CN113493294B - High-lithium microcrystalline glass production system and production method thereof - Google Patents
High-lithium microcrystalline glass production system and production method thereof Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 157
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 61
- 238000002844 melting Methods 0.000 claims abstract description 136
- 230000008018 melting Effects 0.000 claims abstract description 136
- 239000011449 brick Substances 0.000 claims abstract description 112
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 84
- 239000000463 material Substances 0.000 claims abstract description 61
- 239000006060 molten glass Substances 0.000 claims abstract description 57
- 239000007788 liquid Substances 0.000 claims abstract description 53
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 41
- 238000005352 clarification Methods 0.000 claims abstract description 24
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 18
- 239000010703 silicon Substances 0.000 claims abstract description 18
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000006123 lithium glass Substances 0.000 claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 9
- 230000006872 improvement Effects 0.000 claims abstract description 4
- 239000004411 aluminium Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 30
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 27
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 230000004927 fusion Effects 0.000 claims description 17
- 229910052593 corundum Inorganic materials 0.000 claims description 13
- 239000010431 corundum Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004020 conductor Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 6
- 239000000156 glass melt Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 4
- 230000005855 radiation Effects 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000007500 overflow downdraw method Methods 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 239000002241 glass-ceramic Substances 0.000 claims 21
- 210000004127 vitreous body Anatomy 0.000 claims 2
- 238000006124 Pilkington process Methods 0.000 claims 1
- 230000003628 erosive effect Effects 0.000 abstract description 24
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 22
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000010309 melting process Methods 0.000 abstract description 3
- 238000007493 shaping process Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 description 28
- 238000005260 corrosion Methods 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000011734 sodium Substances 0.000 description 11
- 239000011819 refractory material Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229910018068 Li 2 O Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 229910010199 LiAl Inorganic materials 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000003280 down draw process Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000007496 glass forming Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910003250 Na–Li Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 description 1
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- WVMPCBWWBLZKPD-UHFFFAOYSA-N dilithium oxido-[oxido(oxo)silyl]oxy-oxosilane Chemical compound [Li+].[Li+].[O-][Si](=O)O[Si]([O-])=O WVMPCBWWBLZKPD-UHFFFAOYSA-N 0.000 description 1
- 229910000174 eucryptite Inorganic materials 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 229910052670 petalite Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910000500 β-quartz Inorganic materials 0.000 description 1
- 229910052644 β-spodumene Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C03B5/027—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating by passing an electric current between electrodes immersed in the glass bath, i.e. by direct resistance heating
-
- 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
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/18—Stirring devices; Homogenisation
-
- 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
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/225—Refining
-
- 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
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/235—Heating the glass
-
- 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
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
- C03B5/42—Details of construction of furnace walls, e.g. to prevent corrosion; Use of materials for furnace walls
- C03B5/43—Use of materials for furnace walls, e.g. fire-bricks
-
- 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
Abstract
The invention provides a production system and a production method of high-lithium glass ceramics, wherein the production method of the high-lithium glass ceramics comprises a melting step and a step of forming molten glass, and the melting step comprises the following steps: adopt electric melting furnace or electric mixing melting furnace to carry out preliminary melting, along with the improvement of glass liquid temperature, treat that the glass liquid temperature improves to the temperature that glass melting viscosity corresponds, make the glass liquid flow to the platinum clarification tank in, further heat the glass liquid in the platinum clarification tank, heat the glass liquid to the temperature that glass clarification viscosity corresponds, then the glass liquid flows the agitating unit stirring, and molten glass is by shaping behind the stirring, refractory brick material in electric melting furnace or the electric mixing melting furnace is including the refractory brick material that contains one kind or several kinds of elements in zirconium, aluminium or the silicon. The production method and the production system of the high-lithium microcrystalline glass provided by the invention can solve the problem of erosion of the lithium-containing glass to the brick material in the melting process, prolong the service life of the kiln, reduce the impurity of the brick material from entering the glass, and improve the quality of the glass.
Description
Technical Field
The invention relates to a high-lithium microcrystalline glass production system and a production method thereof, belonging to the field of glass production.
Background
In the glass production process flow, glass needs to be melted, clarified and stirred, and then is conveyed to glass forming equipment for forming, wherein the glass is melted by a glass kiln, a furnace body part in contact with molten glass in the glass kiln needs to be made of high-temperature resistant materials, and the high-temperature resistant materials are corroded frequently due to the severe working environment.
The high-lithium microcrystalline glass has excellent secondary strengthening performance, can realize Na-Li and K-Li exchange, realize deep compressive stress and obtain higher strength than basic glass. However, the corrosion of the glass added with lithium to the high-temperature resistant materials is more serious, and the normal production is often influenced, on the other hand, elements in the high-temperature resistant bricks are melted into the glass liquid to cause the pollution of the glass liquid, and the corrosion bubbles and stones are generated when the corrosion substances enter the glass to cause the influence on the quality of the glass, so that the yield of the produced glass is reduced.
