CN110591424B - A kind of preparation method of aluminum phosphate glue-based halogen-free high-expansion flame-retardant heat-insulating fire-retardant coating - Google Patents
A kind of preparation method of aluminum phosphate glue-based halogen-free high-expansion flame-retardant heat-insulating fire-retardant coating Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 100
- 239000011248 coating agent Substances 0.000 title claims abstract description 94
- 239000003063 flame retardant Substances 0.000 title claims abstract description 46
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 title claims abstract description 36
- 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 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003292 glue Substances 0.000 title abstract 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 19
- 239000004816 latex Substances 0.000 claims abstract description 19
- 229920000126 latex Polymers 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 15
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 14
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 9
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 9
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 9
- 229910052902 vermiculite Inorganic materials 0.000 claims abstract description 9
- 239000010455 vermiculite Substances 0.000 claims abstract description 9
- 235000019354 vermiculite Nutrition 0.000 claims abstract description 9
- 229910021538 borax Inorganic materials 0.000 claims abstract description 8
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 8
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 8
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 8
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- 238000005054 agglomeration Methods 0.000 claims description 5
- 230000002776 aggregation Effects 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 2
- 239000001273 butane Substances 0.000 abstract description 12
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 abstract description 12
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 9
- 239000007921 spray Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 6
- 238000005187 foaming Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 3
- 239000002023 wood Substances 0.000 abstract description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000011152 fibreglass Substances 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 13
- 239000010959 steel Substances 0.000 description 13
- 238000007664 blowing Methods 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- NTGGOTYRTOXKMQ-UHFFFAOYSA-K aluminum;potassium;phosphate Chemical compound [Al+3].[K+].[O-]P([O-])([O-])=O NTGGOTYRTOXKMQ-UHFFFAOYSA-K 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
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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)
- Fireproofing Substances (AREA)
- Paints Or Removers (AREA)
Abstract
一种磷酸铝胶基无卤高膨胀型阻燃隔热防火涂料制备方法。其包括利用聚磷酸铵、硼酸钠、硝酸钾、莫来石粉、α‑氧化铝、蛭石粉预制骨料，利用氢氧化铝和磷酸反应生成的乳胶液体作为基体，将骨料与乳胶液体混合制备防火涂料等步骤。本发明效果：涂料界面粘结效果好，可润湿并粘附于多种材料，且在火烧后与被保护基体之间粘结牢固，适用于金属材质、玻璃钢、木制品等多种材料；涂料遇火后发泡膨胀性高，1.5mm的厚度在遇火后可膨胀至11mm，膨胀率高达633％，且内部形成大小不一的孔洞及似海绵层；防火涂料在20min时间内可将的丁烷喷枪火焰(900～1100℃)隔温降低至不高于130℃，10min时间内降低至不高于90℃。
A preparation method of aluminum phosphate glue-based halogen-free high-expansion flame-retardant heat-insulating fire-retardant coating. It includes using ammonium polyphosphate, sodium borate, potassium nitrate, mullite powder, α-alumina, vermiculite powder to prefabricate aggregate, using the latex liquid generated by the reaction of aluminum hydroxide and phosphoric acid as a matrix, and mixing the aggregate and latex liquid to prepare. Fire retardant coating and other steps. Effects of the invention: the coating interface has good bonding effect, can be wetted and adhered to various materials, and is firmly bonded to the protected substrate after burning, and is suitable for various materials such as metal materials, glass fiber reinforced plastics, and wood products; The coating has high foaming expansion after encountering fire. The thickness of 1.5mm can expand to 11mm after encountering fire, and the expansion rate is as high as 633%, and holes of different sizes and sponge-like layers are formed inside; The temperature of the butane spray gun flame (900-1100°C) is reduced to no higher than 130°C, and it is lowered to no higher than 90°C within 10 minutes.
Description
Technical Field
The invention belongs to the technical field of fireproof coating preparation, and particularly relates to a preparation method of an aluminum phosphate gum base halogen-free high-expansion type flame-retardant heat-insulation fireproof coating which is pure inorganic, green, environment-friendly, nontoxic, odorless, strong in universality, high in expansibility and excellent in flame-retardant heat-insulation effect.
