CN118324485A - Refractory material for glass kiln and preparation method and application thereof - Google Patents
Refractory material for glass kiln and preparation method and application thereof Download PDFInfo
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- 239000011819 refractory material Substances 0.000 title claims abstract description 202
- 239000011521 glass Substances 0.000 title claims abstract description 165
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 113
- 239000000843 powder Substances 0.000 claims abstract description 95
- 239000002245 particle Substances 0.000 claims abstract description 79
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 60
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000004927 clay Substances 0.000 claims abstract description 34
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 33
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910021538 borax Inorganic materials 0.000 claims abstract description 28
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 28
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 28
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 28
- 229910000505 Al2TiO5 Inorganic materials 0.000 claims abstract description 27
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 27
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 27
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 claims abstract description 27
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims description 89
- 238000001816 cooling Methods 0.000 claims description 67
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 66
- 239000000463 material Substances 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 47
- 238000003756 stirring Methods 0.000 claims description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 238000002156 mixing Methods 0.000 claims description 35
- 238000000137 annealing Methods 0.000 claims description 33
- 229910052757 nitrogen Inorganic materials 0.000 claims description 32
- 239000000377 silicon dioxide Substances 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 29
- 230000007797 corrosion Effects 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 12
- 239000006060 molten glass Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 description 39
- 238000005299 abrasion Methods 0.000 description 32
- 230000008859 change Effects 0.000 description 21
- 238000004321 preservation Methods 0.000 description 17
- 230000008569 process Effects 0.000 description 16
- 239000002994 raw material Substances 0.000 description 16
- 239000000126 substance Substances 0.000 description 16
- 230000003628 erosive effect Effects 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 238000005485 electric heating Methods 0.000 description 13
- 238000000227 grinding Methods 0.000 description 13
- 230000001965 increasing effect Effects 0.000 description 11
- 238000002844 melting Methods 0.000 description 11
- 230000008018 melting Effects 0.000 description 11
- 238000005336 cracking Methods 0.000 description 10
- 230000009286 beneficial effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000011449 brick Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 4
- 230000008646 thermal stress Effects 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
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- 238000005816 glass manufacturing process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000004901 spalling Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- -1 titanium aluminate Chemical class 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
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- 239000004568 cement Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000009187 flying Effects 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- Ceramic Products (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Furnace Housings, Linings, Walls, And Ceilings (AREA)
Abstract
The invention discloses a refractory material for a glass kiln, and a preparation method and application thereof, wherein the refractory material for the glass kiln comprises the following components in percentage by mass: 48% -52% of silica sol; 11% -15% of alumina particles; 7% -10% of flint clay powder; 5% -8% of silicon carbide; 2.3 to 2.7 percent of aluminum titanate; zirconia 5.5-6.5%; cerium oxide powder 0.8-1.2%; borax 2.8-3.2%; 1.3 to 1.7 percent of sericite powder; mullite 5.5-6.5%; 2.8 to 3.2 percent of magnesium oxide. The refractory material is suitable for glass kilns, has strong thermal shock resistance and is resistant to molten glass corrosion.
Description
Technical Field
The invention relates to a refractory material for a glass kiln, a preparation method and application thereof, and belongs to the technical field of refractory materials.
Background
Glass is mainly made of quartz sand, sodium carbonate and the like through high-temperature melting, and glass kilns are equipment for melting glass, and are various in variety, such as tank kilns, crucible kilns and the like.
The problem that exists at present is that the lining of a glass furnace is often subjected to considerable physical and chemical wear and thermal stresses, since the molten glass and glass raw materials are highly corrosive, and in a continuously molten glass furnace, corrosion is usually continued until the furnace is not in use. In this process, the refractory material of the lining may develop scratches and even cracks, which may grow until the molten glass is infiltrated, thereby affecting the service life of the refractory material.
The temperature, chemical erosion degree and speed of the kiln are closely related to the use position and the type of molten glass, and of course, the quality of a refractory lining is also important, and the service life of the kiln and the production cost of glass are greatly influenced by the refractory material for the glass kiln. The existing refractory materials used in the glass kiln have high strength and high corrosion resistance, but have poor thermal shock resistance, and small cracks can be generated due to rapid cooling or rapid heating when the temperature changes rapidly. Therefore, it is necessary to provide a refractory for a glass furnace having a good molten glass corrosion resistance and a high thermal shock resistance.
Disclosure of Invention
In view of the above, the main object of the present invention is to provide a refractory material for a glass kiln, and a preparation method and application thereof, which aims to solve the technical problems of preparing a refractory material suitable for the glass kiln by controlling the components and the proportion of the materials, and having strong thermal shock resistance and glass liquid erosion resistance.
The aim and the technical problems of the invention are realized by adopting the following technical proposal. The invention provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
48% -52% of silica sol; 11% -15% of alumina particles; 7% -10% of flint clay powder; 5% -8% of silicon carbide; 2.3 to 2.7 percent of aluminum titanate; zirconia 5.5-6.5%; cerium oxide powder 0.8-1.2%; borax 2.8-3.2%; 1.3 to 1.7 percent of sericite powder; mullite 5.5-6.5%; 2.8 to 3.2 percent of magnesium oxide.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
Preferably, the refractory for a glass kiln, wherein the mass concentration of silica in the silica sol is 40% -45%.
Preferably, the refractory for glass kiln, wherein the particle size of the flint clay powder is less than 0.3mm.
