High-temperature-resistant anti-ultraviolet polycarbonate material and preparation method thereof

Abstract

The invention relates to the technical field of polycarbonate materials, in particular to a high-temperature-resistant anti-ultraviolet polycarbonate material and a preparation method thereof. The flame retardant is prepared by adding a hydroxylated flame-retardant substance, an aminated flame-retardant substance and phytic acid. The antistatic modified carbon black is obtained by adding carbon black, gamma-(methacryloyloxy) propyltrimethoxysilane, 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a sulfhydrylated flame-retardant substance and a photoinitiator. And mixing the polycarbonate resin, the polyaryletherketone resin, the flame retardant, the antistatic modified carbon black, the anti-ultraviolet agent, the anti-dripping agent and the dispersing agent, and carrying out melt blending, extrusion granulation and extrusion film forming to obtain the polycarbonate film material. The polycarbonate film material prepared by the invention has excellent flame retardant property and antistatic property, so that the polycarbonate film material has a wide application prospect in the technical field of polycarbonate materials.

Description

Technical Field

[0001] The present invention relates to the technical field of polycarbonate materials, in particular to a high-temperature resistant and ultraviolet resistant polycarbonate material and a preparation method thereof. Background Art

[0002] In today's rapidly advancing technological world, polycarbonate film, with its exceptional performance and wide range of applications, has demonstrated its irreplaceable value. In the electronics and information technology sector, polycarbonate film's high transparency and excellent flexibility make it an ideal material for flexible display screens. Furthermore, its excellent insulation properties ensure the stable operation of electronic components, reduce the risk of short circuits and failures, and enhance the reliability and service life of equipment. In the construction sector, polycarbonate film is widely used in skylights, curtain walls, and other applications. Its excellent thermal and sound insulation properties effectively reduce building energy consumption and create a comfortable indoor environment. In the packaging industry, polycarbonate film, with its excellent chemical resistance and barrier properties, provides reliable packaging protection for food, pharmaceuticals, and other products.

[0003] However, in the field of electronic appliances, circuit failures can easily cause fires, necessitating the development of polycarbonate films with excellent flame retardancy. When exposed to a fire source, these films can effectively reduce the burning rate and inhibit the spread of flames, minimizing the likelihood and severity of fire. Furthermore, due to their excellent insulating properties, polycarbonate films are prone to static electricity, which can damage and malfunction electronic components. Therefore, there is an urgent need to improve the antistatic properties of polycarbonate films to prevent interference and damage to electronic components caused by static electricity accumulation, thereby ensuring stable operation of equipment.

[0004] In order to overcome the defects of the prior art, the present invention provides a high-temperature resistant and UV-resistant polycarbonate material and a preparation method thereof. Summary of the Invention

[0005] The object of the present invention is to provide a high-temperature resistant and UV-resistant polycarbonate material and a preparation method thereof, so as to solve the problems raised in the prior art.

[0006] To achieve the above object, the present invention provides the following technical solutions: A method for preparing a high-temperature resistant and UV-resistant polycarbonate material comprises the following steps: fully mixing a polycarbonate resin, a polyaryletherketone resin, a flame retardant, an antistatic modified carbon black, an anti-UV agent, an anti-dripping agent and a dispersant for 8-15 minutes, and then performing melt blending, extrusion granulation and extrusion film formation to obtain a polycarbonate film material.

[0007] More optimally, the content of each component of the polycarbonate film material is: by mass fraction, 60-75% polycarbonate resin, 10-15% polyaryletherketone resin, 10-13% flame retardant, 3-5% antistatic modified carbon black, 1-3% anti-ultraviolet agent, 0.5-0.7% anti-dripping agent, and the balance is dispersant; the anti-ultraviolet agent is 2-hydroxy-4-methoxybenzophenone; the anti-dripping agent is polytetrafluoroethylene; and the dispersant is pentaerythritol stearate.

[0008] More optimally, the melt blending temperature is 250-270°C; the extrusion granulation temperature is 270-300°C; the extrusion film forming temperature is 280-300°C; and the thickness of the polycarbonate film material is 0.2-0.3 mm.

[0009] More optimally, the preparation process of the flame retardant is: Step S1: adding 5-amino-1H-tetrazole and p-hydroxybenzaldehyde to ethanol, reflux reacting at 77-80° C. for 5-6 hours, cooling, filtering, washing, and drying after completion of the reaction to obtain a hydroxylated flame retardant; adding hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane to anhydrous toluene under a nitrogen atmosphere, stirring evenly, and then adding triethylamine, stirring and reacting at 70-75° C. for 13-15 hours, cooling, filtering, washing, and drying after completion of the reaction to obtain an amino flame retardant; Step S2: uniformly mixing a 75-80 wt% phytic acid aqueous solution and anhydrous ethanol to obtain a phytic acid reaction solution; dropwise adding the phytic acid reaction solution to an amino flame retardant, reacting at 5-10° C. for 6-8 hours; after the reaction is completed, adding a hydroxylated flame retardant, heating to 120-130° C. and stirring to react for 3.5-4.5 hours; and after the reaction is completed, cooling and drying to obtain a flame retardant.

