Flame retardant nylon material and method for producing the same

Abstract

The application discloses a halogen-free flame-retardant nylon material, which comprises PA, a toughening agent, a P-series flame retardant, an N-series flame retardant and a modified polyhedral oligomeric silsesquioxane and derivative flame-retardant synergist. The modified polyhedral oligomeric silsesquioxane and derivative flame-retardant synergist contains boron elements, a cyclic structure R2 with a carbon-hydrogen ratio greater than 1 and two inorganic silicon cage cores. These structures form protective layers such as carbon layers, ceramic barrier layers, protective films or heat-insulating coke layers during combustion, greatly improving the drip-proof effect. At the same time, the heat and oxygen transmission are isolated, and the release of flammable gas is reduced. Multiple mechanisms work together to significantly improve the flame-retardant performance of the material. Further, the modified polyhedral oligomeric silsesquioxane and derivative flame-retardant synergist cooperates with the P-series flame retardant and the N-series flame retardant to synergistically flame-retardant, reduces the amount of flame retardant and improves the flame-retardant performance of the flame-retardant nylon material. The halogen-free flame-retardant nylon material provided by the application has excellent flame-retardant performance.

Description

Technical Field

[0001] This invention relates to the field of materials, specifically to a halogen-free flame-retardant nylon material. Background Technology

[0002] Polyhedral oligomeric silsesquioxane (POSS) is a special type of organic amorphous material. It is a polycyclic organic monomer composed of a silicon framework and its intercalated oxygen atoms. It is an inorganic-organic hybrid nanomaterial. The inorganic silicon cage core in POSS decomposes upon heating to form a dense ceramic barrier layer, which isolates the release of flammable gases and the entry of external heat into the interior, thereby delaying further decomposition of the material. POSS shows great application potential in the field of flame retardants.

[0003] Nylon (PA) is a highly polar polymer material. Its molecules can form hydrogen bonds, resulting in a high melting temperature and a narrow melting range, with a distinct melting point. It is widely used in various industries. However, because nylon lacks flame-retardant properties, flame-retardant modification has become a new direction for nylon materials. Currently, there are two main types of flame-retardant modification for nylon: chemical modification and physical modification. Chemical flame-retardant modification involves introducing flame-retardant components into the main chain or side chains of nylon through chemical reactions, thereby endowing the molecular chain itself with flame-retardant properties. Physical flame-retardant modification involves introducing flame-retardant components or flame retardants into the nylon matrix, followed by mixing and granulation to prepare flame-retardant modified nylon materials. Blending flame-retardant modification is the most convenient and widely used method. Melamine polyphosphate (MPP) is a relatively ideal flame retardant for nylon, with a chemical composition similar to nylon and good compatibility with the nylon matrix. Meanwhile, melamine polyphosphate molecules contain nitrogen and phosphorus elements, resulting in high flame retardant efficiency. Flame-retardant and antistatic nylon materials are produced by melt blending nylon with alkyl phosphinates and melamine polyphosphate as flame retardants and nylon as the matrix through an extruder. Although this method produces flame-retardant and antistatic nylon, the amount of melamine polyphosphate added as a flame retardant is large. The introduction of a large amount of flame retardant will reduce the mechanical properties of the material. Therefore, it is essential to develop a halogen-free flame-retardant PA material with high flame retardancy, crack resistance, excellent physical and mechanical properties, and anti-dripping properties. Summary of the Invention

[0004] In view of the shortcomings of the prior art, the present invention proposes a halogen-free flame-retardant nylon material, which aims to solve the problem of poor flame retardancy of current PA materials.

[0005] The above-mentioned objective of this invention is achieved through the following technical solution:

[0006] In a first aspect, the present invention provides a flame-retardant nylon material, wherein the raw materials of the halogen-free flame-retardant nylon material, by weight, comprise:

[0007] PA50-70 portions,

[0008] 1-5 parts toughening agent

[0009] 3-10 parts of P-series flame retardant

[0010] 3-10 parts of N-series flame retardant

[0011] 2-15 parts of modified polyhedral oligomeric silsesquioxanes and their derivatives as flame retardant synergists.

[0012] The structure of the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist is as follows:

[0013]

[0014] Wherein, R is a non-reactive group, such as isobutyl, isooctyl, ethyl, cyclohexyl, cyclopentyl, or phenyl, and R1 is n-propyl or phenylene;

[0015] R2 is a cyclic structure with a carbon-to-hydrogen ratio greater than 1, including at least one of benzofuran group and polycyclic aromatic group.

[0016] In some embodiments of the present invention, the benzofuran group includes at least one of the benzofuran group and the dibenzofuran group;

[0017] And / or, the polycyclic aromatic group includes at least one of a naphthalene ring group, anthracene ring group, phenanthrene ring group, acenaphthene ring group, fluorene ring group and perylene ring group.

[0018] In some embodiments of the present invention, the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist is prepared by dehydration reaction of compound 1 and compound 2 under the action of a catalyst, and the reaction route is as follows:

[0019]

[0020] In some embodiments of the present invention, the molar ratio of compound 1 to compound 2 is 2:1.

[0021] In some embodiments of the present invention, the preparation method of the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist includes the following steps:

[0022] Compound 1 was dissolved in an organic solvent, and an aqueous solution of compound 2 was added under the action of a catalyst. After catalytic reaction, the mixture was washed and dried to obtain the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist.

[0023] The organic solvent includes at least one of alcohols, aromatic hydrocarbons, aliphatic hydrocarbons, alicyclic hydrocarbons, ethers, ketones, and diol derivatives.

[0024] The catalyst includes at least one of acidic catalysts, metal catalysts, and basic catalysts.

