CN112266633B - 1700 ℃ high-temperature-resistant fireproof coating and preparation method thereof - Google Patents
1700 ℃ high-temperature-resistant fireproof coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 58
- 239000011248 coating agent Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 14
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 13
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims abstract description 13
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 13
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 12
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910033181 TiB2 Inorganic materials 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000292 calcium oxide Substances 0.000 claims abstract description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 11
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000010445 mica Substances 0.000 claims abstract description 11
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 11
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 11
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 229910001868 water Inorganic materials 0.000 claims description 16
- 229920002748 Basalt fiber Polymers 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000003063 flame retardant Substances 0.000 claims description 9
- 239000002518 antifoaming agent Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000012856 weighed raw material Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- 238000009413 insulation Methods 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 11
- 229910019142 PO4 Inorganic materials 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000010452 phosphate Substances 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 8
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- 239000000945 filler Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000011253 protective coating Substances 0.000 description 5
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 229910001387 inorganic aluminate Inorganic materials 0.000 description 4
- 229910052911 sodium silicate Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910014780 CaAl2 Inorganic materials 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 description 2
- 229910052661 anorthite Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 2
- 229910052909 inorganic silicate Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052652 orthoclase Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002694 phosphate binding agent Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention relates to the technical field of fireproof coatings, and particularly discloses a 1700 ℃ high-temperature-resistant fireproof coating and a preparation method thereof. Wherein the aluminum hydroxide, the aluminum dihydrogen phosphate, the sodium carbonate, the silicon dioxide, the titanium diboride, the titanium oxide, the mica powder, the calcium oxide, the magnesium oxide and the double rare earth tantalite are respectively in parts by weight: 10 to 12, 3 to 4, 2 to 3, 1 to 2, 2 to 3, 4 to 5. By adopting the fireproof coating in the patent, the examination is carried out for 20min at the high temperature of 1700 ℃, the temperature of a matrix is 200-300 ℃, and the fireproof coating has an excellent heat insulation effect.
Description
Technical Field
The invention relates to the technical field of fireproof coatings, in particular to a 1700 ℃ high-temperature-resistant fireproof coating and a preparation method thereof.
Background
The development of phosphate-based high-temperature-resistant protective coatings in the last 50 years of the United states is developed, and the phosphate-based high-temperature-resistant protective coatings are mainly prepared by taking aqueous solution of phosphate as a base material and adding fillers. The phosphate-based high-temperature-resistant protective coating is prepared by mixing a phosphate aqueous solution with pigment, filler, auxiliary agent and the like and dispersing at a high speed, the appearance is gray viscous liquid, the filler is allowed to sink when the product is stored and placed for a long time, and the product can be completely uniform paint liquid after being fully stirred. The phosphate-based high-temperature-resistant protective coating is coated and cured to form a phosphate-based high-temperature-resistant protective coating, and the coating system has good performances of corrosion resistance, water resistance, salt mist resistance, lubricating oil resistance, high temperature resistance (up to 650 ℃) and the like, can bear the scouring of high-temperature gas flow, and simultaneously has good physical and mechanical properties, excellent adhesive force, strong weather resistance, outstanding wear resistance and excellent conductivity.
The slow peak and the like add alumina cement as a curing agent and quartz powder, refractory clay and glass fiber as aggregates into a phosphate binder, and the prepared coating has good high-temperature dielectric heat-proof performance, the use temperature can reach 1500 ℃, and the coating is widely applied to antenna parts of missiles. The development of the coatings in China starts to be developed from the 70 th century in the late past, products are not available until the beginning of the century, the problem of metal protection in high-temperature environment work in China is solved, and meanwhile, the development of the phosphate fireproof coating has a large research and development space.
Disclosure of Invention
The invention provides a 1700 ℃ high-temperature-resistant fireproof coating and a preparation method thereof, effectively fills the blank of the domestic high-temperature-resistant fireproof coating, and is an important breakthrough in the fields of aerospace and high-temperature fireproof coatings.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the fire-retardant coating resisting high temperature of 1700 ℃ comprises raw materials of aluminum hydroxide, aluminum dihydrogen phosphate, sodium carbonate, silicon dioxide, titanium diboride, titanium oxide, mica powder, calcium oxide, magnesium oxide, double rare earth tantalite, basalt fiber and a defoaming agent.
The technical principle and the effect of the technical scheme are as follows:
1. the fireproof coating prepared by the scheme is low in heat conductivity and can play a good heat insulation role, and experiments prove that when the fireproof coating is subjected to thermal examination at the high temperature of 1700 ℃ for 10min, the temperature of a matrix is 200-300 ℃, and the temperature gradient is high, so that the fireproof coating plays a good fireproof and heat insulation effect on the matrix material.
