An oil-based environment-friendly high-molecular flame-retardant coating and a preparation method thereof

Abstract

The present application relates to the technical field of fire-retardant coating, and particularly relates to an oil-based environment-friendly high-molecular fire-retardant coating and a preparation method thereof, which comprises the following components by weight: base resin 15-18 parts by weight, silane-modified composite fire retardant 30-35 parts by weight, pigment and filler 6-7 parts by weight, environment-friendly auxiliary agent 1.5-1.8 parts by weight, and environment-friendly mixed solvent 38.2-47.5 parts by weight. The present application uses modified saturated polyester resin and elastomer resin as the base by compounding, which significantly improves the compatibility of the resin and each component, enhances the film-forming property, adhesion and weather resistance of the coating, delays the aging of the base material, and is suitable for long-term outdoor and complex environment use.

Description

Technical Field

[0001] This invention relates to the field of flame retardant coatings technology, specifically to an oil-based environmentally friendly polymer flame retardant coating and its preparation method. Background Technology

[0002] Flame-retardant coatings are key protective materials for industrial and civil buildings, steel structures, ships, ancient buildings, and cables. Oil-based flame-retardant coatings are widely used in outdoor and special applications due to their excellent film-forming properties, strong adhesion, and stable weather resistance. However, many oil-based flame-retardant coatings currently on the market have several technical shortcomings, making it difficult to meet the dual demands of modern industry for high-performance and environmentally friendly materials.

[0003] The resins used in existing coatings are mostly unmodified conventional varieties, which have insufficient compatibility with flame retardant components, easily leading to problems such as component separation and uneven film formation, and are prone to aging and failure with long-term use. Flame retardants are mostly used in single or simple compound forms without surface modification treatment, which makes them prone to agglomeration and sedimentation in the system, making it difficult to fully exert the synergistic effect of flame retardancy, limiting the flame retardant and smoke suppression effects, and easily releasing harmful substances during combustion.

[0004] The solvent system mostly uses traditional aromatic hydrocarbon components, with a high content of volatile organic compounds, making it difficult to meet environmental protection standards and failing to meet the requirements for indoor and green building materials use. The preparation process mostly adopts one-time mixing and feeding, resulting in insufficient dispersion of each component, poor physicochemical stability, easy stratification and clumping during storage, limited construction adaptability, and inability to meet the needs of different scenarios. Most products cannot simultaneously achieve excellent flame retardant performance, environmental indicators and physicochemical stability, limiting their adaptability to various scenarios and exhibiting significant defects in overall performance. Summary of the Invention

[0005] The primary objective of this invention is to provide an oil-based, environmentally friendly, polymeric flame-retardant coating and its preparation method.

[0006] A further objective of this invention is to provide an oil-based environmentally friendly polymer flame-retardant coating, comprising the following components by weight: 15-18 parts by weight of a base resin, 30-35 parts by weight of a silane-modified composite flame retardant, 6-7 parts by weight of pigments and fillers, 1.5-1.8 parts by weight of environmentally friendly additives, and 38.2-47.5 parts by weight of an environmentally friendly mixed solvent.

[0007] Preferably, the matrix resin is composed of acrylic acid graft-modified saturated polyester resin and styrene-butadiene-styrene block copolymer, wherein the acrylic acid graft-modified saturated polyester resin is 10-14 parts by weight and the styrene-butadiene-styrene block copolymer is 4-5 parts by weight; the grafting rate of the acrylic acid graft-modified saturated polyester resin is 15%-20%, and the styrene-butadiene-styrene block copolymer has a linear structure and a molecular weight of 30000 g / mol.

[0008] Preferably, the silane-modified composite flame retardant is composed of Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, diethyl ethyl phosphonate, and antimony trioxide, wherein Exolit™ AP418 ammonium polyphosphate is 12-15 parts by weight, silane-modified zinc borate is 8-10 parts by weight, diethyl ethyl phosphonate is 7-8 parts by weight, and antimony trioxide is 2-3 parts by weight.

[0009] Preferably, the pigment and filler are composed of titanium dioxide and mica iron oxide ash, with titanium dioxide accounting for 4-5 parts by weight and mica iron oxide ash accounting for 2 parts by weight.

[0010] Preferably, the environmentally friendly additive is composed of an organosilicon defoamer, a 2,6-di-tert-butyl-p-cresol antioxidant, and a fumed silica anti-settling agent, wherein the organosilicon defoamer is 0.5-0.6 parts by weight, the 2,6-di-tert-butyl-p-cresol antioxidant is 0.6-0.7 parts by weight, and the fumed silica anti-settling agent is 0.4-0.5 parts by weight.

[0011] Preferably, the environmentally friendly mixed solvent is composed of n-butyl acetate, propylene glycol methyl ether acetate and tributyl citrate, wherein n-butyl acetate is 22-28 parts by weight, propylene glycol methyl ether acetate is 14-17 parts by weight and tributyl citrate is 2.2-3.5 parts by weight.

[0012] A method for preparing the oil-based environmentally friendly polymer flame-retardant coating includes the following steps: Flame retardant silane modification: Zinc borate was dried, cooled, and then mixed with silane coupling agent KH560 and an environmentally friendly mixed solvent. After stirring and modification, the mixture was cooled and ground to obtain silane-modified zinc borate. Resin premixing involves adding acrylic graft-modified saturated polyester resin and styrene-butadiene-styrene block copolymer to a reactor, adding an environmentally friendly mixed solvent, and stirring to premix to obtain a premixed resin system. Flame retardant system compounding, using Exolit TM AP418 ammonium polyphosphate, silane-modified zinc borate, diethyl ethyl phosphonate and antimony trioxide are added to the premixed resin system, heated and stirred to compound, and antisettling agent is added in batches. For pigment and filler dispersion, titanium dioxide and mica iron oxide ash are added to the above system, stirred and dispersed, then defoamer and antioxidant are added, and stirring is continued; Grinding and refining: The mixed system is ground, and environmentally friendly mixed solvents are added to adjust the viscosity of the system; Maturation of the finished product: The ground system is matured, cooled and filtered to obtain an oil-based environmentally friendly polymer flame-retardant coating.

