CN114656131B - Protective coating of glass kiln and preparation process thereof - Google Patents
Protective coating of glass kiln and preparation process thereof Download PDFInfo
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- CN114656131B CN114656131B CN202210488857.7A CN202210488857A CN114656131B CN 114656131 B CN114656131 B CN 114656131B CN 202210488857 A CN202210488857 A CN 202210488857A CN 114656131 B CN114656131 B CN 114656131B
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- 239000011521 glass Substances 0.000 title claims abstract description 82
- 239000011253 protective coating Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005507 spraying Methods 0.000 claims abstract description 33
- 238000001354 calcination Methods 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 23
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- -1 amide compound Chemical class 0.000 claims description 21
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 229910007926 ZrCl Inorganic materials 0.000 claims description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 8
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract description 7
- 239000011819 refractory material Substances 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 5
- 238000005260 corrosion Methods 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000035939 shock Effects 0.000 abstract description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011344 liquid material Substances 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000009991 scouring Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 53
- 239000000203 mixture Substances 0.000 description 17
- 239000011259 mixed solution Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 239000011449 brick Substances 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical group [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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
- 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
- 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
- C03B5/425—Preventing corrosion or erosion
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention is thatThe preparation process of the glass kiln protective coating comprises the following steps: tetraethoxysilane, zrCl 4 Dissolving in an organic solvent, heating and stirring to obtain a solution A; adding urea into the solution A, heating and stirring to obtain a solution B; spraying the solution B on the tank wall of the glass kiln, N 2 Calcining under atmosphere to obtain the protective coating. According to the method, the protective coating with better performance can be obtained without using yttrium oxide materials with higher price, the thermal shock performance and the high-temperature resistant alkaline oxide corrosion performance of the protective coating can meet the use requirements, the protective coating has higher working temperature, lower thermal conductivity coefficient, higher tensile strength and durability, higher flexural strength and higher volume weight, is not easy to fall off when glass is produced at high temperature, lithium ions in glass liquid and refractory materials of the glass kiln pool wall can be prevented from undergoing chemical reaction, the scouring of the glass liquid to the pool wall is reduced, and the service life of the glass kiln is prolonged.
Description
Technical Field
The invention relates to the technical field of glass kilns, in particular to a protective coating of a glass kiln and a preparation process thereof.
Background
With the popularization of large-area touch screen electronic products such as smart phones and tablet computers, consumers put higher demands on the damage resistance of display screens, such as impact resistance, drop resistance and scratch resistance. For this purpose, large terminals continuously update the screen saver material. Glass is used in the field of screen protection with excellent transparency, hardness, corrosion resistance, easy processing and forming and other characteristics. In addition, through the ion exchange process, a compressive stress layer with a certain depth can be formed on the surface of the glass substrate, and the generation and the expansion of microcracks on the surface of the glass are eliminated, so that the strength of the glass is improved. The lithium aluminum silicon electronic glass has greatly improved strength after being toughened, and has very high surface hardness, so that the lithium aluminum silicon electronic glass is widely applied to the field of protective covers, particularly electronic products.
The production of lithium aluminum silicon electronic glass generally requires the use of lithium aluminum silicon glass kilns. Because the production temperature of lithium aluminum silicon electronic glass is generally higher, refractory materials are generally required to be selected for the melting part of the lithium aluminum silicon glass kiln and the crown of the regenerator. The crown of the melting part is preferably 41# fused zirconia corundum brick and alpha-beta fused corundum brick, and the crown of the regenerator is preferably an alkaline brick such as fused magnesia brick, and the fused bricks have excellent fire resistance but are high in price and cost. In lithium aluminum silicon electronic glass production, the refractory materials of the melting part and the crown of the regenerator are corroded due to the influence of dust flying of raw materials, volatilization of alkaline oxide steam, flowing of glass liquid and the like, so that the service life of the lithium aluminum silicon glass kiln is seriously influenced, and the defects of bubbles, stones, stripes and the like in glass can be caused in the glass liquid by the corroded changed materials. In order to produce high-quality lithium aluminum silicon electronic glass, technicians implement protective coating on refractory materials, the existing protective coating process mostly uses zirconite as a main raw material, carbon black as a reducing agent and yttrium oxide as an additive, and a carbothermic reduction method is used for preparing the protective coating, and the prepared protective coating can play a protective role, but the used yttrium oxide has a higher price, so that the protective cost of a lithium aluminum silicon glass kiln is increased.
