CN118125794A - Preparation method of nano silicon dioxide composite heat-insulating material for glass kiln crown - Google Patents
Preparation method of nano silicon dioxide composite heat-insulating material for glass kiln crown Download PDFInfo
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- CN118125794A CN118125794A CN202410207797.6A CN202410207797A CN118125794A CN 118125794 A CN118125794 A CN 118125794A CN 202410207797 A CN202410207797 A CN 202410207797A CN 118125794 A CN118125794 A CN 118125794A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 25
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 25
- 239000011810 insulating material Substances 0.000 title claims abstract description 22
- 239000011521 glass Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 46
- 239000000243 solution Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 28
- 239000011259 mixed solution Substances 0.000 claims description 26
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 239000012774 insulation material Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000000084 colloidal system Substances 0.000 claims description 18
- 238000004321 preservation Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 108090000790 Enzymes Proteins 0.000 claims description 14
- 102000004190 Enzymes Human genes 0.000 claims description 14
- 239000000413 hydrolysate Substances 0.000 claims description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims description 13
- 230000003301 hydrolyzing effect Effects 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 230000004048 modification Effects 0.000 claims description 13
- 238000012986 modification Methods 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000006481 deamination reaction Methods 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- -1 3-methyl-trichloropropyl triethoxysilane Chemical compound 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000003892 spreading Methods 0.000 claims description 7
- 230000007480 spreading Effects 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000009960 carding Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000292 calcium oxide Substances 0.000 claims description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 5
- 239000003518 caustics Substances 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 5
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 5
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 5
- 238000002715 modification method Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 10
- 238000012546 transfer Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 3
- 238000013329 compounding Methods 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005816 glass manufacturing process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Structural Engineering (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of preparation of heat-insulating materials, in particular to a preparation method of a nano silicon dioxide composite heat-insulating material for a glass kiln crown, which comprises the following steps: s1, preparing a fiber body, S2, preparing sol, S3, forming gel, S4, modifying and post-treating; according to the invention, the composite heat-insulating material can effectively reduce heat transfer by compounding nano silicon dioxide, so that the heat-insulating effect of the crown of the kiln is improved, the high specific surface area and the special structure of the nano silicon dioxide can block heat conduction and radiation, the heat energy loss is reduced, the gel thermal resistance can be enhanced by the multi-layer fiber body structure, the heat transfer rate is reduced, the heat-insulating effect of the composite heat-insulating material is improved, the nano silicon dioxide particles in the fiber body can increase the compactness and cohesion of the material, the fiber body can be kept stable in a high-temperature environment, the heat resistance is enhanced, and the service life is prolonged.
Description
Technical Field
The invention relates to the technical field of preparation of heat-insulating materials, in particular to a preparation method of a nano silicon dioxide composite heat-insulating material for a glass kiln crown.
Background
With the rapid development of industry, glass manufacturing industry is also continuously developing. In the glass manufacturing process, the furnace crown is required to heat and melt the glass. However, the conventional kiln crown insulation materials have many problems such as poor insulation performance, easy falling and easy damage, etc., which affect the glass processing efficiency and the product quality. In order to overcome the problems, scientists research and develop a novel nano silicon dioxide composite heat-insulating material for heat insulation of kiln crown.
The nano silicon dioxide composite thermal insulation material consists of nano silicon dioxide and other composite materials. The small size of the nanoparticles can improve the mechanical properties, thermal stability and corrosion resistance of the material. Meanwhile, the nano silicon dioxide can also remarkably improve the heat preservation effect.
However, the nano silicon dioxide composite thermal insulation material still has some defects in the application process, such as high preparation cost, poor sealing performance and easy peeling, the preparation process of the nano silicon dioxide composite thermal insulation material needs higher temperature and pressure, and the manufacturing cost is higher; under the conditions of high temperature and high pressure, the thermoplastic change of the polymer is small, the change of the molecular structure is easy to occur, gaps are generated between the metal and the heat insulation material, and the defect is likely to cause the heat insulation material to be easily peeled off.
