CN115651441B - Preparation method and application of transparent waterproof intumescent flame retardant coating - Google Patents
Preparation method and application of transparent waterproof intumescent flame retardant coating Download PDFInfo
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- CN115651441B CN115651441B CN202211273952.1A CN202211273952A CN115651441B CN 115651441 B CN115651441 B CN 115651441B CN 202211273952 A CN202211273952 A CN 202211273952A CN 115651441 B CN115651441 B CN 115651441B
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- 238000000576 coating method Methods 0.000 title claims abstract description 97
- 239000011248 coating agent Substances 0.000 title claims abstract description 91
- 239000003063 flame retardant Substances 0.000 title claims abstract description 69
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 4
- 230000002195 synergetic effect Effects 0.000 claims abstract description 4
- 239000011247 coating layer Substances 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 36
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 33
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 23
- 229920000877 Melamine resin Polymers 0.000 claims description 22
- 239000004640 Melamine resin Substances 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 239000010410 layer Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 12
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 11
- 235000002949 phytic acid Nutrition 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000467 phytic acid Substances 0.000 claims description 10
- 229940068041 phytic acid Drugs 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 7
- 238000002834 transmittance Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 150000005846 sugar alcohols Polymers 0.000 abstract description 5
- 150000003016 phosphoric acids Chemical class 0.000 abstract description 4
- 238000009413 insulation Methods 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract 1
- -1 melamine modified urea formaldehyde resin Chemical class 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- 238000010907 mechanical stirring Methods 0.000 description 11
- 229920005862 polyol Polymers 0.000 description 11
- 150000003077 polyols Chemical class 0.000 description 11
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 229910000831 Steel Inorganic materials 0.000 description 8
- 239000010959 steel Substances 0.000 description 8
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical class CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 7
- 229920003180 amino resin Polymers 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000002023 wood Substances 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 235000021317 phosphate Nutrition 0.000 description 5
- 239000003973 paint Substances 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical class OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 150000007974 melamines Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- DOKVLJLABBCKOJ-UHFFFAOYSA-N 6-hydrazinyl-1,3,5-triazine-2,4-diamine Chemical compound NNC1=NC(N)=NC(N)=N1 DOKVLJLABBCKOJ-UHFFFAOYSA-N 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical compound NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- NVTPMUHPCAUGCB-UHFFFAOYSA-N pentyl dihydrogen phosphate Chemical compound CCCCCOP(O)(O)=O NVTPMUHPCAUGCB-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000011150 reinforced concrete Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention relates to the technical field of intumescent flame retardance, and particularly discloses a preparation method of an intumescent transparent waterproof flame retardant coating, wherein a main raw material of the coating consists of a component A serving as a film forming agent, a component B serving as a flame retardant and a component C serving as a synergistic flame retardant; the component B is prepared by reacting phosphoric acid compounds with polyalcohol for 3-8 hours at the temperature of 80-150 ℃, and the mol ratio of the phosphoric acid compounds to the polyalcohol is 1:12-1:1; mixing the component A, the component B and the component C with a solvent to obtain the intumescent transparent waterproof flame-retardant coating. The invention also discloses application of the intumescent transparent waterproof flame-retardant coating: coating the expansion type transparent waterproof flame-retardant coating on a substrate, and then curing at a low temperature to form a coating layer; has high-efficiency heat insulation and flame retardance on the base material.
Description
Technical Field
The invention relates to the technical field of intumescent flame retardance, in particular to a preparation method and application of a transparent waterproof intumescent flame retardant coating.
Background
With the development of society, most of buildings and daily necessities are made of inflammable wood, organic polymer materials and the like, and fire disasters are easy to cause; in addition, as the thermal stability of the steel structure is inferior to that of reinforced concrete, the critical temperature for losing stability is only 540 ℃, so that the steel structure is easy to deform and distort in a fire disaster (the temperature is 800-1200 ℃), is a main cause for the collapse of the building, and is easy to cause casualties and property loss. For high polymer composite materials, wood, steel structures and other materials incapable of being internally modified, a general method for improving the flame retardant property is to coat a layer of flame retardant coating, and the intumescent flame retardant coating is widely applied due to durable heat resistance and high flame retardant efficiency.