[0010] More optimally, when preparing hydroxylated flame retardants, the reaction molar ratio of 5-amino-1H-tetrazole and p-hydroxybenzaldehyde is (1.1-1.2):1; when preparing amination flame retardants, the molar mass ratio of hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane is (1.05-1.10):6.

[0011] More optimally, when preparing the flame retardant, the reaction molar ratio of the phosphate group in the phytic acid molecule, the amino group in the aminated flame retardant, and the hydroxyl group in the hydroxylated flame retardant in the phytic acid reaction solution is 1: (1.1-1.2): 1.

[0012] More optimally, the preparation process of antistatic modified carbon black is: Step S1: adding γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and an ammonia solution to carbon black, ball milling the mixture at a rotation speed of 250-300 r / min for 10-15 hours, and drying the mixture after ball milling to obtain modified carbon black; Step S2: Under a nitrogen environment, the hydroxylated flame retardant, p-toluenesulfonic acid, and hydroquinone are added to toluene, stirred evenly, and then 3-mercaptopropionic acid is added dropwise at 110-120° C. After the addition is completed, stirring is continued for 5-7 hours. After the reaction is completed, the mixture is cooled, diluted, and rotary evaporated to obtain a thiolated flame retardant; Step S3: 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a thiolated flame retardant, and a photoinitiator, 2-hydroxy-2-methyl-1-phenyl-1-propanone, are added to toluene, stirred evenly, and then modified carbon black is added. The stirring is continued for 30-50 minutes, and then the reaction is stirred under ultraviolet light for 50-60 minutes. After the reaction is completed, the antistatic modified carbon black is obtained by filtering, washing, and drying.

[0013] More optimally, the mass volume ratio of carbon black, γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and ammonia solution is (6-8) g: (0.10-0.12) g: (18-20) mL: 0.15 mL: 2 mL; when preparing thiol flame retardants, the reaction mass ratio of hydroxylated flame retardants, p-toluenesulfonic acid, hydroquinone, and 3-mercaptopropionic acid is (7.5-7.8): 0.25: 0.05: 4.

[0014] More optimally, when preparing antistatic modified carbon black, the reaction mass ratio of 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, mercapto flame retardant, photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, and modified carbon black is 0.3:0.1:0.2:0.02:(1.5-2.0); the wavelength of ultraviolet light is 365-370nm.

[0015] Beneficial effects of the present invention: The present invention is characterized by preparing a flame retardant by adding a hydroxylated flame retardant, an aminated flame retardant, and phytic acid. The specific reaction mechanism is as follows: 5-amino-1H-tetrazole and p-hydroxybenzaldehyde react to form a Schiff base structure, resulting in the hydroxylated flame retardant; hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane undergo a nucleophilic substitution reaction to produce the aminated flame retardant. In step S2, the phytic acid reaction solution is first added to the aminated flame retardant, undergoing a process similar to an acid-base neutralization reaction, whereby some of the phosphate groups in the phytic acid react with the amino groups to produce a phytate; further, the hydroxylated flame retardant is added to the remaining phosphate groups to undergo an esterification reaction, resulting in the flame retardant. Phytic acid is rich in phosphorus, while 5-amino-1H-tetrazole and 4,4'-diaminodiphenylmethane introduce nitrogen. At high temperatures, the nitrogen-containing structure decomposes to produce non-flammable gases such as nitrogen. These gases can dilute the oxygen concentration in the combustion zone, reducing the combustion reaction rate. Phosphorus promotes the formation of a carbonized layer, while nitrogen helps stabilize it and exerts a flame retardant effect in the gas phase. The two work together to significantly improve flame retardancy. Furthermore, the Schiff base structure formed by the reaction possesses a certain degree of thermal stability and is not easily broken at high temperatures. This maintains the integrity of the flame retardant molecules to a certain extent, extending the duration of the flame retardant effect.

