CN108585511A - A kind of preparation method of high-performance devitrified glass - Google Patents
A kind of preparation method of high-performance devitrified glass Download PDFInfo
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- CN108585511A CN108585511A CN201810471131.6A CN201810471131A CN108585511A CN 108585511 A CN108585511 A CN 108585511A CN 201810471131 A CN201810471131 A CN 201810471131A CN 108585511 A CN108585511 A CN 108585511A
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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
- 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
-
- 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
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
Abstract
The invention discloses a kind of preparation methods of high-performance devitrified glass, include the following steps：Step 1 weighs following corresponding weight percent raw material for standby：SiO222 28%, Al2O316 20%, MgO 8 14%, Fe2O30.2 0.8%, MnO 0.2 0.6%, CaO 0.04 0.08%, ZrO20.02 0.06%, CrO 0.01 0.03%, pretreatment granite waste residues 14 18%, rich magnalium magnesia spinel 8 12%.A kind of preparation method of high-performance devitrified glass of the present invention, the glass-ceramic doping granite reduce cost of manufacture, while can improve the intensity of glass, have higher use value and good application prospect.
Description
Technical field
The present invention relates to devitrified glass preparing technical fields, and in particular to a kind of preparation method of high-performance devitrified glass.
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 as ceramics crystal, that is to say, that its atomic arrangement is regular, so, crystallite
Glass is higher than the brightness of ceramics, stronger than glass toughness, and devitrified glass preparation method includes whole crystallization method (fusion method), sintering
Method, sol-gel method etc., the method for domestic industrial applications is the above two at present, and the present invention adulterates flower in devitrified glass
Gang Yan, and granite contains oxide needed for the industrial productions such as a large amount of silica, alchlor, therefore to devitrified glass
It can further probe into.
The how rare earth doped mine of devitrified glass in the prior art, and Rare Earth Mine have radioactivity, be not to body it is fine, simultaneously
Rare Earth Mine is of high cost, is not suitable for large-scale production.
Invention content
In view of the drawbacks of the prior art, the object of the present invention is to provide a kind of preparation methods of high-performance devitrified glass, should
Glass-ceramic doping granite reduces cost of manufacture, while can improve the intensity of glass, has higher use value and good
Good application prospect.
The present invention solves technical problem and adopts the following technical scheme that：
The present invention provides a kind of preparation methods of high-performance devitrified glass, include the following steps：
Step 1 weighs following corresponding weight percent raw material for standby：SiO222-28%, Al2O316-20%, MgO
8-14%, Fe2O 30.2-0.8%, MnO 0.2-0.6%, CaO 0.04-0.08%, ZrO20.02-0.06%, CrO
0.01-0.03%, pretreatment granite waste residues 14-18%, rich magnalium magnesia spinel 8-12%；
Raw material in step 1 is sent into corundum crucible by step 2 after mixing, is carried out melting, is subsequently sent to mold
Middle cast molding, then anneals, and is then cooled to room temperature again to get the high-performance crystallite of the present invention with 20-30 DEG C/min
Glass.
Preferably, it is that granite waste residues are sent into jaw crushing that granite waste residues preparation method is pre-processed in the step 1
Machine crushes, and broken rear granite is risen to 750 DEG C with 5 DEG C/min from room temperature to be calcined, and 25- is kept the temperature at 750 DEG C
35min is then cooled to room temperature, is sent into mass fraction and is acidified for 40-60% sulfuric acid solutions, then carries out ball milling and crosses 20 mesh sieve,
Up to pretreatment granite waste residues.
Preferably, rich magnalium magnesia spinel grain size is 20-100 mesh in the step 1.
Preferably, content of magnesia is 25-35%, alumina content 45- in the step 1 richness magnalium magnesia spinel
55%.
Preferably, the step 2 melting condition is 1500 DEG C of smelting temperature, smelting time 2h.
Preferably, 950 DEG C first are cooled the temperature to 2-4 DEG C/min before the step 2 annealing, is then kept the temperature
35min。
Preferably, crystallization processing is carried out before the temperature is down to 950 DEG C.
