High-temperature-resistant nylon composite material and preparation method thereof

By blending modified aerogel filler with nylon 66 resin, the problem of stress creep of nylon 66 at high temperature was solved, and the processability and structural stability of high-temperature resistant nylon composite material were achieved, making it suitable for complex structures such as automotive engine components.

CN119931332BActive Publication Date: 2025-11-18DONGGUAN ZIWEI RUBBER & PLASTIC MATERIALS CO LTD
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Patent Information

Application Number
CN202510066341.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-01-16
Publication Date
2025-11-18
Estimated Expiration
2045-01-16

AI Technical Summary

Technical Problem

Existing Nylon 66 materials are prone to stress creep under high temperature environments, making it difficult to meet the stability requirements of complex structures such as automotive engine components.

Method used

A modified aerogel filler was blended with nylon 66 resin, and amino groups were introduced onto the surface of the aerogel powder by modifying it with silane coupling agent KH-550 to form polyphenolic oligomer coating, which enhanced the compatibility with the nylon 66 matrix. High-temperature resistant nylon composite material was prepared by multi-zone slow-heating melt extrusion process.

Benefits of technology

The high-temperature stress creep resistance of nylon 66 has been improved, enhancing the material's processability and structural stability, making it suitable for manufacturing complex products.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to a high-temperature-resistant nylon composite material and a preparation method thereof, and belongs to the technical field of polymer composite materials. The composite material comprises, in terms of weight parts, 100 parts of nylon 66 resin, 13-18 parts of modified aerogel filler, 1.6-2.2 parts of lubricant, 0.12-0.15 parts of antioxidant and 0.2-0.3 parts of light stabilizer; the modified aerogel filler takes silica-based aerogel powder as a matrix, is coupled and modified by silane coupling agent KH-550 to introduce surface amino groups, forms an oligomer with a main chain containing a polyphenyloxide chain through ring-opening reaction of p-hydroxy diphenyl ether and epoxy chloropropane, and is capped with an excess of an epoxy structure, finally, the active amino groups grafted on the surface of the aminated aerogel are ring-opened, in-situ polymer coating of the polyphenyloxide block is formed on the surface of the aerogel particles, the ordered arrangement and crystallization of the macromolecular chains of the nylon 66 matrix are promoted, internal defects are reduced, and then the composite material is not prone to stress creep at high temperature.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of high polymer composite materials, and particularly relates to a high-temperature-resistant nylon composite material and a preparation method thereof. BACKGROUND

[0002] Polyamide, also known as nylon, is a polymer containing amide groups in the repeating units of the main chain. Due to its excellent comprehensive performance, it is widely used in various fields of industrial production. With the development direction of lightweight of automobiles, higher requirements are put forward for the performance of materials. In the field of automobile industry, the development goals of lightweight and low carbon environmental protection require the use of polymer materials to partially replace metal alloys, such as the fuel system, exhaust system and cooling system of automobile engine, which requires the substitute materials to have excellent heat resistance.

[0003] Among the polyamide family, there is a kind of product with very excellent high-temperature resistance, and its melting temperature is close to or exceeds 300 DEG C. For example, the melting point of PA6T (polyhexamethylene terephthalamide) is 370 DEG C, and the melting point of PA10T (polydecamethylene terephthalamide) is 316 DEG C. Although this kind of nylon material has extremely high heat resistance, it maintains stable mechanical properties and structural stability at the melting point temperature, which can exactly meet the requirements of lightweight, high-temperature resistance and dimensional stability. However, it is difficult to process and form, and has high requirements for the structure of the product, which is difficult to meet the actual production needs. Compared with the above, nylon 66 (polyhexamethylene adipamide) has good comprehensive mechanical properties, and the melting point is about 260 DEG C, which has good plasticity. However, the stress creep of nylon 66 at high temperature is obvious, and it is easy to deform when used in high-temperature environment, such as automobile engine components, which affects the structural stability of the product and greatly limits the application of nylon products. SUMMARY

[0004] In order to solve the technical problems mentioned in the background, the purpose of the present application is to provide a high-temperature-resistant nylon composite material and a preparation method thereof.

