CN116162372A - A flame retardant thermal insulation coating - Google Patents

Abstract

The invention relates to a flame-retardant thermal insulation coating, which belongs to the technical field of thermal insulation coatings. The flame retardant thermal insulation coating of the present invention is mainly made of water, emulsion, aerogel, flame retardant-coated hollow glass microspheres and auxiliary agents; The ratio is 20-50:3-10:30-50. The flame retardant and thermal insulation coating of the present invention uses airgel and flame retardant-coated hollow glass microspheres as the main thermal insulation material, and utilizes the flame retardant coated on the surface of the hollow glass microspheres in the flame retardant coating hollow glass microspheres, Increase the wall thickness of the hollow glass microspheres, improve the pressure resistance of the hollow glass microspheres in the coating, reduce the breakage rate of the hollow glass microspheres in the coating and coating, and avoid the attenuation of the thermal insulation performance of the coating; and The flame retardant is coated on the surface of the hollow glass microspheres and added to the paint, which can also increase the contact surface of the flame retardant in the paint and improve the flame retardancy of the paint.

Description

A flame retardant thermal insulation coating

technical field

The invention relates to a flame-retardant thermal insulation coating, which belongs to the technical field of thermal insulation coatings.

Background technique

In the existing technology, traditional thermal insulation materials such as rock wool felt, inorganic thermal insulation mortar, polystyrene foam board, etc. are widely used, but the use of these traditional thermal insulation materials must reach a certain thickness to have good thermal insulation performance , It is time-consuming and labor-intensive in construction, and the construction quality determines its poor waterproof performance. For outdoors, there is still sunlight exposure that is prone to cracking and water seepage of the insulation layer, which directly affects the anti-corrosion performance of the metal surface. The use of organic polymer foam material insulation layer, its flame resistance is relatively poor, there is a certain fire hazard. For example, the process of installing traditional thermal insulation materials on the surface of large oil tanks and gas tanks in the factory is complicated, the cost is high, and the fire hazard is great. Therefore, in recent years, new insulation materials are being developed at home and abroad to replace traditional insulation materials.

Thermal insulation coating is a new type of thermal insulation material, a coating that achieves thermal insulation through low thermal conductivity and high thermal resistance. Among them, the development of lightweight, thin-layer nano-insulation coatings with hollow microspheres as the main filler has become a research hotspot in this field. For example, in the prior art, the application publication number is CN108329780A, which discloses a waterproof and heat-insulating exterior wall coating. The waterproof and heat-insulating exterior wall coating mainly includes the following components: 22-42 parts of silicon acrylic emulsion, ₁₂ parts of nano-SiO2 airgel -18 parts, 5-12 parts of aluminum silicate fiber, 8-15 parts of hollow glass microspheres, 4-9 parts of pigments and fillers, 3-7 parts of expanded vermiculite, 1.3-2.8 parts of dispersant, 0.6-1.4 parts of leveling agent 1.6-3.8 parts of coalescent, 13-18 parts of deionized water. This new type of thermal insulation coating uses nano- _SiO2 airgel, hollow glass microspheres and expanded vermiculite as thermal insulation materials to add to the coating, which can improve the thermal insulation performance of the coating. However, because the hollow glass microspheres are hollow and the walls are thin, The compressive capacity is small, and the coating is easy to break during the actual coating construction (such as spraying construction) and subsequent coating use, resulting in attenuation of the coating's thermal insulation performance, making it difficult to meet the use requirements.

Contents of the invention

The purpose of the present invention is to provide a flame-retardant thermal insulation coating, which can solve the above-mentioned problem that the existing thermal insulation coating easily leads to the attenuation of the thermal insulation performance of the coating.

In order to achieve the above object, the technical solution adopted in the present invention is:

A flame-retardant thermal insulation coating, mainly made of water, emulsion, aerogel, flame retardant-coated hollow glass microspheres and additives; the quality of the emulsion, aerogel and flame-retardant-coated hollow glass The ratio is 20-50:3-10:30-50.

