Preparation method of flame-retardant fluorocarbon coating and product thereof

Abstract

The invention discloses a preparation method of a flame-retardant fluorocarbon coating and a product thereof. According to the idea of the invention, fluorocarbon resin and fire extinguishing capsules are combined to realize the self-cleaning and precise fire extinguishing functions of the coating, specifically, the coating is obtained through solvent type coating and subsequent electrostatic spraying multi-layer covering and finally ultraviolet curing, the contact angle of the coating is not smaller than 100 degrees, and the coating has good stain resistance and self-cleaning capacity. When the coating surface is baked by an alcohol lamp, the time from the time when flame directly touches the coating to the time when the flame is extinguished does not exceed 3 seconds, the capsule breaking synchronization rate is high, and it can be guaranteed that a large amount of medicine is released in a short time to achieve the extinguishment effect with small fire and large fire.

Description

Technical Field

[0001] This invention belongs to the field of polymer coating technology, specifically relating to a method for preparing a flame-retardant fluorocarbon coating and its product. Background Technology

[0002] Fluorocarbon resins, with their high bond energy and unique molecular structure, have become "all-rounders" in the materials field, offering advantages across multiple dimensions, from extreme environment tolerance and precision functional implementation to long-term safety assurance. From high-temperature components in car engine compartments to medical catheters implanted in the human body, from solar panels exposed to ultraviolet radiation to chemical equipment resistant to strong acids and alkalis, this material redefines durability standards with its stable performance. Its weather resistance is exceptional; it does not powder or fade even after 20 years of outdoor exposure, and its resistance to ultraviolet radiation ensures the stability of solar panel encapsulation films under intense sunlight. In terms of chemical inertness, it is "immune" to highly corrosive media such as 98% concentrated sulfuric acid and 50% sodium hydroxide. Using fluorocarbon resin for chemical pipeline linings extends service life by 3-5 times. Its temperature resistance ranges from -200℃ to 200℃, and it can withstand short-term high temperatures of 205℃, outperforming traditional engineering plastics in high-heat environments such as car engine compartments. Its low surface energy properties give it a dual advantage: a coefficient of friction as low as 0.04 (close to ice), making it suitable for manufacturing wear-resistant parts such as bearings; and its anti-adhesion properties enable food processing equipment to achieve "zero residue," with tomato sauce production lines achieving a 40% improvement in cleaning efficiency after adopting fluorocarbon coatings. PVDF resin plays a dual role in lithium batteries: as a positive electrode binder to improve cycle life, and as a separator coating to reduce the risk of thermal runaway by 60%.

[0003] These properties make fluorocarbon resins indispensable in strategic fields such as new energy, high-end manufacturing, and life sciences. Fire extinguishing capsules (microcapsule fire extinguishing agents) are miniature fire extinguishing units that encapsulate highly efficient fire extinguishing agents in a special shell. Their core structure employs a "core-shell dual-layer design," achieving active fire extinguishing functionality through a combination of materials science and thermal response technology. This allows for the stable storage of volatile fire extinguishing agents and precise release triggered in the early stages of a fire, making it a key technology for fire prevention in confined spaces and concealed areas. This invention attempts to combine the advantages of fluorocarbon resins with the benefits of microcapsule fire extinguishing to achieve self-cleaning coatings and active fire extinguishing. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing a flame-retardant fluorocarbon coating, which utilizes the combination of fluorocarbon resin and fire extinguishing capsule to achieve the coating's self-cleaning and precise fire extinguishing functions.

[0005] Another object of the present invention is to provide a flame-retardant fluorocarbon coating product prepared by the above method.