The expansion type flame retardant coating generally comprises a film forming agent, a flame retardant and a synergistic flame retardant, wherein the carbon layer can expand in the combustion process and needs to contain an acid source, a carbon source and an air source, namely, in the combustion process, the acid source can catalyze the carbon source to form a compact carbon layer, the air source serves as a foaming agent to foam the carbon layer, so that the carbon layer forms a heat-insulating expansion carbon layer with a foam structure which is tens of times or hundreds of times of the carbon layer. For example, patent (CN 104194504 a) discloses a nano fire-retardant coating, and a preparation method and application thereof, wherein the nano fire-retardant coating is prepared by physically blending nano silicon dioxide, ethylene acetate copolymer, melamine phosphate, talcum powder and the like, and the nano silicon dioxide exists in the fire-retardant coating in a physical form for flame retardance, so that the nano fire-retardant coating has high flame retardance. Based on the flame retardant added with inorganic filler, most of the current coatings have low transparency, but for some wooden buildings or letter paper and the like, the flame retardant coatings not only need to be endowed with high flame retardance, but also need to keep the surface morphology of the flame retardant coatings clear and visible, in other words, the flame retardant coatings have higher transparency, and patent (CN 104046201A) discloses a flexible expansion type transparent fireproof coating which is prepared from polyphosphate (containing polyethylene glycol) of an A component and amino resin of a B component, has good flexibility, can be cured at room temperature, and has an expansion rate of 53 after the coating is burnt. Patent (CN 105802436 a) discloses a transparent flame-retardant coating containing nano-materials, which is grafted onto phosphate to successfully apply the nano-materials in the coating in a reactive mode, so as to reduce the influence of the nano-materials on the transparency of the coating. Patent (CN 108912939A) discloses a transparent intumescent water-based flame-retardant coating, which is prepared from phosphate, melamine resin and glass beads. However, the water resistance of the coating has a great influence on transparency, and the coating also has high water resistance, and the transparent coating is generally ultrathin, so that the strength of the carbon layer in the combustion process is low, and the expansion ratio cannot be compared with that of the non-transparent coating, so that the heat insulation resistance of the transparent coating is poor. Therefore, it is necessary to develop a high-efficiency intumescent flame-retardant transparent water-resistant coating.
Disclosure of Invention
The invention aims to provide a preparation method and application of an intumescent transparent waterproof flame-retardant coating.
In order to solve the technical problems, the invention provides a preparation method of an intumescent transparent waterproof flame retardant coating, wherein the main raw material of the coating consists of three parts, namely an A component serving as a film forming agent, a B component serving as a flame retardant and a C component serving as a synergistic flame retardant;
and (3) a component A: the mass ratio of the component B=10:1-1:10 (preferably 0.65-1.7:1), and the component C accounts for 1-10 percent (preferably 1-2.5 percent) of the total mass of the main raw materials of the coating;
the component A is amino resin or modified amino resin;
the component B is prepared by reacting phosphoric acid compounds with polyalcohol for 3-8 hours at the temperature of 80-150 ℃, and the molar ratio of the phosphoric acid compounds to the polyalcohol is 1:12-1:1 (preferably 1:1-1.6);
mixing the component A, the component B and the component C with a solvent to obtain the intumescent transparent waterproof flame-retardant coating;
the solvent accounts for 10 to 70 percent (preferably 30 to 55 percent) of the weight of the intumescent transparent waterproof flame retardant coating.
Namely, the solvent: (solvent+a component+b component+c component) =10 to 70% (preferably 30 to 55%).
As the improvement of the preparation method of the intumescent transparent waterproof flame retardant coating of the invention:
the A component is at least one (i.e., one or more) of amino resin or modified amino resin;
the amino resins include, but are not limited to, urea-formaldehyde resins, melamine resins;
the modified amino resin is melamine modified urea formaldehyde resin, starch modified urea formaldehyde resin, polyethylene glycol modified urea formaldehyde resin, methylol melamine resin, methylated melamine resin, butanol etherified melamine resin, amino melamine resin and mixed ether melamine resin.
As a further improvement of the preparation method of the intumescent transparent waterproof flame retardant coating of the invention:
the phosphoric acid compound in the component B is at least any one of the following: phytic acid, phosphoric acid, polyphosphoric acid, phytates, phosphates and derivatives thereof;
the polyol in the component B is at least any one of the following: (poly) ethylene glycol of molecular weight 62-1000, isobutanol, n-butanol, pentaerythritol, glycerol.
As a further improvement of the preparation method of the intumescent transparent waterproof flame retardant coating of the invention:
the component C is at least any one of the following: boric acid, boric acid derivatives, gamma-aminopropyl triethoxysilane derivatives.
