High-temperature-resistant para-aramid fiber oiling agent as well as preparation method and application thereof

Abstract

The invention relates to the technical field of spinning oil agents, in particular to a high-temperature-resistant para-aramid fiber oil agent as well as a preparation method and application of the high-temperature-resistant para-aramid fiber oil agent. The para-aramid fiber oiling agent is prepared from 28 to 37 parts of a lubricant, 15 to 20 parts of an emulsifier, 13.5 to 20.5 parts of an antistatic agent, 10 to 15 parts of a cohesive agent, 10 to 12 parts of an additive, 8 to 12 parts of a diluent, 0.8 to 1.2 parts of three-dimensional interpenetrating ZIF-8 fluorinated graphene aerogel and 2.5 to 3.5 parts of confined ionic liquid, the lubricant is prepared from epoxy group modified phenyl silicone oil and phosphorus-nitrogen flame-retardant polyether polyol; the additives comprise an antioxidant, a preservative and a solubilizer. The para-aramid fiber oiling agent has excellent high-temperature stability, antistatic performance and bundling effect, can keep stable performance in a high-temperature environment, has good water solubility, and effectively improves the processing quality and efficiency of para-aramid fibers.

Description

TECHNICAL FIELD

[0001] The present application relates to a kind of high-temperature-resistant para-aramid fiber oil and preparation method and application, belong to spinning oil technical field. BACKGROUND

[0002] Para-aramid fiber is a kind of high-performance synthetic fiber, with excellent high-temperature resistance, chemical corrosion resistance and high strength, etc., is widely used in aviation, national defense, communication, transportation and individual protection, etc.. In the spinning process of para-aramid fiber, the use of oil is essential. The main role of oil includes reducing the frictional resistance between fiber and equipment, eliminating static electricity, increasing the cohesion of the tow and improving the subsequent processing performance of fiber. However, the current para-aramid spinning oil has some problems in high-temperature environment. For example, the existing aramid oil still has three major problems of volatilization, lubricating film rupture and antistatic agent failure at 350-380℃, resulting in high fiber hairiness rate, difficult to clean in the later stage, and difficult to meet the demand of new generation 350℃ dry spinning process.

[0003] Patent application with publication number CN109722744A discloses a preparation method of para-aramid oil, wherein the composition of para-aramid oil is as follows: smoothing agent 35%-45%, cohesion agent 5%-15%, antistatic agent 7%-17%, emulsifier 35%-40%, and balance adjusting agent 3%-5%. The para-aramid oil of the invention is suitable for para-aramid oiling after heating, but not suitable for high-temperature conditions. Patent application with publication number CN104947424A discloses a preparation method of para-aramid oil, wherein the lubricant is 92-82%, the bundling agent is 3-10%, the composite antistatic agent is 5-8%, and the rest is additive; the lubricant is fatty acid isooctyl ester. The para-aramid oil of the invention is suitable for use in different humidity environments, but not suitable for high-temperature conditions.

[0004] Therefore, it is of great value to develop a high-temperature-resistant para-aramid fiber oil to overcome the shortcomings of existing oils in high-temperature environment and improve the water solubility of the oil, making it easy to clean for downstream applications. SUMMARY

[0005] The present application provides a kind of "three-dimensional interpenetrating skeleton-restricted ionic liquid" high-temperature-resistant para-aramid fiber oil and preparation method and application to overcome the shortcomings of existing technology, the para-aramid fiber oil has excellent high-temperature stability, antistatic performance and bundling effect, can keep stable performance in high-temperature environment, reduce volatilization and decomposition, has good water solubility, effectively improves the processing quality and efficiency of para-aramid fiber.

[0006] The technical scheme for solving the above technical problems is as follows: a high-temperature-resistant para-aramid fiber oil agent, according to weight parts, the para-aramid fiber oil agent comprises: 28-37 parts of lubricant, 15-20 parts of emulsifier, 13.5-20.5 parts of antistatic agent, 10-15 parts of cohesive agent, 10-12 parts of additive, 8-12 parts of diluent, 0.8-1.2 parts of three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel, and 2.5-3.5 parts of confined ionic liquid; The lubricant comprises epoxy-modified phenyl silicone oil and phosphorus-nitrogen flame-retardant polyether polyol. The additive comprises antioxidant, preservative and solubilizer.

[0007] Further, the epoxy value of the epoxy-modified phenyl silicone oil is 0.10-0.15 mol / 100g. The hydroxyl content value of the phosphorus-nitrogen flame-retardant polyether polyol is 20-45 mg / KOH.

[0008] Further, according to weight parts, the addition amount of the epoxy-modified phenyl silicone oil in the para-aramid fiber oil agent is 18-22 parts, and the addition amount of the phosphorus-nitrogen flame-retardant polyether polyol is 10-15 parts.

[0009] Further, in the para-aramid fiber oil agent, the weight part ratio of the epoxy-modified phenyl silicone oil to the phosphorus-nitrogen flame-retardant polyether polyol is (1.4-2):1.

[0010] Further, the emulsifier is hyperbranched polyester-polyether block copolymer (HBPE-PEG).

[0011] Further, according to weight parts, the antistatic agent in the para-aramid fiber oil agent comprises 12-18 parts of fatty alcohol polyoxyethylene ether phosphate potassium salt, and 1.5-2.5 parts of bimodal imidazole ionic liquid.

[0012] Further, the antioxidant comprises 2,6-di-tert-butyl-4-methylphenol, the preservative comprises methyl hydroxybenzoate, and the solubilizer comprises polyethylene glycol.

[0013] Further, according to weight parts, in the para-aramid fiber oil agent, 2,6-di-tert-butyl-4-methylphenol is 3-4 parts, methyl hydroxybenzoate is 3-4 parts, and polyethylene glycol is 3-4 parts.

[0014] Further, the confined ionic liquid is 1-butyl-3-methylimidazolium hexafluorophosphate, the cohesive agent is oleic acid polyethylene glycol 400 diester, and the diluent is deionized water.