Preferably, the refractory for a glass kiln, wherein the zirconia has a particle size of 1 to 2mm.
Preferably, the refractory for a glass kiln, wherein each part of alumina particles comprises the following grain fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The aim and the technical problems of the invention are realized by adopting the following technical proposal. The invention provides a preparation method of a refractory material for a glass kiln, which comprises the following steps:
s1, 48 to 52 percent of silica sol, 11 to 15 percent of alumina particles, 7 to 10 percent of flint clay powder, 5 to 8 percent of silicon carbide, 2.3 to 2.7 percent of aluminum titanate, 5.5 to 6.5 percent of zirconia, 0.8 to 1.2 percent of cerium oxide powder, 2.8 to 3.2 percent of borax, 1.3 to 1.7 percent of sericite powder, 5.5 to 6.5 percent of mullite and 2.8 to 3.2 percent of magnesium oxide are mixed and stirred for 28 to 32 minutes, and then the mixture is obtained after standing for 3 to 4 hours;
S2, under the protection of nitrogen, heating the mixture after standing to 105-115 ℃, then preserving heat for 3.2-3.6 hours, cooling to 68-75 ℃ and carrying out casting and cooling annealing to obtain the glass kiln to enable the refractory material.
Preferably, in the method for preparing the refractory material for a glass kiln, in S1, the mixing and stirring are: and mixing and stirring the granularity materials with the granularity of more than 2mm uniformly, adding the silica sol and stirring uniformly, and finally adding the fine powder with the granularity of less than or equal to 2mm and mixing uniformly.
Preferably, in the method for preparing a refractory material for a glass kiln, in step S2, the volume percentage concentration of the nitrogen gas is 98% or more.
Preferably, in the preparation method of the refractory material for a glass kiln, in the step S2, the cooling rate of the cooling annealing is 2.8-3.3 ℃/min.
The aim of the invention and the solution of the technical problems can also be achieved by adopting the following technical measures. The invention provides a glass kiln, which comprises the refractory material.
Compared with the prior art, the refractory material for the glass kiln and the preparation method and application thereof have the following beneficial effects:
1. The refractory material is suitable for glass kilns, has strong thermal shock resistance and glass liquid corrosion resistance, and can effectively solve the technical problem that the refractory material for glass kilns in the prior art has poor thermal shock resistance;
2. The refractory material can bear extremely high temperature without melting, and for equipment which needs to run for a long time in a high temperature environment such as a glass kiln, the refractory material ensures the structural stability and the service life of a furnace body;
4. the refractory material has good heat insulation performance, and is beneficial to reducing heat loss, so that energy consumption is reduced, and cost is saved;
5. The refractory material disclosed by the invention has fewer pollutants released in the use process, is favorable for environmental protection and meets the requirement of sustainable development;
6. The refractory material has the load softening temperature of 1858-1868 ℃, the normal-temperature compressive strength of 60.5-62.4Mpa, the flexural strength after being treated for 3 hours at 1450 ℃ of 21.1-21.9Mpa, and then is quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20min, and the flexural strength is 12.1-12.4Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the heat conductivity coefficient is 0.5-0.7W/(m.times.K) measured by a steady state method; 300g of refractory material is put on a Taber abrasion tester, and the abrasion loss is 50.9-51.5g by 1000 times of rotation of an abrasive wheel, and the change of a heating permanent line (1450 ℃ multiplied by 2 h)/% is 0.10-0.11;
8. the preparation method of the refractory material has the advantages of simple production process, no need of high-temperature sintering under reaction conditions, and relatively low cost compared with the high-temperature sintering refractory material.
The foregoing description is only an overview of the present invention, and is intended to provide a more thorough understanding of the present invention, and is to be accorded the full scope of the present invention.
Detailed Description
In order to further describe the technical means and effects adopted by the invention to achieve the preset aim, the following is a detailed description of a refractory material for a glass kiln, a preparation method thereof, a specific implementation mode, a structure, characteristics and effects thereof, which are provided by the invention, and the specific implementation mode, the structure, the characteristics and the effects thereof, which are combined with the preferred embodiment. In the following description, different "an embodiment" or "an embodiment" do not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
Unless otherwise indicated, materials, reagents, and the like referred to below are commercially available products well known to those skilled in the art; unless otherwise indicated, the methods are all methods well known in the art. Unless otherwise defined, technical or scientific terms used should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The following operations or conditions of conventional experimental procedures described in the literature in this field may be performed without reference to specific experimental procedures or conditions.
Some embodiments of the invention provide a refractory material for a glass kiln, comprising the following components in percentage by mass:
48% -52% of silica sol; 11% -15% of alumina particles; 7% -10% of flint clay powder; 5% -8% of silicon carbide; 2.3 to 2.7 percent of aluminum titanate; zirconia 5.5-6.5%; cerium oxide powder 0.8-1.2%; borax 2.8-3.2%; 1.3 to 1.7 percent of sericite powder; mullite 5.5-6.5%; 2.8 to 3.2 percent of magnesium oxide.