Disclosure of Invention
The invention provides a preparation method of a nano silicon dioxide composite heat-insulating material for a glass kiln crown, which aims at the defects of the prior art and comprises the following steps:
S1, preparing a fiber body:
according to the mass percentage, 12-16% of sodium oxide, 8-12% of calcium oxide, 2-5% of magnesium oxide, 1-3% of aluminum oxide, 0.5-2% of rare earth element, 1-3% of silicone oil and the balance of nano silicon dioxide are mixed, and melt is obtained after melt refining; drawing the melt into filaments, cleaning the filaments, drying, and then carrying out fluffing treatment to obtain a fiber body;
s2, preparing sol:
mixing and stirring uniformly 10-13% of tetraethoxysilane, 40-60% of ethanol, 1-5% of hydrochloric acid, 0.1-3% of polyacrylamide, 0.1-3% of polyvinyl alcohol, 0.1-5% of cetyltrimethylammonium bromide and the balance of water according to mass percent to obtain a mixed solution, regulating the pH value of the mixed solution, and then stirring and hydrolyzing to obtain sol;
S3, gel forming:
Pouring the sol into a mold, spreading the fiber body in the sol, and placing the filled mold into water bath equipment for thermal insulation molding to obtain gel;
s4, modification and post-treatment:
Heating the gel in water bath continuously to age the gel, putting the gel into normal hexane solution, fully stirring and heating to perform exchange reaction to obtain composite colloid; and (3) putting the composite colloid into a modifying solution for soaking and washing, and drying at 110-130 ℃ to obtain the composite heat-insulating material.
Description: due to the addition of the nano silicon dioxide and the structures of the fiber body and the sol, the composite heat-insulating material has excellent heat-insulating performance, can effectively reduce heat transfer, improves the heat-insulating effect of the kiln crown, and reduces energy consumption; by adding nano silicon dioxide into the fiber body and sol, the stability and strength of the composite thermal insulation material can be enhanced. The nano silicon dioxide particles have higher specific surface area and special structure, and can improve the permeation resistance, compression resistance and high temperature resistance of the material; the preparation of the fiber body, the preparation of the sol, the gel forming, the subsequent modification treatment and other steps, the process is relatively simple, and the mass production is easy.
Further, the cleaning and drying method of the filament in the step S1 is as follows: the filaments are sequentially washed by reflux with ethanol and deionized water with the mass concentration of 50 to 70 percent, and then dried for 12 to 24 hours at the temperature of 120 to 140 ℃.
Description: the ethanol with the concentration of 50-70 wt% has better decontamination and dissolution performance, can effectively remove dirt, impurities and residues on the surface of the filament, and ensures the purity of the filament. Meanwhile, deionized water is used for secondary cleaning, so that the filaments can be further purified, and precipitation and residue of hardness substances in water can be avoided by using deionized water for cleaning, so that pollution and corrosion effects on the filaments are reduced; after cleaning, drying can further remove residual ethanol and water, and the purity of the filaments is improved. Drying is carried out at a higher temperature, so that the evaporation and volatilization of water can be accelerated, the dryness of filaments is ensured, and the influence of water residues on the subsequent process is reduced.
Further, the filaments in the step S1 are fluffed by a fiber carding machine, so as to obtain a fiber body.
Description: the fiber bundles or clusters can be effectively separated by processing the filaments by a fiber carding machine, so that the fiber body obtains better bulk. The fluffy fiber body has larger surface area and more gaps, and can provide more heat insulation air layers, thereby enhancing the heat insulation effect; the fiber carding machine can uniformly card and disperse the fibers, so that the fibers are distributed in a fiber body more uniformly, and the formation of fiber clusters is avoided. The uniform fiber distribution is beneficial to maintaining the uniformity and consistency of materials and improving the stability and reliability of heat preservation performance; the fiber body processed by the fiber carding machine has loose connection among fibers and improved softness and bendability of the fibers, so that the fiber body is easier to control and adjust in the subsequent processing steps such as mixing, forming and the like, and the processability of the material is improved.
Further, the concentration of the hydrochloric acid in the step S2 is 15-25 wt%; the pH value of the mixed solution is regulated to 3-4.
Description: the solubility and the reactivity of the hydrochloric acid can be enhanced by properly increasing the concentration of the hydrochloric acid, so that the reaction process is accelerated, the reaction time is shortened, and the production efficiency is improved; the pH value of the mixed solution is regulated to 3-4, the reaction and the composition of the product can be controlled, and side reactions and adverse effects caused by too high or too low pH value are avoided, so that the purity and stability of the product are improved.