2. In the scheme, titanium diboride, titanium oxide and double rare earth tantalite are used as high-temperature-resistant fillers in the fireproof coating, so that the coating has the advantages of high melting point, high hardness, high wear resistance, low thermal conductivity, good chemical stability and the like; the aluminum dihydrogen phosphate is used as a binding material and simultaneously generates high-melting-point fireproof coating aluminum phosphate with alkalescent aluminum hydroxide; the refractory coatings such as aluminum hydroxide, aluminum dihydrogen phosphate, silicon dioxide, calcium oxide and mica powder react to generate aluminum phosphate, aluminate, silicate, aluminosilicate and the like, the reaction products are different at different temperatures, and the silicon dioxide and the sodium carbonate generate refractory sodium silicate, and SiO in the silicate4A part of tetrahedron is made of AlO4Aluminosilicates of tetrahedrally substituted composition, e.g. orthoclase K [ (AlO)2)(SiO2)3]Denotes that one quarter of the oxygen-containing tetrahedron is occupied by aluminum atoms, and anorthite CaAl2SiO8Or Ca [ (AlO)2)2(SiO2)2]Wherein half is AlO4Tetrahedron, the other half being SiO4Tetrahedra, and the like, refractory aluminosilicate structures; the magnesium oxide is used as a curing agent to absorb water generated in the chemical reaction process, so that the phenomenon that the water generated in the reaction overflows from the coating to damage the coating is avoided.
2Al(OH)3+Al(H2PO4)3→6H2O+3AlPO4
Na2CO3+SiO2→Na2SiO3+CO2↑
MgO+H2O→Mg(OH)2
3. The aluminum hydroxide, the aluminum dihydrogen phosphate, the sodium carbonate, the silicon dioxide, the titanium diboride, the titanium oxide, the mica powder, the calcium oxide, the magnesium oxide and the double rare earth tantalite are respectively prepared from the following components in parts by weight: 10 to 12, 3 to 4, 2 to 3, 1 to 2, 2 to 3, 4 to 5.
Has the advantages that: the raw materials in the proportion can enable the coating to have the best heat insulation effect.
Further, the mass percentage of the basalt fibers is 1-1.5%.
Has the advantages that: the basalt fibers with the mass ratio are added, so that a uniform fiber layer can be formed in the coating, and the fiber layer generates great resistance to air in the coating and is arranged perpendicular to the heat transfer direction, so that heat transfer can be effectively prevented, and heat loss is reduced.
Further, the mass ratio of the defoaming agent is 1-1.5 per mill.
Has the advantages that: suitable defoamers can reduce the generation of bubbles in the starting materials during the reaction.
Further, the diameter of the basalt fiber is 0.8-1 mm, and the length of the basalt fiber is 3-4 mm.
Has the advantages that: the diameter of the added basalt fiber is controlled to be 0.8-1 mm, the basalt fiber can be dispersed in the coating more uniformly, the heat insulation performance is better, the fiber length is controlled to be 3-4 mm, the strength of the coating is high, and the vibration resistance is good.
The application discloses a preparation method of a 1700 ℃ high-temperature-resistant fireproof coating, which comprises the following steps:
step 1: weighing raw materials of aluminum hydroxide, aluminum dihydrogen phosphate, sodium carbonate, silicon dioxide, titanium diboride, titanium oxide, mica powder, calcium oxide, magnesium oxide and double rare earth tantalite, taking absolute ethyl alcohol as a medium, placing the weighed raw materials into a planetary ball mill for ball milling, and drying and sieving the mixed powder;
step 2: and (3) putting the powder sieved in the step (1) into a beaker with deionized water, putting the beaker into a water bath kettle, adding basalt fibers, stirring, adding a defoaming agent, and obtaining the high-temperature-resistant fireproof coating after the solution is in a gel state.
Has the advantages that: the technical scheme is simple in process, the raw materials subjected to ball milling, drying and sieving treatment can be reacted more fully in the coating, and meanwhile, the components in the obtained raw materials are more uniform.
Further, in the step 1, the rotating speed of the ball mill is 300-500 r/min, the ball milling time is 600-1200 min, the temperature in the drying process is 60-80 ℃, the drying time is 10-24 h, and the powder firstly passes through a 300-mesh sieve and then passes through a 500-mesh sieve in the sieving process.
Has the advantages that: can accomplish the abundant ball-milling of raw materials powder under this parameter range and mix, let the ball-milling medium fully volatilize simultaneously to through sieving step by step, make the particle size distribution of raw materials powder more even, play the promotion effect to the reaction between the raw materials.
Further, the temperature of the water bath kettle in the step 2 is 83-95 ℃, and the stirring speed is 500-700 r/min.
Has the advantages that: the temperature can ensure that the reaction between the raw materials can be fully carried out, and meanwhile, the reaction is not easy to control because of no boiling.