Background
The fire-retardant coating is a non-combustible or flame-retardant substance which is coated on the surface of a combustible substrate and effectively prevents the substrate from burning or has a retarding effect on the burning spread of the substrate by reducing the heat conductivity coefficient or improving the thermal resistance. The fire-retardant coating is classified according to its components, and can be classified into oil-based organic type, all-inorganic type and organic/inorganic composite type coatings. The all-inorganic coating has the advantages of wide and cheap sources of required raw materials, simple preparation process, low production cost, A-level fireproof standard, no need of any organic auxiliary agent and the like, so that no unpleasant or toxic odor is released in the production, construction and use processes before fire hazard occurs, and the all-inorganic coating highly meets the requirements of environmental protection.
However, most of all-inorganic fire-retardant coatings belong to non-intumescent thick-coating steel structure fire-retardant coatings, and have the defects of single universality, poor decorative finish and the like. Compared with non-expansion type coating, the expandable coating has the advantages of light weight, better heat insulation effect, higher fire resistance limit, stronger decoration, wider applicability and the like. However, most of the expandable coatings are organic type or organic/inorganic composite type, and there are few reports on all-inorganic type fire-retardant coatings capable of expanding with high foaming. Meanwhile, most of all inorganic fireproof coatings use water as a matrix solution, so that the defects of poor fluidity, low interface bonding strength and the like exist. Based on the analysis, the preparation of the all-inorganic fireproof coating with strong universality, good bonding effect, high foaming expansion and excellent flame-retardant and heat-insulating effects is urgently needed.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of an aluminum phosphate gum base halogen-free high-expansion flame-retardant heat-insulating fireproof coating.
In order to achieve the aim, the preparation method of the aluminum phosphate gum base halogen-free high-expansion flame-retardant heat-insulating fireproof coating provided by the invention comprises the following steps in sequence:
(1) mixing ammonium polyphosphate, sodium borate, potassium nitrate, mullite powder, alpha-alumina and vermiculite powder according to the mass ratio of 3.5-7: 0.7-1.3: 1.5-2.5: 5-7: 1-3: 0.1-0.45, then putting the mixture into a planetary ball mill, and carrying out ball milling for 5 hours at the rotating speed of 250r/min to obtain aggregate with refined granularity and uniform mixing;
(2) diluting concentrated phosphoric acid with the concentration of 85% with water to obtain diluted phosphoric acid with the concentration of 60%, and then putting the diluted phosphoric acid into a water bath kettle with a stirrer to heat to 80-85 ℃ for later use;
(3) slowly adding aluminum hydroxide powder into the diluted phosphoric acid prepared in the step (2) while stirring to prevent flowability from being reduced due to agglomeration, wherein the molar ratio of aluminum to phosphorus is 0.5-1: 1, so as to prepare a white aluminum phosphate latex liquid, and continuously stirring until the viscosity of the liquid reaches 1400-1800 mPa & s;
(4) and (3) mixing the aggregate prepared in the step (1) and the aluminum phosphate latex liquid prepared in the step (3) at normal temperature according to the mass ratio of 1.3-1.7: 1, and uniformly stirring to prepare the aluminum phosphate gum base halogen-free high-expansion type flame-retardant heat-insulating fireproof coating.