Preferably, the crystallization treatment temperature is 1020-1100 DEG C, processing time 35-45min.
Preferably, the step 2 annealing conditions are to be placed in 550-650 DEG C of annealing furnace to anneal.
Compared with prior art, the present invention has following advantageous effect：
(1) preparation method of a kind of high-performance devitrified glass of the invention, addition pretreatment flower hilllock in prepared by devitrified glass
Rock waste residue can reduce cost, while be found by multigroup experiment, and the strong of glass can be remarkably reinforced by adding rich magnalium magnesia spinel
Degree, when content of magnesia is 25-35%, and alumina content is 45-55%, intensity is best.
(2) preparation method of a kind of high-performance devitrified glass of the invention is first cooled the temperature to 2-4 DEG C/min before annealing
950 DEG C, heat preservation 35min is then carried out, nucleus can be improved and formed, can additionally make to form relatively orderly complex phase crystal knot between crystalline phase
Structure, and then strength character is improved, crystallization processing is carried out when temperature is 1020-1100 DEG C, it is found that crystal structure is more stable.
(3) preparation method of a kind of high-performance devitrified glass of the invention, the glass-ceramic doping granite are reduced and are made
Cost, while the intensity of glass can be improved, there is higher use value and good application prospect.
Specific implementation mode
With reference to specific embodiment, technical scheme in the embodiment of the invention is clearly and completely described, shows
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1.
A kind of preparation method of high-performance devitrified glass of the present embodiment, includes the following steps：
Step 1 weighs following corresponding weight percent raw material for standby：SiO222%, Al2O316%, MgO 8%,
Fe2O30.2%, MnO 0.2%, CaO 0.04%, ZrO20.02%, CrO 0.01%, pretreatment granite waste residues 14%,
Rich magnalium magnesia spinel 8%；
Raw material in step 1 is sent into corundum crucible by step 2 after mixing, is carried out melting, is subsequently sent to mold
Middle cast molding, then anneals, and is then cooled to room temperature again to get the high-performance crystallite glass of the present invention with 20 DEG C/min
Glass.
It is that granite waste residues are sent into jaw crushing that granite waste residues preparation method is pre-processed in the step of the present embodiment one
Machine crushes, and broken rear granite is risen to 750 DEG C with 5 DEG C/min from room temperature to be calcined, and 25min is kept the temperature at 750 DEG C, with
Postcooling is sent into mass fraction and is acidified for 40% sulfuric acid solution to room temperature, and then progress ball milling is crossed 20 mesh sieve and spent to get pretreatment
Hilllock rock waste residue.
Rich magnalium magnesia spinel grain size is 20 mesh in the step of the present embodiment one.
Content of magnesia is 25% in the step of the present embodiment one rich magnalium magnesia spinel, alumina content 45%.
The step of the present embodiment, two melting conditions was 1500 DEG C of smelting temperature, smelting time 2h.
The step of the present embodiment two, first cools the temperature to 950 DEG C before annealing with 2 DEG C/min, then carries out heat preservation 35min.
The temperature of the present embodiment carries out crystallization processing before being down to 950 DEG C.
The crystallization treatment temperature of the present embodiment is 1020 DEG C, processing time 35min.
The step of the present embodiment, two annealing conditions were to be placed in 550 DEG C of annealing furnaces to anneal.
Embodiment 2.
A kind of preparation method of high-performance devitrified glass of the present embodiment, includes the following steps：
Step 1 weighs following corresponding weight percent raw material for standby：SiO228%, Al2O320%, MgO 14%,
Fe2O30.8%, MnO 0.6%, CaO 0.08%, ZrO20.06%, CrO 0.03%, pretreatment granite waste residues 18%,
Rich magnalium magnesia spinel 12%；
Raw material in step 1 is sent into corundum crucible by step 2 after mixing, is carried out melting, is subsequently sent to mold
Middle cast molding, then anneals, and is then cooled to room temperature again to get the high-performance crystallite glass of the present invention with 30 DEG C/min
Glass.