Disclosure of Invention
The invention aims to overcome the defects that the yttrium oxide raw material used in the preparation process of the protective coating in the prior art has higher price and the protective cost of a lithium aluminum silicon glass kiln is improved.
Therefore, the invention provides a preparation process of a glass kiln protective coating, which comprises the following steps:
obtaining a solution A: tetraethoxysilane, zrCl 4 Dissolving in an organic solvent, heating and stirring to obtain a solution A;
obtaining a solution B: adding an amide compound into the solution A, heating and stirring to obtain a solution B;
and (3) spray-coating and calcining: spraying the solution B on the tank wall of the glass kiln, N 2 Calcining under atmosphere to obtain the protective coating.
Optionally, the amide compound is at least one selected from urea, formamide, acetamide and dimethylformamide.
Optionally, the solution a further comprises cetyltrimethylammonium bromide.
Optionally, in the step of obtaining the solution A, cetyltrimethylammonium bromide and ZrCl 4 Ethyl orthosilicate is sequentially dissolved in an organic solvent. .
Optionally, the cetyl trimethyl ammonium bromide and ZrCl 4 The mass ratio of (2) to (8) is 1;
the mass ratio of the ethyl orthosilicate to the cetyl trimethyl ammonium bromide is 3:1.
Optionally, the solution B further includes an alkali metal chloride, preferably, the alkali metal chloride is at least one selected from sodium chloride, potassium chloride and lithium chloride.
Optionally, the mass ratio of the amide compound to the alkali metal chloride is 3:1.
Optionally, in the step of obtaining the solution A, heating to 80-100 ℃, and then preserving heat and stirring for 30-40min;
in the step of obtaining the solution B, the solution B is heated to 80-100 ℃, and then is stirred for 8-10 hours with heat preservation.
Optionally, in the step of obtaining the solution A, cetyltrimethylammonium bromide, tetraethoxysilane and ZrCl 4 Sequentially dissolving in organic solvent.
Optionally, the calcination time in the spray calcination step is 2-3h, and the calcination temperature is 1700-1850 ℃.
The invention provides a glass kiln protective coating, which is prepared by the preparation process of the glass kiln protective coating.
The technical scheme of the invention has the following advantages:
1. the invention provides a glass kilnPreparation process of protective coating by tetraethyl orthosilicate and ZrCl 4 And an amide compound is used as a raw material, and is calcined in a nitrogen atmosphere to obtain a protective coating with a main component of zirconia-silicon carbide composite material; the amide compound can introduce nitrogen atoms and carbon atoms, and an electron channel is formed between the nitrogen atoms and zirconium atoms, so that the stability of the zirconia is improved, the zirconia has higher oxygen reducibility, and the conversion of silicon dioxide into silicon carbide is promoted in a calcination stage; the calcination is carried out in the nitrogen atmosphere, so that nitrogen atoms can be continuously introduced, and the reaction is promoted; when the process is used for preparing the glass, the yttrium oxide material with higher price is not required to be used, the protective coating with basically equivalent performance to the yttrium oxide material with higher price can be obtained, the thermal shock performance and the high-temperature alkaline oxide corrosion resistance of the yttrium oxide material are similar to those of the existing protective coating, the use requirement of the protective coating is met, the high-temperature alkaline oxide corrosion resistant glass has higher working temperature, lower thermal conductivity coefficient, higher tensile strength and durability, higher breaking strength and higher volume weight, lithium ions in glass liquid and refractory materials of the tank wall of a glass kiln are prevented from being subjected to chemical reaction when glass is produced at a high temperature, the scouring of the glass liquid to the tank wall is reduced, and the service life of the glass kiln is prolonged.
