Photocuring flame-retardant coating and preparation method thereof
By using composite flame retardant in photocuring coatings, using materials such as pentaerythritol and phosphorus trichloride to form composite flame retardant containing end double bonds and thiol groups, and compounding them with organic sepiolite, the problem of insufficient flame retardant performance of existing photocuring coatings is solved, and more efficient flame retardant effect and improved curing rate and mechanical properties are achieved.
Patent Information
- Application Number
- CN202510492245.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-18
- Publication Date
- 2025-06-27
AI Technical Summary
The flame retardant performance of existing photocuring coatings is insufficient, which makes it impossible to meet the conditions where the flame retardant performance requirements are high, and the addition of flame retardant will lead to a reduced curing rate and uneven dispersion, affecting product performance.
Using a composite flame retardant, the flame retardant is reacted by reaction of pentaerythritol and phosphorus oxychloride, followed by esterification with thiol succinic acid and p-toluenesulfonic acid, followed by monosubstitution reaction with triplecyanochloride and acetone, and then vulcanized with sodium sulfide nucleic acid and hydrochloric acid solution, and finally a click reaction with trimethylol propane triacrylate and intermediate 5 to form a composite flame retardant containing end double bonds and thiol groups, and is compounded with organic sepiolite.
The flame retardant performance and curing rate are improved, the amount of flame retardant is added is reduced, the dispersion effect and mechanical properties of the coating are improved, and the flame retardant effect and product performance are achieved.
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Abstract
Description
Technical Field
[0001] The present invention relates to the field of coatings, and particularly to a photocurable flame retardant coating and a preparation method thereof. Background Art
[0002] The ultraviolet photocuring technology has the advantages of rapid curing, less environmental pollution, good product quality, low process cost, high chemical stability, etc., and is widely used in fields such as coatings, adhesives, and inks. In the field of coatings, traditional matrix materials for ultraviolet photocuring resins, such as epoxy acrylate and polyurethane acrylate, have certain defects in flame retardancy and cannot be applied to some occasions with high requirements for flame retardancy. In order to improve the flame retardancy of photocurable coatings, flame retardants are usually added to the substrate and physically mixed with polymers to achieve this.
[0003] At present, according to the flame retardant, it is usually only physically mixed with the flame-retarded material and other components, which is convenient to use. However, to achieve excellent flame retardant effects, more flame retardants need to be added, which usually leads to problems such as a decrease in the coating curing rate. At the same time, there is also the problem that the flame retardant is not evenly dispersed in the matrix material, resulting in the precipitation of the flame retardant during the material processing or use process, affecting the performance of the product, and the flame retardant performance also cannot reach the ideal effect. Summary of the Invention
[0004] In order to solve the above problems, the purpose of the present invention is to provide a photocurable flame retardant coating and a preparation method thereof.
[0005] The purpose of the present invention can be achieved by the following technical solutions: A photocurable flame retardant coating includes the following raw materials in parts by weight: 50 - 60 parts of acrylate resin, 10 - 15 parts of composite flame retardant, 5 - 10 parts of diluent, 1 - 3 parts of defoamer, and 1 - 3 parts of photoinitiator; The photocurable flame retardant coating is prepared by the following steps: adding acrylate resin, composite flame retardant, diluent, and defoamer into a stirring container, stirring at a stirring rate of 800 - 1000 rpm and at room temperature for 20 - 30 min, and then adding the photoinitiator and stirring to mix, obtaining a photocurable flame retardant coating; The composite flame retardant is prepared by the following steps: A1: Adding pentaerythritol and phosphorus oxychloride into a container, stirring and mixing, reacting at a stirring rate of 200 - 300 rpm and at 140 - 150 °C for 10 - 12 h, adding deionized water, cooling and filtering by suction, obtaining intermediate 1. The dosage ratio of phosphorus oxychloride, pentaerythritol, and deionized water is 0.1 mol: 0.1 - 0.12 mol: 50 - 100 mL; During the reaction process, the hydroxyl group in pentaerythritol reacts with phosphorus oxychloride to obtain intermediate 1, as shown below;