Further, the hydrolysis method in step S2 is as follows: according to the mass percentage, adding 5-15% of the hydrolysate into the mixed solution at 40-50 ℃, stirring and hydrolyzing, adopting 0.01-5 wt% of enzyme hydrolysate as the hydrolysate, stopping hydrolyzing after the enzyme hydrolysate is cooled to room temperature, adding 0.1-1 mol/L of ammonia water solution accounting for 0.1-2% of the mixed solution, and stirring uniformly to obtain the sol.
Description: the hydrolysis reaction is carried out at the temperature of 40-50 ℃, so that the catalytic activity of enzyme can be promoted, the hydrolysis reaction rate can be accelerated, and the enzyme hydrolysate with the concentration of 0.01-5 wt% can provide high-efficiency catalytic action to accelerate the hydrolysis reaction; the hydrolysis reaction is carried out until the enzyme hydrolysate is cooled to room temperature, so that the hydrolysis reaction can be ensured to be fully carried out, and the enzyme activity is maintained at a stable level; adding 0.1-1 mol/L ammonia water solution and stirring uniformly, which is helpful for adjusting the pH value of the solution. Regulating pH can affect the formation and stability of the product, thus controlling the quality and performance of the product.
Further, in step S3, the method for tiling the fiber body in the sol is as follows: pouring the sol into a mould with a shape for the arch of the glass kiln in a layering manner, dividing the fiber body into a plurality of times, and uniformly spreading the fiber body into sol of each layer; the heat preservation method comprises the following steps: and (3) placing the filled mould into water bath equipment with the temperature of 40-50 ℃ for heat preservation for 5-15 min, and then forming to obtain the gel.
Description: the fiber body is divided into a plurality of layers to be evenly spread in each layer of sol, so that the bonding force between the fiber body and the sol is enhanced, the strength and the stability of the product are improved, the gel thermal resistance can be enhanced through the multi-layer fiber body structure, the heat transfer rate is reduced, and the heat preservation effect of the composite heat preservation material is improved; the gel formation can be accelerated by the proper heat preservation temperature, the molding time is shortened, and the production efficiency is improved; during the heat preservation process, the components and the structure in the sol can be stabilized. The method has the advantages of keeping a certain temperature and time, helping to ensure the quality and the performance stability of the product and reducing the influence of external environment factors on the sol.
Further, the modification method of the gel in step S4 is as follows: preparing water bath equipment with the temperature of 40-50 ℃, aging the gel in the water bath for 4-6 hours, putting the gel into a normal hexane solution with the weight of 6-13%, fully stirring and heating to perform exchange reaction, and then performing deamination reaction to obtain a composite colloid; adding 3-methyl-trichloropropyl triethoxysilane accounting for 0.5-2 wt% of the normal hexane solution into the normal hexane solution for modification, and then preserving heat for 18-24 hours in water bath equipment at 45-55 ℃ to obtain modified liquid; the composite colloid is put into the modifying liquid to be soaked for 0.5 to 2 hours and then washed.
Description: aging the gel in a water bath, so that the internal structure of the gel is more stable, and chemical substances contained in the solution can be further reacted and converted, thereby improving the stability of the gel; the gel is subjected to exchange reaction and deamination reaction, alkyl in the n-hexane solution can react with alkyl in the gel to improve the breaking elongation of the gel, and in the surface modification, the surface of the gel can be smoother and more uniform through the n-hexane solution exchange reaction; the gel modification can enhance the surface activity of the gel, so that the gel is easier to interact with other substances, the adsorption performance of the sol on water is enhanced, the heat preservation is favorable for stabilizing the colloid, the full progress of the modification reaction is ensured, and the organic silicon chemical group 3-methyl-trichloropropyl triethoxysilane is introduced into the surface of the gel, so that the full reaction is ensured through a long-time heat preservation reaction; the composite colloid is placed into the modifying liquid for soaking and washing, so that unreacted chemical substance residues can be removed, and the preparation quality of the modified gel can be improved.
Further, the method for deamination comprises the following steps: according to mass percent, adding corrosive accounting for 1-10% of the mass of the gel into the gel after the exchange reaction, and reacting for 1-5 h at 160-230 ℃; the corrosive agent adopts hydrofluoric acid with the concentration of 30-40 wt%.
