Luminescent powder coating and preparation method thereof

By using end carboxylic polyester resin, fluorine-containing acrylic resin and carbon nanotubes, combined with ball milling and bonding technology, the problems of short luminescence time, low intensity and poor stability of luminescence coatings are solved, and high-performance luminescence powder coatings are realized Prepared for outdoor applications.

CN119264789AActive Publication Date: 2025-01-07SHANDONG QIANJIANG POWDER TECH CO LTD
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Patent Information

Application Number
CN202411413866.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-11
Publication Date
2025-01-07
Estimated Expiration
2044-10-11

AI Technical Summary

Technical Problem

Existing luminescent paints have problems such as short luminescence time, low luminescence intensity and poor stability, which limits their application range.

Method used

Using end carboxylic polyester resin, fluorine-containing acrylic resin, carbon nanotubes and other materials, the specific surface area and conductivity of the luminescent material are improved through ball milling and coating technology, and the luminescent material is uniformly adhered to the surface of powder particles through bonding technology. , combined with the synergistic effect of components in a specific proportion, a high-performance luminescent powder coating is prepared.

Benefits of technology

It significantly improves the luminous intensity and stability of the luminous powder coating, enhances weather resistance, ensures uniform and long-term luminous effect when used outdoors, avoids deterioration in leveling and surface pollution problems, and has excellent overall stability.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention discloses a luminescent powder coating and a preparation method thereof, and belongs to the field of powder coating preparation. The carboxyl-terminated polyester resin is added to provide excellent mechanical properties for the powder coating, and the fluorine-containing acrylic resin is easy to coat a luminescent material, can keep stable performance in outdoor exposure for a long time, and is not easy to fade, pulverize and age; therefore, the weather resistance of the powder coating system can be obviously improved by adding the luminescent material coated with the fluorine-containing acrylic resin into the powder coating system. The bonding process enables the luminescent material to be firmly, uniformly and orderly arranged on the surface of the coating film, so that the luminescence is more uniform. On the whole, through compound use of the components and mutual synergistic effect of the components, the powder coating shows more excellent performance, and compared with a traditional powder coating added with a fluorescent agent, the powder coating is better in weather resistance, high in afterglow brightness, capable of being effectively used in outdoor places, capable of achieving decoration and warning effects and excellent in overall stability, and after being stored and used for a long time, the powder coating does not fall off easily. And excellent luminescence performance is still maintained.
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Description

Technical Field

[0001] The invention relates to the field of powder coating preparation, and in particular to a luminous powder coating and a preparation method thereof. Background Art

[0002] With the development of society and the improvement of people's living standards, the performance and functional requirements of coatings are becoming more and more diverse. Among them, powder coating is a coating with 100% solid components. Unlike traditional solvent-based and water-based coatings, its VOC (volatile organic compound) is almost zero, and it is more energy-saving and environmentally friendly without solvent pollution. It is an environmentally friendly coating. Luminescent coating is one of the high-tech functional materials that is developing rapidly in the world. This coating is made of luminescent materials, organic resins or resins, organic solvents or solvents, inorganic pigments, fillers, additives, etc. in a certain proportion. It can absorb and store light energy under visible light such as sunlight or lamplight, and then slowly release the absorbed energy in the form of visible light in the dark. The luminescence time can last for more than 10 hours. Due to its ability to emit light in a dark environment, luminescent coating has broad application prospects in the fields of traffic safety, building decoration, fire emergency, etc. In the prior art, alkaline earth metal aluminate luminescent materials are added to give powder coatings a certain luminescent effect. Due to the different ratios of added strontium oxide and aluminum oxide, the wavelength and afterglow time of fluorescence are also different. By changing the content of strontium oxide and aluminum oxide, the doping amount of europium and dysprosium, and partially or completely replacing strontium oxide with calcium oxide, magnesium oxide, barium oxide, etc., or adding them in combination, a series of rare earth-activated alkaline earth metal aluminate luminescent coatings with different initial luminescent intensities and afterglow times can be obtained, but the luminescent coatings still have the problems of short luminescent time, low luminescent intensity and poor stability, which limits their scope of application. Summary of the invention

[0003] The purpose of the present invention is to provide a luminescent powder coating and a preparation method thereof to solve the problems of short luminescent time, low luminescent intensity and poor stability of luminescent coatings.