2. According to the preparation process of the glass kiln protective coating, the main component of the obtained protective coating is the zirconia-silicon carbide composite material, if the protective coating enters lithium aluminum silicon glass liquid under the flushing of glass liquid, silicon and zirconium are components of the lithium aluminum silicon glass, and glass cannot be polluted after entering the glass liquid.
3. According to the preparation process of the glass kiln protective coating, provided by the invention, the hexadecyl trimethyl ammonium bromide and the alkali metal chloride are added in the preparation process, wherein the hexadecyl trimethyl ammonium bromide can play a role of a surfactant, and the alkali metal chloride plays a role of a salt seal, so that the dispersibility of the coating particles is excellent, agglomeration does not occur, and the overall performance of the protective coating is improved through the interaction of the salt seal and the surfactant.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Cetyl trimethylammonium bromide product number H6269, brand Sigma, available from Sigma aldrich (shanghai) trade company;
the product number of ethyl orthosilicate was 131903, the brand name Aldrich, available from sigma Aldrich (shanghai) trade company.
Example 1
The embodiment provides a glass kiln protective coating, which comprises the following steps:
s1, weighing 5g of cetyl trimethyl ammonium bromide, dissolving in 2mL of absolute ethyl alcohol, stirring until the mixture is clear, and then sequentially adding 40g of ZrCl 4 And 15g of ethyl orthosilicate are stirred until the mixture is clarified to obtain a mixed solution, and then the mixed solution is heated to 90 ℃ and then is stirred for 30min at a constant temperature to obtain a solution A;
s2, adding 15g of urea and 5g of sodium chloride into the solution A, and then heating to 90 ℃, keeping the temperature and stirring for 9 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 3h under the atmosphere to obtain the protective coating, wherein the calcining temperature is 1750 ℃.
Example 2
The embodiment provides a glass kiln protective coating, which comprises the following steps:
s1, weighing 5g of cetyl trimethyl ammonium bromide, dissolving in 2mL of absolute ethyl alcohol, stirring until the mixture is clear, and then sequentially adding 20g of ZrCl 4 And 15g of orthosilicic acidStirring the ethyl ester until the mixture is clear to obtain a mixed solution, heating the mixed solution to 90 ℃, and then preserving heat and stirring for 30min to obtain a solution A;
s2, adding 15g of urea and 5g of sodium chloride into the solution A, and then heating to 90 ℃, keeping the temperature and stirring for 9 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 3h under the atmosphere to obtain the protective coating, wherein the calcining temperature is 1750 ℃.
Example 3
The embodiment provides a glass kiln protective coating, which comprises the following steps:
s1, weighing 5g of cetyl trimethyl ammonium bromide, dissolving in 2mL of absolute ethyl alcohol, stirring until the mixture is clear, and then sequentially adding 15g of ZrCl 4 And 15g of ethyl orthosilicate are stirred until the mixture is clarified to obtain a mixed solution, and then the mixed solution is heated to 80 ℃ and then is stirred for 40min at a constant temperature to obtain a solution A;
s2, adding 15g of urea and 5g of lithium chloride into the solution A, and then heating to 100 ℃, keeping the temperature and stirring for 8 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 3h under the atmosphere to obtain the protective coating, wherein the calcining temperature is 1700 ℃.
Example 4
The embodiment provides a glass kiln protective coating, which comprises the following steps:
s1, weighing 5g of cetyl trimethyl ammonium bromide, dissolving in 2mL of absolute ethyl alcohol, stirring until the mixture is clear, and then sequentially adding 10g of ZrCl 4 And 15g of ethyl orthosilicate are stirred until the mixture is clarified to obtain a mixed solution, and then the mixed solution is heated to 100 ℃ and then is stirred for 30min at a constant temperature to obtain a solution A;
s2, adding 15g of urea and 5g of potassium chloride into the solution A, and then heating to 80 ℃ and stirring for 10 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 2h under atmosphere to obtain the protective coating, wherein the calcining temperature is 1800 ℃.