The flame retardant and thermal insulation coating of the present invention uses airgel and flame retardant-coated hollow glass microspheres as the main material for thermal insulation, and uses the flame retardant to coat hollow glass microspheres (that is, flame-retardant thermal insulation fillers) to coat hollow glass microspheres. The flame retardant on the surface of the microspheres increases the wall thickness of the hollow glass microspheres, improves the pressure resistance of the hollow glass microspheres in the coating, reduces the breakage rate of the hollow glass microspheres in the coating and the coating, and thus avoids coating The attenuation of the thermal insulation performance of the layer; and the flame retardant is coated on the surface of the hollow glass microspheres and added to the coating, which can also increase the contact surface of the flame retardant in the coating and improve the flame retardancy of the coating. In addition, airgel and flame retardant-coated hollow glass microspheres are used as the main thermal insulation material to improve the thermal insulation performance of the coating while reducing the PVC value of the coating and improving the cost performance.

Airgel is a porous amorphous solid material with a three-dimensional network structure formed by the aggregation of nanometer-scale colloidal particles, and the pores are filled with gaseous media. It has good light transmission, good sound absorption, and low low-temperature infrared radiation rate. As well as good hydrophobicity, using it as an insulation material for thermal insulation and flame retardant coatings can reduce the energy loss caused by heat convection and heat conduction and improve thermal insulation performance.

Further, the thermal conductivity of the airgel at room temperature is ≤0.018W/(m·K), the bulk density is 40-60kg/m ³ , the pore size is 20-50nm, and the particle size is 40-60μm. The testing standard for thermal conductivity at room temperature is ISO22007-2-2008, the testing standard for bulk density is GB/T5211.4-1985, the pore size is measured by nitrogen adsorption and desorption, and the testing standard for particle size is GB/T19077-2016. Further, the specific surface area of the airgel is 600-800m ² /g, and the porosity is 90-95%. The specific surface area is tested according to GB/T 19587-2004, and the porosity is obtained by back-calculating the skeleton density.

Further, the airgel is silica airgel.

Compared with the case of using hollow glass microspheres and flame retardants alone, by coating hollow glass microspheres with flame retardants, the gaps between powders can be reduced, the volume of powders can be reduced, the PVC value can be reduced, and the The contact area of the flame retardant improves the flame retardancy of the coating; at the same time, due to the reduction in the volume of the filler, the same amount of emulsion can cover the powder more densely, effectively improving the adhesion and water resistance of the coating. Pigment volume concentration (PVC) refers to the percentage of the volume of pigments and fillers in the coating to the total volume of all non-volatile (resin, emulsion solid components and pigments, fillers) in the formula, that is, PVC (%) = [( Airgel+flame retardant coated hollow glass microspheres)/(aerogel+flame retardant coated hollow glass microspheres+emulsion)]×100.

In order to further improve the flame retardancy, heat preservation and compression resistance of the thermal insulation coating, the flame retardant coated hollow glass microspheres are hydrophobic modified ammonium polyphosphate coated hollow glass microspheres and/or polyphosphate ester coated hollow glass microspheres. beads. The hydrophobically modified ammonium polyphosphate and polyphosphate ester coated on the surface of hollow glass microspheres do not produce harmful substances at high temperatures, are environmentally friendly and pollution-free, and have a wide range of raw material sources and are easy to use.

In order to further improve the compressive performance on the basis of optimizing the heat preservation and flame retardant performance, and better prevent the heat preservation performance from decaying, further, the flame retardant-coated hollow glass microspheres are hydrophobically modified ammonium polyphosphate-coated hollow glass Microbeads and polyphosphate-coated hollow glass microspheres; the mass ratio of hydrophobically modified ammonium polyphosphate-coated hollow glass microspheres to polyphosphate-coated hollow glass microspheres is 1 to 4:1 to 3, for example, 1 :1.