[0004] To achieve the above purpose, the present invention provides a luminescent powder coating, which includes the following raw materials in parts by weight: 55-70 parts of terminal carboxyl polyester resin, 5-10 parts of fluorine-containing acrylic resin, 4-5.3 parts of triglycidyl isocyanurate, 10-20 parts of filler, 10-20 parts of luminescent material, 0.5-2 parts of leveling agent, 0.5-2 parts of brightener, 0.5-1 parts of carbon nanotubes, 0.2-0.3 parts of anti-scratch agent, 0.2-0.5 parts of benzoin, 0.5-2 parts of defoaming agent, 0.5-2 parts of antioxidant, 0-3.0 parts of pigment, 0.1-0.2 parts of desiccant, 0.1-0.3 parts of bonding aid and 0.3-0.5 parts of silicon dioxide.

[0005] Furthermore, the acid value of the carboxyl-terminated polyester resin is 32 mgKOH / g to 38 mgKOH / g. Viscosity@200℃ (mPa.s) The temperature is 1500~2500, and the glass transition temperature is 67℃~70℃.

[0006] Furthermore, the filler is at least one of calcium carbonate, mica powder and barium sulfate.

[0007] Furthermore, the luminescent material includes a matrix and an activator, and the activator accounts for 10% to 30% of the mass of the matrix.

[0008] Furthermore, the activator is a rare earth element.

[0009] Furthermore, the matrix is ​​one or a mixture of aluminate and silicate.

[0010] Furthermore, the carbon nanotubes have an electrical conductivity of >150s / cm, a length of 10-20um, and are obtained by curling graphene sheets.

[0011] Furthermore, the anti-scratch agent is at least one of micronized polypropylene wax, PTFE-modified PE wax and PP wax.

[0012] In addition, the present invention also provides a method for preparing a luminous powder coating, the preparation method comprising the following steps:

[0013] The luminescent material is added to a drum ball mill for ball milling, and then the ball-milled luminescent material and silicon dioxide are added to a mixing device for high-speed airflow impact treatment to obtain a mixture A, and then the mixture A, carbon nanotubes and fluorine-containing acrylic resin are added to a grinding device for stirring, grinding and coating treatment to obtain a mixture B;

[0014] Adding carboxyl-terminated polyester resin, triglycidyl isocyanurate, filler, leveling agent, brightener, anti-scratch agent, benzoin, defoamer, antioxidant and pigment into a mixing tank for premixing; then, melt extrusion, cooling and ACM grinding are performed to obtain a mixture C;

[0015] The mixture B, the mixture C and the bonding aid are mixed, subjected to a bonding process, and then a desiccant is added and mixed, and then sieved through a 160-180 mesh sieve to obtain a luminous powder coating.

[0016] Furthermore, the conditions for the melt extrusion are: a screw speed of 40 Hz to 45 Hz, a melting zone temperature of 120° C. to 125° C., and a mixing zone temperature of 130° C. to 135° C.

[0017] Furthermore, the conditions of the bonding process are: bonding temperature is 65℃~68℃, heating speed is 900rpm~1000rpm, bonding speed is 600rpm~700rpm, cooling speed is 400pm~500pm, cold water temperature is 17℃~19℃, hot water temperature is 70℃~75℃, and the bonding stage time is 300s~500s.

[0018] The luminous powder coating and its preparation method and application provided by the above technical solution have the following beneficial effects compared with the prior art:

[0019] The carboxyl-terminated polyester resin in the present invention has the characteristics of low viscosity and excellent leveling performance, and provides excellent mechanical properties for the coating. The fluorine atoms in the fluorine-containing acrylic resin have large electronegativity and small atomic radius, so that the fluorine-containing acrylic resin has a lower surface energy, making the luminescent material easier to be coated. At the same time, the luminescent material after ball milling has a larger specific surface area, further promoting the coating effect of the fluorine-containing acrylic resin. The presence of fluorine atoms makes the resin have good ultraviolet resistance and antioxidant properties. Fluorine-containing acrylic resin can maintain its stable performance in outdoor exposure for a long time, and is not prone to fading, powdering and aging. The added carbon nanotubes make the luminescent material after coating have good conductivity, which is conducive to the luminescent material being more easily adsorbed on the surface of the substrate during the powder coating spraying process, and can effectively enhance the luminous intensity of the luminescent powder coating. Adding the luminescent material after coating to the powder coating system can significantly improve its weather resistance, so that the luminescent material can also be stably used outdoors and has significant durability. The coating resin has the characteristics of low surface energy. During the melting process of the powder coating, the luminescent material can float to the surface of the coating as much as possible to increase the luminescent area.