Disclosure of Invention
The invention aims to provide a production process and a production system for prolonging the service life of a refractory material in a melting furnace and improving the quality of glass.
A production method of high-lithium glass ceramics comprises a melting step and a forming step of molten glass, and is characterized in that the melting step comprises the following steps: adopt electric melting furnace or electric mixed melting furnace to carry out preliminary melting, along with the improvement of glass liquid temperature, treat that glass liquid temperature improves to the temperature (T) that glass melting viscosity corresponds Fusion furnace ) Flowing the glass liquid into a platinum clarifying tank, further heating the glass liquid in the platinum clarifying tank, and heating the glass liquid to a temperature (T) corresponding to the clarifying viscosity of the glass Clarifying ) Then the molten glass flows to a stirring device for stirring, the molten glass is uniformly stirred and then formed, and the refractory brick material in the electric melting furnace or the electric mixing melting furnace comprises refractory brick material containing one or more elements of zirconium, aluminum or silicon.
Further, the molten glass is formed by float molding, horizontal drawing molding, overflow down-drawing molding or roll molding.
Further, the glass melt viscosity is LogP =2.4-2.6, preferably, the glass melt viscosity is LogP =2.5; the glass fining viscosity is LogP =1.6-1.8, preferably, the glass fining viscosity is LogP =1.7.
Further, in the high-lithium microcrystalline glass, calculated by mol percent, li 2 O content of 10% or more, preferably, li 2 O content of 12% or more, most preferably, li 2 The content of O is more than 15 percent.
Further, the Li in the high-lithium microcrystalline glass is controlled by calculating the mol percentage 2 O+Na 2 O+K 2 The content of O is in the range of 10 to 35%, and Li is more preferable 2 O+Na 2 O+K 2 The content of O is in the range of 15-25%, li being most preferable 2 O+Na 2 O+K 2 The content of O is in the range of 18-22%.
Further, the glass melting viscosity is LogP =2.4-2.6, corresponding to the temperature T Fusion furnace 1400 ℃ or less, more preferably, the corresponding temperature T Fusion furnace 1350 ℃ or less, most preferably the corresponding temperature T Fusion furnace ≤1300℃。
Further, the clarifying viscosity of the glass is LogP =1.6-1.8, and the corresponding temperature is not less than 1450 ℃ and not more than T Clarifying 1620 ℃, more preferably, the corresponding temperature is 1500 ℃ ≦ T Clarifying 1600 ℃ or less, most preferably, the corresponding temperature is 1520 ℃ or less T Clarifying ≤1580℃。
Further, Δ T = T Clarifying -T Fusion furnace The delta T is more preferably more than or equal to 200 ℃ and less than or equal to 300 ℃, and more preferably more than or equal to 200 ℃ and less than or equal to 280 ℃. Most preferably, Δ T is 200 ℃ or more and 250 ℃ or less.
Furthermore, the refractory brick material in direct contact with the molten glass in the electric melting furnace or the electric mixing melting furnace is zirconia corundum, 95 zirconium brick, quartz brick, 41 zirconium brick or corundum brick.
The utility model provides a high lithium microcrystalline glass production system that is used for above-mentioned high lithium microcrystalline glass's production method, production facility system includes electric melting furnace or electric mixing melting furnace, platinum depositing reservoir, agitating unit and forming device, refractory brick material in electric melting furnace or the electric mixing melting furnace includes the refractory brick material that contains one kind or several kinds of elements in zirconium, aluminium or the silicon, sets up at glass liquid level height 1/2 to 3/4 department at least one thermocouple, the thermocouple stretches out the refractory brick material of electric melting furnace or electric mixing melting furnace lateral wall to carry out strict control to the glass liquid temperature that contacts refractory brick material, platinum depositing reservoir has heating system and carries out further heating to the glass liquid. Preferably, the heating may be done electrically with platinum as a conductor or by radiation. The thermocouple extends out of the refractory brick material of the side wall of the electric melting furnace or the electric mixing furnace, preferably the thermocouple extends out of the refractory brick material of the side wall of the electric melting furnace or the electric mixing furnace by 0.5-5mm.
Further, the forming device includes a molten metal bath, an overflow draw down tank, or a pair of rolls.
Furthermore, the refractory brick material in the electric melting furnace or the electric mixing melting furnace is zirconia corundum, 95 zirconium brick, quartz brick, 41 zirconium brick or corundum brick.