[0016] The present invention is characterized in that antistatic modified carbon black is obtained by adding carbon black, γ-(methacryloyloxy)propyltrimethoxysilane, 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a thiol flame retardant, and a photoinitiator. The specific reaction mechanism is as follows: carbon black is modified by adding γ-(methacryloyloxy)propyltrimethoxysilane to obtain modified carbon black with good dispersibility, and a carbon-carbon double bond is introduced on the surface of the carbon black. Then, a hydroxylated flame retardant and 3-mercaptopropionic acid are added to undergo an esterification reaction under the action of a catalyst, p-toluenesulfonic acid, and a stabilizer, hydroquinone, to obtain a thiol flame retardant. Furthermore, 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a thiol flame retardant, a photoinitiator, and the modified carbon black are mixed to undergo a thiol-ene click reaction to obtain an antistatic modified carbon black.

[0017] Among them, carbon black is a material with excellent electrical conductivity. It contains a large number of conjugated systems and free electrons. These free electrons can move within and between carbon black particles, forming conductive pathways, thus providing the basic electron conduction basis for antistatic properties. Furthermore, the organic groups of the silane coupling agent interact with the carbon black surface, reducing the agglomeration force between the carbon black particles and allowing the carbon black to be more evenly dispersed in the system. Evenly dispersed carbon black particles can form more conductive pathways, which is conducive to the transmission of electrons, thereby improving antistatic properties. In addition, the thiol flame retardant obtained by the esterification reaction of hydroxylated flame retardants and 3-mercaptopropionic acid retains flame retardant properties while introducing thiol groups. Mercapto groups have high reactivity, so the mercapto-flame retardant, 3-mercaptopropionic acid, and 4-mercapto-1-butanesulfonic acid together with the carbon-carbon double bonds on the surface of the modified carbon black undergo a mercapto-ene click reaction, connecting the flame retardant structure, hydrophilic sulfonic acid group, carboxylic acid group and carbon black together, forming a complex and continuous electron transport network, enabling electrons to be transmitted quickly and efficiently throughout the system, thereby having both excellent antistatic and flame retardant properties.

[0018] Finally, the polycarbonate resin, polyaryletherketone resin, flame retardant, antistatic modified carbon black, anti-ultraviolet agent, anti-dripping agent, and dispersant are mixed, melt blended, extruded into pellets, and extruded into films to obtain a polycarbonate film material. In summary, the polycarbonate film material prepared by the present invention has excellent flame retardant and antistatic properties, and therefore has broad application prospects in the field of polycarbonate material technology. DETAILED DESCRIPTION

[0019] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0020] Source of raw materials: Carbon black, particle size of 40 nm; polycarbonate resin, provided by Dongguan Shuowei Plastic Raw Materials Co., Ltd., model 1920T-11; polyaryletherketone resin, model Solvay AvaSpire AV-651 GF50, USA; polytetrafluoroethylene, provided by Guangzhou Songbai Chemical Co., Ltd., particle size of 5 μm.

[0021] Example 1: Step S1: 5-amino-1H-tetrazole and p-hydroxybenzaldehyde are added to ethanol, refluxed at 80° C. for 6 hours, and after the reaction is completed, cooled, filtered, washed, and dried to obtain a hydroxylated flame retardant. Under a nitrogen environment, hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane are added to anhydrous toluene, stirred evenly, and then triethylamine is added. The mixture is stirred and reacted at 75° C. for 15 hours. After the reaction is completed, cooled, filtered, washed, and dried to obtain an amination flame retardant. When preparing the hydroxylated flame retardant, the reaction molar ratio of 5-amino-1H-tetrazole and p-hydroxybenzaldehyde is 1.15:1; when preparing the amination flame retardant, the molar mass ratio of hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane is 1.07:6. An 80 wt% phytic acid aqueous solution and anhydrous ethanol are uniformly mixed to obtain a phytic acid reaction solution; the phytic acid reaction solution is dropwise added to an amino flame retardant, and the mixture is reacted at 10° C. for 8 hours. After the reaction is completed, a hydroxylated flame retardant is added, and the mixture is heated to 130° C. and stirred for reaction for 4.5 hours. After the reaction is completed, the mixture is cooled and dried to obtain a flame retardant; when preparing the flame retardant, the reaction molar ratio of the phosphate group in the phytic acid molecule in the phytic acid reaction solution, the amino group in the amino flame retardant, and the hydroxyl group in the hydroxylated flame retardant is 1:1.15:1; Step S2: adding γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and an ammonia solution to carbon black, ball-milling the mixture at a rotation speed of 300 r / min for 15 h, and drying the mixture after ball milling to obtain modified carbon black; Under a nitrogen environment, the hydroxylated flame retardant, p-toluenesulfonic acid, and hydroquinone were added to toluene, stirred evenly, and then 3-mercaptopropionic acid was added dropwise at 120° C. After the addition was completed, stirring was continued for 7 hours. After the reaction was completed, the mixture was cooled, diluted, and rotary evaporated to obtain a thiol flame retardant; 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a mercapto-flame retardant, and a photoinitiator, 2-hydroxy-2-methyl-1-phenyl-1-propanone, are added to toluene, stirred evenly, and then modified carbon black is added. The mixture is stirred for 50 minutes, and then stirred and reacted under ultraviolet light for 60 minutes. After the reaction is completed, the mixture is filtered, washed, and dried to obtain an antistatic modified carbon black. The mass volume ratio of carbon black, γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and ammonia solution is 7g:0.11g:19mL. : 0.15mL: 2mL; when preparing the mercapto flame retardant, the reaction mass ratio of the hydroxylated flame retardant, p-toluenesulfonic acid, hydroquinone, and 3-mercaptopropionic acid is 7.6:0.25:0.05:4; when preparing the antistatic modified carbon black, the reaction mass ratio of 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, mercapto flame retardant, photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, and modified carbon black is 0.3:0.1:0.2:0.02:1.7; the wavelength of the ultraviolet light is 365nm; Step S3: 65 g of polycarbonate resin, 13 g of polyaryletherketone resin, 13 g of flame retardant, 5 g of antistatic modified carbon black, 3 g of 2-hydroxy-4-methoxybenzophenone, 0.5 g of polytetrafluoroethylene and 0.5 g of pentaerythritol stearate are fully mixed for 15 minutes, and then melt blended, extruded into granules, and extruded into films to obtain a polycarbonate film material; the melt blending temperature is 270° C.; the extrusion granulation temperature is 300° C.; the extrusion film forming temperature is 300° C.; and the thickness of the polycarbonate film material is 0.3 mm.