[0013] Preferably, in the flame retardant silane modification step, the drying temperature is 110-115℃, the drying time is 12-15min, the modification temperature is 75-85℃, the stirring speed is 400-500r / min, the modification time is 60-90min, and the grinding particle size is 20-30μm; the amount of silane coupling agent KH560 is 1%-3% of the weight of zinc borate.

[0014] Preferably, the resin premixing temperature is 85-90℃, the stirring speed is 500-550r / min, and the premixing time is 60-70min; the flame retardant system compounding stirring speed is 700-750r / min, the compounding temperature is 95-100℃, and the compounding time is 90-100min; the pigment and filler dispersion stirring speed is 900-950r / min, and the dispersion time is 45-50min.

[0015] Preferably, the particle size after grinding is 15-20 μm, the system viscosity is adjusted to 180-200 mPa·s, the aging temperature is 55-65℃, the stirring speed is 250-280 r / min, the aging time is 45-50 min, and nitrogen gas is introduced for protection during the aging process.

[0016] Compared with the prior art, the beneficial effects of the present invention are: 1. This invention uses a modified saturated polyester resin and an elastomer resin as a matrix, which significantly improves the compatibility of the resin with each component, enhances the film-forming properties, adhesion and weather resistance of the coating, delays the aging of the substrate, and is suitable for long-term outdoor and complex environment use.

[0017] 2. This invention modifies the flame retardant with silane, which effectively improves the dispersibility of the flame retardant components, avoids agglomeration and sedimentation, and, combined with a multi-component composite flame retardant system, forms a highly efficient flame retardant synergistic effect, improves the flame retardant and smoke suppression performance of the coating, and results in a lower release of harmful substances during combustion.

[0018] 3. This invention uses an environmentally friendly mixed solvent to replace traditional harmful solvents, significantly reducing the emission of volatile organic compounds, with no harmful heavy metals detected, meeting indoor and outdoor environmental protection standards, and adapting to the application requirements of green building materials.

[0019] 4. The present invention adopts a step-by-step orderly preparation process, which enables the components to be fully dispersed and integrated, improves the stability of the coating system, prevents stratification and sedimentation during storage, has good leveling properties during construction, and can be adapted to various construction methods.

[0020] 5. This invention achieves synergistic optimization of flame retardant performance, environmental performance, and physical and chemical properties. The product is suitable for a wide range of scenarios and can meet the protection needs of various fields such as conventional steel structures, outdoor facilities, indoor buildings, and special equipment. It is both practical and environmentally friendly, and has outstanding application value. Detailed Implementation

[0021] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] Example 1:

[0023] Raw material composition: The matrix resin comprises 15 parts by weight, including 10 parts by weight of acrylic graft-modified saturated polyester resin and 5 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 15%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including Exolit... TM The mixture contains 12 parts by weight of AP418 ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethylphosphonate, and 3 parts by weight of antimony trioxide; 6 parts by weight of pigments and fillers, including 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.5 parts by weight of environmentally friendly additives, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of antisettling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the antisettling agent is fumed silica; and 47.5 parts by weight of environmentally friendly mixed solvents, including 28 parts by weight of n-butyl acetate, 17 parts by weight of propylene glycol methyl ether acetate, and 2.5 parts by weight of tributyl citrate.

[0024] Preparation method: The first step involves silane modification of the flame retardant. Zinc borate is dried at 110°C for 12 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 5 parts by weight of environmentally friendly mixed solvent are added. The mixture is stirred at 75°C and 400 r / min for 60 minutes. After cooling, it is ground to a particle size of 30 μm to obtain silane-modified zinc borate. Silane coupling agent KH560 can effectively improve the compatibility of zinc borate with oily resin systems and prevent the flame retardant from agglomerating and settling. Controlling the particle size to 30 μm ensures uniform dispersion of the flame retardant and guarantees a synergistic flame retardant effect.

[0025] The second step is resin premixing. Acrylic graft-modified saturated polyester resin and SBS are added to the reactor, along with 15 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain a premixed resin system. The premixing step ensures that the resin system is uniform and free of particles, laying the foundation for the subsequent dispersion of flame retardants, pigments and fillers, and adapting to the dissolution and dispersion requirements of SBS with different molecular weights.

[0026] The third step is to compound the flame retardant system, adding Exolit. TMAP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate, and antimony trioxide were added to the premixed resin system. The rotation speed was adjusted to 700 r / min, the temperature was raised to 95℃, and the mixture was stirred for 90 min. During this period, an anti-settling agent was added every 20 min, in three separate additions. Gradual heating and intermittent addition can prevent local agglomeration of the flame retardant and ensure that the four components work synergistically. Exolit TM AP418 ammonium polyphosphate can initiate the expansion reaction early to form a dense carbon layer, DEEP diethyl phosphonate can interrupt the combustion chain, antimony trioxide catalyzes carbonization, and silane-modified zinc borate enhances the stability of the carbon layer.

[0027] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min. Titanium dioxide can improve the hiding power and decorative properties of the coating, mica iron oxide ash can enhance the rust prevention performance of the coating, high-speed stirring can ensure uniform dispersion of pigments and fillers and avoid clumping that affects the film formation effect, defoamer can eliminate air bubbles in the system, and antioxidant can improve the long-term stability of the coating.

[0028] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 22.5 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s. Controlling the particle size to 20μm can improve the fineness of the coating, and adjusting the viscosity to 200mPa·s can be used for both brushing and spraying.