Wherein, the zirconia corundum refers to a refractory material mainly comprising zirconium dioxide and aluminum trioxide; the 95 zirconium brick is a refractory material with zirconium dioxide content of about 95 percent; the quartz brick is a refractory material mainly composed of silicon dioxide; the 41 zirconium brick is a refractory material with zirconium dioxide content of about 41 percent; corundum bricks refer to refractory materials mainly composed of aluminum trioxide.
Further, a thermocouple is also arranged at the refractory brick material at the bottom of the electric melting furnace or the electric mixing melting furnace.
The production method and the production system of the high-lithium microcrystalline glass provided by the invention can solve the problem of erosion of the lithium-containing glass to the brick material in the melting process, prolong the service life of the kiln, reduce the impurity of the brick material from entering the glass, and improve the quality of the glass.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic view of a glass production process using an electric melting furnace;
FIG. 2 is a schematic view of a process for producing glass using an electric hybrid melting furnace;
FIG. 3 is a corrosion graph after the corrosion test of examples 1 and 5;
FIG. 4 is a corrosion graph after corrosion experiments of comparative examples 1 and 2;
FIG. 5 is a graph showing the corrosion of the firebrick in the case of comparative example 2 after six months.
Reference numerals are as follows: 1-1 electric melting furnace; 1-2 electric mixing melting furnace; 2, a platinum clarification tank; 3, a stirring device; 4, electrodes; and 5, burning the gun.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a production method of high-lithium microcrystalline glass, which is characterized in that molten glass is formed, and the melting step comprises the following steps: adopt electric melting furnace or electric mixed melting furnace to carry out preliminary melting, along with the improvement of glass liquid temperature, treat that glass liquid temperature improves to the temperature (T) that glass melting viscosity corresponds Melting ) The molten glass is flowed into a platinum clarifier, the molten glass is further heated in the platinum clarifier, and the molten glass is heated to a temperature (T) corresponding to the clarifying viscosity of the glass Clarifying the grain ) Then the molten glass flows to a stirring device to be stirred, the molten glass is stirred uniformly and then is formed, the glass forming can adopt float forming, horizontal drawing forming, overflow down-drawing forming or rolling forming, and the refractory brick material in the electric melting furnace or the electric mixing melting furnace is the refractory brick material containing one or more elements of zirconium, aluminum or silicon. When the electric melting furnace or the electric mixing melting furnace is used for preliminary melting, electric energy is used as a heating source, or the electric energy and combustible gas are used as the heating source. The glass raw materials put into the melting furnace are heated by adopting a heat source in the melting furnace, and the heating efficiency of the glass liquid is different according to different heating powers arranged in the furnace. Side wall and bottom of electric melting furnace or electric mixing melting furnaceSince it is required to contact molten glass at a high temperature, refractory bricks which are inevitably eroded by the molten glass and require regular maintenance are used. When the traditional amorphous glass is prepared, the corresponding temperature of the traditional amorphous glass under a certain viscosity is relatively low, and no crystal is precipitated, so that the service life of the general refractory brick material is acceptable. However, when high-lithium glass ceramics are processed, the glass needs to contain a large amount of lithium element so as to form crystals containing Li such as beta quartz and solid solution, beta spodumene and solid solution, eucryptite, petalite, lithium disilicate and lithium silicate in the subsequent forming process of the glass, and further improve the performance of the glass. However, when melting these high-lithium glasses, it has been unexpectedly found that the service life of the refractory brick is greatly shortened, and after a period of use, kiln leakage, i.e., the situation that the kiln is eroded and penetrated to cause leakage, is found. At this time, the furnace needs to be disassembled, and the loss is extremely large. The inventors have made extensive analyses, and have found that the erosion of the refractory bricks by molten glass is increased due to the high melting temperature, generally 1450 ℃ or higher, in melting high-lithium glass, and that a large amount of Li is formed on the surface of the refractory bricks by analyzing the surface components of the eroded refractory bricks 2 SiO 3 And LiAl (SiO) 3 ) 2 The formation of these salts causes the silicon and aluminum networks in the refractory bricks to be destroyed, and accelerates the erosion rate of the refractory bricks. The inventors have found that in melting high lithium glass, the higher the heating temperature, the higher the lithium content, and the more severe the corrosion condition is under high temperature conditions. The inventor probably analyzes that the corrosion of the common brick is caused by eutectic reaction between alkali metal in molten glass and silicon, aluminum and the like in the brick, and lithium has smaller molecules than sodium, more active properties, higher diffusion speed in the molten glass and more violent chemical reaction. Therefore, it is necessary to suppress the formation of undesirable salts, which are salts formed by chemical reaction of lithium ions in the melt with the components in the firebrick material, and the formation of these salts requires the components in the firebrick material to participate in the reaction, thereby destroying the structure of the firebrick material and destroying the firebrick material. The high amount of lithium in the glass melt may be associated with refractory brickThe large amount of silicon, aluminum and other elements contained in the catalyst usually react, including but not limited to the following reaction:
Li 2 O+SiO 2 ＝Li 2 SiO 3 reaction formula (1)
1/2Li 2 O+1/2Al 2 O 3 +2SiO 2 ＝LiAl(SiO 3 ) 2 Reaction type (2)
The reaction speed and the reaction degree of the reaction formulas (1) and (2) have great relationship with the temperature and the lithium content in the molten glass, the higher the temperature and the lithium content are, the faster the reaction speed is, the more serious the reaction degree is, and the corrosion speed of the refractory brick becomes fast and serious, and the period required to be replaced becomes short. Although lithium also reacts with silicon and aluminum in molten glass, under high temperature conditions, silicate formed in the molten glass is in an unstable state and is dissolved into the molten glass again immediately after the formation, and lithium reacts with silicon and aluminum elements in refractory bricks to destroy silicon and aluminum networks in the refractory bricks, so that the refractory bricks are corroded, and silicate and other undesirable salts are formed by the reaction with the refractory bricks. In severe cases, the service life of the glass production line can be greatly shortened, and the yield, the quality and the energy consumption of the glass are influenced.
Through the control of suitable heating efficiency in electric melting furnace or electric mixing melting furnace for the glass liquid is not heated to directly can carry out the temperature of clarifying in electric melting furnace or electric mixing melting furnace, and then adopts and further heats after the glass liquid enters into platinum clarification tank, and heats the glass liquid to clarification temperature. Can effectively avoid or furthest lighten the erosion of the glass liquid to the refractory brick. Among the prior art, generally the heating to the glass liquid is accomplished in the melting furnace, and the effect of depositing reservoir is just to clarify the glass liquid, and this application adopts the platinum depositing reservoir, and the platinum depositing reservoir has heating device, can further heat the glass liquid as required. At the moment, because the side wall and the bottom in the clarification tank, which are in contact with the molten glass, are made of platinum materials, the corrosion phenomenon caused by high temperature and lithium can be avoided, and the quality of the molten glass can be further ensured.
Preferably, the glass melt viscosity is LogP =2.4-2.6, and when the glass liquid is heated in the electric melting furnace or the electric mixing furnace, the temperature of the glass liquid flowing into the platinum fining pool along the platinum channel after being melted in the electric melting furnace or the electric mixing furnace is different due to the difference in heating efficiency, and in order to reduce the erosion speed of the refractory brick material as much as possible and not to damage the fluidity of the glass liquid so as to ensure the coordination of the whole glass preparation process and the production efficiency, the glass liquid is heated to the temperature corresponding to the LogP =2.4-2.6 by controlling the heating efficiency in the electric melting furnace or the electric mixing furnace, and then flows into the platinum pool along the platinum channel, and most preferably, the glass liquid is heated to the temperature corresponding to the LogP =2.5 and then flows into the platinum pool along the platinum channel. Therefore, on one hand, the erosion speed of the refractory bricks is reduced as much as possible, on the other hand, the fluidity of the molten glass can be relatively better, otherwise, the heating temperature is too low, and the fluidity of the molten glass is poor, so that the production efficiency is greatly influenced.
Preferably, the glass fining viscosity is LogP =1.6-1.8. The selection of the corresponding glass clarifying viscosity during the clarification of the molten glass needs to consider the activity degree of the molten glass on one hand and also needs to consider the bearing capacity and the energy-saving requirement of heating equipment on the other hand, the invention preferably adopts LogP =1.6-1.8, more preferably adopts LogP =1.7 as the glass clarifying viscosity, can better clarify the molten glass, does not waste energy, and is relatively friendly to the bearing capacity of the equipment.
Further, in the high-lithium microcrystalline glass, calculated by mol percent, li 2 The content of O is more than 10 percent. Li in molten glass 2 When the content of O is low, the refractory bricks are completely heated in the melting furnace, and the erosion speed of the refractory bricks is relatively controllable. But Li in the melted glass 2 When the content of O is higher, the refractory bricks are completely heated in the melting furnace, the erosion speed of the refractory bricks is obviously accelerated, the erosion degree is obviously deepened, the higher the content of lithium is, the higher the erosion speed is due to the superposition of the factors, and the production system and the production method can bear the melting of the glass with high content of lithium, and reduce the meltingThe production system is affected by severe corrosion caused by low lithium content, preferably Li in the melted glass 2 The content of O is 10% or more, more preferably 12% or more, and most preferably 15% or more.