Drawings
FIG. 1 is an SEM image of a fireproof coating prepared in example 1 of the present invention;
FIG. 2 is a graph showing the thermal conductivity of the fireproof coating prepared in example 1 of the present invention as a function of temperature;
FIG. 3 is a graph showing the temperature change with time during the thermal examination process of the fireproof coating prepared in example 1 of the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
example 1:
a preparation process of a 1700 ℃ high-temperature-resistant fireproof coating comprises the following steps:
step 1: weighing 110.6g of aluminum hydroxide, 110.6g of aluminum dihydrogen phosphate, 32g of sodium carbonate, 32g of silicon dioxide, 32g of titanium diboride, 35g of titanium oxide, 25g of mica powder, 15g of calcium oxide, 25g of magnesium oxide and 48g of double-rare earth tantalate, and putting the weighed raw materials into a planetary ball mill for ball milling by taking absolute ethyl alcohol as a medium, wherein the ball milling rotation speed is 300r/min, the ball milling time is 1200min, so that all the powder can be uniformly mixed, drying the mixed powder at 60 ℃ for 24h, sieving the powder by a 300-mesh sieve, and then sieving the powder by a 500-mesh sieve.
Step 2: and (2) placing a beaker filled with deionized water into a water bath kettle by using a sol-gel method, adding 5g of basalt fiber, stirring, wherein the temperature of the water bath kettle is 83 ℃, the stirring speed is 500r/min, adding the powder sieved in the step (1) into the beaker, stirring for 30min, adding 10ml of defoaming agent, and stopping stirring after the solution is in a gel state to obtain the high-temperature-resistant fireproof coating.
The main reaction equation in step 2 is:
2Al(OH)3+Al(H2PO4)3→6H2O+3AlPO4
Na2CO3+SiO2→Na2SiO3+CO2↑
MgO+H2O→Mg(OH)2
wherein, the titanium diboride, the titanium oxide and the double rare earth tantalite are used as high-temperature resistant fillers in the fireproof coating, so that the coating has the advantages of high melting point, high hardness, high wear resistance, low thermal conductivity, good chemical stability and the like; the aluminum dihydrogen phosphate is used as a binding material and simultaneously generates high-melting-point fireproof coating aluminum phosphate with alkalescent aluminum hydroxide; the refractory coatings such as aluminum hydroxide, aluminum dihydrogen phosphate, silicon dioxide, calcium oxide and mica powder react to generate aluminum phosphate, aluminate, silicate, aluminosilicate and the like, the reaction products are different at different temperatures, and the silicon dioxide and the sodium carbonate generate refractory sodium silicate, and SiO in the silicate4A part of tetrahedron is made of AlO4Aluminosilicates of tetrahedrally substituted composition, e.g. orthoclase K [ (AlO)2)(SiO2)3]Denotes that one quarter of the oxygen-containing tetrahedron is occupied by aluminum atoms, and anorthite CaAl2SiO8Or Ca [ (AlO)2)2(SiO2)2]Wherein half is AlO4Tetrahedron, the other half being SiO4Tetrahedra, and the like, refractory aluminosilicate structures; the magnesium oxide is used as a curing agent to absorb water generated in the chemical reaction process, so that the phenomenon that the water generated in the reaction overflows from the coating to damage the coating is avoided.
Example 2: the difference from example 1 is that:
step 1: 120g of aluminum hydroxide, 120g of aluminum dihydrogen phosphate, 32g of sodium carbonate, 32g of silicon dioxide, 32g of titanium diboride, 35g of titanium oxide, 25g of mica powder, 15g of calcium oxide, 25g of magnesium oxide and 48g of double rare earth tantalate, and putting the weighed raw materials into a planetary ball mill for ball milling by taking absolute ethyl alcohol as a medium, wherein the ball milling speed is 500r/min, the ball milling time is 800min, so that all the powder can be uniformly mixed, drying the mixed powder at 80 ℃ for 18h, sieving the powder by a 300-mesh sieve firstly, and then sieving the powder by a 500-mesh sieve.
Step 2: and (2) placing a beaker filled with deionized water into a water bath pot by using a sol-gel method, adding 1g of basalt fiber, wherein the temperature of the water bath pot is 95 ℃, the stirring speed is 500r/min, adding the powder sieved in the step (1) into the beaker, stirring for 60min, adding 3ml of defoaming agent, and stopping stirring until the solution is in a gel state to obtain the fireproof coating.
Comparative example 1:
the difference from example 1 is that no double rare earth tantalate was added in comparative example 1.
Comparative example 2:
the difference from example 1 is that the temperature of the water bath in comparative example 2 is 70 ℃.
Comparative example 3:
the difference from example 1 is that basalt fiber was not added in comparative example 3.
And (3) experimental detection:
the coatings prepared in examples 1-2 and comparative examples 1-3 were coated on the surface of 45 steel, and were dried in an oven at 35 ℃ to prepare samples.