[0020] The present invention uses a bonding process to enable the treated luminescent material to firmly adhere to the surface of the powder particles. After spray curing, the luminescent material can be evenly and orderly arranged on the surface of the coating, making the luminescence more uniform. At the same time, the luminescent material can be coated to significantly increase its content in the powder coating, avoiding the problem of poor leveling caused by excessive addition. The grinding disc and grinding column surfaces of the ACM grinder involved in the preparation of the luminescent powder coating, as well as the bonding stirring kettle, are carburized to increase the Mohs hardness and wear resistance of the grinder and bonding machine, and avoid the iron metal precipitated during the surface damage of the related equipment during high-speed operation to contaminate the luminescent material, thereby causing the luminescent effect of the luminescent powder coating to become dim and the luminescence to be uneven.

[0021] The present invention uses a compound of ingredients and the ingredients work together to exhibit better performance. Compared with traditional powder coatings with fluorescent agents added, it has better weather resistance and high afterglow brightness. It can be effectively used in outdoor places and can play a decorative and warning role. It has excellent overall stability and still maintains excellent luminous performance after long-term storage and use. In addition, the luminescent material particles of the present invention are relatively large and have high afterglow brightness. After being coated with a fluorine-containing acrylic resin with low surface energy, it can effectively float on the powder coating film, effectively improving the coverage of the luminescent material on the surface of the coating film, and further improving the afterglow brightness. The luminescent material is composed of a matrix and an activator, and has a better decorative effect. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with its embodiments. It should be understood that the specific implementation methods described herein are only used to explain the present invention and do not limit the protection scope of the present invention.

[0023] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more related listed items.

[0024] A luminescent powder coating in one embodiment of the present invention comprises the following raw materials in parts by weight: 55-70 parts of terminal carboxyl polyester resin, 5-10 parts of fluorine-containing acrylic resin, 4-5.3 parts of triglycidyl isocyanurate, 10-20 parts of filler, 10-20 parts of luminescent material, 0.5-2 parts of leveling agent, 0.5-2 parts of brightener, 0.5-1 parts of carbon nanotubes, 0.2-0.3 parts of anti-scratch agent, 0.2-0.5 parts of benzoin, 0.5-2 parts of defoaming agent, 0.5-2 parts of antioxidant, 0-3.0 parts of pigment, 0.1-0.2 parts of desiccant, 0.1-0.3 parts of bonding aid and 0.3-0.5 parts of silicon dioxide.

[0025] In one embodiment, the acid value of the carboxyl-terminated polyester resin is 32 mgKOH / g to 38 mgKOH / g. stick Degree@200℃(mPa.s) The temperature is 1500~2500, and the glass transition temperature is 67℃~70℃.

[0026] In one embodiment, the fluorine-containing acrylic resin is a synthetic resin with fluorine element introduced into the acrylic resin structure.

[0027] In one embodiment, the filler is at least one of calcium carbonate, mica powder and barium sulfate.

[0028] In one embodiment, the luminescent material includes a matrix and an activator, and the activator accounts for 10% to 30% of the mass of the matrix.

[0029] In one embodiment, the activator is a rare earth element.

[0030] In one embodiment, the rare earth element is at least one of europium and dysprosium.

[0031] In one embodiment, the matrix is ​​one or a mixture of aluminate and silicate.

[0032] In one of the embodiments, the carbon nanotubes have an electrical conductivity of >150s / cm, a length of 10-20um, and are obtained by curling graphene sheets.

[0033] In one embodiment, after the matrix and the activator are mixed, the mixture is treated at a temperature of 45° C. to 65° C. for 20 min to 30 min to obtain the luminescent material.