[0006] The specific details of the invention are as follows: Under ice-water bath conditions, 100 parts of isophorone diisocyanate (IPDI) and 1.5 parts of dibutyltin dilaurate (DBTDL) were mixed, and then 110 parts of bisphenol A acrylate were added dropwise. After the addition was complete, the temperature was raised to 35℃-40℃ to continue the reaction and monitor the NCO conversion rate. When the NCO conversion rate reached 50%, 180-220 parts of perfluoropolyether alcohol were added dropwise. After the addition was complete, the temperature was raised to 45℃-50℃ to continue the reaction and monitor the NCO conversion rate. When the NCO conversion rate reached 100%, the reaction ended, and a liquid resin was obtained. 100 parts of the liquid resin, 10-20 parts of diluent, and 3-6 parts of UV curing agent were mixed evenly and then coated onto an aluminum plate with a wire rod for the first coating, with a coating thickness of not less than 1 mm. The coated film was dried in an oven at 60℃ until the resin reached a viscoelastic state. Then, a second coating was applied by electrostatic spraying using a fire extinguishing capsule. The spraying time was adjusted to ensure that the density of the capsule on the plate was not less than 80 g / m³. 2 Based on the actual amount of capsules adhered to the resin coating, a third electrostatic spray coating is applied to the coating using photothermal filler (this can be done in small batches multiple times), ensuring that the amount of photothermal filler on the coating is 1%-2% of the amount of capsules. The resulting coating is then cured in air under a 380 nm UV light source for 60-120 seconds. Care is taken to adjust the UV light intensity so that the surface temperature of the coating does not exceed 120°C, ultimately yielding a flame-retardant fluorocarbon coating.

[0007] The perfluoropolyether alcohols used mentioned above must have a low water content, which can be achieved by pre-treating them with a vacuum oven to remove moisture.

[0008] The diluent used above is one or a mixture of two of toluene, acetone and n-butanol, and the photoinitiator used is a compound of photoinitiator 1173 (2-hydroxy-2-methyl-1-phenyl-1-propanone) and photoinitiator 184 (1-hydroxycyclohexylphenyl ketone) in a 1:1 mass ratio.

[0009] The aforementioned fire extinguishing capsules have a core-shell double-layer structure, a particle size of 500-2000 μm, a drug loading (perfluorohexanone) of not less than 75%, good capsule uniformity, and a capsule trigger (shell breakage and drug release) rate of not less than 95% after being placed at 150°C for 10 seconds.

[0010] The photothermal filler used above is multi-walled carbon nanotubes (CNTs).

[0011] The aforementioned coating has a contact angle of not less than 100° and exhibits good stain resistance and self-cleaning ability. When the coating surface is baked with an alcohol lamp, the time from direct contact of the flame with the coating to the extinguishing of the flame is no more than 3 seconds, and the capsule rupture synchronization rate is high, which can ensure a large release of the drug in a short time to achieve a significant fire extinguishing effect with a small amount of material.

[0012] Fluorocarbon resins are indispensable in strategic fields such as new energy, high-end manufacturing, and life sciences. Fire extinguishing capsules (microencapsulated fire extinguishing agents) are miniature fire extinguishing units that encapsulate highly efficient fire extinguishing agents in a special shell. Their core structure employs a "core-shell dual-layer design," achieving active fire extinguishing functionality through a combination of materials science and thermal response technology. This design can stably store volatile fire extinguishing agents and precisely trigger their release in the early stages of a fire, making it a key technology for fire prevention in confined spaces and concealed areas. This invention attempts to combine the advantages of fluorocarbon resins with the advantages of microencapsulated fire extinguishing to achieve self-cleaning coatings and active fire extinguishing.

[0013] The invention utilizes a combination of fluorocarbon resin and a fire extinguishing capsule to achieve a coating with self-cleaning and precise fire extinguishing functions. Specifically, it involves solvent-based coating followed by multiple layers of electrostatic spraying, and finally UV curing to obtain the coating. The coating has a contact angle of not less than 100° and exhibits good dirt resistance and self-cleaning capabilities. When the coating surface is baked with an alcohol lamp, the time from direct flame contact with the coating to the flame being extinguished is no more than 3 seconds. The capsule rupture synchronization rate is high, ensuring a large release of the extinguishing agent in a short time to achieve a significant fire extinguishing effect with a small amount of material. Detailed Implementation

[0014] The present invention will be described in detail through the following specific examples, but the scope of protection of the present invention is not limited to these embodiments.

[0015] The photoinitiator used is a compound of photoinitiator 1173 (2-hydroxy-2-methyl-1-phenyl-1-propanone) and photoinitiator 184 (1-hydroxycyclohexylphenyl ketone) in a 1:1 mass ratio.

[0016] The fire extinguishing capsules used have a core-shell double-layer structure with a particle size of 500-2000μm and a drug loading (perfluorohexanone) of no less than 75%. The capsules have good uniformity and the capsule triggering (shell breaking and drug release) rate is no less than 95% after being placed at 150℃ for 10 seconds.

[0017] The photothermal filler is multi-walled carbon nanotubes (CNTs).