The functions of the components are as follows:
In the technical scheme, in order to meet the high thermal shock resistance and high glass liquid erosion resistance of the refractory material for the glass kiln, the invention uses silica sol, alumina particles and flint clay powder to form a framework, and forms the refractory material by the cooperation of silicon carbide, aluminum titanate, zirconium oxide, cerium oxide powder, borax, sericite powder and magnesium oxide. By controlling the components and the proportion of the materials, the refractory material for the glass kiln has strong thermal shock resistance and glass liquid corrosion resistance. The functions and the contents of the components are selected as follows:
Silica sol: the silica sol is used as a bonding agent, so that the slag resistance of the refractory material can be obviously improved. This means that refractory materials using silica sol are better resistant to erosion in the face of high temperature slag generated during glass melting, thus maintaining structural stability and extending service life. In addition, silica sols can be used as binders for pure aluminate cements in unshaped refractories, especially in spray coatings, the setting time being adjusted by the addition of setting accelerators. The use of the binder can shorten the construction time and improve the heat strength, which is very important for glass kilns in high temperature environments. Compared with organic resin and tar binder, the silica sol can greatly reduce environmental pollution. This is particularly important for glass manufacturing today where environmental requirements are becoming more stringent. If the content is less than 48wt%, the structural strength of the refractory may be weakened due to the excessively low content, resulting in a decrease in refractoriness; the thermal shock resistance of the refractory material can be affected, so that the refractory material is more easily broken when the temperature is suddenly changed; and simultaneously, the erosion resistance of the refractory material to molten glass and alkaline flyer material can be weakened, so that the service life is shortened. If the content is higher than 52wt%, the content is too high, which may cause the internal structure of the refractory material to be too compact, affecting the function of the expansion joint, and further affecting the thermal expansion and contraction properties of the refractory material; it may also affect the crystallization transformation of the refractory during kiln and cold repair, and appropriate measures are required to accommodate these changes.
Alumina particles: alumina particles mainly play a role in improving refractoriness and softening temperature under load in a refractory material for a glass kiln. Alumina particles are an important component of high alumina refractories, which have higher refractoriness and softening temperature under load than clay refractories. In particular, the role of alumina particles in refractory materials includes: 1. enhancing fire resistance: alumina (Al 2O3) is a high refractory material that significantly increases the refractoriness of the refractory material, enabling it to maintain stability and durability in high temperature environments. This is critical for high temperature industrial equipment such as glass kilns. 2. Increasing the softening temperature under load: the alumina particles also raise the load softening temperature of the refractory material, i.e. the highest temperature at which the shape is maintained under a load. This is also important for the structural stability and the service life of the glass kiln. 3. Optimizing heat conducting capacity: compared with clay refractory, the high-alumina refractory has higher heat conduction capacity. This helps to better manage the temperature distribution within the kiln and improve energy efficiency. 4. Improving thermal shock resistance: the alumina particles also improve the thermal shock resistance of the refractory material so that it is not prone to cracking when the temperature changes sharply, which is particularly important for equipment such as glass kilns that are subject to frequent temperature changes. If the content thereof is less than 11wt%, the refractoriness of the refractory may be lowered due to the decrease in the content thereof, because the alumina content is positively correlated with the refractoriness of the refractory; and its thermal shock resistance may be reduced, which may affect the stability of the refractory material upon rapid temperature changes; and simultaneously, the erosion resistance of the refractory material to molten glass and alkaline flyer materials can be weakened, so that the service life is shortened. If the content is more than 15wt%, the cost of the refractory may be increased because alumina, an important refractory raw material, is relatively expensive; it may also result in a refractory material that is too dense in structure, affecting its function of the expansion joints and thus the thermal expansion and contraction properties of the refractory material.
Flint clay powder: flint clay plays a key role in refractory materials for glass kilns. Flint clay is a high-quality hard refractory clay, the Al 2O3 content in raw ore is about 38%, and the Al 2O3 content after calcination can be improved to about 44%. The high alumina content enables the refractory material made of flint clay to have higher refractoriness and to be capable of withstanding extremely high operating temperatures in glass kilns. Enhancement of load softening temperature: the chemical composition and structural characteristics of flint clay provide it with good stability and compressive strength at high temperatures, which is important for refractory materials to maintain shape and structure at high temperatures and under load. The refractory materials made of flint clay have a small thermal expansion coefficient and good thermal shock resistance, which means that they can maintain stability when temperature changes sharply, reducing the risk of cracking due to thermal shock. The flint clay has a low high temperature creep value, which helps the refractory maintain its shape and dimensional stability under prolonged high temperature conditions. The flint clay refractory also has good resistance to chemical acid corrosion, which is critical to resisting corrosive substances that may be generated during the glass melting process. If the content is less than 7wt%, the content is too low, which may result in insufficient refractoriness of the refractory material and inability to withstand the high temperature environment in the glass kiln; and may also affect the thermal shock stability of the refractory material, making it more prone to cracking when the temperature is suddenly changed. If the content thereof is more than 10wt%, the cost of the refractory may be unnecessarily increased.
Silicon carbide: silicon carbide is mainly used for improving heat conductivity and temperature resistance in refractory materials for glass kilns. Silicon carbide has very good thermal conductivity, which means that refractory materials containing silicon carbide can conduct heat more effectively. This is particularly important in the region of glass furnaces where rapid heat dissipation or maintenance of a uniform temperature is required. The silicon carbide refractory has high refractoriness, so that the silicon carbide refractory can maintain stability and durability under high-temperature environment. This is critical for high temperature industrial equipment such as glass kilns. When the content is lower than 5wt%, the content is too low, so that the heat conductivity coefficient of the refractory material is reduced, and the heat conductivity effect is affected; it may also reduce the performance of the refractory in these respects. When the content thereof is more than 8wt%, the cost of the refractory may be increased correspondingly; too high a silicon carbide content may also affect the structural stability of the refractory, especially under high temperature and load conditions.