Example 5
The comparative example provides a glass kiln protective coating, the preparation process comprises the following steps:
s1, weighing 5g of cetyl trimethyl ammonium bromide, dissolving in 2mL of absolute ethyl alcohol, stirring until the mixture is clear, and then sequentially adding 40g of ZrCl 4 And 15g of ethyl orthosilicate are stirred until the mixture is clarified to obtain a mixed solution, and then the mixed solution is heated to 90 ℃ and then is stirred for 30min at a constant temperature to obtain a solution A;
s2, adding 15g of urea and 5g of sodium chloride into the solution A, and then heating to 90 ℃, keeping the temperature and stirring for 9 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 3h under atmosphere to obtain the protective coating, wherein the calcining temperature is 1850 ℃.
Example 6
The comparative example provides a glass kiln protective coating, the preparation process comprises the following steps:
s1, weighing 5g of cetyl trimethyl ammonium bromide, dissolving in 2mL of absolute ethyl alcohol, stirring until the mixture is clear, and then sequentially adding 40g of ZrCl 4 And 15g of ethyl orthosilicate are stirred until the mixture is clarified to obtain a mixed solution, and then the mixed solution is heated to 90 ℃ and then is stirred for 30min at a constant temperature to obtain a solution A;
s2, adding 15g of urea into the solution A, heating to 90 ℃, preserving heat and stirring for 9 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 3h under the atmosphere to obtain the protective coating, wherein the calcining temperature is 1750 ℃.
Example 7
The comparative example provides a glass kiln protective coating, the preparation process comprises the following steps:
s1, weighing 40g of ZrCl 4 And 15g of tetraethoxysilane are sequentially added into 2mL of absolute ethyl alcohol and stirred until the mixture is clarified to obtain a mixed solution, and then the mixed solution is heated to 90 ℃ and then is kept warm and stirred for 30min to obtain a solution A;
s2, adding 15g of urea and 5g of sodium chloride into the solution A, and then heating to 90 ℃, keeping the temperature and stirring for 9 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 3h under the atmosphere to obtain the protective coating, wherein the calcining temperature is 1750 ℃.
Example 8
The embodiment provides a glass kiln protective coating, which comprises the following steps:
s1, weighing 5g of cetyl trimethyl ammonium bromide, dissolving in 2mL of absolute ethyl alcohol, stirring until the mixture is clear, and then sequentially adding 40g of ZrCl 4 And 15g of ethyl orthosilicate are stirred until the mixture is clarified to obtain a mixed solution, and then the mixed solution is heated to 90 ℃ and then is stirred for 30min at a constant temperature to obtain a solution A;
s2, adding 15g of acetamide and 5g of sodium chloride into the solution A, and then heating to 90 ℃, keeping the temperature and stirring for 9 hours to obtain a solution B;
s3, spraying the solution B on the tank wall of the glass furnace with the spraying thickness of 2mm, and then spraying the solution B on the tank wall of the glass furnace with the thickness of N 2 Calcining for 3h under the atmosphere to obtain the protective coating, wherein the calcining temperature is 1750 ℃.
Comparative example 1
The comparative example provides a glass kiln protective coating, the preparation process comprises the following steps:
20g zircon, 5g carbon black and 5mL Y at 10% concentration were mixed 2 0 3 Mixing to obtain a mixture;
spraying the mixture to the tank wall of a glass furnace by adopting a high-emissivity spray coating method in the glass industry, wherein the spraying thickness is 2mm, and the emissivity coefficient is kept between 0.85 and 0.92 during spraying;
and calcining for 4 hours to obtain the protective coating, wherein the calcining temperature is 1600 ℃.
Test example 1
The thermal shock performance of the protective coatings obtained in the examples and the comparative examples is tested respectively, the test method is GB/T2423-2016 high and low temperature cycle test standard, and the test results are shown in Table 1.