Description: the gel is subjected to deamination reaction, so that organic amine template molecules can be removed, and a nanoscale mesoporous structure is reserved in the gel, so that the thermal resistance of the composite colloid can be increased, the heat transfer rate is reduced, and the heat preservation effect of the composite heat preservation material is improved.
Compared with the prior art, the invention has the beneficial effects that:
According to the invention, by compounding the nano silicon dioxide, the heat transfer of the composite heat-insulating material can be effectively reduced, so that the heat-insulating effect of the crown of the kiln is improved, the high specific surface area and the special structure of the nano silicon dioxide can prevent heat conduction and radiation, and the heat energy loss is reduced, thereby saving energy sources and reducing the production cost; the stability and the strength of the composite thermal insulation material can be enhanced through the preparation of the gel, the compactness and the cohesion of the material can be enhanced by the nano silicon dioxide particles in the fiber body, and the permeation resistance and the compression resistance of the composite thermal insulation material are improved; the gel is subjected to deamination reaction, so that organic amine template molecules can be removed, and a nanoscale mesoporous structure is reserved in the gel, so that the thermal resistance of the composite colloid can be increased, the heat transfer rate is reduced, and the heat preservation effect of the composite heat preservation material is improved; the high temperature resistance of the nano silicon dioxide can also ensure that the fiber body is kept stable in a high temperature environment, strengthen the heat resistance of the composite heat insulation material and prolong the service life.
Detailed Description
The invention will be described in further detail with reference to the following embodiments to better embody the advantages of the invention.
Example 1: the preparation process of nanometer silica composite heat insulating material for glass kiln crown includes the following steps:
S1, preparing a fiber body:
according to the mass percentage, 14 percent of sodium oxide, 10 percent of calcium oxide, 3.5 percent of magnesium oxide, 2 percent of aluminum oxide, 1.25 percent of rare earth element, 2 percent of silicone oil and the balance of nano silicon dioxide are mixed, and melt is obtained after melt refining; drawing the melt into filaments, cleaning the filaments, drying, and then carrying out fluffing treatment by adopting a fiber carding machine to obtain a fiber body;
The cleaning and drying method of the filament comprises the following steps: sequentially carrying out reflux cleaning on the filaments by using ethanol with the mass concentration of 60wt% and deionized water, and then drying at 130 ℃ for 18 hours;
s2, preparing sol:
According to mass percent, mixing and stirring evenly 11.5% of tetraethoxysilane, 50% of ethanol, 3% of hydrochloric acid, 1.5% of polyacrylamide, 1.5% of polyvinyl alcohol, 2.5% of cetyltrimethylammonium bromide and the balance of water to obtain a mixed solution, regulating the pH value of the mixed solution, and then stirring and hydrolyzing to obtain sol;
The concentration of the hydrochloric acid is 20wt%; the pH value of the mixed solution is regulated to 3.5;
the hydrolysis method comprises the following steps: adding 10% of the hydrolysate in the mixed solution at 45 ℃ by mass percent, stirring and hydrolyzing, adopting 2.5% of enzyme hydrolysate by weight, stopping hydrolyzing after the enzyme hydrolysate is cooled to room temperature, adding 0.5mol/L of ammonia water solution accounting for 1% of the mixed solution by mass, and stirring uniformly to obtain sol;
S3, gel forming:
Pouring the sol into a mold, spreading the fiber body in the sol, and placing the filled mold into water bath equipment for thermal insulation molding to obtain gel;
The forming method for spreading the fiber body in the sol comprises the following steps: pouring the sol into a mould with a shape for a glass kiln arch top in five layers, dividing a fiber body into a plurality of times, and uniformly spreading the fiber body in the sol of each layer; the heat preservation method comprises the following steps: placing the filled mould into water bath equipment with the temperature of 45 ℃ for heat preservation for 10min, and then forming;
s4, modification and post-treatment:
The modification method of the gel comprises the following steps: preparing water bath equipment at 45 ℃, aging the gel in the water bath for 5 hours, putting the gel into 9.5wt% of normal hexane solution, fully stirring and heating to perform exchange reaction, and then performing deamination reaction to obtain a composite colloid; adding 3-methyl-trichloropropyl triethoxysilane accounting for 1.25wt% of the normal hexane solution into the normal hexane solution for modification, and then preserving heat for 21 hours in water bath equipment at 50 ℃ to obtain modified liquid; soaking the composite colloid in the modifying liquid for 1.75 hours, and then flushing; drying at 120 ℃ to obtain a composite heat-insulating material;
The deamination reaction method comprises the following steps: adding a corrosive agent accounting for 5% of the mass of the gel into the gel subjected to the exchange reaction according to the mass percentage, and reacting for 3 hours at the temperature of 195 ℃; the etchant adopts hydrofluoric acid with the concentration of 35 weight percent.