Aluminum titanate: titanium aluminic materials generally have a very high degree of fire resistance, which makes them stable in the high temperature environment of the glass kiln, especially at 1600 degrees celsius operating temperature. Under high temperature and load conditions, titanium aluminic acid can provide good creep resistance, which is important for maintaining structural stability and extending service life. Various chemicals, such as alkali vapors, etc., are generated during the operation of the glass kiln. The titanium aluminate refractory is resistant to attack by these chemicals, keeping the refractory performance from being degraded. Titanium aluminic materials generally have good thermal shock stability, which means that they can withstand sharp changes in temperature without cracking, which is particularly important for glass kilns in environments where frequent temperature changes are required. If the content is less than 2.3wt%, the refractory material may have insufficient refractoriness due to the excessively low content, and cannot withstand the high-temperature environment in the glass kiln; it may also affect the thermal shock resistance of the refractory material, making it more prone to cracking when the temperature is suddenly changed. If the content is more than 2.7wt%, the cost of the refractory may be increased accordingly; too high a titanium aluminate content may affect the structural stability of the refractory, especially under high temperature and load conditions.
Zirconia: zirconia plays a main role in enhancing material performance and improving corrosion resistance in refractory materials for glass kilns. The addition of zirconia can improve the thermal shock resistance of the refractory, which is particularly important for glass furnaces that are often affected by high temperature changes. Zirconia can increase the mechanical strength of the refractory, which means that the refractory can withstand greater physical pressures, reducing the likelihood of wear and damage. By adding zirconia, the coefficient of thermal expansion of the refractory material can be effectively reduced, which helps to maintain structural stability in the event of temperature changes. Zirconia has good corrosion resistance, protects refractory materials from being corroded by acid, alkali and other oxides, and maintains durability in high-temperature environments. If the content is less than 5.5wt%, the refractoriness of the refractory material may be lowered, making it unable to withstand the high temperature environment in the glass kiln; it may also affect the thermal shock resistance of the refractory material, making it more prone to cracking when the temperature is suddenly changed. Zirconia is one of the oxides with the strongest resistance to glass attack, and too low a content may also lead to a decrease in the resistance to chemical attack of the refractory. Although the addition of 5.5 to 6.5 weight percent of zirconia can lead the mullite crystal to be small and the material tissue structure to be compact, if the content is higher than 6.5 weight percent, the structural stability of the refractory material can be affected, especially under the conditions of high temperature and load; and the cost of the refractory material may also increase accordingly.
Cerium oxide powder: the cerium oxide plays a main role in the refractory material for glass kilns in improving the performance of the refractory material, in particular to enhance the erosion resistance and improve the thermal shock stability. Cerium oxide can improve erosion resistance of refractory materials, which is critical to environments such as glass kilns where it is exposed to various chemicals at high temperatures. The addition of cerium oxide helps to improve the thermal shock stability of the refractory material, so that the structural stability can be maintained under the condition of rapid temperature change, and the cracking risk caused by temperature fluctuation is reduced. If the content is less than 0.8wt%, the refractory material may have insufficient refractoriness and cannot withstand the high-temperature environment in the glass kiln; the thermal shock resistance of the refractory material can be affected, so that the refractory material is more easily broken when the temperature is suddenly changed; cerium oxide can improve erosion resistance of refractory materials to molten glass and alkaline flyings, and the service life can be shortened when the content is lower than 0.8 wt%. If the content thereof is more than 1.2wt%, the cost of the refractory may be unnecessarily increased; it may also affect the structural stability of the refractory, especially at high temperatures and under load.
Borax: the borax has the main functions of improving the performance of the refractory material, especially enhancing the erosion resistance and improving the thermal shock stability of the refractory material for glass kilns. Borax can increase erosion resistance of refractory materials, which is important for environments such as glass kilns where various chemicals are exposed to high temperatures. The addition of borax is helpful for improving the thermal shock stability of the refractory material, so that the structural stability can be maintained under the condition of rapid temperature change, and the cracking risk caused by temperature fluctuation is reduced. If the content is less than 2.8wt%, the borax plays a role of a flux in the glass manufacturing process, and the insufficient melting of the glass may be caused by the excessively low content, thereby affecting the quality and uniformity of the glass. Borax can reduce the glass melting temperature, and if the content is insufficient, higher temperature can be needed to achieve the same melting effect, so that the energy consumption is increased; if the content is higher than 3.2wt%, the borax is corrosive, and the content is too high, so that chemical attack on the refractory material can be aggravated, and the performance of the refractory material is reduced; excessive borax may affect structural stability of the refractory material, especially under the dual effects of high temperature and chemical reaction.
Sericite powder: the sericite can keep stable physical and chemical properties in a high-temperature environment, and the melting point of the sericite is up to more than 1000 ℃, so that the sericite can still maintain the structure and performance under the high-temperature condition of a glass kiln. Since sericite has a low thermal expansion coefficient and thermal conductivity, it can effectively resist the influence of thermal shock and thermal stress, which is particularly important for glass kilns frequently affected by temperature changes. The sericite has good corrosion resistance and can resist corrosion of corrosive media such as acid and alkali, which is helpful for prolonging the service life of refractory materials and reducing maintenance cost. If the content is less than 1.3wt%, the refractory material may have insufficient refractoriness and cannot withstand the high-temperature environment in the glass kiln; the thermal shock resistance of the refractory material can be affected, so that the refractory material is more easily broken when the temperature is suddenly changed; at the same time, the service life may be shortened; if the content thereof is more than 1.7wt%, the cost of the refractory may be unnecessarily increased; and an excessive amount of sericite may affect structural stability of the refractory material, especially under high temperature and load conditions.