Further, the Li in the high-lithium microcrystalline glass is controlled by calculating the mol percentage 2 O+Na 2 O+K 2 The content of O is in the range of 10-35%. Similarly, the chemical properties of the sodium element and the potassium element are similar to those of the lithium element, but the sodium element and the potassium element are far less active than the lithium element, and can cause chemical reaction with aluminum and silicon in the refractory brick material under certain conditions. Preferably, the production method of the present invention is directed to Li in the molten glass 2 O+Na 2 O+K 2 O is also preferably restricted, preferably suitable for Li 2 O+Na 2 O+K 2 The high-lithium microcrystalline glass with the O content in the range of 10-35 percent is processed by the method. More preferably Li 2 O+Na 2 O+K 2 The content of O is in the range of 15-25%, li being most preferable 2 O+Na 2 O+K 2 The content of O is in the range of 18-22%.
Further, the glass melting viscosity is the temperature T corresponding to LogP =2.4-2.6 Fusion furnace At most 1400 ℃; more preferably, the corresponding temperature T Fusion furnace 1350 ℃ or less, most preferably the corresponding temperature T Fusion furnace Not more than 1300 ℃; the clarifying viscosity of the glass is LogP =1.6-1.8, and the corresponding temperature is not less than 1450 ℃ and not more than T Clarifying Not more than 1620 ℃; more preferably, the corresponding temperature is 1500 ℃ T ≦ T Clarifying 1600 ℃ or less, most preferably, the corresponding temperature is 1520 ℃ or less T Clarifying Less than or equal to 1580 ℃. The temperature corresponding to the glass melting viscosity and the glass clarifying viscosity is determined by the inherent components of the glass, in the invention, when the glass melting viscosity and the corresponding temperature condition are selected, the erosion speed and the erosion degree of refractory brick materials are mainly considered, on the basis, the problems of the fluidity of the glass liquid, the performance requirement of the produced glass and the production efficiency are comprehensively considered, the melting viscosity and the corresponding temperature, the clarifying viscosity and the corresponding temperature are comprehensively determined, and the temperature T corresponding to the control of the glass melting viscosity to LogP =2.4-2.6 Fusion furnace At most 1400 ℃; more preferably, correspond toTemperature T of Fusion furnace 1350 ℃ or less, most preferably the corresponding temperature T Fusion furnace When the temperature is less than or equal to 1300 ℃, the erosion speed and the erosion degree of the refractory brick material are completely controllable, the fluidity of the glass liquid is good, and the clarifying viscosity of the glass liquid is controlled to be between 1450 ℃ and less than or equal to T corresponding to the temperature of LogP =1.6-1.8 Clarifying Not more than 1620 ℃; more preferably, the corresponding temperature is 1500 ℃ T ≦ T Clarifying 1600 ℃ or less, most preferably, the corresponding temperature is 1520 ℃ or less T Clarifying When the temperature is less than or equal to 1580 ℃, the glass liquid can be better clarified, the produced glass has good performance, no energy waste is caused, and the bearing capacity of equipment is relatively friendly.
Further, Δ T = T Clarifying -T Fusion furnace And delta T is more than or equal to 200 ℃ and less than or equal to 300 ℃. Within a certain range, the larger the difference of the delta T, the more suitable the method of the invention is for producing glass, when the delta T is too low, the platinum crucible may not need relatively large heating power, and the melting and even the clarification of the glass are basically completed in a melting furnace. At this time, the advantage of the present invention for protecting the refractory bricks of a melting furnace cannot be exerted. Namely, the molten glass is basically melted to a specified temperature or close to a specified clarification temperature in the melting furnace, the specified clarification temperature is the temperature corresponding to the glass clarification viscosity of LogP =1.6-1.8, the erosion to refractory brick materials is also reached or close to the maximum degree, and then the molten glass is sent to a platinum clarification tank for further heating, so that the significance is not great. When the range of delta T is larger, the temperature control is more favorable, and the temperature control in the melting furnace and the platinum clarifying pool is favorable. However, when the Δ T range is too large, it may cause deterioration of the fluidity of the molten glass in the melting furnace or cause the fining temperature to be too high and consume too much energy. Preferably, 200 ℃ to DELTA.T to 300 ℃. More preferably, 200 ℃ to. DELTA.T to 280 ℃. Most preferably, Δ T is 200 ℃ or more and 250 ℃ or less. Within the above range, particularly, within the preferable range, the control of the temperature is facilitated, the control of the temperature in the melting furnace and in the platinum clarification tank is facilitated, and the purpose of protecting the refractory brick of the melting furnace can be well realized.