In the step (1), the ammonium polyphosphate, the sodium borate and the potassium nitrate are purchased from Guangzhou Kogyo of Tianjin and have high-grade quality;
in the step (1), the mullite powder and the alpha-alumina are purchased from Shanghai Liangjiang titanium white chemical products, Inc., and the particle size is 3-8 μm;
in the step (1), the vermiculite powder is purchased from an Anda mineral powder factory in Lingshou county, and the granularity is 600 meshes;
in the step (3), the liquid viscosity test adopts an NDJ-8S viscosity test instrument produced by Shanghai Changji geological instruments GmbH;
the preparation method of the aluminum phosphate gum base halogen-free high-expansion flame-retardant heat-insulating fireproof coating provided by the invention has the following beneficial effects:
1. the coating has good interface bonding effect, uses white aluminum phosphate latex liquid as a substrate material, has high viscosity, can be wetted and adhered to various materials, is firmly bonded with a protected matrix after being fired, and is not easy to fall off;
2. the coating has high universality, and can be suitable for the surfaces of various materials such as metal materials, glass fiber reinforced plastics, wood products, fiber cloth, polyurethane, even organic gel coats and the like;
3. the foaming expansibility is high, and for a coating with the coating thickness of 1.5mm, the coating can be expanded to 8-11 mm under the flame (900-1100 ℃) of a butane spray gun, and the linear expansion rate is 433-633%; after burning, the coating is filled with a plurality of bubbles with different sizes;
4. the flame-retardant heat-insulation effect is excellent, and for a thin steel plate coated with a coating with the thickness of 1.5mm, after the thin steel plate is directly blown by a butane flame spray gun (900-1100 ℃) for about 10min, the surface temperature of the coating is 941 ℃, and the back temperature of the thin steel plate is only 84.1 ℃; after a butane flame spray gun (900-1100 ℃) is used for direct blowing for about 20min, the surface temperature of the coating is 1005.2 ℃, and the back surface temperature of the thin steel plate is only 128.1 ℃. In addition, the coating has no combustion and no carbonization in the whole burning process;
5. the high-temperature product has low heat conductivity, and after being treated by a butane flame spray gun, the coating mainly comprises ceramic phases such as mullite, alumina and aluminum phosphate which have low heat conductivity and high temperature resistance.
Drawings
FIG. 1 is a macro-micro-topography observation of a coating formed by applying the fire retardant coating prepared in example 3 on a polymer latex board after butane flame direct blowing for 10min, wherein FIG. 1a is an appearance performance, FIG. 1b is a topography of a protected part under the coating, FIG. 1c is a cross-sectional topography of the coating after expansion in fire, and FIG. 1d is a micro-topography of the coating after expansion in fire;
FIGS. 2a and 2b are thickness comparisons of a coating layer formed by applying the fireproof paint prepared in example 1 on a steel sheet before and after burning of butane flame, respectively;
FIG. 3 is an XRD pattern of the fire retardant coating prepared in example 1 after flame ignition at different temperatures.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1 (aluminum phosphate gum based halogen-free high expansion type flame retardant, heat insulating and fire retardant coating for metal material)
The preparation method of the aluminum phosphate gum base halogen-free high-expansion flame-retardant heat-insulating fireproof coating provided by the embodiment comprises the following steps in sequence:
(1) mixing ammonium polyphosphate, sodium borate, potassium nitrate, mullite powder, alpha-alumina and vermiculite powder according to the mass ratio of 3.5:1:2.5:6:2:0.45, then putting the mixture into a planetary ball mill, and carrying out ball milling for 5 hours at the rotating speed of 250r/min to obtain aggregate with refined granularity and uniformly mixed;
(2) diluting concentrated phosphoric acid with concentration of 85% with water to obtain diluted phosphoric acid with concentration of 60%, and heating to 85 deg.C in water bath with stirring;
(3) slowly adding aluminum hydroxide powder into the diluted phosphoric acid prepared in the step (2) while stirring to prevent the fluidity from being reduced due to agglomeration, wherein the molar ratio of aluminum to phosphorus is 0.5:1, so as to prepare a white aluminum phosphate latex liquid, and continuously stirring until the viscosity of the liquid reaches 1400mPa & s;
(4) and (3) mixing the aggregate prepared in the step (1) and the aluminum phosphate latex liquid prepared in the step (3) at normal temperature according to the mass ratio of 1.7:1, and uniformly stirring to prepare the aluminum phosphate gum base halogen-free high-expansion type flame-retardant heat-insulating fireproof coating.