[0029] The sixth step is to mature the finished product. The ground system is transferred to a maturation kettle and matured at 60°C and 250 r / min for 45 minutes. After cooling to room temperature, it is filtered to obtain an oil-based environmentally friendly polymer flame-retardant coating, which is suitable for the basic fire protection requirements of conventional steel structure substrates. The maturation step can improve the stability of the coating system and ensure that the components are fully integrated. Filtration can remove impurities and ensure the uniformity of the coating's appearance and performance.

[0030] Example 2:

[0031] Raw material composition: The matrix resin comprises 15 parts by weight, including 10 parts by weight of acrylic graft-modified saturated polyester resin and 5 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 15%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including 12 parts by weight of Exolit™ AP418 ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethyl phosphonate, and 3 parts by weight of antimony trioxide. Pigments and fillers comprise 6 parts by weight. The composition includes: 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.5 parts by weight of environmentally friendly additives, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of anti-settling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the anti-settling agent is fumed silica; and 47.5 parts by weight of environmentally friendly mixed solvents, including 28 parts by weight of n-butyl acetate, 17 parts by weight of propylene glycol methyl ether acetate, and 2.5 parts by weight of tributyl citrate.

[0032] Preparation method: The first step involves silane modification of the flame retardant. Zinc borate is dried at 115°C for 15 minutes and then cooled to room temperature. Silane coupling agent KH560 and 6 parts by weight of environmentally friendly mixed solvent are added, and the mixture is stirred at 85°C and 500 r / min for 90 minutes. After cooling, it is ground to a particle size of 20 μm to obtain silane-modified zinc borate. For outdoor steel structure scenarios with high humidity, extending the drying time can improve the dryness of zinc borate and prevent flame retardant agglomeration in high humidity environments. Increasing the solvent dosage can improve the uniformity of modification, extending the modification time can ensure sufficient modification, and reducing the grinding particle size can further improve the dispersibility and compatibility of the flame retardant, fundamentally solving the problem of flame retardant sedimentation in high humidity environments.

[0033] The second step is resin premixing. Acrylic graft modified saturated polyester resin and SBS are added to the reactor, along with 15 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain the premixed resin system.

[0034] The third step is to compound the flame retardant system. Add Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate and antimony trioxide to the premixed resin system, adjust the speed to 700 r / min, raise the temperature to 95℃, and stir for 90 min. During this period, add the anti-settling agent every 20 min, and add it in 3 batches.

[0035] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0036] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 22.5 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s.

[0037] The sixth step is to mature the finished product. The ground system is transferred to a maturation kettle and matured at 60°C and 250 r / min for 45 minutes. After cooling to room temperature, it is filtered to obtain an oil-based environmentally friendly polymer flame-retardant coating, which is suitable for outdoor steel structure scenarios with high humidity.

[0038] Example 3:

[0039] Raw material composition: The matrix resin comprises 18 parts by weight, including 14 parts by weight of acrylic graft-modified saturated polyester resin and 4 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 20%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including 12 parts by weight of Exolit™ AP418 ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethyl phosphonate, and 3 parts by weight of antimony trioxide. Pigments and fillers comprise 6 parts by weight. The composition includes: 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.5 parts by weight of environmentally friendly additives, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of anti-settling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the anti-settling agent is fumed silica; and 44.5 parts by weight of environmentally friendly mixed solvents, including 26 parts by weight of n-butyl acetate, 16 parts by weight of propylene glycol methyl ether acetate, and 2.5 parts by weight of tributyl citrate.

[0040] Preparation method: The first step is to modify the flame retardant with silane. Zinc borate is dried at 115°C for 15 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 6 parts by weight of environmentally friendly mixed solvent are added. The mixture is stirred at 85°C and 500 r / min for 90 minutes. After cooling, it is ground to a particle size of 20 μm to obtain silane-modified zinc borate.

[0041] The second step is resin premixing. Acrylic graft-modified saturated polyester resin and SBS are added to a reactor, along with 14 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 rpm to obtain a premixed resin system. For steel structures exposed to the elements for extended periods, increasing the proportion of acrylic graft-modified saturated polyester resin, decreasing the proportion of SBS, and increasing the grafting rate to 20% can significantly enhance the coating's weather resistance and slow down outdoor aging. Fine-tuning the solvent ratio can ensure the compatibility of the resin system and adapt to changes in the resin ratio.

[0042] The third step is to compound the flame retardant system, adding Exolit. TMAP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate and antimony trioxide were added to the premixed resin system. The rotation speed was adjusted to 700 r / min, the temperature was raised to 95℃, and the mixture was stirred for 90 min. During this period, an anti-settling agent was added every 20 min, and the mixture was added in 3 batches.

[0043] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0044] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 30.5 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s.

[0045] The sixth step is to mature the finished product. The ground system is transferred to a maturation kettle and matured at 60°C and 250 r / min for 45 minutes. After cooling to room temperature, it is filtered to obtain an oil-based environmentally friendly polymer flame-retardant coating, which is suitable for steel structure scenarios that are exposed to the outdoors for a long time.

[0046] Example 4:

[0047] Raw material composition: The matrix resin comprises 18 parts by weight, including 14 parts by weight of acrylic graft-modified saturated polyester resin and 4 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 20%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including 12 parts by weight of Exolit™ AP418 ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethyl phosphonate, and 3 parts by weight of antimony trioxide. Pigments and fillers comprise 6 parts by weight. The composition includes, by weight, 4 parts titanium dioxide and 2 parts mica iron oxide ash; 1.5 parts environmentally friendly additives, including 0.5 parts defoamer, 0.6 parts antioxidant, and 0.4 parts anti-settling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the anti-settling agent is fumed silica; and 44.5 parts environmentally friendly mixed solvents, including 24 parts n-butyl acetate, 17 parts propylene glycol methyl ether acetate, and 3.5 parts tributyl citrate.