Mullite: the refractoriness of mullite is about 1850 ℃, which enables the mullite-containing refractory material to maintain stability at extremely high temperatures, and is particularly suitable for use in high temperature environments such as glass kilns. Mullite bricks have a higher high temperature load softening point, which means that they can withstand higher temperatures without deformation under certain loads. Mullite bricks have a dense fine grain structure which helps to reduce bubble formation in the glass liquid and is very important for ensuring glass quality. The mullite brick has good thermal shock resistance, can bear abrupt change of temperature and is not easy to break, and is an important characteristic for glass kilns which frequently experience temperature fluctuation. Mullite bricks are resistant to attack by acid slag, which is particularly important in environments where various chemicals may be exposed to during glass manufacturing. If the content is less than 5.5wt%, the refractory material may have insufficient refractoriness and cannot withstand the high-temperature environment in the glass kiln; the thermal shock resistance of the refractory material can be affected, so that the refractory material is more easily broken when the temperature is suddenly changed; at the same time, the service life may be shortened; if the content thereof is more than 6.5wt%, the cost of the refractory may be unnecessarily increased; and excessive mullite may affect the structural stability of the refractory, especially under conditions of high temperature and load.
Magnesium oxide: magnesium oxide (MgO) is an important refractory material that plays a key role in glass kiln refractories. The melting point of magnesium oxide is very high, up to 2800 ℃, which makes refractory materials containing magnesium oxide extremely refractory, typically above 2000 ℃. Such refractoriness enables the magnesia bricks to maintain stability and durability in high temperature environments such as glass kilns. The magnesium oxide can significantly improve the slag resistance of the refractory material, i.e. the erosion resistance of the high temperature slag. During the glass manufacturing process, the refractory material needs to withstand attack by various chemicals, and the addition of magnesium oxide helps to extend the useful life of the refractory material. The magnesium oxide can also improve the thermal shock stability of the refractory material, i.e. resistance to cracking caused by temperature spikes. The glass kiln can undergo frequent temperature change in the use process, and the magnesium oxide has the characteristics of helping to keep the structure of the refractory stable and reducing the damage caused by temperature fluctuation. If the content is less than 2.8wt%, the refractoriness of the refractory material may be insufficient due to the excessively low content of magnesium oxide, failing to withstand the high temperature environment in the glass kiln; the structural stability of the refractory material at high temperature may also be affected, making it more susceptible to melting and deformation; while the service life may be shortened. If the content is more than 3.2wt%, the cost of the refractory may be increased accordingly. Although magnesium oxide can improve the refractoriness and high temperature structural strength of the refractory, magnesium oxide in an amount of more than 3.2wt% may affect the structural stability of the refractory, especially under high temperature and load conditions.
Through testing, the load softening temperature of the refractory material for the glass kiln is 1858-1868 ℃, the normal-temperature compressive strength is 60.5-62.4Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours is 21.1-21.9Mpa, then the refractory material is subjected to heat preservation at 1100 ℃ for 20 minutes and then is quenched in cold water at 20 ℃, and the flexural strength is 12.1-12.4Mpa after repeated 30 times; is not corroded by glass; the heat conductivity coefficient is 0.5-0.7W/(m.times.K) measured by a steady state method; 300g of the refractory material was put on a Taber abrasion tester and rotated 1000 times to obtain an abrasion loss of 50.9 to 51.5g and a heating permanent line change (1450 ℃ C. Times.2 h)/% of 0.10 to 0.11.
In some embodiments, optionally, the silica concentration in the silica sol may be 40% to 45% by mass. If the content is less than 40%, the refractoriness of the refractory is insufficient; if the content is more than 45%, the cost becomes too high.
In some embodiments, optionally, wherein the flint clay powder has a particle size of less than 0.3mm. This is advantageous in increasing the erosion level of the refractory. If the particle size is more than 0.3mm, the erosion degree of the refractory is reduced.
In some embodiments, optionally, wherein the zirconia has a particle size of 1 to 2mm. This is chosen to increase the strength of the refractory material, either above 2mm or below 1mm may result in a decrease in strength.
In some embodiments, optionally, wherein the alumina particles comprise the following mass percent size fractions: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; alumina 10% with particle size less than 0.088 mm; this is provided to ensure that there are enough 5-3 mm particles to make the particle size distribution more uniform and thus the strength higher. In addition, the alumina particles are too large and may not be completely dissolved in the glass melt, resulting in the generation of stones and other defects.
Some embodiments of the present invention also provide a method for preparing a refractory material for a glass kiln, the method comprising the steps of:
1) Preparing materials according to mass percent;
2) Pouring all the raw materials into a stirrer to mix and stir for 28-32 minutes, and standing for 3-4 hours to obtain a mixture; if the temperature is less than 28 minutes, the mixture is not uniform, and the refractory material is segregated; if the temperature is more than 32 minutes, the material temperature is too high, and the refractory material is easy to crack. Standing for 3-4 hours to enhance the viscosity of the pug; less than 3 hours or more than 4 hours, the strength of the refractory is insufficient.