[0015] The application further discloses a preparation method of the high-temperature-resistant para-aramid fiber oil agent. S1, disperse fluorinated graphene in methanol, add Zn salt and 2-methyl imidazole to carry out sol-gel, freeze-dry, and carbonize at 350-400℃ in nitrogen for 2-3h to obtain three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel; S2, after the three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel is immersed in limited ionic liquid under vacuum conditions, drying to obtain IL@3D-FG-ZIF; S3, the lubricant, emulsifier, adhesion agent, antistatic agent and solubilizer are put into the reaction kettle, pre-emulsified at 160-170℃ under nitrogen for 30-60min; Then add IL@3D-FG-ZIF, antioxidant, preservative, and heat to 180-200℃ for in-situ crosslinking for 60-90min; S4, cool to below 40℃, add diluent, emulsify and disperse, and filter through 0.22-0.50μm to obtain the high-temperature-resistant para-aramid fiber oil.

[0016] The application also discloses an application of the high-temperature-resistant para-aramid fiber oil.

[0017] The application has the following beneficial effects: The high-temperature-resistant para-aramid fiber oil has good temperature resistance under 350℃, is not easy to oxidize and emit black smoke, meets the application of para-aramid in the fields of rubber and optical cable, effectively reduces the generation of para-aramid fiber hair, enhances the adhesion of the fiber, has good water-soluble stability, and further improves the quality and application effect of the para-aramid fiber.

[0018] In the high-temperature-resistant para-aramid fiber oil, the epoxy-modified phenyl silicone oil and the phosphorus-nitrogen flame-retardant polyether polyol are compounded at a ratio of 1.5-2:1 and in-situ crosslinked to form the core lubricating layer of the oil. The epoxy group and the polyether hydroxyl group are rapidly ring-opened at 170-200℃ to form a three-dimensional interpenetrating network, so that the silicone oil molecular chain is chemically anchored, the volatilization rate is less than 4% at 400℃, and the friction coefficient is reduced to 0.08. The phosphorus-nitrogen groups generate a phosphorus-containing carbon layer and a nitrogen expansion layer under heat, which double-blocks oxygen and heat, increases the initial decomposition temperature from 320℃ to 423℃, and synchronously increases the smoke temperature by 60℃. The network polar end group forms a hydrogen bond with the aramid surface hydroxyl group, and the adhesion of the lubricating film is increased by 3 times. Meanwhile, the polyether chain segment with a hydroxyl value of 45mg KOH / g remains water-soluble, and the residual oil after water washing in the later stage is less than 0.01%. The two achieve the integration of "high-temperature lubrication-flame-retardant smoke suppression-easy cleaning".

[0019] In addition, the three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel is used as a rigid skeleton to physically anchor the silicone oil, which is the core of the temperature resistance, migration resistance and antistatic synergy of the application. The 800m2 g -1 Ultra-high specific surface area and 2-4 nm uniform mesoporous, first, provides a huge amount of adsorption sites, which can be in situ cross-linked at 170-200 ℃ during the process of modifying the epoxy phenyl silicone oil and phosphorus-nitrogen polyether chain segment, forming a nanoscale "mechanical lock", so that the high temperature migration rate of the silicone oil is reduced from 5.2 μg cm -2 To <1 μg cm -2 , which completely eliminates the traditional silicone oil "shrink ball" and volatilization problems. Secondly, the rigid ZIF-8 metal-organic framework still maintains the lattice integrity at 400 ℃, and the thermal conductivity of the fluorinated graphene sheet layer is as high as 500 Wm -1 K -1 , which can quickly export local heat and inhibit the formation of hot spots, so that the overall thermal decomposition starting temperature of the oil agent is increased by more than 40 ℃. Thirdly, 2.5-3.5 parts of [BMIM][PF6] ionic liquid are pre-confined in the pores of the aerogel, and the evaporation temperature of the IL (ionic liquid) is increased to 420 ℃ by means of nano-confinement effect, while the negative charge of the pore wall and the positive ion of the IL form an electrostatic anchor, ensuring that the surface resistance is stable at the level of 108Ω at 400 ℃; The oleophobicity of fluorinated graphene further prevents IL from migrating to the surface of the fiber, realizing "long-term antistatic - zero leakage". Fourthly, the three-dimensional framework and the cross-linked lubricating layer form a soft-hard double network, which gives the emulsion shear thinning characteristics, and the viscosity can be reduced by 30% under high-speed shear, which is beneficial to uniform oiling; After stopping shearing, the high viscosity is quickly restored to prevent dripping. The aerogel is simple to prepare, the raw materials are cheap, and it can be recycled and regenerated, providing a scalable ultra-high temperature solution for aramid oil agent.

[0020] In addition, the 1-butyl-3-methylimidazolium hexafluorophosphate added in the application can be evaporated in the 2-4 nm pore channel, and the evaporation temperature is increased to 420 ℃, and the ion conductivity is maintained at 400 ℃, and the surface resistance is stable at 10 8 Ω, realizing long-term antistatic and no leakage; The HLB of the HBPE-PEG hyperbranched emulsifier is approximately 12, the viscosity is instantaneously reduced by 30% under high-temperature shear, and the viscosity is restored after stopping shearing for 10s, preventing dripping, and the emulsion is not layered after 3000 rpm x 30 min. Both of them: the ionic liquid provides continuous charge discharge, and the HBPE-PEG ensures uniform oiling at high speed and easy cleaning at low temperature, with water-washed residual oil <0.01wt%, and both high-temperature resistance and low friction, green process.

[0021] In summary, the high-temperature-resistant para-aramid fiber oil agent described in the application provides high-temperature lubrication and smoke suppression through the epoxy-phosphorus-nitrogen cross-linking lubricating system, anchors and conducts heat through the 3D-FG-ZIF aerogel (three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel), realizes long-acting antistatic through the confined ionic liquid, and the antioxidant, preservative and emulsifier synergistically stabilize through the HBPE-PEG intelligent emulsion. These components are linked together, which pushes the temperature resistance limit of the oil agent from 320 DEG C to greater than or equal to 380 DEG C, while realizing low friction, zero migration, easy cleaning and scalable 380 DEG C level para-aramid fiber processing. DETAILED DESCRIPTION

[0022] The specific embodiments of the application are described in detail below. The application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the spirit of the application, so the application is not limited by the disclosed specific embodiments.