[0022] Example 2: Step S1: 5-amino-1H-tetrazole and p-hydroxybenzaldehyde are added to ethanol, and the mixture is refluxed at 78° C. for 5.5 hours. After the reaction is completed, the mixture is cooled, filtered, washed, and dried to obtain a hydroxylated flame retardant. Under a nitrogen environment, hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane are added to anhydrous toluene, stirred evenly, and then triethylamine is added. The mixture is stirred and reacted at 73° C. for 14 hours. After the reaction is completed, the mixture is cooled, filtered, washed, and dried to obtain an amination flame retardant. When preparing the hydroxylated flame retardant, the reaction molar ratio of 5-amino-1H-tetrazole and p-hydroxybenzaldehyde is 1.15:1; when preparing the amination flame retardant, the molar mass ratio of hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane is 1.07:6. A 77 wt% phytic acid aqueous solution and anhydrous ethanol are uniformly mixed to obtain a phytic acid reaction solution; the phytic acid reaction solution is dropwise added to an amino flame retardant, and the mixture is reacted at 7°C for 7 hours. After the reaction is completed, a hydroxylated flame retardant is added, and the mixture is heated to 125°C and stirred for reaction for 4 hours. After the reaction is completed, the mixture is cooled and dried to obtain a flame retardant; when preparing the flame retardant, the reaction molar ratio of the phosphate group in the phytic acid molecule in the phytic acid reaction solution, the amino group in the amino flame retardant, and the hydroxyl group in the hydroxylated flame retardant is 1:1.15:1; Step S2: adding γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and an ammonia solution to carbon black, ball-milling the mixture at a rotation speed of 270 r / min for 13 h, and drying the mixture after ball milling to obtain modified carbon black; Under a nitrogen environment, the hydroxylated flame retardant, p-toluenesulfonic acid, and hydroquinone were added to toluene, stirred evenly, and then 3-mercaptopropionic acid was added dropwise at 115° C. After the addition was completed, stirring was continued for 6 hours. After the reaction was completed, the mixture was cooled, diluted, and rotary evaporated to obtain a thiol flame retardant; 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a mercapto-flame retardant, and a photoinitiator, 2-hydroxy-2-methyl-1-phenyl-1-propanone, were added to toluene, stirred evenly, and then the modified carbon black was added. The mixture was stirred for 40 minutes, and then stirred and reacted under ultraviolet light for 55 minutes. After the reaction was completed, the mixture was filtered, washed, and dried to obtain an antistatic modified carbon black. The mass volume ratio of carbon black, γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and ammonia solution was 7 g:0.11 g:19 mL. : 0.15mL: 2mL; when preparing the mercapto flame retardant, the reaction mass ratio of the hydroxylated flame retardant, p-toluenesulfonic acid, hydroquinone, and 3-mercaptopropionic acid is 7.6:0.25:0.05:4; when preparing the antistatic modified carbon black, the reaction mass ratio of 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, mercapto flame retardant, photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, and modified carbon black is 0.3:0.1:0.2:0.02:1.7; the wavelength of the ultraviolet light is 365nm; Step S3: 65 g of polycarbonate resin, 13 g of polyaryletherketone resin, 13 g of flame retardant, 5 g of antistatic modified carbon black, 3 g of 2-hydroxy-4-methoxybenzophenone, 0.5 g of polytetrafluoroethylene and 0.5 g of pentaerythritol stearate are fully mixed for 10 minutes, and then melt blended, extruded into granules, and extruded into films to obtain a polycarbonate film material; the melt blending temperature is 260° C.; the extrusion granulation temperature is 280° C.; the extrusion film forming temperature is 290° C.; and the thickness of the polycarbonate film material is 0.3 mm.