3) Heating the mixture after standing to 105-115 ℃ under the protection of nitrogen, preserving heat for 3.2-3.6 hours, cooling to 68-75 ℃ and pouring the mixture into a conventional prefabricated die; wherein the volume percentage concentration of the nitrogen is more than 98 percent; if the concentration is less than 98%, the concentration is too low, and the protection effect is poor. The heating rate is 4.8-5.2 ℃/min, and the refractory material is difficult to form and has cracks on the surface when the heating rate is higher than 5.2 ℃/min or lower than 4.8 ℃/min. Temperatures below 105 ℃ or above 115 ℃ can make the refractory less susceptible to forming and cracking on the surface. The heat preservation time is less than 3.2 hours or more than 3.6 hours, and the strength of the refractory material is insufficient. If the temperature is lower than 68 ℃ or higher than 75 ℃, the refractory material has low strength and is not easy to mold.
4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the prefabricated mold, and cooling to 67-73 ℃ to obtain the glass kiln to make the refractory material. Wherein the volume percentage concentration of the nitrogen is more than 98 percent; if the concentration is less than 98%, the concentration is too low, and the protection effect is poor. The cooling rate of the cooling annealing is set to be 2.8-3.3 ℃/min, so that cracks or spalling are not easy to occur. If the temperature is reduced to be lower than 67 ℃, the refractory material has internal cracks due to the excessively low temperature; if the temperature is reduced to be higher than 73 ℃, the annealing effect is not obvious due to the overhigh temperature, so that the strength of the refractory material is low. If the cooling rate is lower than 2.8 ℃/min or higher than 3.3 ℃/min, cracks or spalling can occur.
In other embodiments, optionally, wherein in step 2), the mixing and stirring is: and mixing and stirring the granularity materials with the granularity of more than 2mm uniformly, adding the silica sol and stirring uniformly, and finally adding the fine powder with the granularity of less than or equal to 2mm and mixing uniformly. The setting of the compounding is more even like this, and then makes refractory material can not segregation, and corrosion-resistant effectual, intensity is big.
Some embodiments of the invention also provide a glass kiln comprising the aforementioned refractory material.
The invention will be further described with reference to specific examples, which are not to be construed as limiting the scope of the invention, but rather as falling within the scope of the invention, since numerous insubstantial modifications and adaptations of the invention will now occur to those skilled in the art in light of the foregoing disclosure.
The refractories of the following examples and comparative examples were tested for their softening temperature under load by a load softening temperature tester, and for their compressive strength at room temperature by a pressure tester.
Example 1
The embodiment provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (mass concentration of silica 42%) 50%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; cerium oxide powder 1%; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1861 ℃, the normal-temperature compressive strength of 62.4Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours of 21.2Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20 minutes, and the flexural strength is 12.4Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.58W/(m.times.K) measured by a steady state method; a300 g refractory was put on a Taber abrasion tester and the abrasion loss was 51.2g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.11.
Example 2
The embodiment provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (42% mass concentration of silica) 50.2%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; 0.8% of cerium oxide powder; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the load softening temperature of the refractory material for the glass kiln is 1858 ℃, the normal-temperature compressive strength is 61.7Mpa, the flexural strength after being treated for 3 hours at 1450 ℃ is 21.3Mpa, then the refractory material is subjected to heat preservation at 1100 ℃ for 20min and then is quenched in cold water at 20 ℃, and the flexural strength is 12.1Mpa after repeated 30 times; is not corroded by glass; the thermal conductivity is 0.55W/(m.times.K) measured by a steady state method; a300 g refractory was put on a Taber abrasion tester and the abrasion loss was 51.5g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.10.
Example 3
The embodiment provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (mass concentration of silica 42%) 49.8%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; 1.2% of cerium oxide powder; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1868 ℃, the normal-temperature compressive strength of 60.5Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours of 21.2Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20 minutes, and the flexural strength is 12.4Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.62W/(m.times.K) measured by a steady state method; a300 g refractory was put on a Taber abrasion tester and the abrasion loss was 51.3g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.11.
Example 4
The embodiment provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
silica sol (42% mass concentration of silica) 50.2%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; cerium oxide powder 1%; 3% of borax; sericite powder 1.3%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1866 ℃, the normal-temperature compressive strength of 62.2Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours of 21.9Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20 minutes, and the flexural strength is 12.2Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.61W/(m.times.K) measured by a steady state method; 300g of the refractory was put on a Taber abrasion tester and the abrasion loss was 50.9g by rotating the grinding wheel 1000 times, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.11.
Example 5
The embodiment provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (mass concentration of silica 42%) 49.8%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; cerium oxide powder 1%; 3% of borax; sericite powder 1.7%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1862 ℃, the normal-temperature compressive strength of 62.1Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours of 21.8Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20 minutes, and the flexural strength is 12.3Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.54W/(m.times.K) measured by a steady state method; a300 g refractory was put on a Taber abrasion tester and the abrasion loss was 51g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. Times.2 h)/% was 0.11.
Example 6
The embodiment provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (42% mass concentration of silica) 50.2%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.3% of aluminum titanate; zirconia (1-2 mm) 6%; cerium oxide powder 1%; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the load softening temperature of the refractory material for the glass kiln is 1859 ℃, the normal-temperature compressive strength is 62Mpa, the flexural strength after being treated for 3 hours at 1450 ℃ is 21.1Mpa, then the refractory material is subjected to heat preservation at 1100 ℃ for 20min and then is quenched in cold water at 20 ℃, and the flexural strength is 12.2Mpa after repeated 30 times; is not corroded by glass; the thermal conductivity is 0.59W/(m.times.K) measured by a steady state method; a300 g refractory was put on a Taber abrasion tester and the abrasion loss was 51.5g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.11.