[0034] In one embodiment, the anti-scratch agent is at least one of micronized polypropylene wax, PTFE-modified PE wax and PP wax.

[0035] In one embodiment, the leveling agent is a polyester modified silicone leveling agent.

[0036] In one embodiment, the defoaming agent is a polyether-modified silicone defoaming agent.

[0037] In one embodiment, the antioxidant is a hindered phenol antioxidant.

[0038] In one embodiment, the median particle size of the silicon dioxide is 7 nm to 10 nm.

[0039] In one embodiment, the desiccant is imported alumina C, a fine-grained pure alumina with a surface area (m2 / g): 100±10, an average particle size (nm): 10-13, and an average particle size (nm). 2 O 3 Content: ≥99.7.

[0040] In one embodiment, the bonding agent is a white ultra-fine powder, the main component of which is a composite amide wax, with a solid content of more than 99.5% and a particle size (D 50 ) is 2-3um. Adding bonding aids in the bonding process can prevent agglomeration and improve the bonding effect of metal powder.

[0041] In one embodiment, the grinding disc and grinding column surface of the ACM grinder and the bonded stirring kettle are carburized, and the carburized hardened layer thickness is 2-6mm. The specific treatment process is: placing the metal and the carburizing agent together in a closed cavity, using heating, vacuum and other measures to activate the metal surface, and then decomposing, absorbing, diffusing and other processes to make carbon enter the metal matrix.

[0042] In addition, the present invention also provides a method for preparing a luminous powder coating, the preparation method comprising the following steps:

[0043] The luminescent material is added to a drum ball mill for ball milling, the ball-milled luminescent material and silicon dioxide are added to a mixing device for high-speed airflow impact treatment to obtain a mixture A, and then the mixture A, carbon nanotubes and fluorine-containing acrylic resin are added to a grinding device for stirring, grinding and coating treatment to obtain a mixture B;

[0044] Adding carboxyl-terminated polyester resin, triglycidyl isocyanurate, filler, leveling agent, brightener, anti-scratch agent, benzoin, defoamer, antioxidant and pigment into a mixing tank for premixing; then, melt extrusion, cooling and ACM grinding are performed to obtain a mixture C;

[0045] The mixture B, the mixture C and the bonding aid are mixed, subjected to a bonding process, and then a desiccant is added and mixed, and then sieved through a 160-180 mesh sieve to obtain a luminous powder coating.

[0046] In one of the embodiments, the melt extrusion conditions are: screw speed is 40HZ~45HZ, melting zone temperature is 120℃~125℃, and mixing zone temperature is 130℃~135℃.

[0047] In one of the embodiments, the setting conditions of the grinding mill during the ACM grinding process are: main grinding frequency 30HZ~35HZ, auxiliary grinding frequency 20HZ~30HZ, and feeding frequency 18HZ~25HZ.

[0048] In one of the embodiments, the conditions of the bonding process are: bonding temperature is 65℃~68℃, heating speed is 900rpm~1000rpm, bonding speed is 600rpm~700rpm, cooling speed is 400pm~500pm, cold water temperature is 17℃~19℃, hot water temperature is 70℃~75℃, and the bonding stage time is 300s~500s.

[0049] The present invention exhibits better performance through the compound use of components and the synergistic effect between the components. Compared with traditional powder coatings with added fluorescent agents, it has better weather resistance and high afterglow brightness, can be effectively used in outdoor places, can play a decorative and warning effect, has excellent overall stability, and still maintains excellent luminous performance after long-term storage and use.

[0050] The embodiments of the present invention will be described in detail below with reference to specific examples.

[0051] It should be noted that the following raw materials are all in weight ratios. The grinding disc and grinding column surfaces of the ACM grinder and the bonded stirring kettle in the following examples are carburized.