[0018] Example 1 A flame-retardant fluorocarbon coating achieves self-cleaning and precise fire extinguishing functions by combining fluorocarbon resin and a fire extinguishing capsule. The coating is prepared through solvent-based coating, subsequent electrostatic spraying, multi-layer coverage, and finally UV curing. The preparation steps are as follows: Under ice-water bath conditions, 100g of isophorone diisocyanate and 1.5g of dibutyltin dilaurate were mixed, and then 110g of bisphenol A acrylate was added dropwise. After the addition was completed, the temperature was raised to 35℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 50%, 180g of perfluoropolyether alcohol was added dropwise. After the addition was completed, the temperature was raised to 46℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 100%, the reaction ended and liquid resin was obtained. After mixing 100g of liquid resin, 12g of toluene, and 3g of UV curing agent evenly, the mixture was applied to an aluminum plate using a wire rod coating method for the first coating, with a thickness of 1mm. The coated film was then dried in an oven at 60℃ until the resin reached a viscoelastic state. A second coating was then applied using an electrostatic spraying technique with a fire extinguishing capsule. The actual plate density of the capsule was 82g / m³. 2 Based on the actual amount of the capsules adhered to the resin coating, a third electrostatic spray coating (in small amounts and multiple times) is applied to the coating using photothermal filler. The actual amount of photothermal filler on the coating is 1.8% of the amount of the capsules. The resulting coated plate was cured in air under an ultraviolet light source for 60-120 seconds. The wavelength of the light source was 380 nm. The intensity of the ultraviolet light was adjusted so that the surface temperature of the coated plate did not exceed 120℃, thus obtaining a flame-retardant fluorocarbon coating.

[0019] The final coated plate was cured in air under an ultraviolet light source with a wavelength of 380 nm for 70 seconds. The surface temperature of the coated plate remained below 120℃ throughout the process, meeting the process requirements. Finally, flame-retardant fluorocarbon coating sample 1 was obtained.

[0020] Subsequent contact angle and fire extinguishing tests were conducted on sample 1 with flame-retardant fluorocarbon coating. The results are shown in Table 1.

[0021] Example 2 A flame-retardant fluorocarbon coating, similar to that in Example 1, is prepared according to the following steps: Under ice-water bath conditions, 100g of isophorone diisocyanate and 1.5g of dibutyltin dilaurate were mixed, and then 110g of bisphenol A acrylate was added dropwise. After the addition was completed, the temperature was raised to 37℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 50%, 196g of perfluorinated polyether alcohol was added dropwise. After the addition was completed, the temperature was raised to 48℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 100%, the reaction ended and liquid resin was obtained. Mix 100g of liquid resin, 8g of toluene, 12g of acetone, and 4g of UV curing agent thoroughly. Apply the mixture to an aluminum plate using a wire rod coating method for the first coating layer, achieving a thickness of 1.2mm. After drying the coating at 60℃ in an oven until the resin reaches a viscoelastic state, apply a second coating layer using an electrostatic spraying process with a fire extinguishing capsule. The actual plate density of the capsule is 88g / m³. 2 Based on the actual amount of the capsules adhered to the resin coating, a third electrostatic spray coating (in small amounts and multiple times) is applied to the coating using photothermal filler. The actual amount of photothermal filler on the coating is 1.2% of the amount of the capsules. The final coated plate was cured in air under an ultraviolet light source with a wavelength of 380 nm for 100 seconds. The surface temperature of the coated plate remained below 120℃ throughout the process, meeting the process requirements. Finally, flame-retardant fluorocarbon coating sample 2 was obtained.

[0022] Subsequent contact angle and fire extinguishing tests were conducted on sample 2 with flame-retardant fluorocarbon coating. The results are shown in Table 1.