Example 2: this example is different from example 1 in that 12% of sodium oxide, 8% of calcium oxide, 2% of magnesium oxide, 1% of aluminum oxide, 0.5% of rare earth element, 1% of silicone oil and the balance of nano silica are mixed, and melt-refined to obtain a melt.
Example 3: this example is different from example 1 in that 16% of sodium oxide, 12% of calcium oxide, 5% of magnesium oxide, 3% of aluminum oxide, 2% of rare earth element, 3% of silicone oil and the balance of nano silica are mixed, and melt-refined to obtain a melt.
Example 4: the present example was different from example 1 in that 10% of ethyl orthosilicate, 40% of ethanol, 1% of hydrochloric acid, 0.1% of polyacrylamide, 0.1% of polyvinyl alcohol, 0.1% of cetyltrimethylammonium bromide and the balance of water were uniformly mixed and stirred to obtain a mixed solution.
Example 5: the present example was different from example 1 in that 13% of ethyl orthosilicate, 60% of ethanol, 5% of hydrochloric acid, 3% of polyacrylamide, 3% of polyvinyl alcohol, 5% of cetyltrimethylammonium bromide and the balance of water were uniformly mixed to obtain a mixed solution.
Example 6: this example differs from example 1 in that a water bath apparatus at 40 ℃ was prepared, the gel was aged in the water bath for 4 hours, the gel was put into a 6wt% n-hexane solution, sufficiently stirred and heated to perform an exchange reaction, and then a deamination reaction was performed to obtain a complex gel; adding 3-methyl-trichloropropyl triethoxysilane accounting for 0.5 weight percent of the normal hexane solution into the normal hexane solution for modification, and then preserving heat for 18 hours in water bath equipment at 45 ℃ to obtain modified liquid; soaking the composite colloid in the modifying liquid for 0.5h and then flushing; drying at 110 ℃ to obtain the composite heat-insulating material.
Example 7: this example differs from example 1 in that a water bath apparatus at 50 ℃ was prepared, the gel was aged in the water bath for 6 hours, the gel was put into a 13wt% n-hexane solution, sufficiently stirred and heated to perform an exchange reaction, and then a deamination reaction was performed to obtain a complex gel; adding 3-methyl-trichloropropyl triethoxysilane accounting for 2wt% of the normal hexane solution into the normal hexane solution for modification, and then preserving heat for 24 hours in water bath equipment at 55 ℃ to obtain modified liquid; soaking the composite colloid in the modifying liquid for 2 hours and then flushing; drying at 130 ℃ to obtain the composite heat-insulating material.
Example 8: this example differs from example 1 in that the cleaning and drying method of the filaments is: the filaments were sequentially washed with 50wt% ethanol and deionized water by reflux, and then dried at 120℃for 12 hours.
Example 9: this example differs from example 1 in that the cleaning and drying method of the filaments is: the filaments were sequentially washed with 70wt% ethanol and deionized water under reflux and then dried at 140℃for 24 hours.
Example 10: this example differs from example 1 in that the concentration of the hydrochloric acid is 15wt%; the hydrolysis method comprises the following steps: according to the mass percentage, adding the hydrolysate accounting for 5 percent of the mass of the mixed solution into the mixed solution at 40 ℃, stirring and hydrolyzing, adopting the enzyme hydrolysate with the concentration of 0.01 weight percent as the hydrolysate, stopping hydrolyzing after the enzyme hydrolysate is cooled to room temperature, adding the ammonia water solution accounting for 0.1 percent of the mass of the mixed solution, and stirring uniformly to obtain the sol.