[0025] In some embodiments of the present invention, the raw materials of the halogen-free flame-retardant nylon material, by weight, include:

[0026] PA50-70 portions,

[0027] 1-5 parts toughening agent

[0028] 3-7 parts of P-series flame retardant

[0029] 3-7 parts of N-series flame retardant

[0030] 2-15 parts of modified polyhedral oligomeric silsesquioxane and its derivatives flame retardant synergist.

[0031] In some embodiments of the present invention, the toughening agent includes at least one of ethylene-octene copolymer, ethylene-propylene copolymer, EMA, and EBA.

[0032] In some embodiments of the present invention, the P-based flame retardant includes an inorganic phosphorus flame retardant or an organic phosphorus flame retardant, wherein the inorganic phosphorus flame retardant includes at least one of red phosphorus, phosphate, and polyphosphate; the organic phosphorus flame retardant includes at least one of phosphate ester, phosphite ester, and phosphine oxide; and / or, the N-based flame retardant includes at least one of melamine urate, melamine phosphate, and melamine inorganic acid salt.

[0033] In some embodiments of the present invention, the raw materials of the halogen-free flame-retardant nylon material further include at least one of a lubricant and an antioxidant; wherein, by weight, the lubricant is 0.2-1 parts and the antioxidant is 0.5-2 parts.

[0034] In a second aspect, the present invention provides a method for preparing the above-mentioned halogen-free flame-retardant nylon material, comprising the following steps: mixing the raw materials evenly, extruding and granulating them through an extruder to obtain granules, i.e., the flame-retardant nylon material.

[0035] In some embodiments of the present invention, the raw materials further include at least one of lubricant and antioxidant.

[0036] This invention relates to a flame-retardant nylon material comprising PA, a toughening agent, a P-based flame retardant, an N-based flame retardant, and a modified polyhedral oligomeric silsesquioxane and its derivative flame-retardant synergist. In this invention, PA material, along with the modified POSS and its derivative flame-retardant synergist, the P-based flame retardant, and the N-based flame retardant, serve as the main components of the flame-retardant nylon material. These components work synergistically with each other. Because the modified polyhedral oligomeric silsesquioxane and its derivative flame-retardant synergist contains boron, a cyclic structure R2 with a carbon-to-hydrogen ratio greater than 1, and two inorganic silicon cage cores, the boron forms boric acid during combustion. The boric acid dehydrates and carbonizes the material surface, forming a carbon layer. The two inorganic silicon cage cores decompose upon heating, forming a dense ceramic barrier layer that isolates the release of combustible gases and the entry of external heat into the interior. The cyclic structure with a carbon-to-hydrogen ratio greater than 1... R2 has a high carbon-to-hydrogen ratio, and its benzofuran and polycyclic aromatic groups contain a large amount of carbon. During combustion, this abundant carbon forms a glassy protective film or an insulating coke layer. These protective films or coke layers isolate air, prevent heat transfer, and reduce the release of flammable gases. These structures, through the formation of protective layers such as carbon layers, ceramic barrier layers, protective films, or insulating coke layers during combustion, significantly improve the anti-dripping effect. Simultaneously, they isolate heat and oxygen transfer, reducing the release of flammable gases. The combined effect of these multiple mechanisms significantly enhances the flame-retardant properties of the material. During combustion, the Si element reacts with the C in the R2 groups. The element can rapidly react to generate a large number of Si-C bonds. Simultaneously, the boron element can form a glassy film on the surface of the flame-retardant nylon material, and the generated boric acid rapidly dehydrates the polymer, producing a char layer. The boron element in the modified POSS and its derivative synergistic flame retardants can also coordinate with the phosphorus element in the system to produce a synergistic effect, thereby improving the flame-retardant effect. By adding modified POSS and its derivative synergistic flame retardants in synergy with P-based and N-based flame retardants, a relatively hard char layer is rapidly generated to prevent the flame-retardant nylon from dripping during combustion and to isolate it from air, thus improving the flame retardancy of the nylon material. The P-based flame retardant provides the acid source, while the N-based flame retardant... The modified POSS and its derivatives provide a gas source, while the synergistic flame retardant provides an abundant carbon source, enabling the P-based and N-based flame retardants to exert stronger flame retardant properties. As a result, the prepared halogen-free flame-retardant nylon material can maintain the original good processing performance, elasticity, and flame retardant properties of thermoplastic elastomers, while improving the crack resistance, flame retardancy, and physical and mechanical properties of the halogen-free flame-retardant nylon material. The modified POSS and its derivatives are colorless viscous liquids, and their addition to the halogen-free flame-retardant nylon material has little impact on the performance of the flame-retardant nylon material. Moreover, a high addition amount is not required to obtain a halogen-free flame-retardant nylon material with excellent flame retardant properties. Attached Figure Description

[0037] Figure 1 This is a molecular structure diagram of the modified POSS flame retardant synergist 1 of the present invention;

[0038] Figure 2This is a molecular structure diagram of the modified POSS flame retardant synergist 2 of the present invention. Detailed Implementation

[0039] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It should be understood that the following embodiments are only used to explain the present invention and are not intended to limit the present invention.

[0040] Unless otherwise specified, all technical and scientific terms used herein have their usual meaning within the field to which the subject matter is claimed.

[0041] PA: Polyamide, also known as nylon or polyamide fiber, is a general term for thermoplastic resins containing repeating amide groups (-NHCO-) ​​in their molecular chains. It includes aliphatic PA, aliphatic-aromatic PA, and aromatic PA. Aliphatic PA has the most varieties and the largest production volume, and is mainly used in the automotive, electrical and electronic, transportation, and machinery manufacturing industries to manufacture various bearings, gears, oil pipes, oil reservoirs, protective covers, and other components.