[0023] Example 3: Step S1: 5-amino-1H-tetrazole and p-hydroxybenzaldehyde are added to ethanol, refluxed at 77° C. for 5 hours, cooled, filtered, washed, and dried after the reaction to obtain a hydroxylated flame retardant; under a nitrogen environment, hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane are added to anhydrous toluene, stirred evenly, and then triethylamine is added, stirred at 70° C. for 13 hours, cooled, filtered, washed, and dried to obtain an amination flame retardant; when preparing the hydroxylated flame retardant, the reaction molar ratio of 5-amino-1H-tetrazole and p-hydroxybenzaldehyde is 1.15:1; when preparing the amination flame retardant, the molar mass ratio of hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane is 1.07:6; A 75 wt% phytic acid aqueous solution and anhydrous ethanol are uniformly mixed to obtain a phytic acid reaction solution; the phytic acid reaction solution is dropwise added to an amino flame retardant, and the mixture is reacted at 5° C. for 6 hours. After the reaction is completed, a hydroxylated flame retardant is added, and the mixture is heated to 120° C. and stirred for reaction for 3.5 hours. After the reaction is completed, the mixture is cooled and dried to obtain a flame retardant; when preparing the flame retardant, the reaction molar ratio of the phosphate group in the phytic acid molecule in the phytic acid reaction solution, the amino group in the amino flame retardant, and the hydroxyl group in the hydroxylated flame retardant is 1:1.15:1; Step S2: adding γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and an ammonia solution to carbon black, ball-milling the mixture at a rotation speed of 250 r / min for 10 h, and drying the mixture after ball milling to obtain modified carbon black; Under a nitrogen environment, the hydroxylated flame retardant, p-toluenesulfonic acid, and hydroquinone were added to toluene, stirred evenly, and then 3-mercaptopropionic acid was added dropwise at 110° C. After the addition was completed, stirring was continued for 5 hours. After the reaction was completed, the mixture was cooled, diluted, and rotary evaporated to obtain a thiol flame retardant; 3-Mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a mercapto-flame retardant, and a photoinitiator, 2-hydroxy-2-methyl-1-phenyl-1-propanone, are added to toluene, stirred evenly, and then modified carbon black is added. The mixture is stirred for 30 minutes, and then stirred and reacted under ultraviolet light for 50 minutes. After the reaction is completed, the mixture is filtered, washed, and dried to obtain an antistatic modified carbon black. The mass volume ratio of carbon black, γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and ammonia solution is 7g:0.11g:19mL. : 0.15mL: 2mL; when preparing the mercapto flame retardant, the reaction mass ratio of the hydroxylated flame retardant, p-toluenesulfonic acid, hydroquinone, and 3-mercaptopropionic acid is 7.6:0.25:0.05:4; when preparing the antistatic modified carbon black, the reaction mass ratio of 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, mercapto flame retardant, photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, and modified carbon black is 0.3:0.1:0.2:0.02:1.7; the wavelength of the ultraviolet light is 365nm; Step S3: 65 g of polycarbonate resin, 13 g of polyaryletherketone resin, 13 g of flame retardant, 5 g of antistatic modified carbon black, 3 g of 2-hydroxy-4-methoxybenzophenone, 0.5 g of polytetrafluoroethylene and 0.5 g of pentaerythritol stearate were fully mixed for 8 minutes, and then melt blended, extruded into granules, and extruded into films to obtain a polycarbonate film material; the melt blending temperature was 250° C.; the extrusion granulation temperature was 270° C.; the extrusion film forming temperature was 280° C.; and the thickness of the polycarbonate film material was 0.3 mm.