[0052] Embodiment 1:

[0053] A method for preparing a luminous powder coating comprises the following steps:

[0054] Aluminate and 20% by mass of europium of the aluminate are mixed and treated at a temperature of 50° C. for 25 minutes to obtain a luminescent material;

[0055] 16 parts of luminescent material are added to a drum ball mill for ball milling, the ball-milled luminescent material and 0.4 parts of silicon dioxide are added to a mixing device for high-speed airflow impact treatment to obtain a mixture A, and then the mixture A, 0.8 parts of carbon nanotubes and 8 parts of fluorine-containing acrylic resin are added to a grinding device for stirring, grinding and coating treatment to obtain a mixture B;

[0056] 65 parts of carboxyl-terminated polyester resin, 4.9 parts of triglycidyl isocyanurate, 15 parts of calcium carbonate, 1 part of polyester-modified silicone leveling agent, 0.5 parts of brightener, 0.2 parts of micronized polypropylene wax, 0.2 parts of benzoin, 0.8 parts of polyether-modified silicone defoamer, 1 part of hindered phenol antioxidant and 1 part of pigment are added into a mixing tank for premixing; then melt-extruded and the melt-extruded conditions are: screw speed of 45 Hz, melting zone temperature of 120° C., mixing zone temperature of 130° C., cooled and ACM ground and the setting conditions of the mill during the ACM grinding process are: main grinding frequency of 30 Hz, auxiliary grinding frequency of 20 Hz, feeding frequency of 18 Hz, to obtain a mixture C;

[0057] The mixture B, the mixture C and the bonding aid are mixed and subjected to a bonding process. The conditions of the bonding process are as follows: a bonding temperature of 65°C, a heating speed of 900rpm, a bonding speed of 600rpm, a cooling speed of 400pm, a cold water temperature of 17°C, a hot water temperature of 70°C, and a bonding stage time of 300s. Imported alumina C is then added, mixed, and sieved through a 160-mesh sieve to obtain a luminous powder coating.

[0058] Embodiment 2:

[0059] A method for preparing a luminous powder coating comprises the following steps:

[0060] Aluminate and 18% by mass of europium of the aluminate are mixed and treated at a temperature of 60° C. for 30 minutes to obtain a luminescent material;

[0061] 19 parts of luminescent material are added to a drum ball mill for ball milling, the ball-milled luminescent material and 0.5 parts of silicon dioxide are added to a mixing device for high-speed airflow impact treatment to obtain a mixture A, and then the mixture A, 0.8 parts of carbon nanotubes and 8 parts of fluorine-containing acrylic resin are added to a grinding device for stirring, grinding and coating treatment to obtain a mixture B;

[0062] 67 parts of carboxyl-terminated polyester resin, 5 parts of triglycidyl isocyanurate, 17 parts of calcium carbonate, 1 part of polyester-modified silicone leveling agent, 0.5 parts of brightener, 0.3 parts of micronized polypropylene wax, 0.5 parts of benzoin, 1 part of polyether-modified silicone defoamer, 0.5 parts of hindered phenol antioxidant and 1 part of pigment are added into a mixing tank for premixing; then melt-extruded and the melt-extruded conditions are as follows: screw speed is 42 Hz, melting zone temperature is 125° C., mixing zone temperature is 132° C., cooled and ACM ground and the setting conditions of the mill during the ACM grinding process are as follows: main grinding frequency is 35 Hz, auxiliary grinding frequency is 30 Hz, and feeding frequency is 20 Hz, to obtain a mixture C;

[0063] The mixture B, the mixture C and the bonding aid are mixed and subjected to a bonding process. The bonding process conditions are as follows: a bonding temperature of 66°C, a heating speed of 1000rpm, a bonding speed of 700rpm, a cooling speed of 500pm, a cold water temperature of 19°C, a hot water temperature of 75°C, and a bonding stage time of 300s. Imported alumina C is then added, mixed, and sieved through a 160-mesh sieve to obtain a luminous powder coating.

[0064] Embodiment 3:

[0065] A method for preparing a luminous powder coating comprises the following steps:

[0066] Aluminate and 20% dysprosium by mass of the aluminate are mixed and treated at a temperature of 60° C. for 30 minutes to obtain a luminescent material;

[0067] 20 parts of luminescent material are added to a drum ball mill for ball milling, the ball-milled luminescent material and 0.5 parts of silicon dioxide are added to a mixing device for high-speed airflow impact treatment to obtain a mixture A, and then the mixture A, 0.8 parts of carbon nanotubes and 10 parts of fluorine-containing acrylic resin are added to a grinding device for stirring, grinding and coating treatment to obtain a mixture B;