[0023] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terms used are only for describing specific embodiments, not for limiting the application.

[0024] A high-temperature-resistant para-aramid fiber oil agent, according to the weight fraction, the para-aramid fiber oil agent comprises: a lubricant 28-37 parts, an emulsifier 15-20 parts, an antistatic agent 13.5-20.5 parts, a cohesive agent 10-15 parts, an additive 10-12 parts, a diluent 8-12 parts, a three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel 0.8-1.2 parts, and a confined ionic liquid 2.5-3.5 parts; The lubricant comprises epoxy-modified phenyl silicone oil and phosphorus-nitrogen flame-retardant polyether polyol. The additive comprises an antioxidant, a preservative and a solubilizer.

[0025] Specifically, the epoxy value of the epoxy-modified phenyl silicone oil is 0.10-0.15 mol / 100g. The hydroxyl content value of the phosphorus-nitrogen flame-retardant polyether polyol is 20-45 mg / KOH.

[0026] Specifically, according to the weight fraction, the amount of the epoxy-modified phenyl silicone oil added in the para-aramid fiber oil agent is 18-22 parts, and the amount of the phosphorus-nitrogen flame-retardant polyether polyol added is 10-15 parts.

[0027] Specifically, the weight fraction ratio of the epoxy-modified phenyl silicone oil to the phosphorus-nitrogen flame-retardant polyether polyol in the para-aramid fiber oil agent is (1.4-2):1.

[0028] Preferably, the mass ratio of the three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel and the confined ionic liquid is 1: (2.5-3.8).

[0029] Specifically, the emulsifier is a hyperbranched polyester-polyether block copolymer (HBPE-PEG).

[0030] Specifically, according to weight parts, the antistatic agent in the para-aramid fiber oil agent includes 12-18 parts of fatty alcohol polyoxyethylene ether phosphate potassium salt, 1.5-2.5 parts of a bimodal ionic liquid.

[0031] Specifically, the antioxidant includes 2,6-di-tert-butyl-4-methylphenol, the preservative includes methylparaben, and the solubilizer includes polyethylene glycol.

[0032] Specifically, according to weight parts, the 2,6-di-tert-butyl-4-methylphenol in the para-aramid fiber oil agent is 3-4 parts, the methylparaben is 3-4 parts, and the polyethylene glycol is 3-4 parts.

[0033] Specifically, the confined ionic liquid is 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF6]); confined in the pore channel of the aerogel to prevent high-temperature volatilization; the three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel is used as a rigid skeleton to inhibit the high-temperature migration of the lubricant.

[0034] The adhesion agent is oleic acid polyethylene glycol 400 diester. The diluent is deionized water for adjusting the solid content of the emulsion.

[0035] The application also discloses a preparation method of the high-temperature-resistant para-aramid fiber oil agent. S1, dispersing fluorinated graphene in methanol, adding Zn salt (zinc nitrate hexahydrate) and 2-methylimidazole for sol-gel, freeze-drying, and carbonizing at 350-400 DEG C in nitrogen for 2-3 h to obtain three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel; S2, after the three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel is impregnated with a confined ionic liquid under vacuum conditions, drying obtains IL@3D-FG-ZIF; S3, the lubricant, the emulsifier, the adhesion agent, the antistatic agent and the solubilizer are put into a reaction kettle, and pre-emulsified at 160-170 DEG C under nitrogen for 30-60 min; Then, IL@3D-FG-ZIF, antioxidant and preservative are added, and in-situ crosslinking is carried out at 180-200 DEG C for 60-90 min; the epoxy group and the polyether hydroxyl group are ring-opening reaction to form a three-dimensional interpenetrating network, so that the initial decomposition temperature of the oil agent is greater than or equal to 423 DEG C.

[0036] S4, cooling to 40℃ or below, adding diluent, emulsifying and dispersing (emulsifying for 15-30 min under the condition of 1500-2000 rpm), and filtering through 0.22-0.50 μm to obtain the high-temperature-resistant para-aramid fiber oiling agent.

[0037] Specifically, the preparation method of the epoxy-modified phenyl silicone oil is as follows: 100-110 g of IOTA-255A, 6-10 g of 3-glycidyloxypropyl trimethoxysilane and 0.1-0.5 g of stannous octoate are put into a reaction kettle, vacuum stirring is carried out at 120-150℃ for 2-3 h, so that the epoxy group is grafted to the side group of the silicon chain; then 0.2-0.4 g of acetic acid neutralization catalyst is added, low-boiling substances are removed under reduced pressure for 30-60 min, and cooling is carried out to obtain the epoxy-modified phenyl silicone oil (epoxy value 0.10-0.15 mol / 100 g, different epoxy values of the epoxy-modified phenyl silicone oil can be obtained by adjusting the amount ratio of IOTA-255A and 3-glycidyloxypropyl trimethoxysilane).

[0038] The preparation method of the phosphorus-nitrogen flame-retardant polyether polyol is as follows: 90-120 g of polyether polyol, 5-10 g of DOPO and 3-8 g of melamine are melt-mixed at 130-150℃, 0.5-1.0 g of tetrabutyl titanate is added dropwise as a catalyst, and nitrogen is bubbled and stirred for 3-6 h until the hydroxyl value is reduced to 20-45 mgKOH / g to obtain the phosphorus-nitrogen flame-retardant polyether polyol (hydroxyl value 20-45 mg / KOH, different hydroxyl values of the phosphorus-nitrogen flame-retardant polyether polyol can be obtained by controlling the nitrogen bubbling and stirring time).