Furthermore, the refractory brick material in direct contact with the molten glass in the electric melting furnace or the electric mixing melting furnace is zirconia corundum, 95 zirconium brick, quartz brick, 41 zirconium brick or corundum brick. These bricks contain a large amount of silicon or aluminum elements and are liable to chemically react with lithium in molten glass at high temperatures.
A high-lithium microcrystalline glass production system used for the production method of the high-lithium microcrystalline glass comprises an electric melting furnace or an electric mixing melting furnace, a platinum clarification tank, a stirring device and a forming device, wherein the forming device comprises a molten metal bath, an overflow pull-down tank or a pair of rollers, refractory bricks in the electric melting furnace or the electric mixing melting furnace comprise refractory bricks containing one or more elements of zirconium, aluminum or silicon, at least one thermocouple is arranged at the position of 1/2 to 3/4 of the height of the glass liquid level, the thermocouple slightly extends out of the refractory bricks on the side wall of the electric melting furnace or the electric mixing melting furnace so as to strictly control the temperature of glass liquid contacting the refractory bricks, and the platinum clarification tank is provided with a heating system which can further heat the glass liquid. Preferably, the heating may be by electrical heating with platinum as a conductor or by radiation.
Further, the refractory brick material in the electric melting furnace or the electric mixing melting furnace is corundum-zirconia, 95-zirconia brick, quartz brick, 41-zirconia brick or corundum brick.
Further, a thermocouple is also arranged at the refractory brick material at the bottom of the electric melting furnace or the electric mixing melting furnace.
The production method and the production system of the high-lithium microcrystalline glass provided by the invention can solve the problem of erosion of the lithium-containing glass to the brick material in the melting process, prolong the service life of the kiln, reduce the impurity of the brick material from entering the glass, and improve the quality of the glass.
Examples
According to the lithium content in the high-lithium glass of each example in table 1, the element in the glass which most affects the corrosion of the firebrick material is Li, although aluminum and silicon contained in the molten glass can also form crystals with lithium, it has been mentioned that, when melting in a high melting furnace, the silicate formed in the molten liquid is in an unstable state and is re-dissolved into the molten glass immediately after formation, and lithium reacts with the silicon and aluminum elements in the firebrick material to destroy the silicon and aluminum networks in the firebrick material, thereby causing the erosion of the firebrick material, and the bad salts such as silicate formed by the reaction with the firebrick material, and in severe cases, the service life of the glass production line can be greatly shortened, and the yield, quality and energy consumption of the glass can be affected.
According to the production method of the high-lithium microcrystalline glass provided by the invention, firstly, an electric melting furnace 1-1 (shown in figure 1) or an electric-gas mixing melting furnace 1-2 (shown in figure 2) is adopted for melting, the temperature of glass raw materials (fed from arrows in figures 1 and 2) is gradually increased to be gradually melted into molten glass as the glass raw materials are heated, and the temperature of the molten glass is increased to the temperature corresponding to the melting viscosity of the glass (specifically, see data in table 2), wherein the electric melting furnace 1-1 is heated by an electrode 4, and the electric-gas mixing melting furnace 1-2 is heated by the electrode 4 and a fuel gun 5. The glass liquid flows into a platinum clarification tank 2, the glass liquid is further heated in the platinum clarification tank 2, the heating can be conducted by taking platinum as a conductor for heating or heating in a radiation mode, the embodiment adopts a conductor energization heating mode, namely, the characteristic that the platinum is used as the conductor is utilized, the conductors are connected to two sides of the platinum clarification tank, an external power supply is used for conducting platinum conductor energization heating, the glass liquid is heated to the temperature corresponding to the clarification viscosity of the glass (specifically, see the data in the table 2), then the glass liquid flows into a stirring device 3 for stirring, and the molten glass flows onto a molten metal bath after being stirred uniformly or is formed by an overflow downward drawing method (namely, forming equipment is used for forming, not shown). The refractory brick material in the electric melting furnace or the electric mixing furnace adopted in the embodiment is 41AZS (No. 41 electric melting zirconia corundum brick) or 95 zirconium brick.
Comparative examples 1 and 2 were conducted by melting in an electric melting furnace or an electric hybrid melting furnace, and as the glass raw material was heated, the temperature of the glass raw material was gradually increased to gradually melt the glass raw material into molten glass, and the temperature of the molten glass was increased to a temperature corresponding to the clearing viscosity of the glass (see data in table 2). Wherein the glass liquid of comparative example 1 flows into a platinum clarifying tank, then the glass liquid flows into a stirring device for stirring, and the glass liquid of comparative example 2 directly flows into the stirring device for stirring. The molten glass is stirred uniformly and then flows onto a molten metal bath or is formed by an overflow downdraw method (namely, is formed by connecting forming equipment). The refractory brick material in the electric melting furnace or the electric mixing melting furnace adopted in the comparative example is 41AZS (No. 41 electric melting zirconia corundum brick) or 95 zirconium brick.