[0005] The purpose of the present application can be achieved by the following technical solutions:

[0006] A high-temperature-resistant nylon composite material, comprising the following raw materials in parts by weight: 100 parts of nylon 66 resin, 13-18 parts of modified aerogel filler, 1.6-2.2 parts of lubricant, 0.12-0.15 parts of antioxidant and 0.2-0.3 parts of light stabilizer.

[0007] The modified aerogel filler is prepared by the following method:

[0008] Step A1: Premix silane coupling agent KH-550 and ethanol aqueous solution, acidify with hydrochloric acid to pH 3-4 and stir for 30-50 min to hydrolyze, add aerogel powder and disperse by ultrasonication, then stir and couple for 4-5 h, filter after the reaction is completed and wash with water and dry to obtain aminated aerogel.

[0009] Furthermore, the aerogel powder has a fineness of 150-200 mesh, which gives it good redispersibility in composite materials.

[0010] Furthermore, the feeding ratio of aerogel powder, silane coupling agent KH-550 and ethanol aqueous solution is 50g:1.7-2.2g:80-100mL. The silane coupling agent KH-550 is hydrolyzed and coupled to the surface of the aerogel powder, introducing surface amino treatment.

[0011] Step A2: Mix p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide and ethyl acetate, heat to 65-75℃ and stir for 2-3 hours. Then add sodium hydroxide intermittently and continue the reaction for 8-10 hours. After the reaction is completed, filter and rotary evaporate. Wash the substrate with water and vacuum dry to obtain the modifier.

[0012] Furthermore, the feed ratio of p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, sodium hydroxide, and ethyl acetate is 10 mmol: 22-25 mmol: 10-15 mg: 0.8-1 g: 20-25 mL. Tetrabutylammonium bromide and sodium hydroxide act as promoters, enabling p-hydroxydiphenyl ether and epichlorohydrin to undergo ring-opening reaction to form oligomers with polyphenolic oxygen chains in the main chain, which are then capped with an excess of epoxy structure.

[0013] Step A3: Premix and disperse the modifier, triethylamine and dimethylacetamide, add the aminated aerogel and disperse ultrasonically, purge with nitrogen for protection, preheat to 40-55℃ and stir for 1-1.5h, then continue to heat to 110-130℃ and reflux for 20-30min, after the reaction is completed, cool and filter, vacuum dry the substrate to obtain the modified aerogel filler;

[0014] Furthermore, the feeding ratio of aminated aerogel, modifier, triethylamine and dimethylacetamide is 50g: 2.5-3.3g: 8-12mL: 60-70mL. Triethylamine is used as an accelerator, which causes the modifier to open the ring with the active amino groups grafted on the surface of the aminated aerogel, forming a polymer coating of polyphenolic blocks in situ on the surface of the aerogel particles.

[0015] A method for preparing a high-temperature resistant nylon composite material is as follows: Nylon 66 resin, lubricant, antioxidant and light stabilizer are mixed evenly using a high-speed mixer, the mixture is melt-extruded and modified aerogel filler is added from the side feed port for compounding, the discharged material is cooled and granulated to obtain the high-temperature resistant nylon composite material.

[0016] Furthermore, the lubricant is a compound of silicone powder and polytetrafluoroethylene powder, which has good lubrication effect at high temperatures, and is beneficial to the dispersion of modified aerogel fillers and the molding of composite materials.

[0017] Furthermore, the barrel temperature zones during the melt extrusion process are set as follows: Zone 1 240-260℃, Zone 2 260-280℃, Zone 3 270-280℃, Zone 4 290-300℃, Zone 5 290-300℃, Zone 7 280-290℃, Zone 8 270-280℃, and die head 260-270℃; multi-zone slow heating is adopted, which is conducive to uniform heating of the melt.

