, corrosion resistant
Corrosion is strong, has good chemical stability and thermal stability, weatherability is strong, plasticity is superior.In recent years in the world
Quick development and application are arrived.
Titanium slag be using the v-ti magnetite ore of magnetic separation as raw material, through electric furnace smelting, remove most of iron and formed one
Kind rich-titanium material is the primary raw material for producing the products such as titanium tetrachloride, titanium dioxide and titanium sponge.In these production process
In will produce a large amount of smelting titanium tailings, and the TiO in these tailings2Content is low, complicated component, granularity is small, recycles difficulty big,
Generate a large amount of industrial solid wastes.It is found in research, in devitrified glass preparation, since smelting titanium tailings itself contains composition glass
Oxide necessary to glass, such as Al2O3、CaO、SiO2Deng TiO2It is also a kind of good Nucleating Agent, it is certain outer by being added
Add agent, it is made to have the condition to form glass, by being controllably heat-treated, devitrified glass is made.
Its component list of smelting titanium tailings is as follows：
Invention content
The purpose of the present invention is to provide a kind of methods preparing devitrified glass new material using smelting titanium tailings, improve industry
Solid waste resource recovery utilizes dynamics, diversifies.
The invention is realized in this way：
A method of devitrified glass new material being prepared using smelting titanium tailings, is included the following steps：
Step 1: raw material selects
Raw material is selected according to following weight ratio：
In the present invention, using quartz sand and smelting titanium tailings as primary raw material, other additives can be bought on periphery, and chemistry
Composition is relatively stable, and production cost is relatively low.Titanium dioxide can be used as devitrified glass Nucleating Agent contained in smelting titanium tailings, be not required to outer
Add Nucleating Agent.
Step 2: raw material mixes
It is mixed after being sent to mixing machine after above-mentioned raw materials are weighed well in proportion, and the water for accounting for raw material gross weight 2% is added, mixed
Conjunction 3~after five minutes, it send to All Electric Melting Furnace feeding chamber.
Step 3: the fusing of mixture
(1) it feeds：It is fed using automatic charging equipment, is controlled and fed by infrared ray liquid level indicator.
(2) fusing of mixture is carried out using All Electric Melting Furnace
All Electric Melting Furnace is divided into main melting tank, dog-hole, increased channel and several parts of material path, the fusing (fusion temperature of mixture
1350 DEG C~1500 DEG C), 8 hours or so (1400~1450 DEG C of the clarification and homogenization temperature) time of clarification and homogenization, in main molten
Change pond to carry out, clarification, the glass being homogenized enter material path through dog-hole, increased channel, and temperature is controlled at 1250 DEG C~1300 DEG C, warp
After material path cooling, calendaring molding (1150 DEG C~1250 DEG C of forming temperature) is carried out into calender.
Step 4: calendaring molding
Every production line uses two table glass calender (the using and the reserved) calendaring moldings, and plate thickness, width can be according to lifes
Production requires to be adjusted, and the communicated roller-way of glass tape of forming enters annealing kiln annealing.
Step 5: annealing
Glass tape enter annealing kiln temperature be 650~800 DEG C, at 680~750 DEG C keep the temperature 10~after twenty minutes, by 3 DEG C/
Divide~5 DEG C/minute of speed to be cooled to 580~620 DEG C, then 300 DEG C are cooled to by 7 DEG C/minute~12 DEG C/minute of speed, using
40 DEG C of kiln discharges are cooled within 40~60 minutes, subsequently into cold end cutting action.Cold end cutting action is wanted by sets requirement or client
The length asked cuts glass tape, forms semi-finished product (annealed sheet) after cutting, is sent to crystallization kiln crystallization through transition roller table.
Step 6: crystallization
The qualified annealed sheet of detection enters crystallization kiln, and 600 DEG C~720 DEG C were warming up to through 30~90 minutes, 600 DEG C~
720 DEG C of heat preservations coring in 30~90 minutes, then 820 DEG C~920 DEG C were warming up to through 30~90 minutes, 30 are kept the temperature at 820 DEG C~920 DEG C
~120 minutes crystallization were cooled to 40 DEG C of kiln discharges through 60~120 minutes, complete crystallization process.As hair plates (crystallization plate), send to
Mill cuts workshop finishing.
Step 7: grinding and polishing
Detection qualified crystallization plate such as is polished through ZDML-16 full-automatic mills, is polished at the surfaces processing, and then storage is protected
It deposits.