[0006] A2: Add intermediate 1, mercaptosuccinic acid, and p-toluenesulfonic acid into a container, stir and mix them. React for 12 - 16 h under the conditions of a stirring rate of 100 - 200 rpm and 80 °C. Then conduct vacuum distillation. Add ethyl acetate, and wash three times with saturated sodium bicarbonate solution and saturated brine solution. Dry in vacuum at 60 °C for 12 h, filter and rotary evaporate to obtain intermediate 2. The dosage ratio of intermediate 1, mercaptosuccinic acid, ethyl acetate, and p-toluenesulfonic acid is 0.2 mol : 0.1 mol : 40 - 60 mL : 0.05 g; During the reaction process, the hydroxyl group in intermediate 1 reacts with the carboxyl group in mercaptosuccinic acid to undergo an esterification reaction to obtain intermediate 2, as shown below;
[0007] A3: Add cyanuric chloride and acetone into a container, stir and mix them. Slowly dropwise add diallylamine. React for 3 h under the conditions of a stirring rate of 100 - 150 rpm and 5 - 10 °C. Filter and wash three times with acetone. Dry in vacuum at 60 °C for 6 - 8 h to obtain intermediate 3. The dosage ratio of cyanuric chloride, diallylamine, and acetone is 0.1 mol : 0.1 mol : 200 - 300 mL; During the reaction process, by controlling the reaction temperature, cyanuric chloride undergoes a monosubstitution reaction with diallylamine to obtain intermediate 3, as shown below;
[0008] A4: Add sodium sulfide nonahydrate into deionized water, stir and slowly add hydrochloric acid solution. Then add intermediate 3. React for 2 - 4 h under the conditions of a stirring rate of 200 - 300 rpm and 0 - 10 °C. Wash three times with acetone, add water for chromatography until the effluent is neutral to obtain intermediate 4. The molar concentration of the hydrochloric acid solution is 2 mol / L. The dosage ratio of sodium sulfide nonahydrate, deionized water, intermediate 3, and hydrochloric acid solution is 120 g : 100 - 150 mL : 50 g : 150 - 200 mL; During the reaction process, using sodium sulfide nonahydrate as a sulfidizing agent to sulfidize the chlorine group in intermediate 3 to obtain intermediate 4, as shown below;
[0009] A5: Add intermediate 2, methanol, and deionized water into a container, stir and heat to 70 °C. Add azobisisobutyronitrile and stir and mix. Then dropwise add intermediate 4. React for 4 - 6 h under the conditions of a stirring rate of 200 - 300 rpm and 70 °C. Cool and filter, wash three times with methanol. Dry in vacuum at 65 °C for 24 h to obtain intermediate 5. The dosage ratio of intermediate 2, intermediate 4, methanol, azobisisobutyronitrile, and deionized water is 0.2 - 0.22 mol : 0.1 mol : 100 - 200 mL : 0.2 - 0.4 g : 100 mL; During the reaction process, a click reaction occurs between the double bond in intermediate 4 and the mercapto group in intermediate 2 to obtain intermediate 5; A6: Add trimethylolpropane triacrylate and triphenylphosphine into a container, stir and mix them, then add p-methoxyphenol and intermediate 5, and react for 4 - 6 h under the conditions of a stirring rate of 200 - 300 rpm, room temperature and ultraviolet lamp irradiation. Then add acetone and organic sepiolite, stir and mix them, ultrasonically disperse for 50 - 60 min, and then mix for 1 h under the conditions of a stirring rate of 150 - 300 rpm and 50 - 60 °C. Rotate evaporate and filter to obtain a composite flame retardant. The dosage ratio of trimethylolpropane triacrylate, intermediate 5, triphenylphosphine, p-methoxyphenol, acetone and organic sepiolite is 0.2 - 0.22 mol: 0.1 mol: 0.1 g: 0.1 g: 150 - 200 mL: 50 g; During the reaction process, trimethylolpropane triacrylate first undergoes a thiol-ene click reaction with intermediate 5, and then is compounded and adsorbed with organic sepiolite to obtain a composite flame retardant; Furthermore, the organic sepiolite is silane-modified sepiolite; Furthermore, the diluent is one or more of 1,6-hexanediol diacrylate or dipropylene glycol diacrylate; Furthermore, the defoamer is a polyether defoamer; Furthermore, the photoinitiator is a cleavage-type photoinitiator; Advantages of the present invention: The present invention provides a photocurable flame retardant coating and a preparation method thereof. In