Further, the hydrophobically modified ammonium polyphosphate-coated hollow glass microspheres are obtained by hydrophobically modifying ammonium polyphosphate II-coated hollow glass microspheres. The ammonium polyphosphate II-coated hollow glass microspheres are obtained by converting the ammonium polyphosphate I in the ammonium polyphosphate I-coated hollow glass microspheres into ammonium polyphosphate II. Ammonium polyphosphate II is an insoluble unbranched chain polymer. It is a high-efficiency inorganic flame retardant with good thermal and chemical stability, low water solubility and moisture absorption. It is volatile during application and does not produce corrosive gases. , long-lasting effect, good safety performance and so on. Hydrophobic modification of the ammonium polyphosphate II-coated hollow glass beads cannot greatly enhance the wall thickness of the hollow glass beads in thermal insulation coatings, and improve the compression resistance of the hollow glass beads in the use of coatings; it can also increase the resistance The contact surface of the flame retardant in the coating improves the flame retardancy of the coating; reduces the amount of emulsion and improves the thermal insulation performance of the coating.

Ammonium polyphosphate I-coated hollow glass microspheres are insoluble in water, but ammonium polyphosphate molecular chains contain hydrophilic amino groups, resulting in hygroscopicity of ammonium polyphosphate. Ammonium phosphate I was transformed into ammonium polyphosphate II and then hydrophobically modified. The ammonium polyphosphate I-coated hollow glass microspheres are made by a non-uniform nucleation method.

Further, the preparation method of the ammonium polyphosphate I-coated hollow glass microspheres comprises the following steps: dispersing the hollow glass microspheres in the ammonium polyphosphate I solution, separating the solid and liquid after aging, and calcining the separated solid , to obtain ammonium polyphosphate I-coated hollow glass microspheres. The ammonium polyphosphate I solution is obtained by dispersing the ammonium polyphosphate I and a dispersant in a solvent, and the solvent is preferably a mixture of water and an alcoholic solvent; the alcoholic solvent is preferably ethanol. The volume ratio of water and alcohol solvent in the solvent is 8-10:1, for example 9:1. The mass of the dispersant is 3-5% of the total mass of the ammonium polyphosphate I and the solvent, for example 4%. The dispersant is preferably cetyltrimethylammonium bromide. The mass ratio of the ammonium polyphosphate I to the dispersant is 12˜18:85, for example 15:85. The mass ratio of the hollow glass microspheres to the ammonium polyphosphate solution is 8-12:100, for example 10:100. The calcination is performed at 180-230°C for 3-5 hours, and then at 280-330°C for 3-5 hours; for example, at 200°C for 4 hours, and then at 300°C for 2 hours. Organic substances such as solvents and dispersants introduced during the preparation process can be effectively removed by calcination.

Further, ammonium polyphosphate II-coated hollow glass microspheres are prepared by a method comprising the following steps: the ammonium polyphosphate I-coated hollow glass microspheres are first incubated at 160-180°C for 2-3 hours in a mixed atmosphere, and then Keep warm at 270-290°C for 2-3 hours, then cool down. The method can convert the ammonium polyphosphate I and the low polyammonium polyphosphate (ammonium polyphosphate I) into a high polyammonium polyphosphate with a degree of polymerization ≥ 1000, that is, type II ammonium polyphosphate. For example, the ammonium polyphosphate I-coated hollow glass microspheres are first kept at 170°C for 2.5h in a mixed atmosphere, and then kept at 280°C for 2.5h. The mixed atmosphere is a mixed atmosphere of ammonia and water vapor, and the water vapor and ammonia in the mixed atmosphere can accelerate the conversion of ammonium polyphosphate from type I to type II. Because ammonium polyphosphate has many crystal forms and is easy to convert each other, by controlling the pressure of water vapor and ammonia, the reaction is always in the environment of forming type II ammonium polyphosphate, which can improve the purity of converted type II ammonium polyphosphate. In order to form high-purity Type II ammonium polyphosphate, further, the pressure of the mixed atmosphere is 100-120kPa, such as 110kPa; the pressure of the water vapor is 25-35kPa, such as 30kPa; the pressure of the ammonia gas 75 to 85 kPa, for example, 80 kPa. In order to avoid that at a lower temperature, ammonia gas in the mixed gas dissolves in water to form ammonia water as a by-product, thereby affecting the purity and performance of converted type II ammonium polyphosphate, further, the cooling is to cool the system to 90-110°C, preferably first cooled to 100-110°C, for example, first cooled to 100°C, and then the mixing atmosphere is closed, and then continued to cool to room temperature.