[0068] 68 parts of carboxyl-terminated polyester resin, 5.1 parts of triglycidyl isocyanurate, 18 parts of calcium carbonate, 1 part of polyester-modified silicone leveling agent, 0.8 parts of brightener, 0.3 parts of micronized polypropylene wax, 0.4 parts of benzoin, 0.8 parts of polyether-modified silicone defoamer, 0.7 parts of hindered phenol antioxidant and 1 part of pigment are added into a mixing tank for premixing; then melt-extruded and the melt-extruded conditions are as follows: screw speed is 45 Hz, melting zone temperature is 125° C., mixing zone temperature is 135° C., cooled and ACM ground and the setting conditions of the mill during the ACM grinding process are as follows: main grinding frequency is 33 Hz, auxiliary grinding frequency is 28 Hz, and feeding frequency is 22 Hz, to obtain a mixture C;

[0069] The mixture B, the mixture C and the bonding aid are mixed and subjected to a bonding process. The conditions of the bonding process are as follows: a bonding temperature of 67°C, a heating speed of 1000rpm, a bonding speed of 700rpm, a cooling speed of 450pm, a cold water temperature of 19°C, a hot water temperature of 74°C, and a bonding stage time of 400s. Imported alumina C is then added, mixed, and sieved through a 160-mesh sieve to obtain a luminous powder coating.

[0070] Embodiment 4:

[0071] A method for preparing a luminous powder coating comprises the following steps:

[0072] Aluminate and 20% dysprosium by mass of the aluminate are mixed and treated at a temperature of 65° C. for 30 minutes to obtain a luminescent material;

[0073] 20 parts of luminescent material are added to a drum ball mill for ball milling, the ball-milled luminescent material and 0.5 parts of silicon dioxide are added to a mixing device for high-speed airflow impact treatment to obtain a mixture A, and then the mixture A, 0.8 parts of carbon nanotubes and 10 parts of fluorine-containing acrylic resin are added to a grinding device for stirring, grinding and coating treatment to obtain a mixture B;

[0074] 70 parts of carboxyl-terminated polyester resin, 5.3 parts of triglycidyl isocyanurate, 20 parts of calcium carbonate, 0.9 parts of polyester-modified silicone leveling agent, 0.6 parts of brightener, 0.3 parts of micronized polypropylene wax, 0.4 parts of benzoin, 0.8 parts of polyether-modified silicone defoamer, 0.8 parts of hindered phenol antioxidant and 1 part of pigment are added into a mixing tank for premixing; then melt-extruded and the melt-extruded conditions are as follows: screw speed is 45 Hz, melting zone temperature is 125° C., mixing zone temperature is 135° C., cooled and ACM ground and the setting conditions of the mill during the ACM grinding process are as follows: main grinding frequency is 35 Hz, auxiliary grinding frequency is 30 Hz, and feeding frequency is 25 Hz, to obtain a mixture C;

[0075] The mixture B, the mixture C and the bonding aid are mixed and subjected to a bonding process. The conditions of the bonding process are as follows: a bonding temperature of 68°C, a heating speed of 1000rpm, a bonding speed of 700rpm, a cooling speed of 500pm, a cold water temperature of 19°C, a hot water temperature of 75°C, and a bonding stage time of 500s. Imported alumina C is then added, mixed, and sieved through a 160-mesh sieve to obtain a luminous powder coating.

[0076] Comparative Example 1:

[0077] The difference between Comparative Example 1 and Example 4 is that the luminescent material in Comparative Example 1 is not coated, and the rest is the same as Example 4, that is, the preparation method in Comparative Example 1 includes the following steps:

[0078] Aluminate and 20% dysprosium by mass of the aluminate are mixed and treated at a temperature of 65° C. for 30 minutes to obtain a luminescent material;

[0079] 20 parts of luminescent material, 0.5 parts of silicon dioxide, 10 parts of fluorine-containing acrylic resin, 70 parts of carboxyl-terminated polyester resin, 5.3 parts of triglycidyl isocyanurate, 20 parts of calcium carbonate, 0.9 parts of polyester-modified silicone leveling agent, 0.6 parts of brightener, 0.8 parts of carbon nanotubes, 0.3 parts of micronized polypropylene wax, 0.4 parts of benzoin, 0.8 parts of polyether-modified silicone defoamer, 0.8 parts of hindered phenol antioxidant and 1 part of pigment are added into a mixing tank for premixing; then melt extrusion is performed under the conditions of: screw speed of 45 Hz, melting zone temperature of 125° C., mixing zone temperature of 135° C., cooling and ACM grinding, and the setting conditions of the mill during the ACM grinding process are: main grinding frequency of 35 Hz, auxiliary grinding frequency of 30 Hz, and feeding frequency of 25 Hz to obtain a mixture;