[0042] EMA: Ethylene-methyl acrylate copolymer, is a copolymer of ethylene, methacrylate, and auxiliary monomers. EMA is transparent, low-density, and elastic, while also exhibiting excellent waterproof, chemical stability, heat resistance, and insulation properties. This material has a wide range of applications, primarily in food packaging, pharmaceutical packaging, electronic and electrical equipment, construction, and automotive parts.

[0043] EBA: Ethylene Butyl Acrylate, is a high-performance polymer material with excellent reactivity, crystallinity, and flowability. It is flexible, has a high melting point, high thermal stability, good heat-sealing properties, and good low-temperature impact resistance. It also has strong compatibility with pigments and inorganic fillers and good compatibility with a variety of polymers. It is widely used in adhesives, food packaging, films, wires and cables, and plastic modification.

[0044] POE: Polyolefin elastomer is a thermoplastic elastomer that is polymerized in situ using metallocene catalysts to polymerize ethylene and octene. It has excellent toughness, processability, weather resistance, heat aging resistance and UV resistance. Its molecular structure gives it a narrow relative molecular mass distribution and a uniform short branch distribution, resulting in excellent physical and mechanical properties (such as high elasticity, high strength and high elongation) and good low-temperature performance.

[0045] PE: Polyethylene, is a thermoplastic resin polymerized from ethylene monomers, possessing excellent low-temperature resistance and chemical stability. PE materials are widely used in various fields, including packaging, containers, pipes, wires and cables, etc. Due to its excellent chemical stability and wide applicability, PE materials are commonly used in food packaging, cling film, water pipes, bubble wrap, etc.

[0046] Polyhedral oligomeric silsesquioxane (POSS) is a special type of organic amorphous material. It is a polycyclic organic monomer composed of a silicon framework and its intercalated oxygen atoms. It is an inorganic-organic hybrid nanomaterial. The inorganic silicon cage core in POSS decomposes upon heating to form a dense ceramic barrier layer, which isolates the release of flammable gases and the entry of external heat into the interior, thereby delaying further decomposition of the material. POSS shows great application potential in the field of flame retardants.

[0047] Flame-retardant nylon (PA) is a highly polar polymer material. Its molecules can form hydrogen bonds, resulting in a high melting temperature and a narrow melting range, along with a distinct melting point. It is widely used in various industries. However, since nylon itself lacks flame-retardant properties, flame-retardant modification has become a new direction for nylon materials. Currently, there are two main types of flame-retardant modification for nylon: chemical modification and physical modification. Chemical flame-retardant modification involves introducing flame-retardant components into the main chain or side chains of nylon through chemical reactions, thereby endowing the molecular chain itself with flame-retardant properties. Physical flame-retardant modification involves introducing flame-retardant components or flame retardants into the nylon matrix, followed by mixing and granulation to prepare flame-retardant modified nylon materials. Blending flame-retardant modification is the most convenient and widely used method. Melamine polyphosphate (MPP) is a relatively ideal flame retardant for nylon, with a chemical composition similar to nylon and good compatibility with the nylon matrix. Meanwhile, melamine polyphosphate molecules contain nitrogen and phosphorus elements, resulting in high flame retardant efficiency. Flame-retardant and antistatic nylon materials are produced by melt blending nylon with alkyl phosphinates and melamine polyphosphate as flame retardants and nylon as the matrix through an extruder. Although this method produces flame-retardant and antistatic nylon, the amount of melamine polyphosphate added as a flame retardant is large. The introduction of a large amount of flame retardant will reduce the mechanical properties of the material. Therefore, it is essential to develop a halogen-free PA material with high flame retardancy, crack resistance, excellent physical and mechanical properties, and anti-dripping properties.

[0048] To address the aforementioned problems, in a first aspect, this invention provides a halogen-free flame-retardant nylon material, wherein the raw materials of the flame-retardant nylon material, by weight, comprise:

[0049] PA50-70 portions,

[0050] 1-5 parts toughening agent

[0051] 3-10 parts of P-series flame retardant

[0052] 3-10 parts of N-series flame retardant

[0053] 2-15 parts of modified polyhedral oligomeric silsesquioxanes and their derivatives as flame retardant synergists.

[0054] The structure of the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist is as follows:

[0055]

[0056] Wherein, R is a non-reactive group, such as isobutyl, isooctyl, ethyl, cyclohexyl, cyclopentyl, or phenyl, and R1 is n-propyl or phenylene;

[0057] R2 is a cyclic structure with a carbon-to-hydrogen ratio greater than 1, including at least one of benzofuran group and polycyclic aromatic group.

[0058] Understandably, when R1 connected to Si in the inorganic silicon cage core is a phenylene ring, the phenylene ring contains a benzene ring with a high carbon-hydrogen ratio and high carbon content. During combustion, it works together with the large amount of Si in the inorganic silicon cage core to further improve the flame retardant properties of the inorganic silicon cage core, thereby improving the flame retardant properties of the modified polyhedral oligomeric silsesquioxane flame retardant synergist.