the raw materials of the photocurable flame retardant coating, the composite flame retardant is obtained by reacting trimethylolpropane triacrylate with intermediate 5 and then compounding with organic sepiolite, so that the composite flame retardant contains terminal double bond groups. The terminal double bonds can enable the composite flame retardant to participate in the curing process of the matrix material, resulting in better dispersion of the composite flame retardant in the matrix material, effectively improving the decline in the flame retardant performance of the matrix material caused by agglomeration. At the same time, the composite flame retardant also contains a certain amount of mercapto groups, which can improve the oxygen inhibition effect during the photocuring process to a certain extent, reduce the coating curing time, and improve the film performance. The composite flame retardant is composed of sepiolite inorganic filler and intermediate 5, and intermediate 5 is obtained by reacting intermediate 4 with intermediate 2, so that intermediate 5 contains melamine groups and phosphate flame retardant groups. These two groups can be used as a gas source and an acid source respectively to form an intumescent flame retardant system, forming a continuous and dense carbon layer during combustion. At the same time, this flame retardant system also cooperates with S to form an N-P-S flame retardant system, achieving a better flame retardant effect. Due to the good high-temperature resistance of sepiolite, it can play a synergistic flame retardant role with the N-P-S flame retardant system in intermediate 5 under high-temperature conditions, promoting the formation of the carbon layer and making the carbon layer more dense and uniform, thereby better inhibiting the overflow of gas and heat transfer during combustion, achieving a good flame retardant effect. And due to the special crystal structure of sepiolite, it can also improve the mechanical properties of the coating to a certain extent. Specific embodiments
[0010] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts shall fall within the protection scope of the present invention. Embodiment
[0011] The composite flame retardant is prepared through the following steps: A1: Add pentaerythritol and phosphorus oxychloride into a container, stir and mix, react for 12 h under the conditions of a stirring rate of 200 rpm and 140 °C, add deionized water, cool and filter to obtain intermediate 1. The dosage ratio of phosphorus oxychloride, pentaerythritol and deionized water is 0.1 mol: 0.1 mol: 100 mL; A2: Add intermediate 1, mercaptosuccinic acid, and p-toluenesulfonic acid into a container, stir and mix them. React for 16 h under the conditions of a stirring rate of 100 rpm and 80 °C. Conduct vacuum distillation. Then add ethyl acetate, and wash three times with saturated sodium bicarbonate solution and saturated brine solution. Dry in vacuum at 60 °C for 12 h, filter and rotary evaporate to obtain intermediate 2. The dosage ratio of intermediate 1, mercaptosuccinic acid, ethyl acetate, and p-toluenesulfonic acid is 0.2 mol: 0.1 mol: 40 mL: 0.05 g; A3: Add cyanuric chloride and acetone into a container, stir and mix them. Slowly dropwise add diallylamine. React for 3 h under the conditions of a stirring rate of 100 rpm and 5 °C. Filter, and wash three times with acetone. Dry in vacuum at 60 °C for 6 h to obtain intermediate 3. The dosage ratio of cyanuric chloride, diallylamine, and acetone is 0.1 mol: 0.1 mol: 200 mL; A4: Add sodium sulfide nonahydrate into deionized water, stir and slowly add hydrochloric acid solution. Then add intermediate 3. React for 4 h under the conditions of a stirring rate of 300 rpm and 0 °C. Wash three times with acetone, add water for chromatography until the effluent is neutral to obtain intermediate 4. The molar concentration of the hydrochloric acid solution is 2 mol / L. The dosage ratio of sodium sulfide nonahydrate, deionized water, intermediate 3, and hydrochloric acid solution is 120 g: 100 mL: 50 g: 200 mL; A5: Add intermediate 2, methanol, and deionized water into a container, stir and heat up to 70 °C. Add azobisisobutyronitrile and stir and mix. Then dropwise add intermediate 4. React for 4 h under the conditions of a stirring rate of 300 rpm and 70 °C. Cool and filter, and wash three times with methanol. Dry in vacuum at 65 °C for 24 h to obtain intermediate 5. The dosage ratio of intermediate 2, intermediate 4, methanol, azobisisobutyronitrile, and deionized water is 0.2 mol: 0.1 mol: 200 mL: 0.4 g: 100 mL; A6: Add trimethylolpropane triacrylate and triphenylphosphine into a container, stir and mix them. Then add p-methoxyphenol and intermediate 5. React for 4 h under the conditions of a stirring rate of 300 rpm, room temperature, and ultraviolet lamp irradiation. Then add acetone and commercially available silane-modified sepiolite, stir and mix, ultrasonically disperse for 50 min, and then mix at a stirring rate of 150 rpm and 50 °C for 1 h. Rotary evaporate and filter to obtain the composite flame retardant. The dosage ratio of trimethylolpropane triacrylate, intermediate 5, triphenylphosphine, p-methoxyphenol, acetone, and commercially available silane-modified sepiolite is 0.22 mol: 0.1 mol: 0.1 g: 0.1 g: 200 mL: 50 g; Example
[0012] The said composite flame retardant is prepared through the following steps: A1: Add pentaerythritol and phosphorus oxychloride into a container, stir and mix them. React for 10 h under the conditions of a stirring rate of 300 rpm and 150 °C. Add deionized water, cool and filter by suction to obtain Intermediate 1. The dosage ratio of phosphorus oxychloride, pentaerythritol and deionized water is 0.1 mol: 0.1 mol: 50 mL; A2: Add Intermediate 1, mercaptosuccinic acid and p-toluenesulfonic acid into a container, stir and mix them. React for 12 h under the conditions of a stirring rate of 200 rpm and 80 °C. Distill under reduced pressure, then add ethyl acetate, and wash three times with saturated sodium bicarbonate solution and saturated brine solution. Dry in vacuum at 60 °C for 12 h, filter and rotary evaporate to obtain Intermediate 2. The dosage ratio of Intermediate 1, mercaptosuccinic acid, ethyl acetate and p-toluenesulfonic acid is 0.2 mol: 0.1 mol: 40 mL: 0.05 g; A3: Add cyanuric chloride and acetone into a container, stir and mix them. Slowly dropwise add diallylamine. React for 3 h under the conditions of a stirring rate of 100 rpm and 8 °C. Filter and wash three times with acetone. Dry in vacuum at 60 °C for 6 h to obtain Intermediate 3. The dosage ratio of cyanuric chloride, diallylamine and acetone is 0.1 mol: 0.1 mol: 200 - 300 mL; A4: Add sodium sulfide nonahydrate into deionized water, stir and slowly add hydrochloric acid solution, then add Intermediate 3. React for 2 h under the conditions of a stirring rate of 300 rpm and 10 °C. Wash three times with acetone, add water for chromatography until the effluent is neutral to obtain Intermediate 4. The molar concentration of the hydrochloric acid solution is 2 mol / L. The dosage ratio of sodium sulfide nonahydrate, deionized water, Intermediate 3 and hydrochloric acid solution is 120 g: 150 mL: 50 g: 150 mL; A5: Add Intermediate 2, methanol and deionized water into a container, stir and heat up to 70 °C, add azobisisobutyronitrile and stir and mix. Then dropwise add Intermediate 4. React for 4 h under the conditions of a stirring rate of 300 rpm and 70 °C. Cool and filter, wash three times with methanol. Dry in vacuum at 65 °C for 24 h to obtain Intermediate 5. The dosage ratio of Intermediate 2, Intermediate 4, methanol, azobisisobutyronitrile and deionized water is 0.2 mol: 0.1 mol: 200 mL: 0.2 g: 100 mL; A6: Add trimethylolpropane triacrylate and triphenylphosphine into a container, stir and mix them, then add p-hydroxyanisole and Intermediate 5. React for 4 h under the conditions of a stirring rate of 300 rpm, room temperature and ultraviolet lamp irradiation. Then add acetone and commercially available silane-modified sepiolite, stir and mix them, ultrasonically disperse for 50 min, and then mix at a stirring rate of 300 rpm and 50 °C for 1 h. Rotate evaporate and filter to obtain the composite flame retardant. The dosage ratio of trimethylolpropane triacrylate, Intermediate 5, triphenylphosphine, p-hydroxyanisole, acetone and commercially available silane-modified sepiolite is 0.22 mol: 0.1 mol: 0.1 g: 0.1 g: 1200 mL: 50 g; Example
[0013] The composite flame retardant is prepared by the following steps: A1: Add pentaerythritol and phosphorus oxychloride into a container, stir and mix them. React for 10 h under the conditions of a stirring rate of 300 rpm and 150 °C. Add deionized water, cool and filter by suction to obtain Intermediate 1. The dosage ratio of phosphorus oxychloride, pentaerythritol and deionized water is 0.1 mol: 0.12 mol: 100 mL; A2: Add Intermediate 1, mercaptosuccinic acid and p-toluenesulfonic acid into a container, stir and mix them. React for 16 h under the conditions of a stirring rate of 200 rpm and 80 °C. Distill under reduced pressure, then add ethyl acetate, wash three times with saturated