[0080] The mixture and the bonding aid are mixed, and a bonding process is performed. The conditions of the bonding process are as follows: a bonding temperature of 68°C, a heating speed of 1000rpm, a bonding speed of 700rpm, a cooling speed of 500pm, a cold water temperature of 19°C, a hot water temperature of 75°C, and a bonding stage time of 500s. Imported alumina C is then added, mixed, and sieved through a 160-mesh sieve to obtain a luminous powder coating.

[0081] Comparative Example 2:

[0082] The difference between Comparative Example 2 and Example 4 is that the luminescent material in Comparative Example 2 is a single dysprosium component, that is, it does not include a matrix, and the rest is the same as Example 4.

[0083] Comparative Example 3:

[0084] The difference between Comparative Example 3 and Example 4 is that the luminescent material in Comparative Example 3 is: aluminate and 5% dysprosium by mass of the aluminate are mixed and treated at a temperature of 65° C. for 30 minutes to obtain the luminescent material. The rest is the same as Example 4.

[0085] Comparative Example 4:

[0086] The difference between Comparative Example 4 and Example 4 is that the fluorine-containing acrylic resin is replaced by polyester resin in Comparative Example 4, and the rest is the same as Example 4.

[0087] Comparative Example 5:

[0088] The difference between Comparative Example 5 and Example 4 is that in Comparative Example 5, epoxy resin is used to replace the terminal carboxyl polyester resin, and the rest is the same as Example 4.

[0089] Comparative Example 6:

[0090] The difference between Comparative Example 6 and Example 4 is that Comparative Example 6 is not subjected to bonding process, and the rest is the same as Example 4.

[0091] Comparative Example 7:

[0092] The difference between Comparative Example 7 and Example 4 is that the bonding process conditions in Comparative Example 7 are as follows: bonding temperature is 40°C, heating speed is 1000rpm, bonding speed is 500rpm, cooling speed is 500pm, cold water temperature is 15°C, hot water temperature is 55°C, and bonding stage time is 200s. Others are the same as Example 4.

[0093] Comparative Example 8:

[0094] The difference between Comparative Example 8 and Example 4 is that no luminescent material is added in Comparative Example 8, and the rest is the same as Example 4.

[0095] Comparative Example 9:

[0096] The difference between Comparative Example 9 and Example 4 is that the ratio of the preparation raw materials in Comparative Example 9 is different, and the others are the same as Example 4. The ratio of the preparation raw materials in Comparative Example 9 is as follows: 50 parts of terminal carboxyl polyester resin, 3 parts of fluorine-containing acrylic resin, 1 part of triglycidyl isocyanurate, 5 parts of filler, 15 parts of luminescent material, 0.5 parts of leveling agent, 0.5 parts of brightener, 0.2 parts of anti-scratch agent, 0.2 parts of benzoin, 0.5 parts of defoaming agent, 0.5 parts of antioxidant, 1 part of pigment, 0.1 parts of desiccant, 0.3 parts of bonding aid and 0.1 parts of silica.

[0097] The luminous powder coatings prepared in Examples 1 to 4 and the powder coatings prepared in Comparative Examples 1 to 9 were subjected to performance tests.

[0098] 1. Mechanical properties refer to GB / T5237.4-2017, and the test results are shown in Table 1 below.

[0099] Table 1: Mechanical properties

[0100]

[0101] From the data analysis of Table 1, it can be seen that after optimizing the preparation of raw materials and the preparation ratio of raw materials, the present application obtains a coating film with significant mechanical properties as a whole.

[0102] 2. Aging resistance test: UVB lamp test conditions are carried out according to German standard GSBAL631.2017, and xenon lamp test conditions are carried out according to national standard GB / T1865-2009. The test results are shown in Table 2 below.