[0059] This invention relates to a halogen-free flame-retardant nylon material comprising PA, a toughening agent, a P-based flame retardant, an N-based flame retardant, and a modified polyhedral oligomeric silsesquioxane and its derivative flame-retardant synergist. In this invention, PA material, along with the modified POSS and its derivative flame-retardant synergist, the P-based flame retardant, and the N-based flame retardant, serve as the main components of the flame-retardant nylon material. These components work synergistically with each other. Because the modified polyhedral oligomeric silsesquioxane and its derivative flame-retardant synergist contains boron, a cyclic structure R2 with a carbon-to-hydrogen ratio greater than 1, and two inorganic silicon cage cores, the boron forms boric acid during combustion. The boric acid dehydrates and carbonizes the material surface, forming a carbon layer. The two inorganic silicon cage cores decompose upon heating, forming a dense ceramic barrier layer that isolates the release of combustible gases and the entry of external heat. The cyclic structure with a carbon-to-hydrogen ratio greater than 1... Structure R2 has a high carbon-to-hydrogen ratio. The benzofuran and polycyclic aromatic groups contain a large amount of carbon. During combustion, this abundant carbon forms a glassy protective film or a heat-insulating coke layer. These protective films or coke layers isolate air, prevent heat transfer, and reduce the release of flammable gases. Through the formation of protective layers such as carbon layers, ceramic barrier layers, protective films, or heat-insulating coke layers during combustion, the anti-dripping effect is greatly improved. Simultaneously, it isolates heat and oxygen transfer and reduces the release of flammable gases. These multiple mechanisms work together to significantly improve the flame-retardant properties of the material. During combustion, Si elements react with R2... The carbon element in the group can rapidly react to generate a large number of Si-C bonds. Simultaneously, the boron element can form a glassy film on the surface of the flame-retardant nylon material, and the generated boric acid rapidly dehydrates the polymer, producing a char layer. The boron element in the modified POSS and its derivative synergistic flame retardants can also coordinate with the phosphorus element in the system to produce a synergistic effect, thereby improving the flame-retardant effect. By adding modified POSS and its derivative synergistic flame retardants in synergy with P-based and N-based flame retardants, a relatively hard char layer is rapidly generated to prevent the flame-retardant nylon from dripping during combustion and to isolate it from air, thus improving the flame retardancy of the flame-retardant nylon material. The P-based flame retardants provide the acid... The N-series flame retardants provide a gas source, while the modified POSS and its derivative synergistic flame retardants provide an abundant carbon source, enabling the P-series and N-series flame retardants to exert stronger flame retardant properties. As a result, the prepared flame-retardant nylon material can maintain the original good processing performance, elasticity, and flame retardant properties of thermoplastic elastomers, while improving the crack resistance, flame retardancy, and physical and mechanical properties of the flame-retardant nylon material. The modified POSS and its derivative flame retardant synergists are colorless viscous liquids, and their addition to the flame-retardant nylon material has little impact on the performance of the flame-retardant nylon material. Moreover, a high addition amount is not required to obtain flame-retardant nylon material with excellent flame retardant properties.

[0060] Furthermore, the benzofuran group includes at least one of the benzofuran group and the dibenzofuran group.

[0061] Phenyl groups have a high carbon-to-hydrogen ratio and a high carbon content, which can slow down the spread of flames during combustion. They can also self-extinguish quickly after the flames are removed, reducing the duration and intensity of combustion. Furan groups, while having a high carbon content, also contain oxygen elements that do not participate in combustion. The combination of these two groups forms benzofuran groups or dibenzofuran groups, which have both a high carbon-to-hydrogen ratio and low combustion elements. Together, they form a glassy protective film or heat-insulating coke layer during combustion. These protective films or coke layers can isolate air, prevent heat transfer, reduce the content of combustibles, and indirectly promote char formation.

[0062] In some embodiments, R2 is a benzofuran group.

[0063] In some embodiments, the polycyclic aromatic group includes at least one of a naphthalene ring group, anthracene ring group, phenanthrene ring group, acenaphthene ring group, fluorene ring group, and perylene ring group.

[0064] Naphthyl ring groups, anthracene ring groups, phenanthrene ring groups, acenaphthene ring groups, fluorene ring groups, and perylene ring groups have a high hydrocarbon ratio and contain a large amount of carbon, making them more likely to form a glassy protective film or heat-insulating coke layer during combustion.

[0065] In some embodiments, R2 is a naphthalene ring group.

[0066] Furthermore, the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist was prepared by dehydration reaction of compound 1 and compound 2 under the action of a catalyst, and the reaction route is as follows:

[0067]

[0068] Furthermore, the molar ratio of compound 1 to compound 2 in the above reaction process is 2:1.

[0069] Compound 1, a polyhedral oligomeric silsesquioxane, has a relatively large spatial structure. During the reaction, compound 2 needs to have sufficiently small steric hindrance to react with compound 1 and yield compound 3, a modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist. In the reaction, each compound 2 is connected to two compounds 1, meaning the molar ratio of compound 1 to compound 2 is 2:1. This ensures sufficient space for compound 3 and achieves structural stability. Compound 2 contains two hydroxyl groups. The two hydroxyl groups of one compound 2 react with one amino group from each of the two compounds 1 to undergo a dehydration reaction, yielding compound 3. The overall reaction requires only a single substance, is simple to operate, and is easy to implement.

[0070] In some embodiments, compound 1 is aminopropylheptaisobutyl cage-like polysilsesquioxane.

[0071] In some embodiments, compound 1 is aminophenyl heptaisobutyl cage-like polysilsesquioxane.

[0072] In some embodiments, compound 2 is benzo[B]naphtho[2,3-D]furan-2-hydroxyboronic acid.

[0073] In some embodiments, compound 2 is dibenzofuran-4-boronic acid.

[0074] In some embodiments, the structural formula of compound 3 is:

[0075]

[0076] The following is counted as modified POSS flame retardant synergist 1.

[0077] In some embodiments, the structural formula of compound 3 is:

[0078]

[0079] The following is counted as modified POSS flame retardant synergist 2.

[0080] Furthermore, the preparation method of compound 3 includes the following steps:

[0081] Compound 1 was dissolved in an organic solvent, and an aqueous solution of compound 2 was added under the action of a catalyst. After catalytic reaction, the mixture was washed and dried to obtain compound 3.