sodium bicarbonate solution and saturated brine solution, dry in vacuum at 60 °C for 12 h, filter and rotate evaporate to obtain Intermediate 2. The dosage ratio of Intermediate 1, mercaptosuccinic acid, ethyl acetate and p-toluenesulfonic acid is 0.2 mol: 0.1 mol: 60 mL: 0.05 g; A3: Add cyanuric chloride and acetone into a container, stir and mix them. Slowly dropwise add diallylamine. React for 3 h under the conditions of a stirring rate of 150 rpm and 5 - 10 °C. Filter, wash three times with acetone, dry in vacuum at 60 °C for 8 h to obtain Intermediate 3. The dosage ratio of cyanuric chloride, diallylamine and acetone is 0.1 mol: 0.1 mol: 300 mL; A4: Add sodium sulfide nonahydrate into deionized water, stir and slowly add hydrochloric acid solution, then add Intermediate 3. React for 2 h under the conditions of a stirring rate of 300 rpm and 0 °C. Wash three times with acetone, add water for chromatography until the effluent is neutral to obtain Intermediate 4. The molar concentration of the hydrochloric acid solution is 2 mol / L. The dosage ratio of sodium sulfide nonahydrate, deionized water, Intermediate 3 and hydrochloric acid solution is 120 g: 150 mL: 50 g: 200 mL; A5: Add intermediate 2, methanol, and deionized water into a container, stir and heat up to 70 °C, add azobisisobutyronitrile and stir to mix, then dropwise add intermediate 4, react for 6 h under the conditions of a stirring rate of 300 rpm and 70 °C, cool and filter, wash three times with methanol, and dry in vacuum at 65 °C for 24 h to obtain intermediate 5. The dosage ratio of intermediate 2, intermediate 4, methanol, azobisisobutyronitrile, and deionized water is 0.22 mol: 0.1 mol: 200 mL: 0.4 g: 100 mL; A6: Add trimethylolpropane triacrylate and triphenylphosphine into a container, stir to mix, then add p - methoxyphenol and intermediate 5, react for 6 h under the conditions of a stirring rate of 300 rpm, room temperature, and ultraviolet lamp irradiation, then add acetone and commercially available silane - modified sepiolite, stir to mix, ultrasonically disperse for 60 min, then mix at a stirring rate of 300 rpm and 60 °C for 1 h, rotary evaporate and filter to obtain a composite flame retardant. The dosage ratio of trimethylolpropane triacrylate, intermediate 5, triphenylphosphine, p - methoxyphenol, acetone, and commercially available silane - modified sepiolite is 0.22 mol: 0.1 mol: 0.1 g: 0.1 g: 200 mL: 50 g; Example
[0014] A photocurable flame - retardant coating comprises the following raw materials in parts by weight: 50 parts of commercially available 4680 acrylate resin, 10 parts of the composite flame retardant of Example 1, 5 parts of commercially available 1,6 - hexanediol diacrylate diluent, 1 part of commercially available THIX - 286 defoamer, and 1 part of commercially available 1173 photoinitiator; The said photocurable flame - retardant coating is prepared by the following steps: Add acrylate resin, composite flame retardant, commercially available 1,6 - hexanediol diacrylate diluent, and commercially available THIX - 286 defoamer into a stirring container, stir at a stirring rate of 1000 rpm and room temperature for 20 min, then add commercially available 1173 photoinitiator and stir to mix to obtain a photocurable flame - retardant coating; Example
[0015] A photocurable flame - retardant coating comprises the following raw materials in parts by weight: 50 parts of commercially available 4680 acrylate resin, 10 parts of the composite flame retardant of Example 2, 10 parts of commercially available 1,6 - hexanediol diacrylate diluent, 3 parts of commercially available THIX - 286 defoamer, and 3 parts of commercially available 1173 photoinitiator; The said photocurable flame - retardant coating is prepared by the following steps: Add acrylate resin, composite flame retardant, commercially available 1,6 - hexanediol diacrylate diluent, and commercially available THIX - 286 defoamer into a stirring container, stir at a stirring rate of 1000 rpm and room temperature for 20 min, then add commercially available 1173 photoinitiator and stir to mix to obtain a photocurable flame - retardant coating; Example