The present invention can be used for producing decoration devitrified glass, and specifically, the present invention has the following technical effect that：
1, devitrified glass is prepared using smelting titanium tailings for the first time, smelting titanium tailings accounts for the 30~41.5% of raw material weight, by adding
Enter a certain amount of alkali metal oxide, changes smelting titanium tailings activity (Al3+The network structure for taking part in smelting titanium tailings is formed, aluminic acid
The oxygen-octahedron and Al of silica chain breaking part in salt network3+Instead of Si4+The aluminum-oxygen tetrahedron of formation is unstable, meeting quilt
Highly basic is dissociated into silicate and aluminate, and in the case where smelting titanium tailings activity is not activated, inside glass occurs after fusing
More calculus and dross, such defect occurred in glass cannot be resolved by increasing temperature, have change its work only
Property), make it that can prepare devitrified glass.The technological difficulties of glass cannot be prepared by solving it.
2, since smelting titanium tailings wherein contains part of the metal oxide, during forming glass, it may appear that metal
Grain doping in glass, seriously affects glass quality, and by outer doping, (glass is being added in such as some metal oxides
The middle appearance that can effectively prevent metallic particles, increases substantially glass melting quality), solve metallic particles occur in glass
Technological difficulties.
3, the introducing of smelting titanium tailings, reduces glass melting temperature.(1400 DEG C~1450 DEG C) (vanadium titanium tailings can regard one as
Kind double salt has saved many reaction institutes calorific requirement in glass melting, and lattice is centainly destroyed, and is easy and other oxygen
Compound carries out solid-liquid phase reaction), in the case where not introducing smelting titanium tailings, glass melting temperature is at 1550~1580 DEG C.
4, due to, containing 10% or so titanium dioxide, during preparing devitrified glass, being not required to outer in smelting titanium tailings
Add Nucleating Agent, significantly saves cost of material.(expensive about 1.2~1.8 ten thousand yuan/ton of titanium dioxide).
5, final devitrified glass product 200~300MPa of compression strength, 40~80MPa of bending strength prepared by the present invention,
2.6~2.7g/cm3 of density, 5~6 grades of Mohs' hardness, water absorption rate<0.01%, finish 90~98, acidproof soda acid, radioactivity inspection
Survey meets national A classes examination criteria.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated.
Embodiment one
A method of devitrified glass new material being prepared using smelting titanium tailings, including：
1, by following raw material precises, and the water for accounting for raw material gross weight 2% is added, is sent into batch mixer mixing (when mixing
Between 4 minutes).
2, above-mentioned mixture is sent into All Electric Melting Furnace fusing, 1500 DEG C of fusion temperature, the glass melted is clarified and equal
After change, material path is entered by dog-hole, increased channel, temperature is down to 1300 DEG C, enters back into calendering work pool, is rolled into through calender
Shape (1250 DEG C of forming temperature) enters annealing kiln afterwards.
3, the glass board material annealing kiln after rolling is annealed, and is 700 DEG C into kiln temperature degree, after keeping the temperature 15 minutes at 650 DEG C,
580 DEG C are cooled to by 3 DEG C/minute of speed, then 300 DEG C are cooled to by 9 DEG C/minute of speed, 40 DEG C were cooled to using 60 minutes
Kiln discharge, subsequently into cold end cutting line.Cold end cutting line cuts glass tape by the length of sets requirement or customer requirement, after cutting
Semi-finished product (annealed sheet) are generated, are sent to crystallization kiln crystallization through transition roller table.
4, the qualified annealed sheet of detection enters crystallization kiln, was warming up to 680 DEG C through 60 minutes, 60 minutes core is kept the temperature at 680 DEG C
Change, be warming up to 900 DEG C through 45 minutes, 100 minutes crystallization are kept the temperature at 900 DEG C, 40 DEG C of kiln discharges were cooled to through 120 minutes, completes
Crystallization process.As hair plates (crystallization plate), send to mill and cut workshop finishing.
Embodiment two
A method of devitrified glass new material being prepared using smelting titanium tailings, including：
1, by following raw material precises, and the water for accounting for raw material gross weight 2% is added, is sent into batch mixer mixing (when mixing
Between 4 minutes).
2, above-mentioned mixture is sent into All Electric Melting Furnace fusing, 1500 DEG C of fusion temperature, the glass melted is clarified and equal
After change, material path is entered by dog-hole, increased channel, temperature is down to 1300 DEG C, enters back into calendering work pool, is rolled into through calender
Shape (1250 DEG C of forming temperature) enters annealing kiln afterwards.