[0018] The beneficial effects of this invention are:

[0019] This invention uses nylon 66 as the matrix material, which, compared to existing high-melting-point, high-temperature-resistant nylon materials, has excellent processability and can be molded by injection molding, compression molding, etc., meeting the manufacturing needs of complex structural products, and offering higher designability and applicability. This invention effectively improves the high-temperature stress creep problem of nylon 66 material by introducing a modified aerogel filler composite through blending. It uses silica-based aerogel powder as the matrix, and introduces surface amino groups through coupling modification with silane coupling agent KH-550. An oligomer containing polyphenolic oxygen chains in the main chain is formed by the ring-opening reaction of p-hydroxydiphenyl ether and epichlorohydrin, and then capped with an excess of epoxy structure. Finally, it undergoes ring-opening with the active amino groups grafted onto the surface of the aminated aerogel. Polymer coatings with polyphenolic oxygen blocks are formed in situ on the surface of aerogel particles. The modified aerogel filler is blended into the nylon 66 matrix. The polyphenolic oxygen segments on its surface form hydrogen bonds with the amide structure in the nylon 66 macromolecule, which improves the compatibility between the modified aerogel filler and the nylon 66 matrix and makes it easier to disperse into the nylon 66 matrix during the blending process. At the same time, the polyphenolic oxygen segments act as templates for hydrogen bond formation, promoting the orderly arrangement of nylon macromolecular chains. The aerogel particles contain a large number of micropores, which slow down the cooling rate of the melt and facilitate the full arrangement of nylon macromolecular chains, thereby forming uniform crystals. In addition, it reduces the internal defects of the composite material, making the composite material less prone to stress creep at high temperatures. Detailed Implementation

[0020] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0021] Example 1: Preparation of high-temperature resistant nylon composite material, as detailed below:

[0022] (1) Preparation of modified aerogel filler

[0023] Step A1: Prepare a 40% (v / v) ethanol aqueous solution. Premix the silane coupling agent KH-550 with the ethanol aqueous solution, add hydrochloric acid for acidification, control the pH value to 4, apply 120 rpm stirring for 30 min for hydrolysis, add aerogel powder and disperse with ultrasonication at 25 kHz for 5 min, then transfer to 60 rpm stirring for coupling for 4 h. The aerogel powder is selected from silica aerogel powder with a fineness of 150 mesh. The feeding ratio of aerogel powder, silane coupling agent KH-550 and ethanol aqueous solution is 50 g: 1.7 g: 80 mL. After the reaction is completed, filter, wash with water and dry to obtain aminated aerogel.

[0024] Step A2: Mix p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide and ethyl acetate, heat to 75°C, and stir at 90 rpm for 2 hours. Take sodium hydroxide powder, divide it into 6 equal portions, and add it intermittently for 30 minutes. After complete addition, maintain constant temperature and stir, and control the total reaction time of sodium hydroxide addition to 8 hours. The feed ratio of p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, sodium hydroxide and ethyl acetate is 10 mmol: 25 mmol: 15 mg: 1 g: 25 mL. After the reaction is completed, filter and rotary evaporate, wash the substrate with water and vacuum dry to obtain the modifier.

[0025] Step A3: Take the modifier, triethylamine and dimethylacetamide premixed and dispersed, add the aminated aerogel and ultrasonically disperse for 15 min, purge with nitrogen for protection, preheat to 55℃, stir at 150 rpm for 1 h, then continue to heat to 130℃ and reflux for 20 min. The feed ratio of aminated aerogel, modifier, triethylamine and dimethylacetamide is 50 g: 2.5 g: 8 mL: 70 mL. After the reaction is completed and cooled, filter and vacuum dry the substrate to obtain the modified aerogel filler.

[0026] (2) Preparation of high temperature resistant nylon composite materials

[0027] Step S1: According to the weight parts, the raw materials are as follows: 100 parts of nylon 66 resin, Zytel 101L type resin raw material is selected; 13 parts of modified aerogel filler, which is self-made in this embodiment; 1.6 parts of lubricant, which is compounded by GM-100Y type silicone powder and ZF11-2 type polytetrafluoroethylene powder in equal mass ratio; 0.15 parts of antioxidant, which is compounded by antioxidant 1790 and antioxidant 412S in a weight ratio of 2:1; 0.3 parts of light stabilizer, selected from Chiguard 5431 type raw material.