[0016] A photocurable flame retardant coating comprises raw materials in the following parts by weight: 60 parts of commercially available 4680 acrylate resin, 15 parts of the composite flame retardant in Example 3, 10 parts of commercially available dipropylene glycol diacrylate diluent, 3 parts of commercially available THIX-286 defoamer, and 3 parts of commercially available 1173 photoinitiator; The photocurable flame retardant coating is prepared by the following steps: adding the acrylate resin, the composite flame retardant, the commercially available dipropylene glycol diacrylate diluent, and the commercially available THIX-286 defoamer into a stirring container, stirring for 30 min at a stirring rate of 800 rpm and at room temperature, and then adding the commercially available 1173 photoinitiator and stirring and mixing to obtain a photocurable flame retardant coating; Comparative Example 1 In Comparative Example 1, the composite flame retardant in Example 6 was replaced with a mixture of commercially available silane-modified sepiolite and FR-MPP flame retardant, where the mass ratio of the commercially available silane-modified sepiolite to the FR-MPP flame retardant was 1 g:3 g, and the other steps were exactly the same as those in Example 6 to obtain a photocurable flame retardant coating; Comparative Example 2 In Comparative Example 2, the composite flame retardant in Example 6 was replaced with a mixture of commercially available silane-modified sepiolite and NLD flame retardant, where the mass ratio of the commercially available silane-modified sepiolite to the NLD flame retardant was 1 g:3 g, and the other steps were exactly the same as those in Example 6 to obtain a photocurable flame retardant coating; Take the photocurable flame retardant coatings prepared in Example 4, Example 5, Example 6, Comparative Example 1, and Comparative Example 2, and uniformly coat the photocurable flame retardant coatings on the surface of polished Chinese fir by a spin coater, with the size of 100×10×4 mm 3 , irradiate and cure the coated wood specimens at a position 15 cm away from the UV curing machine lamp tube, and record the surface drying time. Take another batch of photocurable flame retardant coatings prepared in Example 4, Example 5, Example 6, Comparative Example 1, and Comparative Example 2, and uniformly coat the photocurable flame retardant coatings on the surface of polished Chinese fir by a spin coater, with the size of 100×10×4 mm 3 , irradiate and cure the coated wood specimens at a position 15 cm away from the UV curing machine lamp tube for 90 s to obtain specimens, conduct a limiting oxygen index test using an HC-2 type oxygen index meter, conduct a vertical burning test with reference to ASTM D3801 standard, measure the film hardness using the pencil hardness method with reference to GB / T 9754-2007, and measure the film adhesion using the cross-cut method with reference to ISO 2409-2007. The specific test results are as follows in the table:
[0017] As can be seen from the test results shown in the table, by comparing Example 4, Example 5, Example 6 with Comparative Example 1 and Comparative Example 2, it can be found that under the same conditions, the surface drying times of Example 4, Example 5 and Example 6 are significantly better than those of Comparative Example 1 and Comparative Example 2, indicating that the addition of the composite flame retardant can improve the curing time of the coating. At the same time, under the same curing time, the flame retardant properties and mechanical properties of Example 6 are significantly better than those of Comparative Example 1 and Comparative Example 2, indicating that the addition of the composite flame retardant can effectively improve the flame retardant properties of the coating and reduce the decrease in mechanical properties caused by the addition of the flame retardant.
[0018] The above content is only an example and illustration of the concept of the present invention. Those skilled in the art of the present technology can make various modifications or supplements to the specific embodiments described or use similar methods to replace them. As long as they do not deviate from the concept of the invention or exceed the scope defined by this claim book, they should fall within the protection scope of the present invention.
Claims
1. A light-curing flame-retardant coating, characterized in that: The method comprises the following raw materials in parts by weight: 50-60 parts of acrylic resin, 10-15 parts of composite flame retardant, 5-10 parts of diluent, 1-3 parts of defoaming agent and 1-3 parts of photoinitiator; The photocurable flame retardant coating is prepared by the following steps: adding acrylate resin, composite flame retardant, diluent and defoamer into a stirring container, stirring for 20-30 minutes at a stirring rate of 800-1000rpm and room temperature, and then adding photoinitiator and stirring to obtain a photocurable flame retardant coating.