Example 2 (aluminum phosphate gum based halogen-free high expansion type flame retardant, thermal insulating and fire retardant coating for wood products)
(1) Mixing ammonium polyphosphate, sodium borate, potassium nitrate, mullite powder, alpha-alumina and vermiculite powder according to the mass ratio of 5:0.7:2:7:1:0.1, then putting the mixture into a planetary ball mill, and carrying out ball milling for 5 hours at the rotating speed of 250r/min to obtain aggregate with refined granularity and uniform mixing;
(2) diluting concentrated phosphoric acid with concentration of 85% with water to obtain diluted phosphoric acid with concentration of 60%, and heating to 85 deg.C in water bath with stirring;
(3) slowly adding aluminum hydroxide powder into the diluted phosphoric acid prepared in the step (2) while stirring to prevent the flowability from being reduced due to agglomeration, wherein the molar ratio of aluminum to phosphorus is 0.75:1, so as to prepare a white aluminum phosphate latex liquid, and continuously stirring until the viscosity of the liquid reaches 1600mPa & s;
(4) and (3) mixing the aggregate prepared in the step (1) and the aluminum phosphate latex liquid prepared in the step (3) at normal temperature according to the mass ratio of 1.5:1, and uniformly stirring to prepare the aluminum phosphate gum base halogen-free high-expansion type flame-retardant heat-insulating fireproof coating.
Example 3 (Aluminophosphate-based halogen-free high-expansion flame-retardant, insulating and fire-retardant coating for organic articles)
(1) Mixing ammonium polyphosphate, sodium borate, potassium nitrate, mullite powder, alpha-alumina and vermiculite powder according to the mass ratio of 7:1.3:1.5:6:3:0.1, then putting the mixture into a planetary ball mill, and carrying out ball milling for 5 hours at the rotating speed of 250r/min to obtain aggregate with refined granularity and uniformly mixed;
(2) diluting concentrated phosphoric acid with concentration of 85% with water to obtain diluted phosphoric acid with concentration of 60%, and heating to 80 deg.C in water bath with stirring;
(3) slowly adding aluminum hydroxide powder into the diluted phosphoric acid prepared in the step (2) while stirring to prevent the fluidity from being reduced due to agglomeration, wherein the molar ratio of aluminum to phosphorus is 1:1, so as to prepare white aluminum phosphate latex liquid, and continuously stirring until the liquid viscosity reaches 1800mPa & s;
(4) and (3) mixing the aggregate prepared in the step (1) and the aluminum phosphate latex liquid prepared in the step (3) at normal temperature according to the mass ratio of 1.3:1, and uniformly stirring to prepare the aluminum phosphate gum base halogen-free high-expansion type flame-retardant heat-insulating fireproof coating.
In the aluminum phosphate gum base halogen-free high-expansion type flame-retardant heat-insulating fireproof coating provided by the invention, aluminum phosphate white latex liquid generated by the reaction of aluminum hydroxide and phosphoric acid is used as a main binding phase of the fireproof coating, so that effective interface binding strength can be provided for various protected base materials. Meanwhile, the aluminum phosphate latex liquid can be self-cured at normal temperature, so that the applicability of the coating is greatly improved. Ammonium polyphosphate, sodium borate and potassium nitrate are used as foaming agents of the coating, and the coating is rapidly decomposed when encountering fire, so that a compact coating is changed into an expanded coating with a multi-bubble structure, and generated bubbles are utilized to improve thermal resistance and organize flame burn-through. Meanwhile, the ammonium polyphosphate can also be used as a flame retardant of the fireproof coating at a lower temperature. Mullite and alumina are important flame retardants and heat insulators of the fireproof coating as a flame-retardant high-temperature resistant phase with low thermal conductivity. The vermiculite has higher thermal expansion coefficient, and is mainly used for adjusting the thermal expansion of the fireproof coating so as to adapt to the thermal expansion of different substrates.