[0082] The organic solvents include at least one of alcohols, aromatic hydrocarbons, aliphatic hydrocarbons, alicyclic hydrocarbons, ethers, ketones, and diol derivatives;

[0083] Catalysts include at least one of acidic catalysts, metal catalysts, and basic catalysts.

[0084] In some embodiments, the catalyst is acetic acid.

[0085] In some implementations, the solvent is ethanol.

[0086] Furthermore, the raw materials for flame-retardant nylon materials, by weight, include:

[0087] PA50-70 portions,

[0088] 1-5 parts toughening agent

[0089] 3-7 parts of P-series flame retardant

[0090] 3-7 parts of N-series flame retardant

[0091] 2-15 parts of modified polyhedral oligomeric silsesquioxane and its derivatives flame retardant synergist.

[0092] Reducing the amount of P-series and N-series flame retardants can further improve the mechanical properties of flame-retardant nylon materials.

[0093] Furthermore, the toughening agent includes at least one of ethylene-octene copolymer, ethylene-propylene copolymer, EMA, and EBA.

[0094] Toughening agents can increase the flexibility of adhesive films, significantly increasing the flexibility of materials and making them less prone to breakage under external forces. They can also improve the impact resistance and fatigue resistance of materials, effectively prevent crack propagation, and thus extend the service life of materials. Furthermore, they can weaken the interaction between polymer molecular chains, reduce the friction between molecular chains, and increase the mobility of polymer molecular chains, thereby improving the processing fluidity and molding performance of materials.

[0095] Understandably, toughening agents include, but are not limited to, ethylene-octene copolymers, ethylene-propylene copolymers, EMA, and EBA.

[0096] Furthermore, the P-series flame retardants include inorganic phosphorus flame retardants or organic phosphorus flame retardants. Inorganic phosphorus flame retardants include at least one of red phosphorus, phosphates, and polyphosphates; organic phosphorus flame retardants include at least one of phosphate esters, phosphites, and phosphine oxides; and / or, the N-series flame retardants include at least one of melamine urate, melamine phosphate, and melamine inorganic acid salts.

[0097] Understandably, phosphorus-based flame retardants include, but are not limited to, aluminum hypophosphite, calcium hypophosphite, aluminum diethylphosphite, aluminum methyl ethyl hypophosphite, and aluminum phenyl hypophosphite.

[0098] In some embodiments, the P-based flame retardant is preferably aluminum diethylphosphinate.

[0099] In some embodiments, the N-based flame retardant is preferably melamine cyanurate.

[0100] Furthermore, the raw materials for flame-retardant nylon materials also include at least one of lubricant and antioxidant; wherein, by weight, the raw materials are 0.2-1 parts lubricant and 0.5-2 parts antioxidant.

[0101] In some embodiments, antioxidants include, but are not limited to, asymmetric hindered phenolic antioxidants, aromatic amine antioxidants, thioether antioxidants, and phosphite antioxidants.

[0102] Hindered phenolic antioxidants include, but are not limited to, antioxidant 1010 (pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]), BHT (2,6-di-tert-butyl-p-cresol), and antioxidant 1076 (octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate).

[0103] Aromatic amine antioxidants include, but are not limited to, diphenylamine, p-phenylenediamine, and dihydroquinoline and their derivatives or polymers, such as antioxidant 445 (4,4'-bis(α.α-dimethylbenzyl)diphenylamine).

[0104] Thioether antioxidants include, but are not limited to, DLTP (dilauryl thiodipropionate), DSTDP (distearate thiodipropionate), and DSTP (octadecyl thiodipropionate).

[0105] Phosphite antioxidants include, but are not limited to, antioxidant 168 (tris[2,4-di-tert-butylphenyl]phosphite), antioxidant 618 (pentaerythritol diphosphite bis(octadecyl)ester), and antioxidant 626 (bis[2,4-di-tert-butylphenyl]pentaerythritol diphosphite).

[0106] Adding antioxidants can improve the antioxidant properties and aging resistance of polymer materials, thereby extending their service life.

[0107] In some embodiments, the lubricant includes, but is not limited to, PTFE powder, zinc stearate, magnesium stearate, silicone, calcium stearate, or ethylene bis-stearamide. Adding a lubricant helps to promote more uniform mixing of various raw materials, improves the flowability of the polymer resin, reduces the coefficient of friction, makes the surface of the product smoother, improves processing efficiency, and also improves the transparency and gloss of the plastic.

[0108] In a second aspect, the present invention provides a method for preparing the above-mentioned flame-retardant nylon material, comprising the following steps: mixing raw materials, namely PA, toughening agent, P-based flame retardant, N-based flame retardant and modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist, uniformly, and extruding and granulating the mixture through an extruder to obtain granules, namely halogen-free flame-retardant nylon material.

[0109] Furthermore, the raw materials also include at least one of lubricants and antioxidants.

[0110] The following specific embodiments and data explain the content of the present invention.

[0111] Information on the raw materials involved in the specific implementation method is shown in Table 1:

[0112] Table 1 Information on raw materials for the examples and comparative examples

[0113]

[0114] The flame-retardant nylon materials prepared in the examples and comparative examples were injection molded or pressed into sheets, and their flame retardancy rating, oxygen index, tensile strength, and notched impact strength were tested according to the following standards:

[0115] (1) Flame retardancy rating test

[0116] According to GB / T 5455-2014, the samples were subjected to vertical flammability testing. The samples were cut to the specified dimensions and tested under the specified conditions, and key parameters such as flammability time and residual substances were monitored.

[0117] (2) Does it drip when testing flame retardancy rating?

[0118] To determine whether dripping occurs during flame retardancy rating testing, the test was conducted according to UL94 standards. The sample thickness was 3mm, and the test temperature was 23±2℃. The test was performed using the UL94 vertical burning test apparatus from Jiangsu Zhengrui Taibang Electronics Co., Ltd.