As a further improvement of the preparation method of the intumescent transparent waterproof flame retardant coating of the invention:
mode one: the component C is mixed with the component A after reacting with the component B:
mixing the component C and the component B, reacting for 5-24 hours at the reaction temperature of 10-150 ℃, and then uniformly blending the mixture with the component A and the solvent at the temperature of 10-70 ℃ to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating);
mode two, component A, component B and component C are directly blended:
and (3) uniformly mixing the component A, the component B and the component C with a solvent directly to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
As a further improvement of the preparation method of the intumescent transparent waterproof flame retardant coating of the invention:
the solvent is at least any one of the following: water, ethanol, n-butanol, isobutanol.
The invention also provides the intumescent transparent waterproof flame-retardant coating prepared by the method, the light transmittance of the coating is up to more than 85%, the coating has excellent water resistance, and a high-expansion heat-insulating flame-retardant carbon layer can be formed.
The paint can be widely applied to various materials such as wood structures, steel structures, composite plastics and the like.
The invention also provides an application of the intumescent transparent waterproof flame-retardant coating prepared by the method: the expansion type transparent waterproof flame-retardant coating is coated on a plate (comprising a steel plate, a wood plate, quartz glass and the like) and then cured at a low temperature to form a coating layer.
The intumescent transparent waterproof flame-retardant coating has the following technical advantages:
(1) The preparation is simple, the color and luster of the raw materials can be maintained after the coating, the textures are visible, and the light transmittance is as high as more than 85 percent; therefore, the transparency is high;
(2) Has excellent water resistance;
(3) Forming a high-expansion heat-insulating flame-retardant carbon layer: the paint has less smoke yield in the combustion process, can form a compact high-expansion carbon layer, and has high-efficiency heat insulation and flame retardance on a base material (plate);
(4) The paint can be widely applied to various materials such as wood structures, steel structures, composite plastics and the like.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a photograph of an expanded carbon layer of a steel sheet coated with the flame retardant coating prepared in example 1 after burning the large sheet.
In fig. 1, the left side view is a front view of the post-combustion expanded carbon layer, and the right side view is a side view of the post-combustion expanded carbon layer.
Fig. 2 is a photograph of the flame retardant coating prepared in example 1 after it is applied to a wood board and dried.
Detailed Description
The invention will be further described with reference to the following specific examples, but the scope of the invention is not limited thereto:
the normal temperature is 20-30 ℃.
1. The preparation examples of the intumescent transparent waterproof flame retardant coating of the invention are as follows:
example 1
The component A is 35.0g of methylated melamine resin; the component B is prepared by the following method: 10.0g phytic acid, 5g phosphoric acid and 13.6g pentaerythritol were added to a three-necked flask equipped with mechanical stirring (i.e., 3:5 molar ratio of phosphate compound to polyol); reacting at 120 ℃ for 8 hours to prepare a component B; the C component is 1.0g boric acid.
Stirring and reacting the component C and the component B for 10 hours at 120 ℃, cooling the reaction to normal temperature, adding the component A, adding 33.0g of isobutanol (as a solvent), and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
Example 2:
the component A is 40.0g of melamine resin; the component B is prepared by the following method: 10.0g phytic acid, 5g phosphoric acid and 13.6g pentaerythritol were added to a three-necked flask equipped with mechanical stirring (i.e., 3:5 molar ratio of phosphate compound to polyol); reacting at 100 ℃ for 8 hours to prepare a component B; the C component is 1.0g boric acid.
Stirring and reacting the component C and the component B for 8 hours at 120 ℃, cooling the reaction to normal temperature, adding the component A and 48.0g of isobutanol, and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
Example 3:
the component A is 40.0g of melamine resin; the component B is prepared by the following method: 10.0g of phosphoric acid and 13.6g of pentaerythritol are added into a three-neck flask with mechanical stirring (namely, the mol ratio of phosphoric acid compound to polyol is 1:1), and the mixture is reacted for 5 hours at 80 ℃ to prepare a component B; the C component is 1.5g boric acid.
Stirring and reacting the component C and the component B for 10 hours at 120 ℃, cooling the reaction to normal temperature, adding the component A and adding 30.0g of n-butyl alcohol, and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
Example 4:
the component A is 45.0g of melamine resin; the component B is prepared by the following method: 5.0g of phosphoric acid, 10.0g of phytic acid and 20.0g of polyethylene glycol 200 are added into a three-neck flask with mechanical stirring (namely, the mol ratio of phosphoric acid compound to polyalcohol is 3:5), and the mixture is reacted for 7 hours at 110 ℃ to prepare a component B; the C component is 2.0g boric acid.