In order to verify the effect of the fire retardant coating provided by the above embodiment, the inventors performed the following experiment:
1) flatly paving the polished, cleaned and dried thin steel plate and the high polymer latex plate on a smooth and pure glass plate, and placing the glass plate with the protected surface facing upwards;
2) the fireproof coating prepared in the embodiment 1 is simply coated on the protected surface of the thin steel plate by a brush, and then the coating is uniformly coated by a coater, wherein the thickness of the coating is controlled to be 1.5 mm; the fireproof coating prepared in the embodiment 3 is simply coated on the protected surface of the polymer latex plate by a brush, and then the coating is uniformly coated by a coater, wherein the thickness of the coating is controlled to be 1.5 mm;
3) the coating is cured for 2 to 3 days at room temperature and then put into use.
4) And (3) testing the flame-retardant heat-insulating property:
directly blowing the coating formed on the surface of the thin steel plate by the fireproof coating prepared in the embodiment 1 by using a butane flame spray gun (900-1100 ℃), testing the surface temperature of the coating at the flame direct-blowing part by using an infrared thermometer, and simultaneously detecting the back surface temperature of the thin steel plate by using a thermocouple thermometer, wherein after about 10min, the surface temperature of the coating is 941 ℃, and the back surface temperature of the thin steel plate is only 84.1 ℃; after about 20min, the coating surface temperature was 1005.2 ℃ and the steel sheet back surface temperature was only 128.1 ℃. In addition, the fire-retardant coating is free of combustion and carbonization in the whole burning process.
② directly blowing and coating the fire-proof coating prepared in the embodiment 3 on the surface of the polymer latex plate by using a butane flame spray gun (900-1100 ℃), and comparing the combustion state of the peripheral part of the coating and the protected part under the coating after 10min, as shown in figure 1. As can be seen from fig. 1a, the part of the coating not coated with the fireproof paint is already yellow under the action of heat radiation, and the phenomenon of peeling and splashing is generated. Fig. 1b is a photograph of the protected area where the coating was scraped off, and it can be clearly seen that the color of the protected area remains white. The comparison between fig. 1a and fig. 1b can effectively illustrate that the fireproof coating has excellent flame retardant and heat insulation properties.
5) Observing macro-micro morphology of the coating after encountering fire: the cross section of the coating scraped off in the above step (c) was observed with the naked eye as shown in fig. 1 c. From fig. 1c, it is clear that various bubbles with different sizes are generated under the action of the foaming agent, and the thermal conductivity of the coating can be effectively reduced. In addition, the microscopic morphology of the scraped-off coating was observed using a scanning electron microscope, as shown in FIG. 1 d. As can be seen from FIG. 1d, the interior of the coating is filled with a large number of micro-pores, which are shaped like a foam structure.
6) Examination of expansion Properties in foaming: comparative coating with the fire retardant coating prepared in example 1 the thickness of the coating formed on the steel sheet before and after the fire was encountered is shown in FIG. 2. FIG. 2a shows the coating thickness before direct blowing of a butane flame, which is about 1.5 mm; FIG. 2b shows the thickness of the coating layer after 20min of direct blowing of butane flame, at which time the thickness expands to 8-11 mm. Therefore, the linear expansion rate of the fireproof coating is 433-633%.
7) Component analysis of the coating: the components of the fireproof coating prepared in example 1 after flame treatment at different temperatures were analyzed by an XRD tester (D/Max 2500v/PC, Rigaku), and the corresponding XRD pattern is shown in FIG. 3;
after flame combustion treatment at different temperatures, the fireproof coating always contains two components of mullite and alumina. After being burnt by flame (300-400 ℃) of a common lighter, the fireproof coating contains potassium aluminum phosphate, hydroxyl alumina, mullite and alumina; after the household natural gas flame (800-900 ℃) burns, the components are aluminum phosphate, alumina, mullite and aluminum potassium phosphate; and finally, under the combustion of butane spray gun flame (900-1100 ℃), the aluminum potassium phosphate disappears, and only aluminum phosphate, mullite and a small amount of alumina remain in the components. The above products all have very low thermal conductivity.