The grades of inclusion defects such as bubbles and stones in the glass of the examples and the comparative examples and the corrosion amount Gc of the refractory bricks are considered (the corrosion amount Gc is defined by the standard: JC/T806-2013 glass melting furnace refractory material static state molten glass corrosion resistance test method).
Reference standard was examined for erosion of the examples and comparative examples: the static molten glass corrosion resistance test method of the refractory material for the JC/T806-2013 glass melting furnace is characterized in that the temperature of refractory brick strips corresponding to LogP =2.5 is kept for 24h, the corrosion amount Gc of the positions of liquid level lines is observed, and the larger the Gc is, the more serious the corrosion is.
The grade standard of inclusion defects such as bubbles, stones and the like: grading the inclusions in a GB/T903-2019 colorless optical glass standard.
Table 1: components of the examples (calculated by mole percent)
Table 2: process, performance parameters, and Effect conditions of the various embodiments
Fig. 3 shows corrosion graphs after the corrosion experiments in examples 1 (left side of fig. 3) and 5 (right side of fig. 3), and it can be seen from fig. 3 that the erosion amount Gc at the liquid surface line position hardly changes. FIG. 4 shows the corrosion patterns after the corrosion experiments of comparative examples 1 (left side of FIG. 4) and 2 (right side of FIG. 4). As can be seen from fig. 4, the erosion amount Gc at the position of the liquid surface line is large, and the surface erosion is very severe. The compositions of example 1 and comparative example 1 were the same, and the material of the furnace firebrick was the same, and the compositions of example 5 and comparative example 2 were the same, and the material of the furnace firebrick was the same. However, compared with the conventional production in the prior art, the production method provided by the invention has the advantage that the erosion amount Gc of the refractory brick is greatly different. FIG. 5 shows the corrosion of the refractory bricks after disassembly and thorough erosion and leakage of the kiln after actual use for 6 months according to comparative example 2. According to the embodiment, after the kiln is actually used for 12 months, the operation of the kiln is still normal without any leakage (the kiln is generally not dismounted when being normally used, and the dismounting cost is extremely high).
It can be seen from the above examples that, as the content of lithium in the glass increases, the corrosion amount Gc of the refractory brick material generally shows a slight and slow increase trend, but the change is very insignificant, and the total corrosion amount is very small and completely controllable. In the embodiments 1 to 7, the electric melting furnace or the electric mixing melting furnace is adopted to heat the glass to the temperature corresponding to the glass melting viscosity, and then the glass liquid is further heated in the platinum clarification tank to the temperature corresponding to the glass clarification viscosity, so that the delta T is strictly controlled, the overhigh temperature in the electric melting furnace or the electric mixing melting furnace is avoided, and the corrosion to the refractory brick is further effectively avoided. While the comparative examples 1-2 adopt the conventional method of heating the refractory brick material in an electric melting furnace or an electric mixing furnace to the glass fining temperature and further fining the refractory brick material in a fining pool, the refractory brick material is obviously more seriously eroded than the refractory brick material in the examples 1-7 due to the overhigh temperature in the electric melting furnace or the electric mixing furnace, and simultaneously, partial elements of the refractory brick material are transferred into molten glass, so that the grade of inclusion defects such as bubbles, stones and the like of the molten glass can be unqualified.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (21)
1. A production method of high-lithium microcrystalline glass comprises a melting step and a forming step of molten glass, and is characterized in that the melting step comprises the following steps: by means of electric melting furnacesOr the electric mixing melting furnace carries out preliminary melting, and along with the improvement of the temperature of the glass liquid, the temperature of the glass liquid is increased to the temperature (T) corresponding to the melting viscosity of the glass Fusion furnace ) The molten glass is flowed into a platinum clarifier, the molten glass is further heated in the platinum clarifier, and the molten glass is heated to a temperature (T) corresponding to the clarifying viscosity of the glass Clarifying the grain ) Then the molten glass flows to a stirring device for stirring, the molten glass is uniformly stirred and then formed, and the refractory brick material in the electric melting furnace or the electric mixing melting furnace comprises refractory brick material containing one or more elements of zirconium, aluminum or silicon; the glass has a melt viscosity of LogP =2.4-2.6, corresponding to a temperature T Fusion furnace The clarifying viscosity of the glass is LogP =1.6-1.8, and the corresponding temperature is 1450 ℃ and T Clarifying ≤1620℃，ΔT＝T Clarifying -T Fusion furnace And the delta T is between 200 and 300 ℃.