Further, the method of hydrophobic modification comprises the following steps: heat-insulate the mixture of ammonium polyphosphate II-coated hollow glass microspheres, methyl hydrogen silicone oil, gas-phase hydrophobic silica and water, then cool and dry . After drying, the hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres are obtained. During the heat preservation process, the methyl hydrogen-containing silicone oil is chemically cross-linked and coated on the surface of the ammonium polyphosphate II-coated hollow glass microspheres, and the gas-phase hydrophobic silica is filled with uncrosslinked ammonium polyphosphate II-coated hollow glass microspheres. In the pores on the surface of the beads, it plays a role in supplementing and enhancing the hydrophobic performance. The temperature of the heat preservation treatment is 30-70°C, for example, 50°C. The time for the heat preservation treatment is 1 to 3 hours, for example, 2 hours. The mass ratio of the ammonium polyphosphate II-coated hollow glass microspheres, methyl hydrogen-containing silicone oil, and gas-phase hydrophobic silica is 100:2˜3:1˜2, for example, 100:2.5:1.5. The mass ratio of the ammonium polyphosphate II-coated hollow glass microspheres to water is 100:8-12, for example, 100:10.

Further, the polyphosphate-coated hollow glass microspheres are made by a liquid coating method. Furthermore, the liquid coating method includes the following steps: uniformly mixing the suspension of the hollow glass microspheres and the polyphosphate solution, separating the solid from the liquid, and drying the obtained solid. The solid-liquid separation of the system obtained by mixing the hollow glass microsphere suspension and the polyphosphate solution is to insulate the obtained system at 50-60°C for 1-3 hours, for example, at 55°C for 2 hours. The liquid was then separated off after cooling to room temperature. The mixing is to mix the hollow glass microsphere suspension and the polyphosphate solution and then stir and mix at 50-60°C, for example, stir and mix at 55°C. The stirring and mixing is first stirred at 200 rpm for 2 hours, and then stirred at 60 rpm for 1 hour.

Further, the polyphosphate solution is obtained by dissolving polyphosphate in butanol. The mass ratio of the polyphosphate to butanol is 10:4-6, for example 10:5. Further, the suspension of hollow glass microspheres is formed by dispersing hollow glass microspheres in water; the mass ratio of hollow glass microspheres to water is 9-11:100, for example, 10:100. Further, the mass ratio of the hollow glass microsphere suspension to the polyphosphate solution is 110:12-18, for example, 110:15.

Polyphosphate is a biodegradable polymer with good biocompatibility and easy structure modification and functionalization. It has high heat resistance, good water resistance, self-sustaining property, high phosphorus content, and flame retardant properties. Excellent, by coating the hollow glass microspheres with liquid, the wall thickness of the hollow glass microspheres in the thermal insulation coating can be greatly enhanced, and the compression resistance of the hollow glass microspheres in the coating can be improved; the contact surface of the flame retardant in the coating can be increased, Improve the flame retardancy of coatings; reduce the amount of emulsion and improve the thermal insulation performance of coatings. Further, the polyphosphate is triphenyl phosphate.

Further, the emulsion is one or any combination of silicone emulsion, polyurethane emulsion, and fluorocarbon emulsion. Among them, the silicone emulsion has strong high temperature resistance, oxidation resistance and weather resistance, which can improve the temperature resistance limit and weather resistance of the coating. The emulsion is preferably an aqueous emulsion with a solid content of 35-50%. Further, the silicone emulsion is a water-based silicone emulsion, the polyurethane emulsion is a water-based polyurethane emulsion; the fluorocarbon emulsion is a water-based fluorocarbon emulsion.