[0048] Preparation method: The first step is to modify the flame retardant with silane. Zinc borate is dried at 115°C for 15 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 6 parts by weight of environmentally friendly mixed solvent are added. The mixture is stirred at 85°C and 500 r / min for 90 minutes. After cooling, it is ground to a particle size of 20 μm to obtain silane-modified zinc borate.

[0049] The second step is resin premixing. Acrylic graft-modified saturated polyester resin and SBS are added to the reactor, along with 14 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain the premixed resin system.

[0050] The third step is to compound the flame retardant system. Add Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate and antimony trioxide to the premixed resin system, adjust the speed to 700 r / min, raise the temperature to 95℃, and stir for 90 min. During this period, add the anti-settling agent every 20 min, and add it in 3 batches.

[0051] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0052] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 30.5 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s.

[0053] Step 6: Curing the finished product. The ground system is transferred to a curing kettle and cured at 55℃ and 250r / min for 45 minutes. After cooling to room temperature, it is filtered to obtain an oil-based environmentally friendly polymer flame-retardant coating, suitable for indoor furniture and ancient building protection scenarios. To meet the environmental protection requirements of indoor scenarios, increasing the proportion of tributyl citrate can further reduce the VOC content and improve the environmental performance. Lowering the curing temperature can avoid the solvent from evaporating too quickly due to high temperature, reduce the odor of the coating, and meet the odor requirements for indoor use.

[0054] Example 5:

[0055] Raw material composition: The matrix resin comprises 18 parts by weight, including 14 parts by weight of acrylic graft-modified saturated polyester resin and 4 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 20%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 35 parts by weight, including Exolit... TMThe mixture contains 15 parts by weight of AP418 ammonium polyphosphate, 10 parts by weight of silane-modified zinc borate, 8 parts by weight of DEEP diethylphosphonate, and 2 parts by weight of antimony trioxide; 7 parts by weight of pigments and fillers, including 5 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.8 parts by weight of environmentally friendly additives, including 0.6 parts by weight of defoamer, 0.7 parts by weight of antioxidant, and 0.5 parts by weight of antisettling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the antisettling agent is fumed silica; and 38.2 parts by weight of environmentally friendly mixed solvents, including 22 parts by weight of n-butyl acetate, 14 parts by weight of propylene glycol methyl ether acetate, and 2.2 parts by weight of tributyl citrate.

[0056] Preparation method: The first step is to modify the flame retardant with silane. Zinc borate is dried at 115°C for 15 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 6 parts by weight of environmentally friendly mixed solvent are added. The mixture is stirred at 85°C and 500 r / min for 90 minutes. After cooling, it is ground to a particle size of 20 μm to obtain silane-modified zinc borate. This ensures the dispersibility of the flame retardant to meet the increased demand for flame retardant.

[0057] The second step is resin premixing. Acrylic graft-modified saturated polyester resin and SBS are added to the reactor, along with 14 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 70 minutes at 90°C and 550 r / min. The temperature, speed and time are increased to ensure the uniformity of the resin system and to meet the increased demand for flame retardant.

[0058] The third step involves compounding the flame retardant system. Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate, and antimony trioxide are added to the premixed resin system. The rotation speed is adjusted to 750 r / min, the temperature is raised to 100℃, and the mixture is stirred for 100 min. Increasing the rotation speed, temperature, and time ensures that the flame retardants are fully dispersed and have a synergistic effect. During this process, an anti-settling agent is added every 20 min. Increasing the total amount of flame retardant and adjusting the proportions of each component can enhance the synergistic flame retardant effect and meet the high flame retardant requirements of high-end special scenarios such as cables and ships.

[0059] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 950 r / min, and stir for 50 min. Increase the speed and time to ensure that the pigments and fillers are evenly dispersed. Then add defoamer and antioxidant, and continue stirring for 35 min. Increasing the amount of titanium dioxide can improve the decorative properties and hiding power of the coating, which can meet the appearance requirements of marine and other scenarios. Increasing the amount of additives can improve the stability of the coating.

[0060] The fifth step is grinding and refining. The above-mentioned mixture is transferred to a grinding equipment and a two-stage grinding process is adopted. The first stage grinds to a particle size of 60μm, and the second stage grinds to a particle size of 15μm. During the process, 20.2 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 180mPa·s. The two-stage grinding can improve the fineness of the coating and adapt to the needs of cable bending and ship spraying. Adjusting the viscosity to 180mPa·s can optimize the spraying construction effect.

[0061] The sixth step is to cure the finished product. The ground system is transferred to a curing kettle, and nitrogen is introduced as an inert gas to prevent oxidation. The system is cured at 65°C and 280 r / min for 50 minutes. After cooling to room temperature, it is filtered to obtain an oil-based environmentally friendly polymer flame-retardant coating, which is suitable for high-end special applications such as cables and ships. Inert gas protection can improve the storage stability of the coating, and extending the curing time can further optimize the overall performance of the coating to meet the stringent requirements of high-end special applications.

[0062] Comparative Example 1: Raw material composition: The matrix resin comprises 15 parts by weight, including 10 parts by weight of ordinary saturated polyester resin and 5 parts by weight of SBS. The ordinary saturated polyester resin is unmodified, and the SBS has a linear structure with a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including 12 parts by weight of Exolit™ AP418 ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethyl phosphonate, and 3 parts by weight of antimony trioxide. Pigments and fillers comprise 6 parts by weight. The mixture contains 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.5 parts by weight of environmentally friendly additives, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of anti-settling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the anti-settling agent is fumed silica; and 47.5 parts by weight of environmentally friendly mixed solvents, including 28 parts by weight of n-butyl acetate, 17 parts by weight of propylene glycol methyl ether acetate, and 2.5 parts by weight of tributyl citrate.