Example 11: this example differs from example 1 in that the concentration of the hydrochloric acid is 25wt%; the hydrolysis method comprises the following steps: adding a hydrolysis solution accounting for 15% of the mass of the mixed solution into the mixed solution at 50 ℃ according to the mass percentage, stirring and hydrolyzing, adopting an enzyme hydrolysis solution with the concentration of 5wt%, stopping hydrolyzing after the enzyme hydrolysis solution is cooled to room temperature, adding an ammonia water solution accounting for 1mol/L of the mass of the mixed solution, and stirring uniformly to obtain the sol.
Example 12: this example differs from example 1 in that the filled mold was placed in a 40 ℃ water bath apparatus for 5 minutes and then molded.
Example 13: this example differs from example 1 in that the filled mold was placed in a 50 ℃ water bath apparatus for 15 minutes and then molded.
Example 14: the difference between this example and example 1 is that the corrosive agent accounting for 1% of the gel mass is added into the gel after the exchange reaction, and the reaction is carried out for 1 hour at 160 ℃; the etchant adopts hydrofluoric acid with the concentration of 30 weight percent.
Example 12: the difference between this example and example 1 is that the corrosive agent accounting for 10% of the gel mass is added into the gel after the exchange reaction, and the reaction is carried out for 5 hours at 230 ℃; the etchant adopts hydrofluoric acid with the concentration of 40 weight percent.
Experimental example: the samples obtained in examples 1to 7 and comparative example were examined for material density, porosity and thermal conductivity, and the results of specific detailed performance tests are shown in table 1.
Comparative example differs from example 1 in that no fibrous body was added to the sol;
Table 1: 8 different sample Performance test tables tested according to examples 1-7 and comparative examples
1. The influence of proportioning parameters of the prepared melt on the performance of the prepared composite heat-insulating material is explored.
Conclusion: from the data in table 1, it can be seen that the composite thermal insulation material prepared by proportioning the melt in example 1 has better thermal insulation performance, and compared with examples 1 and 3, the composite thermal insulation material in example 3 has the greatest density, and the composite thermal insulation material in example 1 has better comprehensive performance in comprehensive view.
2. The influence of the proportioning parameters of the prepared mixed solution on the performance of the prepared composite heat-insulating material is explored.
Conclusion: as can be seen from the data in table 1, the thermal insulation performance of the samples prepared by using the mixing parameters of the mixed solution in example 5 is better than that of example 4, and the composite thermal insulation material in example 1 has better comprehensive performance from the comprehensive point of view.
3. The influence of the technological parameters of gel modification on the performance of the prepared composite heat-insulating material is explored.
Conclusion: as can be seen from the data in table 1, the comparative example has better overall performance and better thermal insulation performance than example 1, indicating that the structure of the fiber filaments in the gel can reduce the thermal conductivity of the composite thermal insulation material, increase the thermal resistance, and reduce the heat transfer rate. Compared with the heat conduction coefficient of the embodiment 7, the heat conduction coefficient of the embodiment 6 is slightly higher, and the heat insulation performance of the composite heat insulation material prepared by adopting the embodiment 7 is better.
Claims (9)
1. The preparation method of the nano silicon dioxide composite heat-insulating material for the crown of the glass kiln is characterized by comprising the following steps of:
S1, preparing a fiber body:
according to the mass percentage, 12-16% of sodium oxide, 8-12% of calcium oxide, 2-5% of magnesium oxide, 1-3% of aluminum oxide, 0.5-2% of rare earth element, 1-3% of silicone oil and the balance of nano silicon dioxide are mixed, and melt is obtained after melt refining; drawing the melt into filaments, cleaning the filaments, drying, and then carrying out fluffing treatment to obtain a fiber body;
s2, preparing sol:
mixing and stirring uniformly 10-13% of tetraethoxysilane, 40-60% of ethanol, 1-5% of hydrochloric acid, 0.1-3% of polyacrylamide, 0.1-3% of polyvinyl alcohol, 0.1-5% of cetyltrimethylammonium bromide and the balance of water according to mass percent to obtain a mixed solution, regulating the pH value of the mixed solution, and then stirring and hydrolyzing to obtain sol;
S3, gel forming:
Pouring the sol into a mold, spreading the fiber body in the sol, and placing the filled mold into water bath equipment for thermal insulation molding to obtain gel;
s4, modification and post-treatment:
Heating the gel in water bath continuously to age the gel, putting the gel into normal hexane solution, fully stirring and heating to perform exchange reaction to obtain composite colloid; and (3) putting the composite colloid into a modifying solution for soaking and washing, and drying at 110-130 ℃ to obtain the composite heat-insulating material.