[0024] Comparative Example 1: The flame retardant was removed, and the rest was the same as Example 1, and the specific steps were as follows: Step S1: γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and ammonia solution were added to carbon black, and the mixture was ball-milled at a speed of 300 r / min for 15 h. After the ball milling, the mixture was dried to obtain modified carbon black; Under a nitrogen environment, the hydroxylated flame retardant, p-toluenesulfonic acid, and hydroquinone were added to toluene, stirred evenly, and then 3-mercaptopropionic acid was added dropwise at 120° C. After the addition was completed, stirring was continued for 7 hours. After the reaction was completed, the mixture was cooled, diluted, and rotary evaporated to obtain a thiol flame retardant; 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a mercapto-flame retardant, and a photoinitiator, 2-hydroxy-2-methyl-1-phenyl-1-propanone, are added to toluene, stirred evenly, and then modified carbon black is added. The mixture is stirred for 50 minutes, and then stirred and reacted under ultraviolet light for 60 minutes. After the reaction is completed, the mixture is filtered, washed, and dried to obtain an antistatic modified carbon black. The mass volume ratio of carbon black, γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and ammonia solution is 7g:0.11g:19mL. : 0.15mL: 2mL; when preparing the mercapto flame retardant, the reaction mass ratio of the hydroxylated flame retardant, p-toluenesulfonic acid, hydroquinone, and 3-mercaptopropionic acid is 7.6:0.25:0.05:4; when preparing the antistatic modified carbon black, the reaction mass ratio of 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, mercapto flame retardant, photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, and modified carbon black is 0.3:0.1:0.2:0.02:1.7; the wavelength of the ultraviolet light is 365nm; Step S2: 65 g of polycarbonate resin, 13 g of polyaryletherketone resin, 5 g of antistatic modified carbon black, 3 g of 2-hydroxy-4-methoxybenzophenone, 0.5 g of polytetrafluoroethylene and 0.5 g of pentaerythritol stearate were fully mixed for 15 minutes, and then melt blended, extruded into granules, and extruded into films to obtain a polycarbonate film material; the melt blending temperature was 270° C.; the extrusion granulation temperature was 300° C.; the extrusion film forming temperature was 300° C.; and the thickness of the polycarbonate film material was 0.3 mm.

[0025] Comparative Example 2: The antistatic modified carbon black was replaced with ordinary carbon black, and the rest was the same as Example 1, and the specific steps were as follows: Step S1: 5-amino-1H-tetrazole and p-hydroxybenzaldehyde were added to ethanol, refluxed at 80° C. for 6 hours, and after the reaction was completed, cooled, filtered, washed, and dried to obtain a hydroxylated flame retardant; under a nitrogen environment, hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane were added to anhydrous toluene, stirred evenly, and then triethylamine was added, stirred at 75° C. for 15 hours, and after the reaction was completed, cooled, filtered, washed, and dried to obtain an amino flame retardant; when preparing the hydroxylated flame retardant, the reaction molar ratio of 5-amino-1H-tetrazole and p-hydroxybenzaldehyde was 1.15:1; when preparing the amino flame retardant, the molar mass ratio of hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane was 1.07:6; An 80 wt% phytic acid aqueous solution and anhydrous ethanol are uniformly mixed to obtain a phytic acid reaction solution; the phytic acid reaction solution is dropwise added to an amino flame retardant, and the mixture is reacted at 10° C. for 8 hours. After the reaction is completed, a hydroxylated flame retardant is added, and the mixture is heated to 130° C. and stirred for reaction for 4.5 hours. After the reaction is completed, the mixture is cooled and dried to obtain a flame retardant; when preparing the flame retardant, the reaction molar ratio of the phosphate group in the phytic acid molecule in the phytic acid reaction solution, the amino group in the amino flame retardant, and the hydroxyl group in the hydroxylated flame retardant is 1:1.15:1; Step S2: 65 g of polycarbonate resin, 13 g of polyaryletherketone resin, 13 g of flame retardant, 5 g of carbon black, 3 g of 2-hydroxy-4-methoxybenzophenone, 0.5 g of polytetrafluoroethylene and 0.5 g of pentaerythritol stearate are fully mixed for 15 minutes, and then melt blended, extruded into granules, and extruded into films to obtain a polycarbonate film material; the melt blending temperature is 270° C.; the extrusion granulation temperature is 300° C.; the extrusion film forming temperature is 300° C.; and the thickness of the polycarbonate film material is 0.3 mm.