It can be understood that the additives in the flame-retardant thermal insulation coating of the present invention are commonly used additives in the coating field. Further, the auxiliary agent is one or any combination of dispersants, wetting agents, defoamers, bactericides, antifreeze agents, thickeners, and film-forming aids.

Further, the mass ratio of the auxiliary agent to the emulsion is 0.5-5:20-50, and the mass ratio of water to the emulsion is 7-20:20-50.

The preparation method of the flame retardant thermal insulation paint of the present invention comprises the following steps: taking water, emulsion, aerogel, flame retardant coated hollow glass microspheres and auxiliary agents and mixing to obtain the product.

Detailed ways

The technical solution of the present invention will be further described below in combination with specific embodiments.

The hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres used in Examples 1-5 are made by a non-uniform nucleation method, which specifically includes the following steps:

(1) Take 15 parts of ammonium polyphosphate (oligomeric) with a molecular weight of 309.5 and add 85 parts of a mixed aqueous solution of distilled water and absolute ethanol (the volume ratio of distilled water to absolute ethanol is 9:1) to fully soak, add the total amount of the system 4% cetyltrimethylammonium bromide dispersant by mass was stirred at a stirring speed of 500 rpm for 60 minutes to obtain ammonium polyphosphate I solution.

(2) Get 10 parts of hollow glass microspheres and add 100 parts of ammonium polyphosphate I solution, stir for 60 minutes at a stirring speed of 60 rpm, and ultrasonically vibrate while stirring; filter after aging, and move the gained solid into a high-temperature resistant container, Place it in a high-temperature resistance furnace for calcination at a calcination temperature of 200°C for 4 hours, then raise the temperature to 300°C for 2 hours, leave the furnace and cool naturally to obtain ammonium polyphosphate I-coated hollow glass microspheres.

(3) 100 parts of ammonium polyphosphate I-coated hollow glass microspheres are placed in a microwave tube furnace (with stirring equipment) at 20 rpm, and heated to the microwave tube furnace reactor at a microwave tube furnace temperature of 100°C. The mixture of ammonia and water vapor (pressure is 110kPa, wherein the water vapor pressure is 80kPa, ammonia pressure is 30kPa), and then the temperature of the microwave tube furnace is raised to 170 ℃ and kept under stirring for 2.5 hours, the holding time After that, raise the temperature of the microwave tube furnace to 280°C and keep it under stirring for 2.5 hours, then cool down to 100°C, close the atmosphere, and continue cooling to room temperature to obtain ammonium polyphosphate II-coated hollow glass microspheres.

(4) Hydrophobic modification of methyl hydrogen-containing silicone oil and gas-phase hydrophobic silica: Take 100 parts of ammonium polyphosphate II-coated hollow glass microspheres, 2.5 parts of methyl hydrogen-containing silicone oil, 1.5 parts of gas-phase hydrophobic silica, and 50 parts of water. The parts were mixed and stirred evenly, and then placed in a vacuum drying oven at 50°C for 2 hours. After cooling to room temperature, the obtained solid was dried to obtain hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres.

Polyphosphate-coated hollow glass microspheres are prepared by a liquid coating method, which specifically includes the following steps:

1) After drying and crushing 10 parts of polyphosphate, add 5 parts of butanol to fully soak and dissolve to obtain a polyphosphate solution; the polyphosphate tripolyphosphate used is specifically Dongguan Xingyuan Chemical Co., Ltd. FR-TPP (triphenyl phosphate);

2) Take 10 parts of hollow glass microspheres and add them into 100 parts of distilled water and stir evenly to obtain a suspension of hollow glass microspheres;

The obtained suspension of hollow glass microspheres was added to the polyphosphate solution while stirring with a homogeneous disperser in a constant temperature water bath (the temperature of the water bath was 55°C), and then the temperature of the water bath was kept at 55°C, and the mixture was stirred at 200 rpm. Stir the system at a high speed for 2 hours, then stir the system at a stirring speed of 60 rpm for 60 minutes, keep warm at 55°C, precipitate for 2 hours, cool to room temperature and filter, wash the obtained solid and shake it with a vibrating sieve for 1 hour. Break and disperse, and then dry in an oven at 40°C to obtain polyphosphate-coated hollow glass microspheres.