Test example 2
The high-temperature resistant alkaline oxidation performance of the protective coating obtained in the examples and the comparative examples is tested respectively, and the test method is as follows: the protective material was coated on the refractory bricks according to the methods of examples and comparative examples, the degree of corrosion of one day was tested under an atmosphere of high temperature sodium oxide as a corrosive liquid, the presence or absence of modified dissolution phenomenon of the coating was observed and the dissolution rate was recorded, and the test results are shown in table 1.
Test example 3
The thermal conductivity coefficients of the protective coatings obtained in the examples and the comparative examples are respectively tested, and the test method comprises the following steps: ASTM C201-1998 refractory thermal conductivity Standard test method, test results are shown in Table 1.
Test example 4
The tensile and lasting strength of the protective coatings obtained in the examples and the comparative examples are respectively tested by the displacement test: the protective coating is obtained for the examples and the comparative examples respectively, the protective coating with the size of 5cm multiplied by 5cm is taken as a sample, one corner of the sample is clamped on a clamp at the upper end of an electronic textile strength machine (YG 026 DK), one corner of the opposite corner is clamped on a clamp at the lower end, a rack at the upper end is clamped on the other corner of the opposite corner, the clamp is parallel to the horizontal surface of the sample, the clamp at the upper end is not moved, the clamp at the lower end is moved until the sample is broken, the pressure at the break point is recorded, the pressure value at the break point is compared with the area of the section to obtain the tensile endurance strength, and the test result is shown in the table 1.
Test example 5
The flexural strength of the protective coating obtained in the examples and the comparative examples was tested by the following method: the GB/T3001-2017 refractory material is subjected to normal temperature flexural strength test method, and the test results are shown in Table 1.
Test example 6
The volume weights of the protective coatings obtained in the examples and the comparative examples are respectively tested by using a volume weight device, and the test method comprises the following steps: SIS 16 11 41-1963 plastics the bulk weight of the shaped material was determined and the test results are shown in Table 1.
TABLE 1
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (6)
1. The preparation process of the glass kiln protective coating is characterized by comprising the following steps of:
obtaining a solution A: tetraethoxysilane, zrCl 4 Dissolving in an organic solvent, heating and stirring to obtain a solution A;
obtaining a solution B: adding an amide compound into the solution A, heating and stirring to obtain a solution B;
and (3) spray-coating and calcining: spraying the solution B on the tank wall of the glass kiln, N 2 Calcining under atmosphere to obtain a protective coating;
the protective coating comprises zirconia and silicon carbide;
the solution a also includes cetyl trimethylammonium bromide;
the hexadecyl trimethyl ammonium bromide and ZrCl 4 The mass ratio of (2) to (8) is 1;
the mass ratio of the ethyl orthosilicate to the cetyl trimethyl ammonium bromide is 3:1;
or, the solution B also comprises alkali metal chloride, wherein the alkali metal chloride is at least one selected from sodium chloride, potassium chloride and lithium chloride;
the mass ratio of the amide compound to the alkali metal chloride is 3:1.
2. The process for preparing a protective coating for a glass kiln according to claim 1, wherein the amide compound is at least one selected from urea, formamide, acetamide and dimethylformamide.
3. According to claim 2A preparation process of a glass kiln protective coating is characterized in that in the step of obtaining a solution A, cetyltrimethylammonium bromide and ZrCl are added 4 Ethyl orthosilicate is sequentially dissolved in an organic solvent.
4. The process for preparing a protective coating for a glass kiln according to claim 3, wherein in the step of obtaining the solution A, the solution A is heated to 80-100 ℃ and then stirred for 30-40min at a constant temperature;
in the step of obtaining the solution B, the solution B is heated to 80-100 ℃, and then is stirred for 8-10 hours with heat preservation.
5. The process for preparing a protective coating for a glass kiln according to claim 4, wherein the calcination time in the spray calcination step is 2-3 hours and the calcination temperature is 1700-1850 ℃.
6. A glass kiln protective coating prepared by the process of any one of claims 1-5.
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