[0026] Comparative Example 3: The antistatic modified carbon black was removed, and the rest was the same as Example 1, and the specific steps were as follows: Step S1: 5-amino-1H-tetrazole and p-hydroxybenzaldehyde were added to ethanol, refluxed at 80° C. for 6 hours, and after the reaction was completed, the reaction was cooled, filtered, washed, and dried to obtain a hydroxylated flame retardant; under a nitrogen environment, hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane were added to anhydrous toluene, stirred evenly, and then triethylamine was added, stirred at 75° C. for 15 hours, and after the reaction was completed, the reaction was cooled, filtered, washed, and dried to obtain an amination flame retardant; when preparing the hydroxylated flame retardant, the reaction molar ratio of 5-amino-1H-tetrazole and p-hydroxybenzaldehyde was 1.15:1; when preparing the amination flame retardant, the molar mass ratio of hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane was 1.07:6; An 80 wt% phytic acid aqueous solution and anhydrous ethanol are uniformly mixed to obtain a phytic acid reaction solution; the phytic acid reaction solution is dropwise added to an amino flame retardant, and the mixture is reacted at 10° C. for 8 hours. After the reaction is completed, a hydroxylated flame retardant is added, and the mixture is heated to 130° C. and stirred for reaction for 4.5 hours. After the reaction is completed, the mixture is cooled and dried to obtain a flame retardant; when preparing the flame retardant, the reaction molar ratio of the phosphate group in the phytic acid molecule in the phytic acid reaction solution, the amino group in the amino flame retardant, and the hydroxyl group in the hydroxylated flame retardant is 1:1.15:1; Step S2: 65 g of polycarbonate resin, 13 g of polyaryletherketone resin, 13 g of flame retardant, 3 g of 2-hydroxy-4-methoxybenzophenone, 0.5 g of polytetrafluoroethylene and 0.5 g of pentaerythritol stearate were fully mixed for 15 minutes, and then melt blended, extruded into granules, and extruded into films to obtain a polycarbonate film material; the melt blending temperature was 270° C.; the extrusion granulation temperature was 300° C.; the extrusion film forming temperature was 300° C.; and the thickness of the polycarbonate film material was 0.3 mm.

[0027] Detection test: Flame retardant performance test: Referring to GB / T 2406.2-2009 "Determination of combustion behavior of plastics by oxygen index method Part 2: Room temperature test", the polycarbonate film material prepared by the present invention was used as a sample with a sample size of 70×6.5 mm, and the oxygen index value was recorded.

[0028] Antistatic performance test: Referring to GB / T 1410-2006, "Test method for volume resistivity and surface resistivity of solid insulating materials," the polycarbonate film material prepared in this invention was cut into 70 mm x 70 mm specimens. The test voltage was 400 V, and the surface resistivity of the specimens was recorded. The results are shown in the following table: Conclusion: The dosages used in Examples 1 to 3 remained unchanged, and only some reaction parameters were modified. The experimental data show that there was no significant fluctuation in the performance of the samples.

[0029] Comparative Example 1: The flame retardant was removed, and the rest was the same as Example 1. From the experimental data, it can be seen that compared with Example 1, the oxygen index was reduced to 31.2%. The reason for this is that the flame retardant prepared by the present invention has a phosphorus-nitrogen synergistic flame retardant structure and a Schiff base structure, and therefore has excellent flame retardant properties. Therefore, after removing the flame retardant, the oxygen index is reduced.

[0030] Comparative Example 2: The antistatic modified carbon black was replaced with ordinary carbon black. The rest was the same as in Example 1. From the experimental data, it can be seen that compared with Example 1, the oxygen index was reduced to 36.6%, and the surface resistivity was increased to 3.75×10 12 Ω, the reason is analyzed as follows: antistatic modified carbon black includes thiol flame retardant, hydrophilic sulfonic acid group and carboxylic acid group, so it has excellent antistatic and flame retardant properties. Therefore, after the antistatic modified carbon black is replaced by ordinary carbon black, the oxygen index decreases and the surface resistivity increases.

[0031] Comparative Example 3: The antistatic modified carbon black was removed, and the rest was the same as Example 1. From the experimental data, it can be seen that compared with Example 1, the oxygen index was reduced to 35.1%, and the surface resistivity was increased to 2.93×10 14Ω, the reason is that comparative example 3 further removes the carbon black with good conductivity on the basis of comparative example 2, so the antistatic performance is further reduced, so the surface resistivity is further reduced.

[0032] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "include," "comprise," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a process, method, article, or apparatus comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0033] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or substitute equivalents for some of the technical features. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A method for preparing a high-temperature resistant and UV-resistant polycarbonate material, characterized in that: The following steps are involved: The polycarbonate resin, polyaryletherketone resin, flame retardant, antistatic modified carbon black, anti-ultraviolet agent, anti-dripping agent and dispersant are fully mixed for 8-15 minutes, melt blended, extruded into granules and extruded into films to obtain a polycarbonate film material.

2. The method for preparing a high-temperature resistant and UV-resistant polycarbonate material according to claim 1, characterized in that: The content of each component of the polycarbonate film material is as follows: by mass fraction, 60-75% polycarbonate resin, 10-15% polyaryletherketone resin, 10-13% flame retardant, 3-5% antistatic modified carbon black, 1-3% anti-ultraviolet agent, 0.5-0.7% anti-dripping agent, and the balance is dispersant; the anti-ultraviolet agent is 2-hydroxy-4-methoxybenzophenone; the anti-dripping agent is polytetrafluoroethylene; and the dispersant is pentaerythritol stearate.