2. The method for preparing the nano silica composite thermal insulation material for the crown of the glass kiln according to claim 1, wherein the method for cleaning and drying the filaments in the step S1 is as follows: the filaments are sequentially washed by reflux with ethanol and deionized water with the mass concentration of 50 to 70 percent, and then dried for 12 to 24 hours at the temperature of 120 to 140 ℃.
3. The method for preparing a nano silica composite thermal insulation material for a glass kiln crown according to claim 1, wherein the filaments in step S1 are fluffed by a fiber carding machine to obtain a fiber body.
4. The method for preparing a nano silica composite thermal insulation material for a glass kiln crown according to claim 1, wherein the concentration of hydrochloric acid in the step S2 is 15-25 wt%; the pH value of the mixed solution is regulated to 3-4.
5. The method for preparing the nano silica composite thermal insulation material for the crown of the glass kiln according to claim 1, wherein the hydrolysis method in the step S2 is as follows: according to the mass percentage, adding 5-15% of the hydrolysate into the mixed solution at 40-50 ℃, stirring and hydrolyzing, adopting 0.01-5 wt% of enzyme hydrolysate as the hydrolysate, stopping hydrolyzing after the enzyme hydrolysate is cooled to room temperature, adding 0.1-1 mol/L of ammonia water solution accounting for 0.1-2% of the mixed solution, and stirring uniformly to obtain the sol.
6. The method for preparing the nano silica composite thermal insulation material for the crown of the glass kiln according to claim 1, wherein in the step S3, the method for tiling the fiber body in the sol is as follows: pouring the sol into a mould with a shape for the arch of the glass kiln in a layering manner, dividing the fiber body into a plurality of times, and uniformly spreading the fiber body into sol of each layer; the heat preservation method comprises the following steps: and (3) placing the filled mould into water bath equipment with the temperature of 40-50 ℃ for heat preservation for 5-15 min, and then forming to obtain the gel.
7. The method for preparing the nano silica composite thermal insulation material for the crown of the glass kiln according to claim 1, wherein the modification method of the gel in the step S4 is as follows: preparing water bath equipment with the temperature of 40-50 ℃, aging the gel in the water bath for 4-6 hours, putting the gel into a normal hexane solution with the weight of 6-13%, fully stirring and heating to perform exchange reaction, and then performing deamination reaction to obtain a composite colloid; adding 3-methyl-trichloropropyl triethoxysilane accounting for 0.5-2 wt% of the normal hexane solution into the normal hexane solution for modification, and then preserving heat for 18-24 hours in water bath equipment at 45-55 ℃ to obtain modified liquid; the composite colloid is put into the modifying liquid to be soaked for 0.5 to 2 hours and then washed.
8. The method for preparing the nano silica composite thermal insulation material for the crown of the glass kiln according to claim 7, wherein the method for deamination reaction is as follows: according to mass percent, adding corrosive accounting for 1-10% of the mass of the gel into the gel after the exchange reaction, and reacting for 1-5 h at 160-230 ℃; the corrosive agent adopts hydrofluoric acid with the concentration of 30-40 wt%.
9. The method for preparing the nano silica composite thermal insulation material for the crown of the glass kiln according to claim 1, wherein the modification method of the gel in the step S4 is as follows: preparing water bath equipment with the temperature of 40-50 ℃, aging the gel in the water bath for 4-6 hours, putting the gel into a normal hexane solution with the weight of 6-13%, fully stirring and heating to perform exchange reaction, and then performing deamination reaction to obtain a composite colloid; adding 3-methyl-trichloropropyl triethoxysilane accounting for 0.5-2 wt% of the normal hexane solution into the normal hexane solution for modification, and then preserving heat for 18-24 hours in water bath equipment at 45-55 ℃ to obtain modified liquid; the composite colloid is put into the modifying liquid to be soaked for 0.5 to 2 hours and then washed.
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