2. The method for producing a high-lithium glass-ceramic according to claim 1, wherein the molten glass is formed by a float method, a horizontal drawing method, an overflow down-draw method or a rolling method.
3. The method for producing a high-lithium glass ceramic according to claim 1, wherein the glass melt viscosity is LogP =2.5; the glass fining viscosity is LogP =1.7.
4. The method for producing a high-lithium glass-ceramic according to claim 1, wherein Li is calculated in mol% in the high-lithium glass-ceramic 2 The content of O is more than 10 percent.
5. The production method of a high-lithium glass-ceramic according to claim 1, wherein Li is calculated in mol% in the high-lithium glass-ceramic 2 The content of O is more than 12 percent.
6. The production method of a high-lithium glass-ceramic according to claim 1, wherein Li is calculated in mol% in the high-lithium glass-ceramic 2 The content of O is more than 15 percent.
7. The production method of a high-lithium glass-ceramic according to claim 1 or 4, wherein Li is controlled in the high-lithium glass-ceramic by mol percentage calculation 2 O+Na 2 O+K 2 The content of O is in the range of 10-35%.
8. The production method of a high-lithium glass-ceramic according to claim 1 or 4, wherein Li is controlled in the high-lithium glass-ceramic by mol percentage calculation 2 O+Na 2 O+K 2 The content of O is in the range of 15-25%.
9. The production method of a high-lithium glass-ceramic according to claim 1 or 4, wherein Li is controlled in the high-lithium glass-ceramic by mol percentage calculation 2 O+Na 2 O+K 2 The content of O is in the range of 18-22%.
10. The method for producing a high-lithium glass-ceramic according to claim 1, wherein the glass has a melt viscosity of LogP =2.4-2.6 corresponding to a temperature T Fusion furnace ≤1350℃。
11. The production method of a high-lithium glass ceramic according to claim 1, wherein the glass has a melt viscosity of LogP =2.4-2.6 corresponding to a temperature T Melting ≤1300℃。
12. The method for producing a high-lithium glass ceramic according to claim 1, wherein the glass has a fining viscosity of LogP =1.6-1.8, which corresponds to a temperature of 1500 ℃. Ltoreq.T Clarifying ≤1600℃。
13. The method for producing a high-lithium glass-ceramic according to claim 1, wherein the glass has a fining viscosity of LogP =1.6-1.8, which corresponds to a temperature of 1520 ℃ Tc. Ltoreq. Tfiner. Ltoreq.1580 ℃.
14. The production method of a high-lithium glass ceramic according to claim 1, Δ T = T Clarifying -T Melting And the delta T is between 200 and 280 ℃.
15. The production method of a high-lithium glass ceramic according to claim 1, Δ T = T Clarifying -T Fusion furnace And the delta T is between 200 and 250 ℃.
16. The method for producing high-lithium glass-ceramic according to claim 1, wherein the refractory brick material in direct contact with molten glass in the electric melting furnace or the electric mixing furnace is zirconia alumina, 95 zirconia brick, quartz brick, 41 zirconia brick or corundum brick.
17. A high-lithium glass-ceramic production system for carrying out the production method of high-lithium glass-ceramic according to any one of claims 1 to 16, comprising an electric melting furnace or an electric mixing melting furnace, a platinum clarifier, a stirring device, and a forming device, characterized in that: refractory brick material in electric melting furnace or the electric mixing melting furnace is for including the refractory brick material that contains one kind or several kinds of elements in zirconium, aluminium or the silicon, sets up at least one thermocouple in glass liquid level height 1/2 to 3/4 department, the thermocouple stretches out the refractory brick material of electric melting furnace or the electric mixing melting furnace lateral wall to carry out the strict control to the vitreous humor temperature that contacts refractory brick material, platinum depositing reservoir has heating system to further heat the vitreous humor.
18. The high-lithium glass-ceramic production system according to claim 17, wherein the forming device comprises a molten metal bath, an overflow draw tank, or a pair of rollers.
19. The high-lithium glass-ceramic production system according to claim 17, wherein the refractory brick material in the electric melting furnace or the electric mixing furnace is corundum-zirconia, 95-zirconia brick, quartz brick, 41-zirconia brick or corundum brick.
20. The system for producing the high-lithium microcrystalline glass according to claim 17, wherein the platinum clarification tank is provided with a heating system which is electrified and heated by taking platinum in the platinum clarification tank as a conductor or is heated by radiation.
21. The high-lithium glass-ceramic production system according to claim 17, wherein a thermocouple is also provided at the refractory brick at the bottom of the electric melting furnace or electric hybrid melting furnace.
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