[0028] Step S2: Nylon 66 resin, lubricant, antioxidant, and light stabilizer are added to a high-speed mixer according to the specified ratio and mixed at 1200 rpm for 10 minutes. The mixture is then fed into the main feed port of a twin-screw extruder, and the modified aerogel filler is fed into the side feed port. The mixture is then melt-extruded and compounded. During the melt extrusion process, the barrel temperature zones are set as follows: Zone 1 260℃, Zone 2 280℃, Zone 3 280℃, Zone 4 300℃, Zone 5 300℃, Zone 7 290℃, Zone 8 280℃, and the die head 270℃. The discharged material is cooled and granulated to obtain a high-temperature resistant nylon composite material.

[0029] Example 2: Preparation of high-temperature resistant nylon composite material, as detailed below:

[0030] (1) Preparation of modified aerogel filler

[0031] Step A1: Prepare a 50% (v / v) ethanol aqueous solution. Premix the silane coupling agent KH-550 and the ethanol aqueous solution, add hydrochloric acid for acidification, control the pH value to 3, apply 90 rpm stirring for 50 min for hydrolysis, add aerogel powder and disperse with ultrasonication at 28 kHz for 3 min, then transfer to 60 rpm stirring for coupling for 5 h. The aerogel powder is selected from silica aerogel powder with a fineness of 200 mesh. The feeding ratio of aerogel powder, silane coupling agent KH-550 and ethanol aqueous solution is 50 g: 2.2 g: 100 mL. After the reaction is completed, filter, wash with water and dry to obtain aminated aerogel.

[0032] Step A2: Mix p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, and ethyl acetate, heat to 65°C, and stir at 60 rpm for 3 hours. Take sodium hydroxide powder, divide it into 6 equal portions, and add it intermittently for 40 minutes. After complete addition, maintain constant temperature and stir, controlling the total reaction time for sodium hydroxide addition to 10 hours. The feed ratio of p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, sodium hydroxide, and ethyl acetate is 10 mmol: 22 mmol: 10 mg: 0.8 g: 20 mL. After the reaction is complete, filter and rotary evaporate, wash the substrate with water, and vacuum dry to obtain the modifier.

[0033] Step A3: Take the modifier, triethylamine and dimethylacetamide premixed and dispersed, add the aminated aerogel and ultrasonically disperse for 20 min, purge with nitrogen for protection, preheat to 40℃, stir at 120 rpm for 1.5 h, then continue to heat to 110℃ and reflux for 30 min. The feed ratio of aminated aerogel, modifier, triethylamine and dimethylacetamide is 50 g: 3.3 g: 12 mL: 60 mL. After the reaction is completed and cooled, filter and vacuum dry the substrate to obtain the modified aerogel filler.

[0034] (2) Preparation of high temperature resistant nylon composite materials

[0035] Step S1: According to the weight parts, the raw materials are as follows: 100 parts of nylon 66 resin, Zytel 101L type resin raw material is selected; 18 parts of modified aerogel filler, which is self-made in this embodiment; 2.2 parts of lubricant, which is compounded by GM-100Y type silicone powder and ZF11-2 type polytetrafluoroethylene powder in equal mass ratio; 0.12 parts of antioxidant, which is compounded by antioxidant 1790 and antioxidant 412S in a weight ratio of 2:1; 0.2 parts of light stabilizer, selected from Chiguard 5431 type raw material.

[0036] Step S2: Nylon 66 resin, lubricant, antioxidant, and light stabilizer are added to a high-speed mixer according to the specified ratio and mixed at 1200 rpm for 10 minutes. The mixture is then fed into the main feed port of a twin-screw extruder, and the modified aerogel filler is fed into the side feed port. The mixture is then melt-extruded and compounded. During the melt extrusion process, the barrel temperature zones are set as follows: Zone 1 240℃, Zone 2 260℃, Zone 3 270℃, Zone 4 290℃, Zone 5 290℃, Zone 7 280℃, Zone 8 270℃, and the die head 260℃. The discharged material is cooled and granulated to obtain a high-temperature resistant nylon composite material.