[0119] (3) Oxygen index

[0120] According to GB / T 2406.2-2009, the sample size was prepared according to Type IV sample size. The test was conducted according to Method A - Top Surface Ignition Method. The oxygen index tester was performed using a device from Nanjing Jiangning District Fangshang Analytical Instrument Equipment Factory.

[0121] (4) Tensile strength

[0122] The test was conducted according to Clause 9 of GB 1040—2008, with a test temperature of 23±2℃. The tensile test used a standard dumbbell-shaped specimen with a tensile speed of 250 mm / min. The tensile strength of five specimens was tested using a micro-controlled electronic universal tensile testing machine from Dongguan High-Speed ​​Railway Testing Co., Ltd., and the average value of the results was taken.

[0123] (5) Notched impact strength

[0124] The test was conducted according to the ISO 179-92 standard. The sample was prepared according to the standard requirements, usually in the shape of a cuboid. The key parameters were set as follows: impact velocity, which is usually set to 3.5 m / s; pendulum energy, which can be selected as 1 J, 2.75 J or 5.5 J; pendulum swing angle, which is 150°; and distance from the center of the pendulum to the impact blade, which is 335 mm. The test was conducted 5 times and the average value of the results was taken.

[0125] The test results are detailed in Table 3.

[0126] Example 1:

[0127] 2 mol of aminopropyl heptaisobutyl cage-like polysilsesquioxane was dissolved in 100 ml of tetrahydrofuran solution. 0.2 mol of acetic acid catalyst was added to the solution, and 1 mol of benzo[B]naphtho[2,3-D]furan-2-hydroxyboric acid was added under stirring. The reaction was stirred for 2-4 h, then stopped. The mixture was then rotary evaporated under reduced pressure, washed with water, and dried to obtain modified POSS flame retardant synergist 1.

[0128] 70 parts PA, 5 parts POE, 10 parts modified POSS flame retardant synergist, 3 parts diethyl aluminum hypophosphite, 3 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0129] Example 2:

[0130] The preparation method is the same as in Example 1, except that:

[0131] 50 parts PA, 1 part POE, 12 parts modified POSS flame retardant synergist, 5 parts diethyl aluminum hypophosphite, 3 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0132] Example 3:

[0133] The preparation method is the same as in Example 1, except that:

[0134] 70 parts PA, 3 parts POE, 2 parts modified POSS flame retardant synergist, 1 part diethyl aluminum hypophosphite, 10 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0135] Example 4:

[0136] The preparation method is the same as in Example 1, except that:

[0137] 70 parts PA, 4 parts POE, 10 parts modified POSS flame retardant synergist, 10 parts diethyl aluminum hypophosphite, 9 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0138] Example 5:

[0139] The preparation method is the same as in Example 1, except that:

[0140] 70 parts PA, 5 parts POE, 12 parts modified POSS flame retardant synergist, 7 parts diethyl aluminum hypophosphite, 7 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0141] Example 6:

[0142] The preparation method is the same as in Example 1, except that:

[0143] 50 parts PA, 1 part POE, 12 parts modified POSS flame retardant synergist, 7 parts diethyl aluminum hypophosphite, 7 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0144] Example 7:

[0145] The preparation method is the same as in Example 1, except that:

[0146] 70 parts PA, 4 parts POE, 10 parts modified POSS flame retardant synergist, 5 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0147] Example 8:

[0148] The preparation method is the same as in Example 1, except that:

[0149] 73 parts PA, 1 part POE, 10 parts modified POSS flame retardant synergist, 5 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0150] Example 9:

[0151] 2 mol of aminopropyl heptaisobutyl cage-like polysilsesquioxane was dissolved in 100 ml of tetrahydrofuran solution. 0.2 mol of acetic acid catalyst was added to the solution, and 1 mol of dibenzofuran-3-boric acid was added under stirring. The reaction was stirred for 2-4 h, then stopped. The mixture was then rotary evaporated under reduced pressure, washed with water, and dried to obtain modified POSS flame retardant synergist 2.

[0152] 70 parts PA, 4 parts POE, 10 parts modified POSS flame retardant synergist, 2 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0153] Comparative Example 1:

[0154] The preparation method is the same as in Example 1, except that:

[0155] 70 parts PA, 4 parts POE, 14 parts modified POSS flame retardant synergist, 3 parts diethyl aluminum hypophosphite, 3 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0156] Comparative Example 2:

[0157] 70 parts PA, 4 parts POE, 10 parts aluminum diethyl phosphite, 10 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant are mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material is obtained.

[0158] Comparative Example 3:

[0159] The preparation method is the same as in Example 1, except that:

[0160] 70 parts PA, 4 parts POE, 10 parts modified POSS flame retardant synergist, 10 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame retardant nylon preform. After drying at 80℃, a high flame retardant, crack-resistant, halogen-free flame retardant nylon material was obtained.

[0161] Comparative Example 4:

[0162] The preparation method is the same as in Example 1, except that:

[0163] 70 parts PA, 4 parts POE, 10 parts modified POSS flame retardant synergist, 10 parts diethyl aluminum hypophosphite, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0164] Comparative Example 5:

[0165] The preparation method is the same as in Example 10, except that:

[0166] 70 parts PA, 4 parts POE, 20 parts modified POSS flame retardant synergist, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame retardant nylon preform. After drying at 80℃, a high flame retardant, crack-resistant, halogen-free flame retardant nylon material was obtained.

[0167] Comparative Example 6:

[0168] 70 parts PA, 4 parts POE, 20 parts aluminum diethyl phosphite, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0169] Comparative Example 7:

[0170] 70 parts PA, 4 parts POE, 20 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant are mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material is obtained.