Stirring and reacting the component C and the component B for 10 hours at 120 ℃, cooling the reaction to normal temperature, adding the component A and 40.0g of n-butyl alcohol, and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
Example 5:
the component A is 45.0g of melamine resin; the component B is prepared by the following method: 15.0g of phosphoric acid, 10g of phytic acid and 40.0g of polyethylene glycol 200 are added into a three-neck flask with mechanical stirring (namely, the mole ratio of phosphoric acid compound to polyol is 4:5), and the mixture is reacted for 5 hours at 100 ℃ to prepare a component B; the C component is 2.0g of gamma-aminopropyl triethoxysilane.
Stirring and reacting the component C and the component B for 10 hours at 120 ℃, cooling the reaction to normal temperature, adding the component A, adding 51.0g of mixed solution of n-butanol and ethanol (31.0 g of n-butanol and 20.0g of ethanol), and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
Example 6:
the component A is 45.0g of melamine resin; the component B is prepared by the following method: 15.5g of phosphoric acid, 10.0g of pentaerythritol and 20.0g of polyethylene glycol 200 are added into a three-neck flask with mechanical stirring (namely, the mol ratio of phosphoric acid compound to polyol is 9:10) and reacted for 5 hours at 100 ℃ to prepare a component B; the C component is 1.0g of gamma-aminopropyl triethoxysilane.
Stirring and reacting the component C and the component B for 5 hours at 80 ℃, cooling the reaction to normal temperature, adding the component A, adding 58.0g of isobutanol and ethanol mixed solution (20.0 g of isobutanol and 38.0g of ethanol), and uniformly mixing to obtain the intumescent transparent waterproof flame retardant coating (liquid coating).
Example 7:
the component A is 40.0g of melamine resin; the component B is prepared by the following method: 15.5g of phosphoric acid, 10.0g of pentaerythritol and 20.0g of polyethylene glycol 200 are added into a three-neck flask with mechanical stirring (namely, the mol ratio of phosphoric acid compound to polyol is 9:10), and the mixture is reacted for 8 hours at 150 ℃ to prepare a component B; the C component is 2.0g of gamma-aminopropyl triethoxysilane.
Stirring and reacting the component C and the component B for 10 hours at 80 ℃, cooling the reaction to normal temperature, adding the component A, adding 82.0g of ethanol, and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
Example 8:
the component A is 40.0g of melamine resin; the component B is prepared by the following method: 18.0g of phosphoric acid, 8.0g of phytic acid, 10.0g of pentaerythritol and 20.0g of polyethylene glycol 200 are added into a three-neck flask with mechanical stirring (namely, the mol ratio of phosphoric acid compound to polyol is 1:1), and the mixture is reacted for 4 hours at 150 ℃ to prepare a component B; the C component is 1.0g of gamma-aminopropyl triethoxysilane.
Stirring and reacting the component C and the component B for 10 hours at 120 ℃, cooling the reaction to normal temperature, adding the component A and 50.0g of n-butyl alcohol, and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating (liquid coating).
Example 9:
the component A is 40.0g of melamine resin; the component B is prepared by the following method: 18.0g of phosphoric acid, 8.0g of phytic acid, 10.0g of pentaerythritol and 20.0g of polyethylene glycol 200 are added into a three-neck flask with mechanical stirring (namely, the mol ratio of phosphoric acid compound to polyol is 1:1), and the mixture is reacted for 4 hours at 150 ℃ to prepare a component B; the C component is 1.0g of gamma-aminopropyl triethoxysilane.
The component A, the component B and the component C are evenly mixed at normal temperature, 50.0g of n-butyl alcohol is added and evenly mixed, and the intumescent transparent waterproof flame retardant coating (liquid coating) is obtained.
Comparative example 1:
the component A is 40.0g of melamine resin; the component B is prepared by the following method: 10.0g of phosphoric acid and 13.6g of pentaerythritol are added into a three-neck flask with mechanical stirring (namely, the mol ratio of phosphoric acid compound to polyol is 1:1), and the mixture is reacted for 8 hours at 80 ℃ to prepare a component B; uniformly mixing the component B with the component A and 32.0g of n-butanol at normal temperature; obtaining the coating.
Comparative example 2:
the component A is 40.0g of melamine resin; the component B is prepared by the following method: 20.0g of phytic acid and 13.6g of pentaerythritol are added into a three-neck flask with mechanical stirring (namely, the mole ratio of phosphoric acid compound to polyol is 1:5), and the mixture is reacted for 8 hours at 100 ℃ to prepare a component B; uniformly mixing the component B with the component A and 38.0g of n-butanol at normal temperature; obtaining the coating.