3, the glass board material annealing kiln after rolling is annealed, and is 700 DEG C into kiln temperature degree, after keeping the temperature 15 minutes at 650 DEG C,
580 DEG C are cooled to by 3 DEG C/minute of speed, then 300 DEG C are cooled to by 9 DEG C/minute of speed, 40 DEG C were cooled to using 60 minutes
Kiln discharge, subsequently into cold end cutting line.Cold end cutting line cuts glass tape by the length of sets requirement or customer requirement, after cutting
Semi-finished product (annealed sheet) are generated, are sent to crystallization kiln crystallization through transition roller table.
4, the qualified annealed sheet of detection enters crystallization kiln, was warming up to 700 DEG C through 60 minutes, 60 minutes core is kept the temperature at 700 DEG C
Change, be warming up to 920 DEG C through 60 minutes, 100 minutes crystallization are kept the temperature at 920 DEG C, 40 DEG C of kiln discharges were cooled to through 120 minutes, completes
Crystallization process.As hair plates (crystallization plate), send to mill and cut workshop finishing.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will be fallen in principle disclosed in the present application
Within scope and spirit.
Claims (3)
1. a kind of method preparing devitrified glass new material using smelting titanium tailings, it is characterised in that include the following steps：
Step 1: raw material selects
Raw material is selected according to following weight ratio：
Step 2: raw material mixes
It is mixed after being sent to mixing machine after above-mentioned raw materials are weighed well in proportion, and the water for accounting for raw material gross weight 2% is added, mixing 3
~after five minutes, it send to All Electric Melting Furnace feeding chamber；
Step 3: the fusing of mixture
(1) it feeds：It is fed using automatic charging equipment, is controlled and fed by infrared ray liquid level indicator；
(2) fusing of mixture is carried out using All Electric Melting Furnace
All Electric Melting Furnace is divided into main melting tank, dog-hole, increased channel and several parts of material path, when the fusing of mixture, clarification and homogenization
Between 8 hours or so, carried out in main melting tank, clarification, the glass that has been homogenized enter material path, temperature control through dog-hole, increased channel
System is at 1250 DEG C~1300 DEG C, and after material path cools down, calendaring molding, forming temperature 1150 DEG C~1250 are carried out into calender
℃；
Step 4: calendaring molding
Every production line uses two table glass calender calendaring moldings, plate thickness, width that can be adjusted according to production requirement,
The communicated roller-way of glass tape of forming enters annealing kiln annealing；
Step 5: annealing
Glass tape enter annealing kiln temperature be 650~800 DEG C, at 680~750 DEG C keep the temperature 10~after twenty minutes, by 3 DEG C/minute~5
DEG C/minute speed be cooled to 580~620 DEG C, then 300 DEG C are cooled to by 7 DEG C/minute~12 DEG C/minute of speed, using 40~60
Minute is cooled to 40 DEG C of kiln discharges, subsequently into cold end cutting action；Cold end cutting action is by sets requirement or the length of customer requirement
Degree cuts glass tape, forms semi-finished product annealed sheet after cutting, is sent to crystallization kiln crystallization through transition roller table；
Step 6: crystallization
The qualified annealed sheet of detection enters crystallization kiln, 600 DEG C~720 DEG C is warming up to through 30~90 minutes, at 600 DEG C~720 DEG C
Coring in 30~90 minutes is kept the temperature, then 820 DEG C~920 DEG C were warming up to through 30~90 minutes, 30~120 are kept the temperature at 820 DEG C~920 DEG C
Minute crystallization was cooled to 40 DEG C of kiln discharges through 60~120 minutes, completes crystallization process.
2. the method for preparing devitrified glass new material using smelting titanium tailings according to claim 1, it is characterised in that：
In the main melting tank of All Electric Melting Furnace, 1350 DEG C~1500 DEG C of the fusion temperature of mixture, clarification and homogenization temperature 1400~
1450℃。
3. the method for preparing devitrified glass new material using smelting titanium tailings according to claim 1, it is characterised in that：
In step 6, become crystallization plate after the completion of crystallization, is polished through ZDML-16 full-automatic mills, polished surface processing, so
Storage preserves afterwards.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810322207.9A CN108373266A (en) | 2018-04-11 | 2018-04-11 | A method of preparing devitrified glass new material using smelting titanium tailings |
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Cited By (7)
| 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 |
| 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 |
| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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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