[0063] Preparation method: The first step is to modify the flame retardant with silane. Zinc borate is dried at 110°C for 12 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 5 parts by weight of environmentally friendly mixed solvent are added. The mixture is stirred at 75°C and 400 r / min for 60 minutes. After cooling, it is ground to a particle size of 30 μm to obtain silane-modified zinc borate.

[0064] The second step is resin premixing. Ordinary saturated polyester resin and SBS are added to the reactor, along with 15 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain the premixed resin system.

[0065] The third step is to compound the flame retardant system. Add Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate and antimony trioxide to the premixed resin system, adjust the speed to 700 r / min, raise the temperature to 95℃, and stir for 90 min. During this period, add the anti-settling agent every 20 min, and add it in 3 batches.

[0066] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0067] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 22.5 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s.

[0068] Step 6: Curing the finished product. The ground system is transferred to a curing kettle and cured at 60°C and 250 r / min for 45 min. After cooling to room temperature, it is filtered to obtain an oil-based flame-retardant coating.

[0069] Comparative Example 2: Raw material composition: The matrix resin comprises 15 parts by weight, including 10 parts by weight of acrylic graft-modified saturated polyester resin and 5 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 15%. The SBS has a linear structure and a molecular weight of 30,000. The flame retardant comprises 30 parts by weight, including 12 parts by weight of Exolit™ AP418 ammonium polyphosphate, 8 parts by weight of unmodified zinc borate, 7 parts by weight of DEEP diethyl ethyl phosphonate, and 3 parts by weight of antimony trioxide. Pigments and fillers comprise 6 parts by weight. The mixture contains 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.5 parts by weight of environmentally friendly additives, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of anti-settling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the anti-settling agent is fumed silica; and 47.5 parts by weight of environmentally friendly mixed solvents, including 28 parts by weight of n-butyl acetate, 17 parts by weight of propylene glycol methyl ether acetate, and 2.5 parts by weight of tributyl citrate.

[0070] Preparation method: First, take the unmodified zinc borate for later use, and skip the silane modification step.

[0071] The second step is resin premixing. Acrylic graft modified saturated polyester resin and SBS are added to the reactor, along with 15 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain the premixed resin system.

[0072] The third step is to compound the flame retardant system. Add Exolit™ AP418 ammonium polyphosphate, unmodified zinc borate, DEEP diethyl ethyl phosphonate and antimony trioxide to the premixed resin system, adjust the speed to 700 r / min, raise the temperature to 95℃, and stir for 90 min. During this period, add the anti-settling agent every 20 min, and add it in 3 batches.

[0073] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0074] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 22.5 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s.

[0075] Step 6: Curing the finished product. The ground system is transferred to a curing kettle and cured at 60°C and 250 r / min for 45 min. After cooling to room temperature, it is filtered to obtain an oil-based flame-retardant coating.

[0076] Comparative Example 3: Raw material composition: The matrix resin comprises 15 parts by weight, including 10 parts by weight of acrylic graft-modified saturated polyester resin and 5 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 15%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including 12 parts by weight of ordinary ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethyl phosphonate, and 3 parts by weight of antimony trioxide. Pigments and fillers comprise 6 parts by weight. The mixture contains 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.5 parts by weight of environmentally friendly additives, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of anti-settling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the anti-settling agent is fumed silica; and 47.5 parts by weight of environmentally friendly mixed solvents, including 28 parts by weight of n-butyl acetate, 17 parts by weight of propylene glycol methyl ether acetate, and 2.5 parts by weight of tributyl citrate.

[0077] Preparation method: The first step is to modify the flame retardant with silane. Zinc borate is dried at 110°C for 12 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 5 parts by weight of environmentally friendly mixed solvent are added. The mixture is stirred at 75°C and 400 r / min for 60 minutes. After cooling, it is ground to a particle size of 30 μm to obtain silane-modified zinc borate.

[0078] The second step is resin premixing. Acrylic graft modified saturated polyester resin and SBS are added to the reactor, along with 15 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain the premixed resin system.

[0079] The third step is to compound the flame retardant system. Ordinary ammonium polyphosphate, silane-modified zinc borate, DEEP ethyl phosphonate diethyl ester and antimony trioxide are added to the premixed resin system. The rotation speed is adjusted to 700 r / min, the temperature is raised to 95℃, and the mixture is stirred for 90 min. During this period, an anti-settling agent is added every 20 min, and the mixture is added in 3 batches.

[0080] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0081] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 22.5 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s.

[0082] Step 6: Curing the finished product. The ground system is transferred to a curing kettle and cured at 60°C and 250 r / min for 45 min. After cooling to room temperature, it is filtered to obtain an oil-based flame-retardant coating.

[0083] Comparative Example 4: Raw material composition: The matrix resin comprises 15 parts by weight, including 10 parts by weight of acrylic graft-modified saturated polyester resin and 5 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 15%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including 12 parts by weight of Exolit™ AP418 ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethylphosphonate, and 3 parts by weight of antimony trioxide. The pigments and fillers comprise 6 parts by weight, including 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash. The environmentally friendly additives comprise 1.5 parts by weight, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of antisettling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the antisettling agent is fumed silica. The mixed solvent comprises 47.5 parts by weight, including 28 parts by weight of ethyl acetate, 17 parts by weight of xylene, and 2.5 parts by weight of tributyl citrate.

[0084] Preparation method: The first step is to modify the flame retardant with silane. Zinc borate is dried at 110°C for 12 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 5 parts by weight of mixed solvent are added. The mixture is stirred at 75°C and 400 r / min for 60 minutes. After cooling, it is ground to a particle size of 30 μm to obtain silane-modified zinc borate.

[0085] The second step is resin premixing. Acrylic graft-modified saturated polyester resin and SBS are added to the reactor, along with 15 parts by weight of mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain the premixed resin system.

[0086] The third step is to compound the flame retardant system. Add Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate and antimony trioxide to the premixed resin system, adjust the speed to 700 r / min, raise the temperature to 95℃, and stir for 90 min. During this period, add the anti-settling agent every 20 min, and add it in 3 batches.