Example 7
The embodiment provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (mass concentration of silica 42%) 49.8%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.7% of aluminum titanate; zirconia (1-2 mm) 6%; cerium oxide powder 1%; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1866 ℃, the normal-temperature compressive strength of 61.8Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours of 21.3Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20 minutes, and the flexural strength is 12.4Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.61W/(m.times.K) measured by a steady state method; a300 g refractory was put on a Taber abrasion tester and the abrasion loss was 51.2g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.11.
Comparative example 1
The comparative example provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (42% mass concentration of silica) 50.4%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; 0.6% of cerium oxide powder; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1813 ℃, the normal-temperature compressive strength of 56.5Mpa, the flexural strength after being treated for 3 hours at 1450 ℃ of 16.6Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20min, and the flexural strength is 9.6Mpa after being repeatedly carried out for 30 times; is corroded by glass; the thermal conductivity is 0.83W/(m.times.K) measured by a steady state method; 300g of the refractory was put on a Taber abrasion tester and the abrasion loss was 53.3g by rotating the grinding wheel 1000 times, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.15.
Comparative example 2
The comparative example provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (mass concentration of silica 42%) 49.6%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; 1.4% of cerium oxide powder; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1811 ℃, the normal-temperature compressive strength of 53.3Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours of 19.2Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20 minutes, and the flexural strength is 10.1Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.88W/(m.times.K) measured by a steady state method; 300g of the refractory was put on a Taber abrasion tester and the abrasion loss was 54.1g by rotating the grinding wheel 1000 times, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.14.
Comparative example 3
The comparative example provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (42% mass concentration of silica) 50.4%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; 1.4% of cerium oxide powder; 3% of borax; sericite powder 1.1%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1822 ℃, the normal-temperature compressive strength of 56.2Mpa, the flexural strength after being treated for 3 hours at 1450 ℃ of 17.1Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20min, and the flexural strength is 8.9Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.85W/(m.times.K) measured by a steady state method; 300g of the refractory was put on a Taber abrasion tester and the abrasion loss was 54.4g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.15.
Comparative example 4
The comparative example provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (mass concentration of silica 42%) 49.6%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.5% of aluminum titanate; zirconia (1-2 mm) 6%; 1.0% of cerium oxide powder; 3% of borax; sericite powder 1.9%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1835 ℃, the normal-temperature compressive strength of 52.6Mpa, the flexural strength after being treated for 3 hours at 1450 ℃ of 17.7Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20min, and the flexural strength is 10.2Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.9W/(m.times.K) measured by a steady state method; a300 g refractory was put on a Taber abrasion tester and the abrasion loss was 55.2g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.14.
Comparative example 5
The comparative example provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (42% mass concentration of silica) 50.4%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.1% of aluminum titanate; zirconia (1-2 mm) 6%; 1.0% of cerium oxide powder; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1813 ℃, the normal-temperature compressive strength of 55.3Mpa, the flexural strength after being treated at 1450 ℃ for 3 hours of 17.7Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20 minutes, and the flexural strength is 8.3Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.83W/(m.times.K) measured by a steady state method; 300g of the refractory was put on a Taber abrasion tester and the abrasion loss was 54.1g by 1000 rotations of the grinding wheel, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.15.
Comparative example 6
The comparative example provides a refractory material for a glass kiln, which comprises the following components in percentage by mass:
Silica sol (mass concentration of silica 42%) 49.6%; 13% of alumina particles; flint clay powder (granularity less than 0.088 mm) 8%; silicon carbide (particle size less than 0.3 mm) 6%; 2.9% of aluminum titanate; zirconia (1-2 mm) 6%; 1.0% of cerium oxide powder; 3% of borax; sericite powder 1.5%; 6% of mullite powder; 3% of magnesium oxide; wherein, the alumina particles comprise the following particle fractions in percentage by mass: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
The preparation method of the refractory material for the glass kiln comprises the following steps:
(1) Preparing raw materials according to mass percentage;
(2) Firstly, uniformly mixing and stirring the granularity material larger than 2mm, then adding the silica sol, uniformly stirring, finally adding the fine powder, uniformly mixing, and standing for trapping the material for 3.5 hours to obtain a mixture;
(3) Placing the mixture into an electric heating furnace, under the protection of nitrogen with the concentration of 99% (v/v), heating the mixture from room temperature to 110 ℃, keeping the temperature at the heating rate of 5 ℃/min, keeping the temperature at 110 ℃ for 3 hours, gradually cooling the mixture to 70 ℃ at the speed of 3 ℃/min after the heat preservation is finished, and pouring the mixture into a prefabricated mold;
(4) And (3) under the protection of nitrogen, cooling and annealing the mixture in the die, wherein the cooling rate in the annealing treatment process is 3 ℃/min, and cooling to 70 ℃ to obtain the refractory material for the glass kiln.