The airgel powder used in Examples 1-5 and Comparative Examples is silica airgel powder, specifically the AG-D silica airgel powder of Shenzhen Zhongning Technology Co., Ltd., the silica The thermal conductivity of silicon airgel at room temperature is ≤0.018W/(m·K), the bulk density is 40-60kg/m ³ , the pore diameter is 20-50nm, the particle size is 50μm, the specific surface area is 600-800m ² /g, and the pores The rate is 90-95%.

The fluorocarbon emulsion used in Examples 1 to 5 and the comparative example is ZT-9615 water-based fluorocarbon emulsion of Jiangsu Zhitai Technology Co., Ltd., and the silicone emulsion is AH-071 water-based high-temperature-resistant pure Silicone resin emulsion, polyurethane emulsion is the F0410 water-based polyurethane emulsion of Shenzhen Yoshida Chemical Co., Ltd.

The auxiliary agent that adopts in embodiment 1～5 and comparative example is all the same, is the combination of dispersant, wetting agent, defoamer, film-forming auxiliary agent, bactericide, antifreeze agent and thickener, and dispersant is German Bi gram BYK-163 dispersant, the wetting agent is PE-100 wetting agent from Germany Corning, the defoamer is NXZ defoamer from Japan Nopco, and the film-forming aid is alcohol ester twelve from Eastman , the fungicide is Troy’s MERGALK14, the antifreeze is Dow’s propylene glycol, and the thickener is Dow’s RM-8W; The mass ratio of thickener is 3:1:5:5:3:7:5.

Example 1

The flame-retardant thermal insulation coating of this embodiment is made of the following raw materials in parts by weight: 11.5 parts of water, 50 parts of emulsion, 3 parts of airgel, 35 parts of hollow glass microspheres coated with flame retardant, and 0.5 parts of additives.

Among them, the emulsion is a silicone emulsion with a solid content of 50%; the flame retardant-coated hollow glass microspheres are hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres and polyphosphate-coated hollow glass microspheres. The mass ratio of ammonium polyphosphate II-coated hollow glass microspheres to polyphosphate-coated hollow glass microspheres is 3:2.

Example 2

The flame-retardant thermal insulation coating of this embodiment is made of the following raw materials in parts by weight: 10 parts of water, 40 parts of emulsion, 7 parts of airgel, 40 parts of hollow glass microspheres coated with flame retardant, and 3 parts of additives.

Among them, the emulsion is polyurethane emulsion with a solid content of 35%; the flame retardant-coated hollow glass microspheres are hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres and polyphosphate-coated hollow glass microspheres, hydrophobically modified The mass ratio of ammonium polyphosphate II-coated hollow glass microspheres to polyphosphate-coated hollow glass microspheres is 3:1.

Example 3

The flame-retardant thermal insulation coating of this embodiment is made of the following raw materials in parts by weight: 25 parts of water, 35 parts of emulsion, 5 parts of airgel, 30 parts of hollow glass microspheres coated with flame retardant, and 5 parts of additives.

Among them, the emulsion is a fluorocarbon emulsion with a solid content of 48%. The flame retardant-coated hollow glass microspheres are hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres and polyphosphate-coated hollow glass microspheres. The mass ratio of ammonium polyphosphate II-coated hollow glass microspheres to polyphosphate-coated hollow glass microspheres is 2:1.