When the sample is observed by a scanning electron microscope, taking example 1 as an example, the SEM image of the sample is shown in fig. 1, and the fireproof coating layer has no defects such as air holes and cracks.
The thermal conductivity of the coated side of the fire retardant coating was measured, and the results of the thermal conductivity measured at 800 ℃ are shown in table 1 below, taking the sample prepared in example 1 as an example, and as shown in fig. 2, which is a graph of the thermal conductivity of the sample prepared in example 1 as a function of temperature, from fig. 2, it can be observed that the thermal conductivity of the fire retardant coating coated in example 1, which tends to decrease greatly as the temperature increases, is 0.84W · m at 800 ℃ as the thermal conductivity-1·K-1After reaching 800 ℃, the thermal conductivity tends to rise slowly due to the influence of thermal radiation and photon scattering as the temperature rises further.
Table 1 shows the thermal conductivities of examples 1 to 2 and comparative examples 1 to 3
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Thermal conductivity (W.m)-1·K-1) | 0.84 | 0.86 | 1.15 | 2.15 | 1.31 |
As can be seen from the above table 1, the fireproof coating prepared by the method is low in thermal conductivity and can play a good heat insulation role.
The samples are subjected to thermal examination at 1700 ℃, the examination time is 20 minutes, taking example 1 as an example, the change curve of the temperature along with the time in the thermal examination process is shown in fig. 3, the temperature of the back surface of the sample in the thermal examination process can be observed to be 200-300 ℃, namely the temperature gradient reaches thousands of degrees, and the fireproof coating prepared by the method has an excellent heat insulation effect and plays a good protection role on a base material.
The foregoing is merely an example of the present invention and common general knowledge of the known specific materials and characteristics thereof has not been described herein in any greater extent. It should be noted that, for those skilled in the art, without departing from the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (6)
1. The fire-retardant coating capable of resisting the high temperature of 1700 ℃ is characterized in that: the raw materials comprise aluminum hydroxide, aluminum dihydrogen phosphate, sodium carbonate, silicon dioxide, titanium diboride, titanium oxide, mica powder, calcium oxide, magnesium oxide, double rare earth tantalate, basalt fiber and a defoaming agent; the aluminum hydroxide, the aluminum dihydrogen phosphate, the sodium carbonate, the silicon dioxide, the titanium diboride, the titanium oxide, the mica powder, the calcium oxide, the magnesium oxide and the double rare earth tantalite are prepared from the following components in parts by weight: 10-12, 3-4, 2-3, 1-2, 2-3, 4-5; the mass percentage of the basalt fibers is 1-1.5%.
2. The fire retardant coating capable of resisting the high temperature of 1700 ℃ according to claim 1, wherein: the mass ratio of the defoaming agent is 1-1.5 per mill.
3. The fire retardant coating capable of resisting the high temperature of 1700 ℃ according to claim 1, wherein: the basalt fibers have a diameter of 0.8-1 mm and a length of 3-4 mm.
4. A method of preparing a 1700 ℃ high temperature resistant fire retardant coating of claim 1, wherein: the method comprises the following steps:
step 1: weighing raw materials of aluminum hydroxide, aluminum dihydrogen phosphate, sodium carbonate, silicon dioxide, titanium diboride, titanium oxide, mica powder, calcium oxide, magnesium oxide and double rare earth tantalite, taking absolute ethyl alcohol as a medium, placing the weighed raw materials into a planetary ball mill for ball milling, and drying and sieving the mixed powder;
step 2: and (3) putting the powder sieved in the step (1) into a beaker with deionized water, putting the beaker into a water bath, adding basalt fibers, stirring, adding a defoaming agent, and obtaining the high-temperature-resistant fireproof coating after the solution is in a gel state.
5. The fire retardant coating capable of resisting the high temperature of 1700 ℃ according to claim 4, wherein: in the step 1, the rotating speed of the ball mill is 300-500 r/min, the ball milling time is 600-1200 min, the temperature in the drying process is 60-80 ℃, the drying time is 10-24 h, and the powder is sieved through a 300-mesh sieve and then through a 500-mesh sieve in the sieving process.
6. The fire retardant coating capable of resisting the high temperature of 1700 ℃ according to claim 4, wherein: the temperature of the water bath kettle in the step 2 is 83-95 ℃, and the stirring speed is 500-700 r/min.
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| CN115093725B (en) * | 2022-06-23 | 2023-03-10 | 上海箬宇新材料有限公司 | 1800 ℃ resistant phosphate heat-insulating fireproof coating and preparation method thereof |
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| CN102910928B (en) * | 2012-11-13 | 2014-05-07 | 黑龙江省科学院石油化学研究院 | Preparation method of phosphate base composite material resistant to superhigh temperature of 1700 DEG C |
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