Through testing, the refractories for the glass kiln have the load softening temperature of 1812 ℃, the normal-temperature compressive strength of 50.2Mpa, the flexural strength after being treated for 3 hours at 1450 ℃ of 16.6Mpa, then the refractories are quenched in cold water at 20 ℃ after being kept at 1100 ℃ for 20min, and the flexural strength is 7.8Mpa after being repeatedly carried out for 30 times; is not corroded by glass; the thermal conductivity is 0.87W/(m.times.K) measured by a steady state method; 300g of the refractory was put on a Taber abrasion tester and the abrasion loss was 53.1g by rotating the grinding wheel 1000 times, and the change in the heating permanent line (1450 ℃ C. X2 h)/% was 0.15.
From the performance test data of examples 1-7 and comparative examples 1-6, it can be seen that the addition of 0.8% -1.2% cerium oxide is advantageous for improving the performance of the refractory material because the addition of cerium oxide changes the phase composition and microstructure of the material, reduces the internal thermal stress, and adjusts the thermal expansion of the material, thereby enhancing the strength of the refractory material. The addition of 2.3 to 2.7 percent of aluminum titanate is beneficial to improving the performance of the refractory material, the aluminum titanate material has extremely low thermal expansion coefficient, which means that the volume change of the material is small when the temperature is changed, so that the structural stress caused by temperature fluctuation is reduced, the aluminum titanate has higher melting point, the aluminum titanate can keep good physical form under high-temperature environment and is not easy to melt or deform, the aluminum titanate has very important characteristic for the refractory material which needs to be used for a long time under the high-temperature condition, and the low thermal conductivity of the aluminum titanate is beneficial to slowing down the heat transfer, so that the thermal stress generated by the temperature gradient inside the material can be reduced, and the stability and the service life of the refractory material in the thermal environment are improved. The addition of 1.3 to 1.7 percent of sericite is beneficial to improving the performance of the refractory material, the thermal expansion coefficient of the sericite is lower, which means that the volume change of the material is smaller when the temperature is changed, the structural stress caused by temperature fluctuation can be reduced, the dimensional stability of the material is improved, the sericite has excellent heat-resistant insulating property, which is beneficial to improving the electrical insulating capability of the refractory material at high temperature, is particularly important for the application occasions needing insulation under high temperature conditions, the sericite is difficult to dissolve in an acid-base solution, the chemical property is stable, which is beneficial to improving the stability and the durability of the refractory material under the chemical erosion environment, and the abrasion resistance of the sericite are good, which is beneficial to improving the durability of the refractory material, reducing the material loss caused by abrasion, thereby improving the strength of the refractory material.
In the description of the present invention, numerous specific details are set forth. However, it is understood that embodiments of the invention may be practiced without these specific details. In some embodiments, well-known methods, structures and techniques have not been shown in detail in order not to obscure an understanding of this description.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (10)
1. The refractory material for the glass kiln is characterized by comprising the following components in percentage by mass:
48% -52% of silica sol; 11% -15% of alumina particles; 7% -10% of flint clay powder; 5% -8% of silicon carbide; 2.3 to 2.7 percent of aluminum titanate; zirconia 5.5-6.5%; cerium oxide powder 0.8-1.2%; borax 2.8-3.2%; 1.3 to 1.7 percent of sericite powder; mullite 5.5-6.5%; 2.8 to 3.2 percent of magnesium oxide.
2. The refractory for a glass kiln according to claim 1, wherein the silica content of the silica sol is 40 to 45% by mass.
3. The refractory for a glass kiln according to claim 1, wherein the flint clay powder has a particle size of less than 0.3mm.
4. The refractory for a glass kiln according to claim 1, wherein the zirconia has a particle size of 1 to 2mm.
5. The refractory for a glass kiln according to claim 1, wherein the alumina particles comprise the following fractions in mass percent: 30% of alumina with granularity of 5-3 mm; 40% of alumina with granularity of 3-2 mm; 20% of alumina with granularity of 2-0.088 mm; 10% of alumina with the granularity of less than 0.088 mm.
6. The preparation method of the refractory material for the glass kiln is characterized by comprising the following steps of:
s1, 48 to 52 percent of silica sol, 11 to 15 percent of alumina particles, 7 to 10 percent of flint clay powder, 5 to 8 percent of silicon carbide, 2.3 to 2.7 percent of aluminum titanate, 5.5 to 6.5 percent of zirconia, 0.8 to 1.2 percent of cerium oxide powder, 2.8 to 3.2 percent of borax, 1.3 to 1.7 percent of sericite powder, 5.5 to 6.5 percent of mullite and 2.8 to 3.2 percent of magnesium oxide are mixed and stirred for 28 to 32 minutes, and then the mixture is obtained after standing for 3 to 4 hours;
S2, under the protection of nitrogen, heating the mixture after standing to 105-115 ℃, then preserving heat for 3.2-3.6 hours, cooling to 68-75 ℃ and carrying out casting and cooling annealing to obtain the glass kiln to enable the refractory material.
7. The method for producing a refractory for a glass kiln according to claim 6, wherein in the step S1, the mixing and stirring are: and mixing and stirring the granularity materials with the granularity of more than 2mm uniformly, adding the silica sol and stirring uniformly, and finally adding the fine powder with the granularity of less than or equal to 2mm and mixing uniformly.
8. The method for producing a refractory for a glass kiln according to claim 6, wherein in the step S2, the concentration of the nitrogen gas is 98% by volume or more.
9. The method for producing a refractory for a glass kiln according to claim 6, wherein in the step S2, the cooling rate of the cooling annealing is 2.8 to 3.3 ℃/min.
10. A glass kiln comprising the refractory material of any one of claims 1-5.
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