[0103] Table 2: Aging test results

[0104]

[0105]

[0106] From the data analysis of Table 2, it can be seen that the coating film formed by the luminous powder coating of the present application has excellent gloss retention rate and uniform apparent color.

[0107] III. Brightness test, test conditions and test results are shown in Table 3 below.

[0108] Table 3: Brightness test results

[0109]

[0110]

[0111] From the data analysis in Table 3, it can be seen that the preparation raw materials, preparation raw material ratios and process interactions of the present application result in high afterglow brightness, can be effectively used in outdoor places, can have decorative and warning effects, have excellent overall stability, and still maintain excellent luminous properties after long-term storage and use.

[0112] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0113] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A luminous powder coating, characterized in that: The luminescent powder coating comprises the following raw materials in parts by weight: 55-70 parts of terminal carboxyl polyester resin, 5-10 parts of fluorine-containing acrylic resin, 4-5.3 parts of triglycidyl isocyanurate, 10-20 parts of filler, 10-20 parts of luminescent material, 0.5-2 parts of leveling agent, 0.5-2 parts of brightener, 0.5-1 parts of carbon nanotubes, 0.2-0.3 parts of anti-scratch agent, 0.2-0.5 parts of benzoin, 0.5-2 parts of defoaming agent, 0.5-2 parts of antioxidant, 0-3.0 parts of pigment, 0.1-0.2 parts of desiccant, 0.1-0.3 parts of bonding aid and 0.3-0.5 parts of silicon dioxide.

2. The luminous powder coating according to claim 1, characterized in that: The acid value of the carboxyl-terminated polyester resin is 32 mgKOH / g to 38 mgKOH / g. Viscosity@200℃(mPa.s) The temperature is 1500~2500, and the glass transition temperature is 67℃~70℃.

3. The luminous powder coating according to claim 1, characterized in that: The filler is at least one of calcium carbonate, mica powder and barium sulfate.

4. The luminous powder coating according to claim 1, characterized in that: The luminescent material comprises a matrix and an activator, and the activator accounts for 10% to 30% of the mass of the matrix.

5. The luminous powder coating according to claim 4, characterized in that: The activator is a rare earth element; the matrix is ​​one or a mixture of aluminate and silicate.

6. The luminous powder coating according to claim 1, characterized in that: The carbon nanotube has an electrical conductivity of more than 150 s / cm and a length of 10 to 20 um, and is obtained by curling a graphene sheet.

7. The luminous powder coating according to claim 1, characterized in that: The anti-scratch agent is at least one of micronized polypropylene wax, PTFE-modified PE wax and PP wax.

8. A method for preparing a luminous powder coating, characterized in that: The preparation method is used to prepare the luminescent powder coating according to any one of claims 1 to 7, and the preparation method comprises the following steps: The luminescent material is added to a drum ball mill for ball milling, and then the ball-milled luminescent material and silicon dioxide are added to a mixing device for high-speed airflow impact treatment to obtain a mixture A, and then the mixture A, carbon nanotubes and fluorine-containing acrylic resin are added to a grinding device for stirring, grinding and coating treatment to obtain a mixture B; Adding carboxyl-terminated polyester resin, triglycidyl isocyanurate, filler, leveling agent, brightener, anti-scratch agent, benzoin, defoamer, antioxidant and pigment into a mixing tank for premixing; then, melt extrusion, cooling and ACM grinding are performed to obtain a mixture C; The mixture B, the mixture C and the bonding aid are mixed, subjected to a bonding process, and then a desiccant is added and mixed, and then sieved through a 160-180 mesh sieve to obtain a luminous powder coating.

9. The preparation method according to claim 8, characterized in that: The conditions for the melt extrusion are: a screw speed of 40 Hz to 45 Hz, a melting zone temperature of 120° C. to 125° C., and a mixing zone temperature of 130° C. to 135° C.

10. The preparation method according to claim 8, characterized in that: The bonding process conditions are as follows: bonding temperature is 65℃~68℃, heating speed is 900rpm~1000rpm, bonding speed is 600rpm~700rpm, cooling speed is 400pm~500pm, cold water temperature is 17℃~19℃, hot water temperature is 70℃~75℃, and bonding stage time is 300s~500s.

Citation Information

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