[0039] Preparation of the HBPE-PEG emulsifier: under a nitrogen environment, 2,2-bis-hydroxymethyl propionic acid (bis-MPA) and 1,1,1-tris(hydroxymethyl)propane TMP are melt polycondensed at a hydroxyl molar ratio (10-15):1, water is removed at 140-160℃ for 4 h to obtain hyperbranched polyester HBPE; after cooling, isophorone diisocyanate IPDI is used as a bridge to couple the terminal hydroxyl group of HBPE with PEG-2000 at 70-85℃ for 4-6 h, and the solvent is evaporated to obtain the HBPE-PEG block copolymer.

[0040] More specifically, in the embodiments of the present application: Preparation of the HBPE-PEG emulsifier: under a nitrogen environment, 2,2-bis-hydroxymethyl propionic acid (bis-MPA) and 1,1,1-tris(hydroxymethyl)propane TMP are melt polycondensed at a hydroxyl molar ratio (10-15):1, water is removed at 140-160℃ for 4 h to obtain hyperbranched polyester HBPE; after cooling, isophorone diisocyanate IPDI is used as a bridge to couple the terminal hydroxyl group of HBPE with PEG-2000 at 70-85℃ for 4-6 h, and the solvent is evaporated to obtain the HBPE-PEG block copolymer.

[0041] The related raw materials used in the embodiments of the application can be directly purchased, and the models and purchasing manufacturers of the related raw materials are as follows: Phenyl silicone oil (IOTA-255): ASE-303, manufacturer: Huaiyiota Silicone Oil Co., Ltd.; 3-glycidyloxypropyl trimethoxysilane: KH-560, manufacturer: Nanjing Shuguang Silane Chemical Co., Ltd.; Stannous octoate: T-9 (≥95%), manufacturer: American Gas Chemical Products Company; Polyether polyol: PPG-1000, manufacturer: Shandong Lansheng East Chemical Co., Ltd.; 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO): purchasing manufacturer: Shanghai Maikelin Biochemical Technology Co., Ltd.; Tetrabutyl titanate: TBT (≥99%), manufacturer: Araldite Reagent (Shanghai) Co., Ltd.; 2,2-dimethylol propionic acid: bis-MPA, manufacturer: TCI (Shanghai) Chemical Industry Development Co., Ltd.; 1,1,1-tris(hydroxymethyl)propane: TMP (≥98%), manufacturer: Jiangsu Sanmu Group Co., Ltd.; Isophorone diisocyanate: IPDI, manufacturer: Covestro (China) Co., Ltd.; Polyethylene glycol: PEG-2000 (industrial grade), manufacturer: Jiangsu Hai'an Petrochemical Co., Ltd.; Oleic acid polyethylene glycol 400 diester: PEG400DO, manufacturer: Hai'an Petrochemical Factory of Jiangsu Province; Fatty alcohol polyoxyethylene ether phosphate potassium salt: PK-301, manufacturer: Zhejiang Royaltech Science and Technology Co., Ltd.; Bisimidazole ionic liquid: [BMIM][PF6], manufacturer: Ionic Liquid Center of Lanzhou Institute of Chemical Physics; 2,6-di-tert-butyl-4-methylphenol: BHT, manufacturer: Lanxess, Germany; Methyl hydroxybenzoate: ≥99%, manufacturer: Shandong Xingang Chemical Co., Ltd.; Fluorinated graphene: FG-1, manufacturer: Changzhou Sixth Element Material Technology Co., Ltd.; 2-methylimidazole: purity ≥99%, Araldite Reagent (Shanghai) Co., Ltd.; Zinc nitrate hexahydrate: AR grade, manufacturer: National Pharmaceutical Group Chemical Reagent Co., Ltd.

[0042] The application further discloses an application of the high-temperature-resistant para-aramid fiber oiling agent, and the oiling agent is used for oiling operation of para-aramid fibers.

[0043] Example 1

[0044] Preparation of a high-temperature-resistant para-aramid fiber oil: The raw materials are as follows according to weight parts: Lubricant: epoxy-modified phenyl silicone oil 20 parts (epoxy value 0.12 mol / 100 g), phosphorus-nitrogen flame-retardant polyether polyol 12 parts (hydroxyl value 35 mg / KOH); Emulsifier: HBPE-PEG 18 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 15 parts, bisimidazole ionic liquid 2 parts; Coalescent agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel 1.0 part, confined ionic liquid [BMIM][PF6] 3 parts; Diluent: deionized water 10 parts.

[0045] The specific preparation method is as follows: S1, disperse fluorinated graphene in methanol, add Zn salt and 2-methylimidazole for sol-gel, freeze-dry, and carbonize at 350°C under nitrogen for 3h to obtain three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel; S2, immerse the three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel in confined ionic liquid under vacuum conditions, and dry to obtain IL@3D-FG-ZIF; S3, put the lubricant, emulsifier, coalescent agent, antistatic agent and solubilizer into the reaction kettle, pre-emulsify at 165°C under nitrogen for 30min (stirring speed 300rpm); Then add IL@3D-FG-ZIF, antioxidant, preservative, and heat to 175°C and stir for 75min; S4, cool to 35°C, add diluent, emulsify at 1500rpm for 20min, filter through 0.22μm to remove possible impurities, and store the prepared oil in a container, seal and store to obtain a high-temperature-resistant para-aramid fiber oil.

[0046] Example 2

[0047] Preparation of a high-temperature-resistant para-aramid fiber oil: The raw materials are as follows according to weight parts: Lubricant: epoxy-modified phenyl silicone oil 22 parts (epoxy value 0.15 mol / 100g), phosphorus-nitrogen flame-retardant polyether polyol 15 parts (hydroxyl value 20 mg / KOH); Emulsifier: HBPE-PEG 20 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 18 parts, bisimidazole ionic liquid 2.5 parts; Coalescent agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel 1.2 parts, confined ionic liquid [BMIM][PF6] 3 parts; Diluent: deionized water 12 parts.