2. The light-curing flame-retardant coating according to claim 1, characterized in that: The composite flame retardant is prepared by the following steps: A1: Add pentaerythritol and phosphorus oxychloride into a container, stir and mix, react for 10-12 hours at a stirring rate of 200-300 rpm and 140-150° C., add deionized water, cool and filter, and obtain intermediate 1; A2: Add intermediate 1, mercaptosuccinic acid and p-toluenesulfonic acid into a container, stir and mix, react at a stirring rate of 100-200 rpm and 80° C. for 12-16 h, distill under reduced pressure, add ethyl acetate, wash three times with saturated sodium bicarbonate solution and saturated saline solution, dry under vacuum at 60° C. for 12 h, filter and rotary evaporate to obtain intermediate 2; A3: Add cyanuric chloride and acetone into a container, stir to mix, slowly add diallylamine dropwise, react for 3 h at a stirring rate of 100-150 rpm and 5-10°C, filter, wash three times with acetone, and vacuum dry at 60°C for 6-8 h to obtain intermediate 3; A4: Sodium sulfide nonahydrate was added to deionized water, stirred and hydrochloric acid solution was slowly added, and then intermediate 3 was added, and the reaction was carried out at a stirring rate of 200-300 rpm and 0-10°C for 2-4 hours, washed with acetone three times, and chromatographed with water until the effluent was neutral to obtain intermediate 4; A5: Add intermediate 2, methanol and deionized water into a container, stir and heat to 70°C, add azobisisobutyronitrile and stir to mix, then dropwise add intermediate 4, react at a stirring rate of 200-300 rpm and 70°C for 4-6 hours, cool and filter, wash three times with methanol, and vacuum dry at 65°C for 24 hours to obtain intermediate 5; A6: Add trimethylolpropane triacrylate and triphenylphosphine into a container, stir and mix, then add p-hydroxyanisole and intermediate 5, react for 4-6 hours at a stirring rate of 200-300 rpm, room temperature and ultraviolet light irradiation, then add acetone and organic sepiolite, stir and mix, ultrasonically disperse for 50-60 minutes, then mix for 1 hour at a stirring rate of 150-300 rpm and 50-60°C, and filter by rotary evaporation to obtain a composite flame retardant.
3. A light-curing flame-retardant coating according to claim 2, characterized in that: In step A1: the ratio of phosphorus oxychloride, pentaerythritol and deionized water is 0.1 mol: 0.1-0.12 mol: 50-100 mL; In step A2: the ratio of intermediate 1, mercaptosuccinic acid, ethyl acetate and p-toluenesulfonic acid is 0.2 mol: 0.1 mol: 40-60 mL: 0.05 g; In step A3: the ratio of cyanuric chloride, diallylamine and acetone is 0.1 mol: 0.1 mol: 200-300 mL; In step A4: the molar concentration of the hydrochloric acid solution is 2 mol / L, and the amount ratio of sodium sulfide nonahydrate, deionized water, intermediate 3 and hydrochloric acid solution is 120 g: 100-150 mL: 50 g: 150-200 mL; In step A5: the ratio of intermediate 2, intermediate 4, methanol, azobisisobutyronitrile and deionized water is 0.2-0.22 mol: 0.1 mol: 100-200 mL: 0.2-0.4 g: 100 mL; In step A6: the usage ratio of trimethylolpropane triacrylate, intermediate 5, triphenylphosphine, p-hydroxyanisole, acetone and organic sepiolite is 0.2-0.22 mol: 0.1 mol: 0.1 g: 0.1 g: 150-200 mL: 50 g.
4. The light-curing flame-retardant coating according to claim 2, characterized in that: The organic sepiolite is silane-modified sepiolite.
5. The light-curing flame-retardant coating according to claim 1, characterized in that: The diluent is one or more of 1,6-hexanediol diacrylate and propylene glycol diacrylate.
6. The light-curing flame-retardant coating according to claim 1, characterized in that: The defoamer is a polyether defoamer.
7. The light-curing flame-retardant coating according to claim 1, characterized in that: The photoinitiator type is a cleavage type photoinitiator.
8. The method for preparing a light-curable flame-retardant coating according to claim 1, characterized in that: The method comprises the following steps: adding acrylate resin, composite flame retardant, diluent and defoamer into a stirring container, stirring for 20-30 minutes at a stirring rate of 800-1000 rpm and room temperature, and then adding photoinitiator and stirring to obtain a light-cured flame retardant coating.