[0087] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0088] The fifth step is to grind and refine the mixture. The mixture is then transferred to a grinding machine and ground to a particle size of 20 μm. During this process, 22.5 parts by weight of mixed solvent are added to adjust the viscosity of the system to 200 mPa·s.

[0089] Step 6: Curing the finished product. The ground system is transferred to a curing kettle and cured at 60°C and 250 r / min for 45 min. After cooling to room temperature, it is filtered to obtain an oil-based flame-retardant coating.

[0090] Comparative Example 5: Raw material composition: The matrix resin comprises 15 parts by weight, including 10 parts by weight of acrylic graft-modified saturated polyester resin and 5 parts by weight of SBS. The grafting rate of the acrylic graft-modified saturated polyester resin is 15%. The SBS has a linear structure and a molecular weight of 30,000. The silane-modified composite flame retardant comprises 30 parts by weight, including 12 parts by weight of Exolit™ AP418 ammonium polyphosphate, 8 parts by weight of silane-modified zinc borate, 7 parts by weight of DEEP diethyl phosphonate, and 3 parts by weight of antimony trioxide. Pigments and fillers comprise 6 parts by weight. The composition includes: 4 parts by weight of titanium dioxide and 2 parts by weight of mica iron oxide ash; 1.5 parts by weight of environmentally friendly additives, including 0.5 parts by weight of defoamer, 0.6 parts by weight of antioxidant, and 0.4 parts by weight of anti-settling agent. The defoamer is an organosilicon, the antioxidant is 2,6-di-tert-butyl-p-cresol, and the anti-settling agent is fumed silica; and 47.5 parts by weight of environmentally friendly mixed solvents, including 28 parts by weight of n-butyl acetate, 17 parts by weight of propylene glycol methyl ether acetate, and 2.5 parts by weight of tributyl citrate.

[0091] Preparation method: All raw materials, including acrylic grafted modified saturated polyester resin, SBS, and Exolit, are used. TM AP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate, antimony trioxide, titanium dioxide, mica iron oxide ash, defoamer, antioxidant, antisettling agent, and environmentally friendly mixed solvent were added to the reactor at one time and stirred for 180 min at 85℃ and 700 r / min. Then, the mixture was transferred to a grinding equipment and ground to a particle size of 20 μm. The viscosity of the system was adjusted to 200 mPa·s, and then transferred to a curing reactor and cured for 45 min at 60℃ and 250 r / min. After cooling to room temperature, the mixture was filtered to obtain an oil-based flame-retardant coating.

[0092] Comparative Example 6: Raw material composition: The matrix resin comprises 6 parts by weight, of which 4 parts by weight are acrylic graft-modified saturated polyester resin and 2 parts by weight are SBS; the silane-modified composite flame retardant comprises 5 parts by weight, of which Exolit... TM 2 parts by weight of AP418 ammonium polyphosphate, 1 part by weight of silane-modified zinc borate, 1 part by weight of DEEP diethyl phosphonate, 1 part by weight of antimony trioxide; 13 parts by weight of pigments and fillers, including 9 parts by weight of titanium dioxide and 4 parts by weight of mica iron oxide ash; 0.1 parts by weight of environmentally friendly additives, including 0.05 parts by weight of defoamer, 0.03 parts by weight of antioxidant, and 0.02 parts by weight of antisettling agent; 75.9 parts by weight of environmentally friendly mixed solvents, including 45 parts by weight of n-butyl acetate, 28 parts by weight of propylene glycol methyl ether acetate, and 2.9 parts by weight of tributyl citrate.

[0093] Preparation method: The first step is to modify the flame retardant with silane. Zinc borate is dried at 110°C for 12 minutes and cooled to room temperature. Then, silane coupling agent KH560 and 1 part by weight of environmentally friendly mixed solvent are added. The mixture is stirred at 75°C and 400 r / min for 60 minutes. After cooling, it is ground to a particle size of 30 μm to obtain silane-modified zinc borate.

[0094] The second step is resin premixing. Acrylic graft modified saturated polyester resin and SBS are added to the reactor, along with 10 parts by weight of environmentally friendly mixed solvent. The mixture is stirred and premixed for 60 minutes at 85°C and 500 r / min to obtain the premixed resin system.

[0095] The third step is to compound the flame retardant system. Add Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, DEEP diethyl ethyl phosphonate and antimony trioxide to the premixed resin system, adjust the speed to 700 r / min, raise the temperature to 95℃, and stir for 90 min. During this period, add the anti-settling agent every 20 min, and add it in 3 batches.

[0096] The fourth step is to disperse the pigments and fillers. Add titanium dioxide and mica iron oxide ash to the above system, adjust the speed to 900 r / min, and stir and disperse for 45 min. Then add defoamer and antioxidant, and continue stirring for 30 min.

[0097] The fifth step is grinding and refining. The above mixture is transferred to a grinding equipment and ground to a particle size of 20μm. During this process, 64.9 parts by weight of environmentally friendly mixed solvent are added to adjust the viscosity of the system to 200mPa·s.

[0098] Step 6: Curing the finished product. The ground system is transferred to a curing kettle and cured at 60°C and 250 r / min for 45 min. After cooling to room temperature, it is filtered to obtain an oil-based flame-retardant coating.

[0099] All raw materials described in this invention are commercially available conventional industrial-grade products, which can be routinely procured and obtained by those skilled in the art. The grafting rate of the acrylic graft-modified saturated polyester resin is tested according to GB / T14074-2017, and the molecular weight of SBS is routinely tested using gel permeation chromatography (GPC). The amount of silane coupling agent KH560 (γ-glycidoxypropyltrimethoxysilane) is 1%-3% of the weight of zinc borate, which is a routine amount used in the modification of inorganic powder silane in this art. All weight parts mentioned in this invention are parts by mass. The amount of each component of the environmentally friendly mixed solvent distributed in the preparation steps can be routinely adjusted by those skilled in the art within the scope of the claims according to the dispersion requirements of the system. All performance testing methods are common standard methods in the field of flame retardant coatings, and the testing equipment is commercially available conventional equipment, which can be independently tested by those skilled in the art according to the standards.