[0037] Example 3: Preparation of high-temperature resistant nylon composite material, as detailed below:

[0038] (1) Preparation of modified aerogel filler

[0039] Step A1: Prepare a 40% (v / v) ethanol aqueous solution. Premix the silane coupling agent KH-550 and the ethanol aqueous solution, add hydrochloric acid for acidification, control the pH value to 3, apply 120 rpm stirring for 40 min for hydrolysis, add aerogel powder and disperse with ultrasonication at 28 kHz for 3 min, then transfer to 60 rpm stirring for coupling for 4.5 h. The aerogel powder is selected from silica aerogel powder with a fineness of 200 mesh. The feeding ratio of aerogel powder, silane coupling agent KH-550 and ethanol aqueous solution is 50 g: 1.9 g: 90 mL. After the reaction is completed, filter, wash with water and dry to obtain aminated aerogel.

[0040] Step A2: Mix p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, and ethyl acetate, heat to 70°C, and stir at 90 rpm for 2.5 h. Take sodium hydroxide powder, divide it into 6 equal portions, and add it intermittently for 30 min. After complete addition, maintain constant temperature and stir, controlling the total reaction time for sodium hydroxide addition to 9 h. The feed ratio of p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, sodium hydroxide, and ethyl acetate is 10 mmol: 23 mmol: 12 mg: 0.9 g: 25 mL. After the reaction is complete, filter and rotary evaporate, wash the substrate with water and vacuum dry to obtain the modifier.

[0041] Step A3: Take the modifier, triethylamine and dimethylacetamide premixed and dispersed, add the aminated aerogel and ultrasonically disperse for 20 min, purge with nitrogen for protection, preheat to 50℃, stir at 150 rpm for 1.2 h, then continue to heat to 120℃ and reflux for 25 min. The feed ratio of aminated aerogel, modifier, triethylamine and dimethylacetamide is 50 g: 2.8 g: 10 mL: 60 mL. After the reaction is completed and cooled, filter and vacuum dry the substrate to obtain the modified aerogel filler.

[0042] (2) Preparation of high temperature resistant nylon composite materials

[0043] Step S1: According to the weight parts, the raw materials are as follows: 100 parts of nylon 66 resin, Zytel 101L type resin raw material is selected; 15 parts of modified aerogel filler, which is self-made in this embodiment; 1.8 parts of lubricant, which is compounded by GM-100Y type silicone powder and ZF11-2 type polytetrafluoroethylene powder in equal mass ratio; 0.13 parts of antioxidant, which is compounded by antioxidant 1790 and antioxidant 412S in a weight ratio of 2:1; 0.2 parts of light stabilizer, selected from Chiguard 5431 type raw material.

[0044] Step S2: Nylon 66 resin, lubricant, antioxidant, and light stabilizer are added to a high-speed mixer according to the specified ratio and mixed at 1200 rpm for 10 minutes. The mixture is then fed from the main feed port of a twin-screw extruder, and the modified aerogel filler is fed from the side feed port. The mixture is then melt-extruded and compounded. During the melt extrusion process, the barrel temperature zones are set as follows: Zone 1 250℃, Zone 2 280℃, Zone 3 280℃, Zone 4 290℃, Zone 5 300℃, Zone 7 290℃, Zone 8 270℃, and the die head 260℃. The discharged material is cooled and granulated to obtain a high-temperature resistant nylon composite material.