It is that granite waste residues are sent into jaw crushing that granite waste residues preparation method is pre-processed in the step of the present embodiment one
Machine crushes, and broken rear granite is risen to 750 DEG C with 5 DEG C/min from room temperature to be calcined, and 35min is kept the temperature at 750 DEG C, with
Postcooling is sent into mass fraction and is acidified for 60% sulfuric acid solution to room temperature, and then progress ball milling is crossed 20 mesh sieve and spent to get pretreatment
Hilllock rock waste residue.
Rich magnalium magnesia spinel grain size is 100 mesh in the step of the present embodiment one.
Content of magnesia is 35% in the step of the present embodiment one rich magnalium magnesia spinel, alumina content 55%.
The step of the present embodiment, two melting conditions was 1500 DEG C of smelting temperature, smelting time 2h.
The step of the present embodiment two, first cools the temperature to 950 DEG C before annealing with 4 DEG C/min, then carries out heat preservation 35min.
The temperature of the present embodiment carries out crystallization processing before being down to 950 DEG C.
The crystallization treatment temperature of the present embodiment is 1100 DEG C, processing time 45min.
The step of the present embodiment, two annealing conditions were to be placed in 650 DEG C of annealing furnaces to anneal.
Embodiment 3.
A kind of preparation method of high-performance devitrified glass of the present embodiment, includes the following steps：
Step 1 weighs following corresponding weight percent raw material for standby：SiO225%, Al2O318%, MgO 11%,
Fe2O30.5%, MnO 0.4%, CaO 0.06%, ZrO20.04%, CrO 0.02%, pretreatment granite waste residues 16%,
Rich magnalium magnesia spinel 10%；
Raw material in step 1 is sent into corundum crucible by step 2 after mixing, is carried out melting, is subsequently sent to mold
Middle cast molding, then anneals, and is then cooled to room temperature again to get the high-performance crystallite glass of the present invention with 25 DEG C/min
Glass.
It is that granite waste residues are sent into jaw crushing that granite waste residues preparation method is pre-processed in the step of the present embodiment one
Machine crushes, and broken rear granite is risen to 750 DEG C with 5 DEG C/min from room temperature to be calcined, and 30min is kept the temperature at 750 DEG C, with
Postcooling is sent into mass fraction and is acidified for 50% sulfuric acid solution to room temperature, and then progress ball milling is crossed 20 mesh sieve and spent to get pretreatment
Hilllock rock waste residue.
Rich magnalium magnesia spinel grain size is 60 mesh in the step of the present embodiment one.
Content of magnesia is 30% in the step of the present embodiment one rich magnalium magnesia spinel, alumina content 50%.
The step of the present embodiment, two melting conditions was 1500 DEG C of smelting temperature, smelting time 2h.
The step of the present embodiment two, first cools the temperature to 950 DEG C before annealing with 3 DEG C/min, then carries out heat preservation 35min.
The temperature of the present embodiment carries out crystallization processing before being down to 950 DEG C.
The crystallization treatment temperature of the present embodiment is 1060 DEG C, processing time 40min.
The step of the present embodiment, two annealing conditions were to be placed in 600 DEG C of annealing furnaces to anneal.
Embodiment 4.
A kind of preparation method of high-performance devitrified glass of the present embodiment, includes the following steps：
Step 1 weighs following corresponding weight percent raw material for standby：SiO220%, Al2O314%, MgO 6%,
Fe2O30.1%, MnO 0.1%, CaO 0.02%, ZrO20.01%, CrO 0.005%, pretreatment granite waste residues 12%,
Rich magnalium magnesia spinel 6%；
Raw material in step 1 is sent into corundum crucible by step 2 after mixing, is carried out melting, is subsequently sent to mold
Middle cast molding, then anneals, and is then cooled to room temperature again to get the high-performance crystallite glass of the present invention with 15 DEG C/min
Glass.
It is that granite waste residues are sent into jaw crushing that granite waste residues preparation method is pre-processed in the step of the present embodiment one
Machine crushes, and broken rear granite is risen to 750 DEG C with 5 DEG C/min from room temperature to be calcined, and 20min is kept the temperature at 750 DEG C, with
Postcooling is sent into mass fraction and is acidified for 35% sulfuric acid solution to room temperature, and then progress ball milling is crossed 20 mesh sieve and spent to get pretreatment
Hilllock rock waste residue.