[0048] The specific preparation method is as follows: S1, disperse fluorinated graphene in methanol, add Zn salt and 2-methyl imidazole for sol-gel, freeze-dry, and carbonize at 400°C in nitrogen for 2h to obtain three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel; S2, after immersing the three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel in the confined ionic liquid under vacuum conditions, dry to obtain IL@3D-FG-ZIF; S3, put the lubricant, emulsifier, coalescent agent, antistatic agent and solubilizer into the reaction kettle, pre-emulsify at 165°C under nitrogen for 30min (stirring speed 300rpm); Then add IL@3D-FG-ZIF, antioxidant, preservative, and heat to 185°C and stir for 75min; S4, cool to 35°C, add diluent, emulsify at 1500rpm for 20min, filter through 0.22μm to remove possible impurities, fill the prepared oil agent into a container, seal and store to obtain a high-temperature-resistant p-aramid fiber oil agent.

[0049] Example 3

[0050] Preparation of a high-temperature-resistant p-aramid fiber oil agent: The raw materials are as follows according to weight fraction: Lubricant: epoxy-modified phenyl silicone oil 22 parts (epoxy value 0.15 mol / 100g), phosphorus-nitrogen flame-retardant polyether polyol 15 parts (hydroxyl value 20 mg / KOH); Emulsifier: HBPE-PEG 20 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 12 parts, bisimidazole ionic liquid 1.5 parts; Adhesion agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel 0.8 parts, confined ionic liquid [BMIM][PF6] 3 parts; Diluent: deionized water 8 parts.

[0051] The specific preparation method is: S1, disperse fluorinated graphene in methanol, add Zn salt and 2-methyl imidazole for sol-gel, freeze-dry and carbonize at 380℃ in nitrogen for 2h to obtain three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel; S2, after immersing the three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel in confined ionic liquid under vacuum conditions, dry to obtain IL@3D-FG-ZIF; S3, put the lubricant, emulsifier, adhesion agent, antistatic agent and solubilizer into the reaction kettle, pre-emulsify at 165℃ under nitrogen for 30min (stirring speed 300rpm); Then add IL@3D-FG-ZIF, antioxidant, preservative, heat to 185℃ and stir for 75min; S4, cool to 35℃, add diluent and emulsify at 1500rpm for 20min, filter through 0.22μm to remove possible impurities, fill the prepared oil agent into a container, seal and store to obtain a high-temperature-resistant p-aramid fiber oil agent.

[0052] Example 4

[0053] Preparation of a high-temperature-resistant p-aramid fiber oil agent: The raw materials are as follows according to the weight fraction: Lubricant: epoxy-modified phenyl silicone oil 21 parts (epoxy value 0.10 mol / 100g), phosphorus-nitrogen flame-retardant polyether polyol 11 parts (hydroxyl value 45mg / KOH); Emulsifier: HBPE-PEG 19 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 16 parts, bisimidazole ionic liquid 2.2 parts; Adhesion agent: oleic acid polyethylene glycol 400 diester 13 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 4 parts; Preservative: methyl hydroxybenzoate 4 parts; Solubilizing agent: polyethylene glycol (PEG) 4 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel 1.1 parts, confined ionic liquid [BMIM] [PF6] 3.2 parts; Diluent: deionized water 11 parts.

[0054] The specific preparation method is: S1, disperse fluorinated graphene in methanol, add Zn salt and 2-methyl imidazole to perform sol-gel, freeze dry, and then carbonize at 380℃ in nitrogen for 2.5h to obtain three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel; S2, after immersing the three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel in confined ionic liquid under vacuum conditions, dry to obtain IL@3D-FG-ZIF; S3, put the lubricant, emulsifier, adhesion agent, antistatic agent and solubilizing agent into the reaction kettle, pre-emulsify at 165℃ under nitrogen for 60min (stirring speed 300rpm); Then add IL@3D-FG-ZIF, antioxidant, preservative, and heat to 185℃ and stir for 80min; S4, cool to 35℃, add diluent and emulsify at 1500rpm for 20min, filter through 0.22μm to remove possible impurities, and then put the prepared oil agent into a container, seal and store to obtain a high-temperature-resistant p-aramid fiber oil agent.

[0055] Example 5

[0056] Preparation of a high-temperature-resistant p-aramid fiber oil agent: The raw materials are as follows according to the weight fraction: Lubricant: epoxy-modified phenyl silicone oil 18.5 parts (epoxy value 0.12 mol / 100g), phosphorus-nitrogen flame-retardant polyether polyol 11 parts (hydroxyl value 40mg / KOH); Emulsifier: HBPE-PEG 19 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 16 parts, double imidazole ionic liquid 2.2 parts; Adhesion agent: oleic acid polyethylene glycol 400 diester 13 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 4 parts; Preservative: methyl hydroxybenzoate 4 parts; Solubilizing agent: polyethylene glycol (PEG) 4 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel 1.1 parts, confined ionic liquid [BMIM] [PF6] 3.2 parts; Diluent: deionized water 11 parts.

[0057] The specific preparation method is as follows: S1, dispersing fluorinated graphene in methanol, adding Zn salt and 2-methyl imidazole for sol-gel, freeze-drying, and carbonizing at 380°C in nitrogen for 2h to obtain three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel; S2, after the three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel is immersed in the confined ionic liquid under vacuum, drying to obtain IL@3D-FG-ZIF; S3, the lubricant, emulsifier, adhesion agent, antistatic agent and solubilizer are put into the reaction kettle, pre-emulsified at 170°C under nitrogen for 30min (stirring speed 300rpm); Then add IL@3D-FG-ZIF, antioxidant, preservative, and heat to 185°C and stir for 80min; S4, cool to 35°C, add diluent, emulsify at 1500rpm for 20min, filter through 0.22μm to remove possible impurities, and store the prepared oil agent in a container, seal to obtain high-temperature-resistant p-aramid fiber oil agent.