Comparative example 3:
the component A is 40.0g of melamine resin, the component B is 35.0g of acid amyl phosphate, the component C is 2.0g of gamma-aminopropyl triethoxysilane, and the component A, the component B and the component C are uniformly mixed with 40.0g of n-butanol at normal temperature; obtaining the coating.
Comparative example 4: relative to example 4, the prior preparation of the B component was cancelled, namely specifically:
the component A is 45.0g of melamine formaldehyde resin; the component B consists of 5.0g of phosphoric acid, 10.0g of phytic acid and 20.0g of polyethylene glycol 200; the C component is 2.0g boric acid.
Stirring the component C and the component B at 120 ℃ for reaction for 10 hours, cooling the reaction to normal temperature, adding the component A and adding 40.0g of n-butanol, and uniformly mixing to obtain the coating.
(II) paint performance test:
1. flame retardant test:
the coatings obtained in examples 1 to 9 and comparative examples 1 to 4 were applied to steel sheets, respectively, and cured at low temperature (24 hours at 25 ℃) so that the thickness of the cured coating was 0.4.+ -. 0.02mm. The test was performed as follows:
the water resistance was measured according to GB 1733-1993 and the light transmittance of the coating was measured using a light transmittance meter. The large panel combustion method was tested according to GB 12441-2018. The decomposition temperature was analyzed using thermogravimetric analysis. The expansion ratio of the carbon layer is calculated by adopting the ratio of the expansion height of the carbon layer to the thickness of the coating. The method is simple and easy to implement, and can be used for comparing the basic performances of the flame retardant coating prepared by different schemes.
The results obtained are shown in Table 1 below.
2. Transparency experiment:
the coatings obtained in examples 1 to 9 and comparative examples 1 to 4 were applied to quartz glass, respectively, so that the thickness of the cured coating was 0.2.+ -. 0.02mm. The experimental mode is as follows: and the ultraviolet-visible near-infrared spectrophotometer is adopted for light transmittance test, and the wavelength range is 200-1200nm. The final value of the coating is the average of five determinations.
The results obtained are shown in Table 1 below.
TABLE 1
Finally, it should also be noted that the above list is merely a few specific embodiments of the present invention. Obviously, the invention is not limited to the above embodiments, but many variations are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (4)
1. A preparation method of an intumescent transparent waterproof flame-retardant coating is characterized by comprising the following steps: the main raw material of the coating consists of a component A serving as a film forming agent, a component B serving as a flame retardant and a component C serving as a synergistic flame retardant;
the component A is 45.0g of melamine resin; the component B is prepared by the following method: 5.0g of phosphoric acid, 10.0g of phytic acid and 20.0g of polyethylene glycol 200, and reacting for 7 hours at 110 ℃ to prepare a component B; 2.0g boric acid as component C;
stirring and reacting the component C and the component B for 10 hours at 120 ℃, cooling the reaction to normal temperature, adding the component A and adding 40.0g of n-butyl alcohol, and uniformly mixing to obtain the intumescent transparent waterproof flame-retardant coating.
2. An intumescent transparent water-resistant flame retardant coating prepared by the method of claim 1.
3. The intumescent, transparent, water-resistant, flame retardant coating of claim 2, wherein: the light transmittance of the coating is up to more than 85%, the coating has excellent water resistance, and a high-expansion heat-insulating flame-retardant carbon layer can be formed.
4. The application of the intumescent transparent waterproof flame retardant coating prepared by the method of claim 1, which is characterized in that:
and (3) coating the expansion type transparent waterproof flame-retardant coating on a plate, and then curing at a low temperature to form a coating layer.
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| CN104046201A (en) * | 2014-03-28 | 2014-09-17 | 上海大学 | Flexible expandable transparent fireproof paint and preparation method thereof |
| CN105860742A (en) * | 2016-05-18 | 2016-08-17 | 湖南浩盛消防科技有限公司 | Low-smoke expansive type transparent fire-retardant coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104046201A (en) * | 2014-03-28 | 2014-09-17 | 上海大学 | Flexible expandable transparent fireproof paint and preparation method thereof |
| CN105860742A (en) * | 2016-05-18 | 2016-08-17 | 湖南浩盛消防科技有限公司 | Low-smoke expansive type transparent fire-retardant coating and preparation method thereof |
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