[0023] Example 3 A flame-retardant fluorocarbon coating, similar to that in Example 1, is prepared according to the following steps: Under ice-water bath conditions, 100g of isophorone diisocyanate and 1.5g of dibutyltin dilaurate were mixed, and then 110g of bisphenol A acrylate was added dropwise. After the addition was completed, the temperature was raised to 40℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 50%, 220g of perfluoropolyether alcohol was added dropwise. After the addition was completed, the temperature was raised to 49℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 100%, the reaction ended and liquid resin was obtained. 100g of liquid resin, 16g of n-butanol, and 6g of UV curing agent were mixed evenly and then coated onto an aluminum plate using a wire rod coating method to achieve a first coating thickness of 1.1mm. The coated film was then dried in an oven at 60℃ until the resin reached a viscoelastic state. A second coating was then applied using an electrostatic spraying technique with a fire extinguishing capsule. The actual plate density of the capsule was 89g / m³. 2 Based on the actual amount of the capsules adhered to the resin coating, a third electrostatic spray coating (in small amounts and multiple times) is applied to the coating using photothermal filler. The actual amount of photothermal filler on the coating is 1.4% of the amount of the capsules. The final coated plate was cured in air under an ultraviolet light source for 110 seconds. The wavelength of the light source was 380 nm. The surface temperature of the coated plate was kept below 120℃ throughout the process, which met the process requirements. Finally, flame-retardant fluorocarbon coating sample 3 was obtained.

[0024] Subsequent contact angle and fire extinguishing tests were conducted on sample 3 with flame-retardant fluorocarbon coating. The results are shown in Table 1: .

Claims

1. A method for preparing a flame-retardant fluorocarbon coating, characterized in that, The coating achieves self-cleaning and precise fire extinguishing functions by combining fluorocarbon resin and fire extinguishing capsules. The coating is obtained through solvent-based coating, subsequent electrostatic spraying, multiple layers, and finally UV curing, including the following steps: Under ice-water bath conditions, 100 parts of isophorone diisocyanate (IPDI) and 1.5 parts of dibutyltin dilaurate (DBTDL) were mixed, and then 110 parts of bisphenol A acrylate were added dropwise. After the addition was completed, the temperature was raised to 35℃-40℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 50%, 180-220 parts of perfluoropolyether alcohol were added dropwise. After the addition was completed, the temperature was raised to 45℃-50℃ to continue the reaction and the NCO conversion rate was monitored. When the NCO conversion rate reached 100%, the reaction ended and liquid resin was obtained. Mix 100 parts liquid resin, 10-20 parts diluent, and 3-6 parts UV curing agent thoroughly. Apply the mixture to an aluminum plate using a wire rod coating method for the first coating layer, ensuring a thickness of at least 1 mm. After drying the coating at 60°C in an oven until the resin reaches a viscoelastic state, apply a second coating layer using an electrostatic spraying device with a fire extinguishing capsule. Adjust the spraying time to ensure that the capsule's density on the plate is not less than 80 g / m³. 2 Depending on the amount of adhesion to the resin coating, the film is then electrostatically sprayed with photothermal filler for a third coating, or this can be done in small amounts multiple times, ensuring that the amount of photothermal filler on the plate is 1%-2% of the amount of capsule on the plate; The resulting coated plate was cured in air under an ultraviolet light source for 60-120 seconds. The wavelength of the light source was 380 nm. The intensity of the ultraviolet light was adjusted so that the surface temperature of the coated plate did not exceed 120℃, thus obtaining a flame-retardant fluorocarbon coating.

2. The method for preparing a flame-retardant fluorocarbon coating according to claim 1, characterized in that... The perfluoropolyether alcohol used is first dehydrated using a vacuum oven to ensure a low moisture content.

3. The method for preparing a flame-retardant fluorocarbon coating according to claim 1, characterized in that... The diluent used is one or a mixture of two of toluene, acetone and n-butanol, and the photoinitiator used is a compound of photoinitiator 1173 (2-hydroxy-2-methyl-1-phenyl-1-propanone) and photoinitiator 184 (1-hydroxycyclohexylphenyl ketone) in a 1:1 mass ratio.

4. The method for preparing a flame-retardant fluorocarbon coating according to claim 1, characterized in that... The fire extinguishing capsules used have a core-shell double-layer structure with a particle size of 500-2000μm and a perfluorohexanone loading of no less than 75%. The capsules are placed at 150℃ for 10 seconds and the drug release rate is no less than 95%.

5. The method for preparing a flame-retardant fluorocarbon coating according to claim 1, characterized in that... The photothermal filler used is multi-walled carbon nanotubes (CNTs).

6. A flame-retardant fluorocarbon coating, characterized in that... The coating prepared according to any one of claims 1-5 has a contact angle of not less than 100° and good dirt resistance and self-cleaning ability. When the coating surface is baked with an alcohol lamp, the time from direct contact of the flame with the coating to the extinguishing of the flame does not exceed 3 seconds. The capsule rupture synchronization rate is high, which can ensure a large amount of drug release in a short time to achieve a fire extinguishing effect with a small amount of drug.