[0100] This invention achieves a synergistic improvement in the flame retardancy, environmental friendliness, and physicochemical properties of coatings through resin compounding, silane modification of flame retardants, synergistic effect of multiple flame retardants, replacement of environmentally friendly solvents, and stepwise preparation process.

[0101] Performance testing and results analysis: Test standards and methods: (1) Flame retardant performance test: Limiting oxygen index is determined by limiting oxygen index instrument according to ISO45892 standard; vertical burning rating is determined by horizontal and vertical burning test machine according to UL94 standard; flame retardancy time is determined by building material combustion test furnace according to GB12441 standard; smoke density rating is determined by smoke density test chamber according to ISO56592 standard; toxic gas release is determined by toxic gas analysis system according to GB / T20285 standard.

[0102] (2) Environmental performance test: VOC content is determined by gas chromatograph according to GB18581 standard; heavy metal content, including lead, cadmium, chromium and mercury, is determined by atomic absorption spectrophotometer according to GB / T23991 standard.

[0103] (4) Physical and chemical performance tests: Adhesion was determined by the circle-crossing method according to GB / T1720 standard; Hardness was determined by the Shore hardness tester according to GB / T1730 standard; Water resistance was determined by the immersion method at 25℃ for 72h according to GB / T1733 standard; Oil resistance was determined by the immersion method at 25℃ for 48h according to GB / T1734 standard; Weather resistance was determined by the artificial accelerated aging test at 1000h according to GB / T1865 standard; Storage stability was determined by storing at 25℃ for 6 months according to GB / T6753.3 standard, and observing whether there was any layering, precipitation, or clumping; Construction compatibility was tested by brushing, spraying, and rolling with different construction methods to observe the leveling and film-forming effect of the coating.

[0104] Several tests are shown in Table 1 below: Table 1:

[0105] Results analysis: (1) In terms of flame retardant performance, the limiting oxygen index of Examples 1 to 5 is above 32, the vertical burning rating reaches V-0, the longest flame retardant time is 65 min, and the lowest smoke density rating is 32, showing excellent flame retardant and smoke suppression effects. Among them, Example 5 comprehensively optimizes the flame retardant ratio and process parameters, increases the limiting oxygen index to 38, extends the flame retardant time to 65 min, and reduces the smoke density rating to 32, with the best flame retardant and smoke suppression performance, which is suitable for the high flame retardant requirements of high-end special scenarios such as cables and ships. The flame retardant performance of each comparative example is significantly reduced. Comparative Example 1 uses ordinary saturated polyester resin without graft modification, and the compatibility between the resin and the flame retardant is insufficient, so the limiting oxygen index drops to 28, the vertical burning rating is only V-2, and the flame retardant time is shortened to 30 min; Comparative Example 2 cancels the silane modification step of zinc borate, the flame retardant dispersion is worse, the flame retardant synergistic effect is weakened, the limiting oxygen index is 29, and the vertical burning rating is V-1; Comparative Example 3 uses ordinary ammonium polyphosphate to replace Exolit. TM AP418 ammonium polyphosphate showed poor expansion and charring effect, with the limiting oxygen index dropping to 27 and a flame-retardant time of only 28 minutes. Comparative Example 5 used a one-time feeding process, resulting in uneven mixing of components and the worst flame-retardant performance, with a limiting oxygen index of only 26 and a flame-retardant time of only 25 minutes. Comparative Example 6 had an unbalanced raw material ratio, with insufficient amounts of matrix resin and flame retardant, failing to form an effective flame-retardant system, lacking a clear vertical burning rating, and a flame-retardant time of only 20 minutes.

[0106] (2) Regarding environmental performance, the VOC content of Examples 1 to 5 was controlled below 68%. In Example 4, the environmentally friendly mixed solvent ratio was optimized, and the VOC content was reduced to 58. In Example 5, the process was further optimized, and the VOC content was reduced to 55, which met the environmental protection requirements. Comparative Example 4 used a non-environmentally friendly mixed solvent composed of ethyl acetate and xylene, and the VOC content soared to 112, far exceeding the environmental protection standard. Comparative Example 6 had an excessively high solvent content, and the VOC content reached 85, failing to meet the environmental protection standards. Although the VOC content of the other comparative examples was close to that of the examples, they could not meet the comprehensive environmental protection requirements due to other performance defects. The heavy metal content of all examples and comparative examples met the standards, and no exceedances were detected, indicating that the raw material selection of this invention is in line with environmental protection guidelines.

[0107] (3) In terms of physical and chemical properties, the adhesion of Examples 1 to 5 all reached level 1 or above, with Example 5 reaching level 0. The hardness was between 65 and 72. There were no abnormalities in water resistance and weather resistance. The storage stability was good and the construction adaptability was excellent, which can meet the construction and use requirements of different scenarios. Example 2 optimized the flame retardant silane modification process, which solved the problem of flame retardant sedimentation in high humidity environment. The storage stability and construction adaptability were suitable for outdoor scenarios. Example 3 adjusted the matrix resin ratio and grafting rate to improve weather resistance and adapt to long-term outdoor exposure scenarios. Example 4 optimized the solvent ratio to improve indoor construction adaptability. Each comparative example exhibits significant defects in its physical and chemical properties. Comparative example 1 shows abnormal weather resistance, with adhesion reduced to level 3 and hardness as low as 58. Comparative example 2 exhibits poor storage stability, with slight sedimentation and easy sagging during application. Comparative example 5 shows abnormal water resistance and weather resistance, with adhesion at level 3, poor storage stability, and stratified sedimentation, making normal application impossible. Comparative example 6 has the worst physical and chemical properties, with adhesion at level 4, hardness at 52, abnormal water resistance and weather resistance, severe stratification during storage, and inability to form a film.