Example 4

The flame-retardant thermal insulation coating of this embodiment is made of the following raw materials in parts by weight: 16.5 parts of water, 20 parts of emulsion, 10 parts of airgel, 50 parts of hollow glass microspheres coated with flame retardant, and 3.5 parts of additives.

Among them, the emulsion is polyurethane emulsion with a solid content of 35%; the flame retardant-coated hollow glass microspheres are hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres and polyphosphate-coated hollow glass microspheres, hydrophobically modified The mass ratio of ammonium polyphosphate II-coated hollow glass microspheres to polyphosphate-coated hollow glass microspheres is 1:1.

Example 5

The flame-retardant thermal insulation coating of this embodiment is made of the following raw materials in parts by weight: 13 parts of water, 45 parts of emulsion, 5 parts of airgel, 35 parts of hollow glass microspheres coated with flame retardant, and 2 parts of additives.

Among them, the emulsion is a silicone emulsion with a solid content of 50%; the flame retardant-coated hollow glass microspheres are hydrophobically modified ammonium polyphosphate II-coated hollow glass microspheres and polyphosphate-coated hollow glass microspheres. The mass ratio of ammonium polyphosphate II-coated hollow glass microspheres to polyphosphate-coated hollow glass microspheres is 4:3.

comparative example

The flame-retardant thermal insulation coating of this comparative example is made of the following raw materials in parts by weight: 13 parts of water, 45 parts of emulsion, 5 parts of airgel, 10 parts of hollow glass microspheres, 25 parts of flame retardant, and 2 parts of auxiliary agent .

Among them, the emulsion is a silicone emulsion with a solid content of 50%; the filler is hollow glass microspheres, the flame retardant is type II ammonium polyphosphate (polymerization degree ≥ 1000) and phosphoric acid ester, and the mass ratio of ammonium polyphosphate and phosphoric acid ester is 4:3; the polyphosphate used is FR-TPP (triphenyl phosphate) from Dongguan Xingyuan Chemical Co., Ltd.

When preparing the flame retardant and thermal insulation coatings of the above examples and comparative examples, the respective raw materials in the formulation amount were mixed evenly to obtain the corresponding flame retardant thermal insulation coatings.

Experimental example

1) According to JCT2285-2014 (hollow glass microsphere pressure resistance test industry standard) gas isostatic pressure detection method, using gas as the pressure transmission medium to carry out compressive strength test, determine the hydrophobic modified polyphosphoric acid used in the embodiment before and after compression Ammonium II coated hollow glass microspheres (1#), polyphosphate coated hollow glass microspheres (2#), and the density of hollow glass microspheres, and then calculate the compressive strength by the following formula:

N _f ＝[P _G *(P ₂ -P ₁ )]/[P ₂ *(P _G -P ₁ )]

N _f : Under a certain constant isostatic pressure, the volume percentage of the destroyed hollow microspheres to the total hollow microspheres;

P ₁ : Particle density of hollow glass microspheres before gas compression, unit g/cm ³ ;

P ₂ : Particle density of hollow glass microspheres after gas compression, unit g/cm ³ ;

P _G : the density of the hollow glass microsphere shell, in g/cm ³ .

In addition, the wall thickness of hydrophobically modified ammonium polyphosphate II coated hollow glass microspheres, polyphosphate coated hollow glass microspheres, and hollow glass microspheres were measured by using the calculation formula of hollow microbead wall thickness and laser particle size analyzer. , Particle size measurement test.

The results are shown in Table 1.

Table 1 Compression test results

1# 2# hollow glass microspheres Powder wall thickness 17μm 20μm 2μm Powder particle size μm 70 75 30 Compressive strength (MPa) twenty three 25 4

From the data in Table 1, it can be known that the hydrophobic modification of ammonium polyphosphate II-coated hollow glass microspheres and polyphosphate-coated hollow glass microspheres greatly passes the compression resistance of hollow glass microspheres, thus reducing the thermal insulation performance of coatings. of weakness.