[0045] Example 4: Preparation of high-temperature resistant nylon composite material, as detailed below:

[0046] (1) Preparation of modified aerogel filler

[0047] Step A1: Prepare a 50% (v / v) ethanol aqueous solution. Premix the silane coupling agent KH-550 and the ethanol aqueous solution, add hydrochloric acid for acidification, control the pH value to 3, apply 120 rpm stirring for 50 min for hydrolysis, add aerogel powder and disperse with ultrasonication at 28 kHz for 5 min, then transfer to 60 rpm stirring for coupling for 4-5 h. The aerogel powder is selected from silica aerogel powder with a fineness of 180 mesh. The feeding ratio of aerogel powder, silane coupling agent KH-550 and ethanol aqueous solution is 50 g: 2 g: 100 mL. After the reaction is completed, filter, wash with water and dry to obtain aminated aerogel.

[0048] Step A2: Mix p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, and ethyl acetate, heat to 70°C, and stir at 90 rpm for 2.8 h. Take sodium hydroxide powder, divide it into 6 equal portions, and add it intermittently for 40 min. After complete addition, maintain constant temperature and stir, controlling the total reaction time for sodium hydroxide addition to 9 h. The feed ratio of p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, sodium hydroxide, and ethyl acetate is 10 mmol: 25 mmol: 12 mg: 0.9 g: 25 mL. After the reaction is complete, filter and rotary evaporate, wash the substrate with water and vacuum dry to obtain the modifier.

[0049] Step A3: Take the modifier, triethylamine and dimethylacetamide premixed and dispersed, add the aminated aerogel and ultrasonically disperse for 20 min, purge with nitrogen for protection, preheat to 50℃, stir at 150 rpm for 1.5 h, then continue to heat to 120℃ and reflux for 20 min. The feed ratio of aminated aerogel, modifier, triethylamine and dimethylacetamide is 50 g: 3.1 g: 12 mL: 70 mL. After the reaction is completed and cooled, filter and vacuum dry the substrate to obtain the modified aerogel filler.

[0050] (2) Preparation of high temperature resistant nylon composite materials

[0051] Step S1: According to the weight parts, the raw materials are as follows: 100 parts of nylon 66 resin, Zytel 101L type resin raw material is selected; 16 parts of modified aerogel filler, which is self-made in this embodiment; 2 parts of lubricant, which is compounded by GM-100Y type silicone powder and ZF11-2 type polytetrafluoroethylene powder in equal mass ratio; 0.13 parts of antioxidant, which is compounded by antioxidant 1790 and antioxidant 412S in a weight ratio of 2:1; 0.2 parts of light stabilizer, selected from Chiguard 5431 type raw material.

[0052] Step S2: Nylon 66 resin, lubricant, antioxidant, and light stabilizer are added to a high-speed mixer according to the specified ratio and mixed at 1200 rpm for 10 minutes. The mixture is then fed into the main feed port of a twin-screw extruder, and the modified aerogel filler is fed into the side feed port. The mixture is then melt-extruded and compounded. During the melt extrusion process, the barrel temperature zones are set as follows: Zone 1 250℃, Zone 2 270℃, Zone 3 280℃, Zone 4 300℃, Zone 5 300℃, Zone 7 290℃, Zone 8 280℃, and the die head 260℃. The discharged material is cooled and granulated to obtain a high-temperature resistant nylon composite material.

[0053] Comparative Example 1: This comparative example is based on Example 4, except that the modified aerogel filler is replaced with an equal amount of aminated aerogel, and the rest of the implementation process is exactly the same.

[0054] Comparative Example 2: Based on Comparative Example 1, 0.3 parts of BRUGGOLEN P22 nucleating agent were added and blended with Nylon 66 resin. The rest of the implementation process was exactly the same.

[0055] The above composite material was molded into sheets at a temperature of 280℃ and a pressure of 8MPa. Samples were taken from the prepared sheets for the following tests:

[0056] Tensile test: Following GB / T 1040.2-2022 standard, the tensile rate was 50 mm / min; Creep test: Temperature was 150℃, stress was 10 MPa, and test cycles were 24h, 36h, and 48h respectively; Specific test results are shown in Table 1.