[0171] Comparative Example 8:

[0172] 70 parts PA, 4 parts POE, 10 parts benzo[B]naphtho[2,3-D]furan-2-hydroxyboric acid flame retardant, 5 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0173] Comparative Example 9:

[0174] 70 parts PA, 4 parts POE, 10 parts aminopropyl heptaisobutyl cage-like polysilsesquioxane flame retardant, 5 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, 0.5 parts antioxidant, and 0.3 parts light stabilizer were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain a thermoplastic polyester elastomer flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free thermoplastic polyester elastomer flame-retardant nylon material was obtained.

[0175] Comparative Example 10:

[0176] 70 parts PA, 4 parts POE, 5 parts aminopropyl heptaisobutyl cage-like polysilsesquioxane flame retardant, 5 parts aminopropyl heptaisobutyl cage-like polysilsesquioxane flame retardant, 5 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, 0.5 parts antioxidant, and 0.3 parts light stabilizer were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain a thermoplastic polyester elastomer flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free thermoplastic polyester elastomer flame-retardant nylon material was obtained.

[0177] Comparative Example 11:

[0178] 2 mol of aminopropyl heptaisobutyl cage-like polysilsesquioxane was dissolved in 100 ml of tetrahydrofuran solution. 0.2 mol of acetic acid catalyst was added to the solution, followed by the addition of 1 mol of methylboric acid under stirring. The reaction was stirred for 2-4 hours, then stopped. The mixture was then rotary evaporated under reduced pressure, washed with water, and dried to obtain methylboric acid-modified POSS flame retardant.

[0179] 70 parts PA, 4 parts POE, 10 parts methylboric acid modified POSS flame retardant, 5 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0180] Comparative Example 12:

[0181] 2 mol of aminopropylheptaisobutyl cage-like polysilsesquioxane was dissolved in 100 ml of tetrahydrofuran solution. 0.2 mol of acetic acid catalyst was added to the solution, followed by the addition of 1 mol of phenylboronic acid under stirring. The reaction was stirred for 2-4 hours, then stopped. The mixture was then rotary evaporated under reduced pressure, washed with water, and dried to obtain phenylboronic acid-modified POSS flame retardant.

[0182] 70 parts PA, 5 parts POE, 10 parts phenylboronic acid modified POSS flame retardant, 5 parts diethyl aluminum hypophosphite, 5 parts MCA flame retardant, 0.5 parts lubricant, and 0.5 parts antioxidant were mixed evenly and granulated by twin-screw extrusion at 260℃ to obtain flame-retardant nylon preform. After drying at 80℃, a high flame-retardant, crack-resistant, halogen-free flame-retardant nylon material was obtained.

[0183] Table 2 summarizes the components and key preparation variables of Examples 1-9 and Comparative Examples 1-12. Table 2: Component Tables of Examples 1-9 and Comparative Examples 1-12 of the Present Invention.

[0184] Table 2. Examples and Comparative Formulations of the Invention

[0185]

[0186] According to the specifications of GB / T 1040-2008, GB / T 5455, GB / T 2406.2, UL94 and ISO 179-92, the flame-retardant nylon materials in Examples 1-9 and Comparative Examples 1-12 were tested for tensile strength, flame retardancy rating, oxygen index, whether they dripped during combustion, and notched impact strength. The test results are recorded in Table 3 below:

[0187] Table 3 Performance test table of Examples 1-9 and Comparative Examples 1-12 of the present invention

[0188] Tensile strength / MPa Flame retardant rating Oxygen index (%) Does it drip? Notched impact strength / kJ / m² Example 1 95 V0 25.5 no 13.8 Example 2 64 V0 27 no 11 Example 3 98 V0 26 no 11.8 Example 4 75 V0 29 no 12.2 Example 5 82 V0 31 no 12 Example 6 60 V0 33 no 9.4 Example 7 88 V0 30 no 12.6 Example 8 73 V0 29 no 8.6 Example 9 86 V0 30 no 12.2 Comparative Example 1 70 V2 22 no 12.1 Comparative Example 2 56 V2 24 yes 7.4 Comparative Example 3 86 V1 26 no 12.3 Comparative Example 4 55 V1 27 no 7.2 Comparative Example 5 62 V2 23 no 10.5 Comparative Example 6 57 V2 25 yes 6.4 Comparative Example 7 64 V2 24 yes 9.4 Comparative Example 8 90 V0 27 yes 12.8 Comparative Example 9 86 V2 25 yes 11.9 Comparative Example 10 86 V0 29 yes 12.4 Comparative Example 11 89 V2 24 yes 13 Comparative Example 12 87 V0 28 yes 12