[0058] Comparative Example 1

[0059] The oil agent is prepared by the same method as in Example 1, except that the skeleton IL@3D-FG-ZIF and the confined ionic liquid [BMIM][PF6] are not contained in the present comparative example 1, as follows: Lubricant: epoxy modified phenyl silicone oil 20 parts, phosphorus-nitrogen flame-retardant polyether polyol 12 parts; Emulsifier: HBPE-PEG 18 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 15 parts, bisimidazole ionic liquid 2 parts; Adhesion agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Diluent: deionized water 10 parts.

[0060] The specific preparation method is as follows: S1, the lubricant, emulsifier, adhesion agent, antistatic agent and solubilizer are put into the reaction kettle, pre-emulsified at 165°C under nitrogen for 30min (stirring speed 300rpm); Then add antioxidant, preservative, and heat to 175°C and stir for 75min; S2, cooling to 35℃, adding diluent 1500 rpm emulsification 20 min, 0.22 μm filtration, filtration to remove possible impurities, the prepared oil agent into the container, sealed and stored to obtain high temperature resistant p-aramid fiber oil agent.

[0061] Comparative Example 2

[0062] The same method as in Example 1 was used to prepare the oil agent, except that no confined ionic liquid was added in this comparative example 2, as follows: The raw materials are as follows according to the weight fraction: Lubricant: epoxy modified phenyl silicone oil 20 parts, phosphorus-nitrogen flame-retardant polyether polyol 12 parts; Emulsifier: HBPE-PEG 18 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 15 parts, bisimidazole ionic liquid 2 parts; Coalescent agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel 1.0 part; Diluent: deionized water 10 parts.

[0063] The specific preparation method is as follows: S1, disperse fluorinated graphene in methanol, add Zn salt and 2-methylimidazole for sol-gel, freeze-dry and carbonize at 350℃ under nitrogen for 3h to obtain three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel; S2, put the lubricant, emulsifier, coalescent agent, antistatic agent and solubilizer into the reaction kettle, pre-emulsify at 165℃ under nitrogen for 30 min (stirring speed 300 rpm); Then add three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel, antioxidant, preservative, and heat to 175℃ and stir for 75 min; S3, cooling to 35℃, adding diluent 1500 rpm emulsification 20 min, 0.22 μm filtration, filtration to remove possible impurities, the prepared oil agent into the container, sealed and stored to obtain high temperature resistant p-aramid fiber oil agent.

[0064] Comparative Example 3

[0065] The same method as in Example 1 was used to prepare the oil agent, except that no aerogel skeleton (three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel) was added in this comparative example 3, as follows: The raw materials are as follows in terms of weight parts: Lubricant: epoxy modified phenyl silicone oil 20 parts, phosphorus-nitrogen flame-retardant polyether polyol 12 parts; Emulsifier: HBPE-PEG 18 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 15 parts, bisimidazole ionic liquid 2 parts; Coalescent agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: confined ionic liquid [BMIM][PF6] 3 parts; Diluent: deionized water 10 parts.

[0066] The specific preparation method is as follows: S1, the lubricant, emulsifier, coalescent agent, antistatic agent and solubilizer are put into the reaction kettle, and pre-emulsified at 165°C under nitrogen for 30min (stirring speed 300rpm); Then add confined ionic liquid [BMIM][PF6], antioxidant, preservative, and stir at 175°C for 75min; S2, cool to 35°C, add diluent 1500rpm emulsified for 20min, filter through 0.22μm, remove possible impurities, fill the prepared oil agent into a container, seal and store to obtain a high-temperature-resistant p-aramid fiber oil agent.

[0067] Comparative Example 4

[0068] The oil agent is prepared by the same method as in Example 1, except that the epoxy modified phenyl silicone oil in this comparative example 4 is epoxy grafted, with an epoxy value of 0.06 mol / 100g, and the oil agent preparation ingredients and steps are the same as in Example 1. The preparation of epoxy modified phenyl silicone oil IOTA-255A is as follows: Take 100g of IOTA-255A and 3g of 3-glycidyloxypropyltrimethoxysilane, 0.1g of stannous octoate into the reaction kettle, vacuum stirring at 120°C for 2h, so that the epoxy group is grafted on the side group of the silicon chain; then add 0.2g of acetic acid neutralization catalyst, reduce pressure to remove low boiling point for 30min, cool down to get epoxy modified phenyl silicone oil (epoxy value 0.06mol / 100g).

[0069] Comparative Example 5

[0070] The oil agent is prepared by the same method as in Example 1, except that the phosphorus-nitrogen flame-retardant polyether polyol in this Comparative Example 5 has a hydroxyl content higher than 45 mg / KOH, and the oil agent is prepared by the same composition and steps as in Example 1. The phosphorus-nitrogen flame-retardant polyether polyol is prepared as follows: 90 g of polyether polyol is mixed with 5 DOPO and 3 g of melamine at 130°C, 0.5 g of tetrabutyl titanate is added dropwise as a catalyst, and stirring is carried out under nitrogen for 2 h to obtain a phosphorus-nitrogen flame-retardant polyether polyol with a hydroxyl value of 55 mg / KOH.

[0071] Comparative Example 6

[0072] The oil agent is prepared by the same method as in Example 1, except that the amount of the imidazole-based ionic liquid in this Comparative Example 6 is increased to 5 parts (higher than the amount defined in the present application), and the preparation is as follows: The raw materials are as follows in terms of weight fraction: Lubricant: epoxy-modified phenyl silicone oil 20 parts, phosphorus-nitrogen flame-retardant polyether polyol 12 parts; Emulsifier: HBPE-PEG 18 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 15 parts, imidazole-based ionic liquid 5 parts; Coalescent agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel 1.0 part, confined ionic liquid [BMIM][PF6] 3 parts; Diluent: deionized water 10 parts.

[0073] The specific preparation method is the same as in Example 1.