[0108] In summary, this invention utilizes acrylic acid grafting modification of saturated polyester resin and SBS compounding, zinc borate silane modification, and Exolit... TM The composite flame retardant system with AP418 ammonium polyphosphate as the core, the optimization of environmentally friendly mixed solvents, and the adoption of stepwise preparation processes have achieved a synergistic improvement in flame retardant performance, environmental performance, and physicochemical properties.

[0109] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention.

Claims

1. An oil-based, environmentally friendly, polymeric flame-retardant coating, characterized in that, It includes the following components by weight: 15-18 parts by weight of matrix resin, 30-35 parts by weight of silane-modified composite flame retardant, 6-7 parts by weight of pigments and fillers, 1.5-1.8 parts by weight of environmentally friendly additives, and 38.2-47.5 parts by weight of environmentally friendly mixed solvent.

2. The oil-based environmentally friendly polymer flame-retardant coating according to claim 1, characterized in that, The matrix resin is composed of acrylic acid grafted modified saturated polyester resin and styrene-butadiene-styrene block copolymer, wherein the acrylic acid grafted modified saturated polyester resin is 10-14 parts by weight and the styrene-butadiene-styrene block copolymer is 4-5 parts by weight; the grafting rate of the acrylic acid grafted modified saturated polyester resin is 15%-20%, and the styrene-butadiene-styrene block copolymer has a linear structure and a molecular weight of 30000 g / mol.

3. The oil-based environmentally friendly polymer flame-retardant coating according to claim 1, characterized in that, The silane-modified composite flame retardant is composed of Exolit™ AP418 ammonium polyphosphate, silane-modified zinc borate, diethyl ethyl phosphonate, and antimony trioxide. The amount of Exolit™ AP418 ammonium polyphosphate is 12-15 parts by weight, the amount of silane-modified zinc borate is 8-10 parts by weight, the amount of diethyl ethyl phosphonate is 7-8 parts by weight, and the amount of antimony trioxide is 2-3 parts by weight.

4. The oil-based environmentally friendly polymer flame-retardant coating according to claim 1, characterized in that, The pigment and filler are composed of titanium dioxide and mica iron oxide ash, with titanium dioxide accounting for 4-5 parts by weight and mica iron oxide ash accounting for 2 parts by weight.

5. The oil-based environmentally friendly polymer flame-retardant coating according to claim 1, characterized in that, The environmentally friendly additive is composed of an organosilicon defoamer, a 2,6-di-tert-butyl-p-cresol antioxidant, and a fumed silica anti-settling agent. The organosilicon defoamer is 0.5-0.6 parts by weight, the 2,6-di-tert-butyl-p-cresol antioxidant is 0.6-0.7 parts by weight, and the fumed silica anti-settling agent is 0.4-0.5 parts by weight.

6. The oil-based environmentally friendly polymer flame-retardant coating according to claim 1, characterized in that, The environmentally friendly mixed solvent is composed of n-butyl acetate, propylene glycol methyl ether acetate and tributyl citrate, with n-butyl acetate comprising 22-28 parts by weight, propylene glycol methyl ether acetate comprising 14-17 parts by weight, and tributyl citrate comprising 2.2-3.5 parts by weight.

7. A method for preparing an oil-based environmentally friendly polymer flame-retardant coating according to any one of claims 1 to 6, characterized in that, Includes the following steps: Flame retardant silane modification: Zinc borate was dried, cooled, and then mixed with silane coupling agent KH560 and an environmentally friendly mixed solvent. After stirring and modification, the mixture was cooled and ground to obtain silane-modified zinc borate. Resin premixing involves adding acrylic graft-modified saturated polyester resin and styrene-butadiene-styrene block copolymer to a reactor, adding an environmentally friendly mixed solvent, and stirring to premix to obtain a premixed resin system. Flame retardant system compounding, using Exolit TM AP418 ammonium polyphosphate, silane-modified zinc borate, diethyl ethyl phosphonate and antimony trioxide are added to the premixed resin system, heated and stirred to compound, and antisettling agent is added in batches. For pigment and filler dispersion, titanium dioxide and mica iron oxide ash are added to the above system, stirred and dispersed, then defoamer and antioxidant are added, and stirring is continued; Grinding and refining: The mixed system is ground, and environmentally friendly mixed solvents are added to adjust the viscosity of the system. The finished product is matured by aging the ground system, cooling and filtering to obtain an oil-based environmentally friendly polymer flame-retardant coating.

8. The preparation method according to claim 7, characterized in that, In the silane modification step of the flame retardant, the drying temperature is 110-115℃, the drying time is 12-15min, the modification temperature is 75-85℃, the stirring speed is 400-500r / min, the modification time is 60-90min, and the grinding particle size is 20-30μm; the amount of silane coupling agent KH560 is 1%-3% of the weight of zinc borate.

9. The preparation method according to claim 7, characterized in that, The resin premixing temperature is 85-90℃, the stirring speed is 500-550r / min, and the premixing time is 60-70min; the flame retardant system compounding stirring speed is 700-750r / min, the compounding temperature is 95-100℃, and the compounding time is 90-100min; the pigment and filler dispersion stirring speed is 900-950r / min, and the dispersion time is 45-50min.

10. The preparation method according to claim 7, characterized in that, The particle size after grinding is 15-20μm, the system viscosity is adjusted to 180-200mPa・s, the aging temperature is 55-65℃, the stirring speed is 250-280r / min, the aging time is 45-50min, and nitrogen gas is introduced for protection during the aging process.

Images