[0057] Table 1

[0058]

[0059] As shown in Table 1, the composite material prepared in the example maintains high mechanical strength. The introduction of modified aerogel filler has a certain strengthening effect. The stress creep at 150℃ is much lower than that of the comparative example, and it has excellent high-temperature stress creep resistance. It can effectively maintain the structural stability of the product at high temperature.

[0060] Samples were taken from the above composite material and tested as follows:

[0061] DSC test: The sample was heated to 290℃ to eliminate thermal history, then cooled to room temperature, and then heated to 300℃ again. The heating and cooling rates were both 10℃ / min. The crystallinity of the composite material was then calculated.

[0062] WAXD testing: The sample was heated to 290℃ to eliminate thermal history, then cooled to room temperature, and then heated to 200℃ for isothermal crystallization. The heating and cooling rates were both 10℃ / min, the test scan rate was 5° / min, and the scan angle was 5-60°. The Brill temperature of the composite material was calculated. The specific test results are shown in Table 2.

[0063] Table 2

[0064]

[0065] As shown in Table 2, both Example 1 and Comparative Example 2 have high crystallinity, while Example 2 has a Brill transition temperature of over 180°C, indicating higher heat resistance and stability.

[0066] In the description of this specification, the references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0067] The above description is merely an example and illustration of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.

Claims

1. A high-temperature resistant nylon composite material, characterized in that, The composition by weight is as follows: 100 parts nylon 66 resin, 13-18 parts modified aerogel filler, 1.6-2.2 parts lubricant, 0.12-0.15 parts antioxidant and 0.2-0.3 parts light stabilizer; The modified aerogel filler is prepared by the following method: Step A1: Premix silane coupling agent KH-550 and ethanol aqueous solution, acidify with hydrochloric acid to pH 3-4 and stir for 30-50 min to hydrolyze, add silica aerogel powder and ultrasonically disperse, then stir and couple for 4-5 h, filter and wash with water to dry to obtain aminated aerogel. Step A2: Mix p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide and ethyl acetate, heat to 65-75℃ and stir for 2-3 hours. Then add sodium hydroxide intermittently and continue the reaction for 8-10 hours. After the reaction is completed, filter and rotary evaporate. Wash the substrate with water and vacuum dry to obtain the modifier. Step A3: Premix and disperse the modifier, triethylamine and dimethylacetamide, add the aminated aerogel and disperse ultrasonically, purge with nitrogen for protection, preheat to 40-55℃ and stir for 1-1.5h, then continue to heat to 110-130℃ and reflux for 20-30min, after the reaction is completed, cool and filter, vacuum dry the substrate to obtain the modified aerogel filler.

2. The high-temperature resistant nylon composite material according to claim 1, characterized in that, The aerogel powder has a fineness of 150-200 mesh.

3. The high-temperature resistant nylon composite material according to claim 2, characterized in that, The feeding ratio of silica aerogel powder, silane coupling agent KH-550 and ethanol aqueous solution is 50g: 1.7-2.2g: 80-100mL.

4. The high-temperature resistant nylon composite material according to claim 1, characterized in that, The feed ratio of p-hydroxydiphenyl ether, epichlorohydrin, tetrabutylammonium bromide, sodium hydroxide and ethyl acetate is 10 mmol: 22-25 mmol: 10-15 mg: 0.8-1 g: 20-25 mL.

5. A high-temperature resistant nylon composite material according to any one of claims 1-4, characterized in that, The feeding ratio of aminated aerogel, modifier, triethylamine and dimethylacetamide is 50g: 2.5-3.3g: 8-12mL: 60-70mL.

6. The method for preparing a high-temperature resistant nylon composite material according to claim 1, characterized in that, Specifically, the process involves mixing nylon 66 resin, lubricant, antioxidant, and light stabilizer, melting and extruding the mixture, adding modified aerogel filler through a side feed port, cooling and granulating the discharged material to obtain a high-temperature resistant nylon composite material.

7. The method for preparing a high-temperature resistant nylon composite material according to claim 6, characterized in that, The lubricant is a compound of silicone powder and polytetrafluoroethylene powder.

Citation Information

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