Rich magnalium magnesia spinel grain size is 10 mesh in the step of the present embodiment one.
Content of magnesia is 20% in the step of the present embodiment one rich magnalium magnesia spinel, alumina content 40%.
The step of the present embodiment, two melting conditions was 1500 DEG C of smelting temperature, smelting time 2h.
The step of the present embodiment two, first cools the temperature to 950 DEG C before annealing with 1 DEG C/min, then carries out heat preservation 35min.
The temperature of the present embodiment carries out crystallization processing before being down to 950 DEG C.
The crystallization treatment temperature of the present embodiment is 1000 DEG C, processing time 30min.
The step of the present embodiment, two annealing conditions were to be placed in 500 DEG C of annealing furnaces to anneal.
Embodiment 5.
A kind of preparation method of high-performance devitrified glass of the present embodiment, includes the following steps：
Step 1 weighs following corresponding weight percent raw material for standby：SiO230%, Al2O322%, MgO 16%,
Fe2O31%, MnO 0.8%, CaO 0.10%, ZrO20.08%, CrO 0.04%, pretreatment granite waste residues 20%, richness
Magnalium magnesia spinel 14%；
Raw material in step 1 is sent into corundum crucible by step 2 after mixing, is carried out melting, is subsequently sent to mold
Middle cast molding, then anneals, and is then cooled to room temperature again to get the high-performance crystallite of the present invention with 20-30 DEG C/min
Glass.
It is that granite waste residues are sent into jaw crushing that granite waste residues preparation method is pre-processed in the step of the present embodiment one
Machine crushes, and broken rear granite is risen to 750 DEG C with 5 DEG C/min from room temperature to be calcined, and 25- is kept the temperature at 750 DEG C
35min is then cooled to room temperature, is sent into mass fraction and is acidified for 40-60% sulfuric acid solutions, then carries out ball milling and crosses 20 mesh sieve,
Up to pretreatment granite waste residues.
Rich magnalium magnesia spinel grain size is 60 mesh in the step of the present embodiment one.
Content of magnesia is 40% in the step of the present embodiment one rich magnalium magnesia spinel, alumina content 60%.
The step of the present embodiment, two melting conditions was 1500 DEG C of smelting temperature, smelting time 2h.
The step of the present embodiment two, first cools the temperature to 950 DEG C before annealing with 6 DEG C/min, then carries out heat preservation 35min.
The temperature of the present embodiment carries out crystallization processing before being down to 950 DEG C.
The crystallization treatment temperature of the present embodiment is 1150 DEG C, processing time 50min.
The step of the present embodiment, two annealing conditions were to be placed in 700 DEG C of annealing furnaces to anneal.
Comparative example 1.
It is essentially identical with the material and preparation process of embodiment 3, it has only the difference is that not adding pretreatment granite waste residues.
Comparative example 2.
It is essentially identical with the material and preparation process of embodiment 3, it has only the difference is that not adding rich magnalium magnesia spinel.
Comparative example 3.
It is essentially identical with the material and preparation process of embodiment 3, have only unlike magnesia in rich magnalium magnesia spinel
Content is 25%, alumina content 45%.
Comparative example 4.
It is essentially identical with the material and preparation process of embodiment 3, have only unlike magnesia in rich magnalium magnesia spinel
Content is 35%, alumina content 55%.