[0189] As can be seen from Table 3, the flame-retardant nylon injection-molded sheets of Examples 1-9 have high flame-retardant performance, and all of them reach the V0 level. The V0 level test shows that none of them drip, and the oxygen index is >25.By comparing Examples 1 and 5, and Examples 2 and 6, it can be seen that increasing the amount of P-based and N-based flame retardants improves the flame retardant performance of the prepared flame-retardant nylon material, but reduces its tensile strength and notched impact strength. This indicates that while excessive flame retardants can improve the flame retardant performance of the material, they can also reduce the physical and mechanical properties of the material matrix, resulting in poor plastic deformation ability and easy breakage. By comparing Examples 7 and 9, the structural type of the modified POSS flame retardant synergist added was changed. By comparing the experimental data in the table above, the tensile strength, flame retardant rating, oxygen index, dripping during combustion, and notched impact strength of Examples 7 and 9 were significantly improved. The test results were basically the same, indicating that in this invention, changes in the substrate and the type of modified POSS flame retardant synergist in the system do not affect the performance of the prepared thermoplastic polyester elastomer material. In Comparative Example 1, compared to Example 7, the addition of excessive modified POSS flame retardant synergist 1 actually reduced the physical and mechanical properties and flame retardant properties of the prepared flame-retardant nylon material. When excessive modified POSS flame retardant synergist is added, it cannot form an effective flame retardant system with P-based and N-based flame retardants, reducing the physical and mechanical properties of the system and also resulting in poor plastic deformation ability of the prepared material. In Comparative Examples 2-7, by changing the proportions of the added modified POSS flame retardant synergist, P-based flame retardant, and N-based flame retardant, the following results were obtained: When any of the modified POSS flame retardant synergist, P-type flame retardant, and N-type flame retardant is missing from the system, the flame retardant performance of the prepared flame-retardant nylon material will decrease, and varying degrees of dripping will occur during combustion. Its physical and mechanical properties will also be poor. In this invention, the modified POSS flame retardant synergist, P-type flame retardant, and N-type flame retardant need to work together synergistically to form a glass film and carbon layer on the material surface, thereby improving the flame retardant effect, achieving the anti-dripping effect during combustion, and improving the physical and mechanical properties of the material. In Comparative Examples 8-10, the modified POSS flame retardant synergist was changed to its reactant, and the experimental data of the three could not achieve the anti-dripping effect during combustion. Moreover, the flame retardant performance of Comparative Example 9 was poor. In Comparative Examples 11 and 12, equal parts of methylboronic acid-modified POSS flame retardant synergist and phenylboronic acid-modified POSS flame retardant synergist were added to replace the modified POSS flame retardant synergist of the present invention. The methylboronic acid-modified POSS flame retardant synergist lacks an R2 group with a carbon-hydrogen ratio greater than 1, while the phenylboronic acid-modified POSS flame retardant synergist contains a benzene ring structure. However, the flame retardant rating of Comparative Example 11 is V2, and it cannot achieve the anti-dripping effect during combustion. The flame retardant performance of Comparative Example 12 is relatively high, but it also cannot achieve the anti-dripping effect during combustion. This indicates that the modified POSS flame retardant synergist containing a benzene ring structure cannot generate an effective char layer during combustion to achieve the anti-dripping effect during combustion.

[0190] Therefore, this invention verifies that modifying POSS flame retardant synergist improves the flame retardancy of flame-retardant nylon materials, giving them excellent physical and mechanical properties and excellent anti-dripping effect during combustion. It has extremely high industrial value and can be widely applied and promoted.

[0191] The above are merely preferred embodiments of the present invention and do not limit the patent scope of the present invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the patent protection scope of the present invention.

Claims

1. A flame-retardant nylon material, characterized in that, The raw materials of the flame-retardant nylon material, by weight, include: PA50-70 portions, 1-5 parts toughening agent 3-10 parts of P-series flame retardant 3-10 parts of N-series flame retardant 2-12 parts of modified polyhedral oligomeric silsesquioxanes and their derivatives as flame retardant synergists. The structure of the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist is as follows: Wherein, R is isobutyl, isooctyl, ethyl, cyclohexyl, cyclopentyl or phenyl, and R1 is propylene or phenylene; R2 is a 2-benzo[B]naphtho[2,3-D]furan group or a 3-dibenzofuran group; Wherein, the P-series flame retardant is an inorganic phosphorus flame retardant or an organic phosphorus flame retardant, wherein the inorganic phosphorus flame retardant is at least one of red phosphorus, phosphate, and polyphosphate, and the organic phosphorus flame retardant is at least one of phosphate ester, phosphite ester, and phosphine oxide; and the N-series flame retardant is at least one of melamine inorganic acid salts.

2. The flame-retardant nylon material as described in claim 1, characterized in that, The modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist were prepared by dehydration reaction of compound 1 and compound 2 under the action of a catalyst, and the reaction route is as follows: 。 3. The flame-retardant nylon material as described in claim 2, characterized in that, The molar ratio of compound 1 to compound 2 is 2:

1.

4. The flame-retardant nylon material as described in claim 2, characterized in that, The preparation method of the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist includes the following steps: Compound 1 was dissolved in an organic solvent, and an aqueous solution of compound 2 was added under the action of a catalyst. After catalytic reaction, the mixture was washed and dried to obtain the modified polyhedral oligomeric silsesquioxane and its derivative flame retardant synergist. The organic solvent is at least one of alcohols, aromatic hydrocarbons, aliphatic hydrocarbons, alicyclic hydrocarbons, ethers, ketones, and diol derivatives. The catalyst is at least one of acidic catalysts, metal catalysts, and basic catalysts.

5. The flame-retardant nylon material as described in claim 1, characterized in that, The raw materials of the flame-retardant nylon material, by weight, include: PA50-70 portions, 1-5 parts toughening agent 3-7 parts of P-series flame retardant 3-7 parts of N-series flame retardant 2-12 parts of modified polyhedral oligomeric silsesquioxane and its derivatives flame retardant synergist.

6. The flame-retardant nylon material as described in claim 1, characterized in that, The toughening agent is at least one of ethylene-octene copolymer, ethylene-propylene copolymer, EMA, and EBA.

7. The flame-retardant nylon material as described in claim 1, characterized in that, The raw materials for the flame-retardant nylon material also include at least one of a lubricant and an antioxidant; wherein, by weight, the lubricant comprises 0.2-1 parts and the antioxidant comprises 0.5-2 parts.

8. A method for preparing the flame-retardant nylon material as described in claim 1, characterized in that, The process includes the following steps: mixing the raw materials evenly, extruding and granulating them through an extruder to obtain granules, which are the flame-retardant nylon materials.

9. The method for preparing the flame-retardant nylon material as described in claim 8, characterized in that, The raw materials also include at least one of lubricant and antioxidant.

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