Claims (3)
1. The preparation method of the aluminum phosphate gum base halogen-free high-expansion flame-retardant heat-insulating fireproof coating is characterized by comprising the following steps of: the preparation method of the aluminum phosphate gum base halogen-free high-expansion flame-retardant heat-insulating fireproof coating comprises the following steps in sequence:
(1) mixing ammonium polyphosphate, sodium borate, potassium nitrate, mullite powder, alpha-alumina and vermiculite powder according to the mass ratio of 3.5-7: 0.7-1.3: 1.5-2.5: 5-7: 1-3: 0.1-0.45, then putting the mixture into a planetary ball mill, and carrying out ball milling for 5 hours at the rotating speed of 250r/min to obtain aggregate with refined granularity and uniform mixing;
(2) diluting concentrated phosphoric acid with the concentration of 85% with water to obtain diluted phosphoric acid with the concentration of 60%, and then putting the diluted phosphoric acid into a water bath kettle with a stirrer to heat to 80-85 ℃ for later use;
(3) slowly adding aluminum hydroxide powder into the diluted phosphoric acid prepared in the step (2) while stirring to prevent flowability from being reduced due to agglomeration, wherein the molar ratio of aluminum to phosphorus is 0.5-1: 1, so as to prepare a white aluminum phosphate latex liquid, and continuously stirring until the viscosity of the liquid reaches 1400-1800 mPa & s;
(4) and (3) mixing the aggregate prepared in the step (1) and the aluminum phosphate latex liquid prepared in the step (3) at normal temperature according to the mass ratio of 1.3-1.7: 1, and uniformly stirring to prepare the aluminum phosphate gum base halogen-free high-expansion type flame-retardant heat-insulating fireproof coating.
2. The preparation method of the aluminum phosphate gum based halogen-free high-expansion flame-retardant heat-insulating fireproof coating as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), the grain diameter of the mullite powder and the alpha-alumina is 3-8 μm.
3. The preparation method of the aluminum phosphate gum based halogen-free high-expansion flame-retardant heat-insulating fireproof coating as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), the particle size of the vermiculite powder is 600 meshes.
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| CN115433479B (en) * | 2022-10-18 | 2023-06-27 | 中国民航大学 | Preparation method of phosphate gum base flame-retardant heat-insulating coating with high ceramization degree in fire |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102282221A (en) * | 2008-02-12 | 2011-12-14 | 邦基化肥股份有限公司 | Aluminum phosphate slurry |
| CN102485684A (en) * | 2010-12-02 | 2012-06-06 | 北京仁创科技集团有限公司 | Fireproof coating composition and fireproof steel material |
| CN103467774A (en) * | 2013-09-24 | 2013-12-25 | 北京工商大学 | Composition applicable to surface flame retardance of rigid polyurethane foam insulation board |
| CN108165157A (en) * | 2018-02-02 | 2018-06-15 | 东周化学工业（昆山）有限公司 | A kind of water expansion heat-insulating flame-retardant suppression cigarette coating and its coating process |
| CN110305551A (en) * | 2019-07-12 | 2019-10-08 | 顺德职业技术学院 | Novel water-based intumescent flame retardant coating and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102282221A (en) * | 2008-02-12 | 2011-12-14 | 邦基化肥股份有限公司 | Aluminum phosphate slurry |
| CN102485684A (en) * | 2010-12-02 | 2012-06-06 | 北京仁创科技集团有限公司 | Fireproof coating composition and fireproof steel material |
| CN103467774A (en) * | 2013-09-24 | 2013-12-25 | 北京工商大学 | Composition applicable to surface flame retardance of rigid polyurethane foam insulation board |
| CN108165157A (en) * | 2018-02-02 | 2018-06-15 | 东周化学工业（昆山）有限公司 | A kind of water expansion heat-insulating flame-retardant suppression cigarette coating and its coating process |
| CN110305551A (en) * | 2019-07-12 | 2019-10-08 | 顺德职业技术学院 | Novel water-based intumescent flame retardant coating and preparation method thereof |
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