3. The method for preparing a high-temperature resistant and UV-resistant polycarbonate material according to claim 1, characterized in that: The melt blending temperature is 250-270° C.; the extrusion granulation temperature is 270-300° C.; the extrusion film forming temperature is 280-300° C.; and the thickness of the polycarbonate film material is 0.2-0.3 mm.

4. The method for preparing a high-temperature resistant and UV-resistant polycarbonate material according to claim 1, characterized in that: The preparation process of flame retardant is: Step S1: adding 5-amino-1H-tetrazole and p-hydroxybenzaldehyde to ethanol, reflux reacting at 77-80° C. for 5-6 hours, cooling, filtering, washing, and drying after completion of the reaction to obtain a hydroxylated flame retardant; adding hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane to anhydrous toluene under a nitrogen atmosphere, stirring evenly, and then adding triethylamine, stirring and reacting at 70-75° C. for 13-15 hours, cooling, filtering, washing, and drying after completion of the reaction to obtain an amino flame retardant; Step S2: uniformly mixing a 75-80 wt% phytic acid aqueous solution and anhydrous ethanol to obtain a phytic acid reaction solution; dropwise adding the phytic acid reaction solution to an amino flame retardant, reacting at 5-10° C. for 6-8 hours; after the reaction is completed, adding a hydroxylated flame retardant, heating to 120-130° C. and stirring to react for 3.5-4.5 hours; and after the reaction is completed, cooling and drying to obtain a flame retardant.

5. The method for preparing a high-temperature resistant and UV-resistant polycarbonate material according to claim 4, characterized in that: When preparing hydroxylated flame retardants, the reaction molar ratio of 5-amino-1H-tetrazole and p-hydroxybenzaldehyde is (1.1-1.2):1; when preparing amination flame retardants, the molar mass ratio of hexachlorocyclotriphosphazene and 4,4'-diaminodiphenylmethane is (1.05-1.10):

6.

6. The method for preparing a high-temperature resistant and UV-resistant polycarbonate material according to claim 4, characterized in that: When preparing the flame retardant, the reaction molar ratio of the phosphate group in the phytic acid molecule, the amino group in the aminated flame retardant, and the hydroxyl group in the hydroxylated flame retardant in the phytic acid reaction solution is 1: (1.1-1.2):

1.

7. The method for preparing a high-temperature resistant and UV-resistant polycarbonate material according to claim 4, characterized in that: The preparation process of antistatic modified carbon black is: Step S1: adding γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and an ammonia solution to carbon black, ball milling the mixture at a rotation speed of 250-300 r / min for 10-15 hours, and drying the mixture after ball milling to obtain modified carbon black; Step S2: Under a nitrogen environment, the hydroxylated flame retardant, p-toluenesulfonic acid, and hydroquinone are added to toluene, stirred evenly, and then 3-mercaptopropionic acid is added dropwise at 110-120° C. After the addition is completed, stirring is continued for 5-7 hours. After the reaction is completed, the mixture is cooled, diluted, and rotary evaporated to obtain a thiolated flame retardant; Step S3: 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, a thiolated flame retardant, and a photoinitiator, 2-hydroxy-2-methyl-1-phenyl-1-propanone, are added to toluene, stirred evenly, and then modified carbon black is added. The stirring is continued for 30-50 minutes, and then the reaction is stirred under ultraviolet light for 50-60 minutes. After the reaction is completed, the antistatic modified carbon black is obtained by filtering, washing, and drying.

8. The method for preparing a high-temperature resistant and UV-resistant modified carbon black polycarbonate material according to claim 7, characterized in that: The mass volume ratio of carbon black, γ-(methacryloyloxy)propyltrimethoxysilane, distilled water, ethanol, and ammonia solution is (6-8) g: (0.10-0.12) g: (18-20) mL: 0.15 mL: 2 mL; when preparing the thiol flame retardant, the reaction mass ratio of the hydroxylated flame retardant, p-toluenesulfonic acid, hydroquinone, and 3-mercaptopropionic acid is (7.5-7.8): 0.25: 0.05:

4.

9. The method for preparing a high-temperature resistant and UV-resistant modified carbon black polycarbonate material according to claim 7, characterized in that: When preparing antistatic modified carbon black, the reaction mass ratio of 3-mercaptopropionic acid, 4-mercapto-1-butanesulfonic acid, mercapto flame retardant, photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propanone, and modified carbon black is 0.3:0.1:0.2:0.02:(1.5-2.0); the wavelength of ultraviolet light is 365-370nm.

10. A high temperature resistant and UV resistant polycarbonate material, characterized in that: Prepared according to the preparation method according to any one of claims 1 to 9.

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