Devitrified glass prepared by embodiment 3 and comparative example 1-4 is tested to obtain the performance test results as follows
| Compression strength (MPa) | Flexural strength (MPa) | |
| Embodiment 3 | 627 | 125 |
| Comparative example 1 | 623 | 121 |
| Comparative example 2 | 621 | 120 |
| Comparative example 3 | 624 | 122 |
| Comparative example 4 | 625 | 223 |
The present invention passes through a large amount of experimental demonstration, a kind of preparation method of high-performance devitrified glass, the glass-ceramic doping
Granite reduces cost of manufacture, while can improve the intensity of glass, before having higher use value and good application
Scape.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (9)
1. a kind of preparation method of high-performance devitrified glass, which is characterized in that include the following steps：
Step 1 weighs following corresponding weight percent raw material for standby：SiO222-28%, Al2O316-20%, MgO 8-
14%, Fe2O30.2-0.8%, MnO 0.2-0.6%, CaO 0.04-0.08%, ZrO20.02-0.06%, CrO 0.01-
0.03%, pretreatment granite waste residues 14-18%, rich magnalium magnesia spinel 8-12%；
Raw material in step 1 is sent into corundum crucible by step 2 after mixing, is carried out melting, is subsequently sent to pour in mold
Type casting moulding is then annealed, and is then cooled to room temperature again to get the high-performance devitrified glass of the present invention with 20-30 DEG C/min.
2. a kind of preparation method of high-performance devitrified glass according to claim 1, which is characterized in that in the step 1
Pretreatment granite waste residues preparation method is to crush granite waste residues feeding jaw crusher, will it is broken after granite with
5 DEG C/min rises to 750 DEG C from room temperature and is calcined, and 25-35min is kept the temperature at 750 DEG C, is then cooled to room temperature, is sent into quality point
Number is that 40-60% sulfuric acid solutions are acidified, and then carries out ball milling and crosses 20 mesh sieve to get pretreatment granite waste residues.
3. a kind of preparation method of high-performance devitrified glass according to claim 1, which is characterized in that in the step 1
Rich magnalium magnesia spinel grain size is 20-100 mesh.
4. a kind of preparation method of high-performance devitrified glass according to claim 1, which is characterized in that the step 1 is rich
Content of magnesia is 25-35%, alumina content 45-55% in magnalium magnesia spinel.
5. a kind of preparation method of high-performance devitrified glass according to claim 1, which is characterized in that the step 2 is molten
Refining condition is 1500 DEG C of smelting temperature, smelting time 2h.
6. a kind of preparation method of high-performance devitrified glass according to claim 1, which is characterized in that the step 2 is moved back
950 DEG C first are cooled the temperature to 2-4 DEG C/min before fire, then carries out heat preservation 35min.
7. a kind of preparation method of high-performance devitrified glass according to claim 6, which is characterized in that the temperature is down to
Crystallization processing is carried out before 950 DEG C.
8. a kind of preparation method of high-performance devitrified glass according to claim 7, which is characterized in that the crystallization processing
Temperature is 1020-1100 DEG C, processing time 35-45min.
9. a kind of preparation method of high-performance devitrified glass according to claim 1, which is characterized in that the step 2 is moved back
Fiery condition is to be placed in 550-650 DEG C of annealing furnace to anneal.
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| CN201810471131.6A CN108585511A (en) | 2018-05-17 | 2018-05-17 | A kind of preparation method of high-performance devitrified glass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111439755A (en) * | 2020-04-17 | 2020-07-24 | 中南林业科技大学 | Amorphous igneous rock and preparation method thereof |
| CN111847871A (en) * | 2019-04-30 | 2020-10-30 | 桂林理工大学 | Method for preparing high-physical-property glass by using dilong granite as auxiliary agent |
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| CN103771712A (en) * | 2013-12-27 | 2014-05-07 | 河北省沙河玻璃技术研究院 | Process for preparing glass ceramics from granite tailings by float process and special tin bath for same |
| CN104140209A (en) * | 2014-07-29 | 2014-11-12 | 青岛祥海电子有限公司 | Solid waste reuse type glass ceramic |
| CN104140212A (en) * | 2014-07-30 | 2014-11-12 | 青岛祥海电子有限公司 | Environment-friendly glass ceramic utilizing waste materials |
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| CN102603326A (en) * | 2012-03-21 | 2012-07-25 | 长兴云峰炉料有限公司 | Microcrystalline glass composite ceramic Al2O3-SiC-C-based castable |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111847871A (en) * | 2019-04-30 | 2020-10-30 | 桂林理工大学 | Method for preparing high-physical-property glass by using dilong granite as auxiliary agent |
| CN111439755A (en) * | 2020-04-17 | 2020-07-24 | 中南林业科技大学 | Amorphous igneous rock and preparation method thereof |
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