[0074] Comparative Example 7

[0075] The oil agent is prepared by the same method as in Example 1, except that no epoxy-modified phenyl silicone oil is used in this Comparative Example 7, and phenyl silicone oil IOTA-255A is directly used, and the preparation is as follows: The raw materials are as follows in terms of weight fraction: Lubricant: phenyl silicone oil 20 parts, phosphorus-nitrogen flame-retardant polyether polyol 12 parts; Emulsifier: HBPE-PEG 18 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 15 parts, imidazole-based ionic liquid 5 parts; Coalescent agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel 1.0 parts, confined ionic liquid [BMIM][PF6] 3 parts; Diluent: deionized water 10 parts.

[0076] The specific preparation method is the same as that of Example 1.

[0077] Comparative Example 8

[0078] The oil agent was prepared by the same method as Example 1, except that no phosphorus-nitrogen flame-retardant polyether polyol was used in this comparative example 8, and polyether polyol was directly used, as follows: The raw materials are as follows according to the weight fraction: Lubricant: epoxy modified phenyl silicone oil 20 parts, polyether polyol 12 parts; Emulsifier: HBPE-PEG 18 parts; Antistatic agent: fatty alcohol polyoxyethylene ether phosphate potassium salt 15 parts, bisimidazole ionic liquid 5 parts; Coalescent agent: oleic acid polyethylene glycol 400 diester 12 parts; Antioxidant: 2,6-di-tert-butyl-4-methylphenol 3.5 parts; Preservative: methyl hydroxybenzoate 3.5 parts; Solubilizer: polyethylene glycol (PEG) 3.5 parts; Other ingredients: three-dimensional interpenetrating ZIF-8@ fluorinated graphene aerogel 1.0 parts, confined ionic liquid [BMIM][PF6] 3 parts; Diluent: deionized water 10 parts.

[0079] The specific preparation method is the same as that of Example 1.

[0080] The oil agent prepared in the above examples and comparative examples was tested for performance, and the specific test results are shown in Table 1 below, and the detection methods involved are as follows: Epoxy value: GB / T 1677-2008 "Hydrochloric acid-acetone method"; Hydroxyl value according to GB / T 12008.3-2009 "Phthalic anhydride method"; Conductivity: HG / T 3506 "Surface active agent Test water or water solution Conductivity determination"; Smoke point: GBT 382-2017 Coal oil and jet fuel smoke point determination method; Stability: GB / T 5559-2010; Temperature resistance effect determination: heat the oil to 350℃ and keep at this temperature for 2h, then reduce to room temperature, weigh and calculate the mass loss of the oil before and after heating.

[0081] Fiber hairiness reduction rate: under the condition of 1500 D dry spinning (350 ℃ duct, 250 m / min), use the oil at 1.3wt% oiling rate, determine the hairiness number of 1000 m fiber bundle according to FZ / T 50014-2008, and calculate the hairiness number reduction rate of fiber bundle with and without oil.

[0082] Table 1 Oil performance test results

[0083] From the above table data, it can be seen that: examples 1-5 are the para-aramid fiber oil of the present application, the smoke temperature of the para-aramid fiber oil is higher, so it has better high temperature resistance, in addition, the conductivity of the para-aramid fiber oil is lower, and the stability is better.

[0084] From the comparison of the results of comparative example 1 and example 1, it can be seen that: example 1 introduces three-dimensional interpenetrating skeleton IL@3D-FG-ZIF and confined ionic liquid [BMIM][PF6] at the same time, the smoke temperature is increased from 380℃ to 423℃, the mass loss at 350℃×2h is reduced from 7.5% to 2.9%, the surface resistance is reduced from 8×10 9 Ω to 2×10 7 Ω, the hairiness reduction rate is increased from 45% to 78%, which fully proves that the "skeleton-confined" synergistic structure can significantly enhance the high temperature resistance, antistatic and bunching performance.

[0085] From the comparison of the results of comparative example 2 and example 1, it can be seen that: only the skeleton is retained and the confined ionic liquid is missing, the smoke temperature is only 385℃, the mass loss is 6.2%, the surface resistance is 5×10 9 Ω, which are all worse than example 1, indicating that the skeleton alone can improve the heat resistance, but cannot meet the requirements of long-term antistatic and low migration, and must be combined with the confined ionic liquid to achieve the best effect.

[0086] From the comparison of the results of comparative example 3 and example 1, it can be seen that: only the confined ionic liquid is added and the skeleton is missing, the smoke temperature is 382℃, the mass loss is 6.8%, and the surface resistance is as high as 1×10 10 Ω, the hairiness reduction rate is only 50%, which shows that the lack of skeleton will lead to the high temperature volatilization of ionic liquid and the intensified migration of silicone oil, and the overall performance will decrease significantly.

[0087] From the comparison of the results of Comparative Example 4 and Example 1, it can be seen that the insufficient epoxy value (0.06 mol / 100g) leads to a loose crosslinking network, the smoke temperature drops to 375℃, the mass loss is 7.2%, and the hairiness rate is reduced only by 40%, which shows that the modification degree of epoxy is a key factor affecting the integrity of the high-temperature-resistant lubricating film.

[0088] From the comparison of the results of Comparative Example 5 and Example 1, it can be seen that the excessively high hydroxyl value (55 mgKOH / g) makes the hydrophilic segment too long, the smoke temperature further drops to 370℃, the mass loss is as high as 9.1%, and the water-washed residual oil is as high as 0.05%, which shows that the excessive hydroxyl value will destroy the balance between flame retardation and hydrophilicity, causing high-temperature volatilization and difficulty in subsequent cleaning.

[0089] From the comparison of the results of Comparative Example 6 and Example 1, it can be seen that although the excessive ionic liquid reduces the surface resistance to 4×10 7 Ω, the smoke temperature is only 390℃, the mass loss is 6.8%, and a small amount of precipitate appears, which shows that the excessive limited ionic liquid will lead to uncontrolled viscosity and increased high-temperature volatilization, which is not conducive to the overall stability.