2) Test the flame retardancy and thermal conductivity performance of the flame-retardant thermal insulation coatings of Examples 1 to 5 and the comparative examples respectively, and test the flame retardancy according to GB8624-2012 "Classification of Combustion Behavior of Building Materials and Products". /T3651-2008 "Measurement Method for High Temperature Thermal Conductivity of Metals" standard to test the thermal conductivity, the test results are shown in Table 2. According to the calculation formula of the PVC value of the coating: that is, PVC (%) = [(airgel + flame retardant coated hollow glass beads) / (airgel + flame retardant coated hollow glass beads + emulsion)] × 100 , to calculate the PVC value of the paint.

The performance test result of table 2 embodiment 1-5 thermal insulation coating

From the data in Table 2, it can be seen that the flame retardant efficiency of the flame retardant can be improved by coating the insulating filler hollow glass microspheres with the flame retardant, the PVC value of the coating can be reduced, and the thermal insulation performance and adhesion of the coating can be improved. It also reduces the problem that the actual thermal insulation effect is inconsistent with the design caused by the broken hollow glass beads during the spraying process, ensuring the consistency of thermal insulation coating performance and the stability of construction.

Claims (10)

1. A flame-retardant heat-insulating coating is characterized in that: the hollow glass microsphere is mainly prepared from water, emulsion, aerogel, flame retardant coated hollow glass microsphere and an auxiliary agent; the mass ratio of the emulsion to the aerogel to the hollow glass bead coated by the flame retardant is 20-50:3-10:30-50.

2. The flame retardant and heat insulating coating according to claim 1, wherein: the aerogel isThe normal temperature heat conductivity coefficient is less than or equal to 0.018W/(m.K), and the bulk density is 40-60 kg/m ³ The aperture is 20-50 nm, and the grain diameter is 40-60 mu m.

3. The flame retardant and heat insulating coating according to claim 1, wherein: the aerogel is a silica aerogel.

4. The flame retardant and heat insulating coating according to claim 1, wherein: the flame retardant coated hollow glass beads are hydrophobic modified ammonium polyphosphate coated hollow glass beads and/or polyphosphate coated hollow glass beads.

5. The flame retardant and heat insulating coating according to claim 4, wherein: the flame retardant coated hollow glass beads are hydrophobic modified ammonium polyphosphate coated hollow glass beads and polyphosphate coated hollow glass beads; the mass ratio of the hydrophobic modified ammonium polyphosphate coated hollow glass beads to the polyphosphate coated hollow glass beads is 1-4:1-3.

6. The flame retardant and heat insulating coating according to claim 4 or 5, wherein: the hydrophobic modified ammonium polyphosphate coated hollow glass bead is obtained by carrying out hydrophobic modification on an ammonium polyphosphate II coated hollow glass bead.

7. The flame retardant and heat insulating coating according to claim 6, wherein: the method for converting the ammonium polyphosphate I coated hollow glass beads into the ammonium polyphosphate II coated hollow glass beads comprises the following steps: the hollow glass bead coated with the ammonium polyphosphate I is firstly insulated for 2 to 3 hours at 160 to 180 ℃ in the mixed atmosphere, then is insulated for 2 to 3 hours at 270 to 290 ℃, and is cooled; the mixed atmosphere is a mixed atmosphere of ammonia and steam.

8. The flame retardant and heat insulating coating according to claim 6, wherein: the method for hydrophobically modifying comprises the following steps: and (3) carrying out heat preservation treatment on the mixture of the ammonium polyphosphate II coated hollow glass beads, methyl hydrogen silicone oil, gas phase hydrophobic white carbon black and water, and then cooling and drying.

9. The flame-retardant and heat-insulating coating according to any one of claims 1 to 4, wherein: the emulsion is one or any combination of organosilicon emulsion, polyurethane emulsion and fluorocarbon emulsion.

10. The flame-retardant and heat-insulating coating according to any one of claims 1 to 4, wherein: the mass ratio of the auxiliary agent to the emulsion is 0.5-5:20-50, and the mass ratio of the water to the emulsion is 7-20:20-50.