[0090] From the comparison of the results of Comparative Example 7 and Example 1, it can be seen that if the epoxy-modified phenyl silicone oil is not used and the phenyl silicone oil IOTA-255A is directly used, the lubricating layer lacks crosslinking anchor points due to the absence of epoxy grafting, and the silicone oil only exists in a physically adsorbed state; the molecular chain is easy to slip and volatilize at high temperature, which shows that the "epoxy-hydroxyl in-situ crosslinking" is a necessary condition for forming a dense high-temperature-resistant lubricating film, and the absence of the same will significantly deteriorate the heat resistance and migration resistance.

[0091] From the comparison of the results of Comparative Example 8 and Example 1, it can be seen that if the phosphorus-nitrogen flame-retardant polyether polyol is not used and the polyether polyol is directly used, the system loses the phosphorus-containing carbon layer and the nitrogen gas expansion synergistic flame-retardant mechanism after removing the phosphorus-nitrogen flame-retardant unit, the smoke temperature further decreases, the mass loss increases, and the smoke amount significantly increases at high temperature.

[0092] The application effect of the oiling agent on the para-aramid fiber was further determined: the oiling agent was tested on 1500D para-aramid fiber (the temperature when the para-aramid fiber tows enter the oiling agent tank for oiling is 280-350℃), and the results are shown in Table 2.

[0093] Table 2 Application results of the oiling agent on para-aramid fiber

[0094] From the data in Table 2 above, it can be seen that the application of the para-aramid fiber oiling agent described in the present application to the para-aramid fiber can effectively reduce the generation of para-aramid fiber hairiness, enhance the cohesiveness of the fiber, and at the same time has good water-soluble stability.

[0095] Each technical feature of the above-described embodiments can be combined with any other technical feature, and for the sake of brevity, not all possible combinations are described, but it is understood that the scope of the present disclosure encompasses all such possible combinations.

[0096] Any modifications and improvements made to the present disclosure by those of ordinary skill in the art without departing from the spirit of the present disclosure shall fall within the scope of the present disclosure, and the scope of the present disclosure shall be defined by the appended claims.

Claims

1. A high temperature resistant para-aramid fiber oil, characterized in that: The para-aramid fiber oil comprises, by weight, 28-37 parts of lubricant, 15-20 parts of emulsifier, 13.5-20.5 parts of antistatic agent, 10-15 parts of cohesive agent, 10-12 parts of additive, 8-12 parts of diluent, 0.8-1.2 parts of three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel, and 2.5-3.5 parts of confined ionic liquid. The lubricant includes epoxy-modified phenyl silicone oil and phosphorus-nitrogen flame-retardant polyether polyol; The additives include antioxidants, preservatives and solubilizers.

2. The high-temperature resistant para-aramid fiber oil according to claim 1, characterized in that: The epoxy value of the epoxy-modified phenyl silicone oil is 0.10-0.15 mol / 100 g; The phosphorus-nitrogen flame-retardant polyether polyol has a hydroxyl content of 20-45 mg / KOH.

3. The high-temperature resistant para-aramid fiber oil according to claim 1, characterized in that: In the para-aramid fiber oil, the epoxy-modified phenyl silicone oil is added in an amount of 18-22 parts by weight, and the phosphorus-nitrogen flame-retardant polyether polyol is added in an amount of 10-15 parts by weight; In the para-aramid fiber oil, the weight ratio of the epoxy-modified phenyl silicone oil to the phosphorus-nitrogen flame-retardant polyether polyol is (1.4-2):

1.

4. The high-temperature resistant para-aramid fiber oil according to claim 1, characterized in that: The emulsifier is a hyperbranched polyester-polyether block copolymer.

5. The high temperature resistant para-aramid fiber oil according to claim 1, characterized in that: In the para-aramid fiber oil, the antistatic agent includes 12-18 parts of fatty alcohol polyoxyethylene ether phosphate potassium salt and 1.5-2.5 parts of bisimidazolium ionic liquid.

6. The high-temperature resistant para-aramid fiber oil according to claim 1, characterized in that: The antioxidant includes 2,6-di-tert-butyl-4-methylphenol, the preservative includes methyl hydroxybenzoate, and the solubilizer includes polyethylene glycol.

7. The high-temperature resistant para-aramid fiber oil according to claim 6, characterized in that: In terms of parts by weight, the para-aramid fiber oil comprises 3-4 parts of 2,6-di-tert-butyl-4-methylphenol, 3-4 parts of methyl hydroxybenzoate, and 3-4 parts of polyethylene glycol.

8. The high-temperature resistant para-aramid fiber oil according to claim 1, characterized in that: The confined ionic liquid is 1-butyl-3-methylimidazolium hexafluorophosphate; the chelating agent is oleic acid polyethylene glycol 400 diester; and the diluent is deionized water.

9. A method for preparing a high-temperature resistant para-aramid fiber oil according to any one of claims 1 to 8, characterized in that: The preparation method is: S1. Graphene fluoride was dispersed in methanol, and Zn salt and 2-methylimidazole were added to perform sol-gel formation. After freeze-drying, the mixture was carbonized in nitrogen at 350-400°C for 2-3 h to obtain a three-dimensional interpenetrating ZIF-8@graphene fluoride aerogel. S2, impregnating the three-dimensional interpenetrating ZIF-8@fluorinated graphene aerogel with confined ionic liquid under vacuum conditions and drying to obtain IL@3D-FG-ZIF; S3. Add lubricant, emulsifier, cohesive agent, antistatic agent and solubilizer into the reactor and pre-emulsify at 160-170°C under nitrogen for 30-60 minutes; Then, IL@3D-FG-ZIF, antioxidants, and preservatives were added and the temperature was raised to 180-200°C for in-situ cross-linking for 60-90 min; S4. Cool the mixture to below 40° C., add a diluent for emulsification and dispersion, and filter through a 0.22-0.50 μm filter to obtain the high-temperature resistant para-aramid fiber oil.

10. An application of a high-temperature resistant para-aramid fiber oil according to any one of claims 1 to 8, characterized in that: The oiling agent is used for the oiling operation of para-aramid fiber.

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