Transparent nylon material as well as preparation method and application thereof

By combining transparent nylon prepolymer with polyetheramine, and utilizing the hydrophilicity and polarity of polyetheramine to form a conductive path, the performance balance problem of antistatic transparent nylon material is solved, achieving high antistatic properties, excellent mechanical properties, and high light transmittance.

CN121537784APending Publication Date: 2026-02-17DONGGUAN AONENG ENG PLASTICS CO LTD SHANGHAI BRANCH
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Patent Information

Application Number
CN202511968481.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-24
Publication Date
2026-02-17

AI Technical Summary

Technical Problem

Existing antistatic transparent nylon materials struggle to balance antistatic durability, high light transmittance, and good mechanical properties.

Method used

By combining transparent nylon prepolymer with polyetheramine, the polyether segments in the polyetheramine adsorb moisture to form a conductive path. The interaction between the polarity of the amino group and the molecular chain of the transparent nylon material improves the antistatic properties while maintaining good mechanical properties and light transmittance.

Benefits of technology

The prepared transparent nylon material has excellent antistatic properties, good mechanical properties, high light transmittance and excellent solvent resistance. It also has excellent tensile strength, modulus, flexural strength and hardness, high light transmittance, low surface resistivity and resistance to ethanol and gasoline.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a transparent nylon material as well as a preparation method and application thereof. The transparent nylon material is prepared from the following raw materials: a transparent nylon prepolymer and polyether amine, the transparent nylon prepolymer is prepared from the following raw materials: binary acid, diamine and an end-capping reagent. The transparent nylon prepolymer is prepared from the binary acid, the diamine and the end-capping reagent, and then the transparent nylon prepolymer reacts with the polyether amine to prepare the transparent nylon material, so that the transparent nylon material has excellent antistatic performance, good mechanical properties, high light transmittance and excellent solvent resistance.
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Description

Technical Field

[0001] This invention belongs to the field of nylon material technology, and particularly relates to a transparent nylon material, its preparation method and application. Background Technology

[0002] Transparent nylon, as a high-performance amorphous or microcrystalline thermoplastic engineering plastic, occupies an important position in the materials field due to its unique performance advantages. It not only inherits the excellent mechanical strength, abrasion resistance, chemical resistance, and fatigue resistance of traditional nylon, but more importantly, it possesses high light transmittance and low haze. This characteristic allows it to successfully overcome the milky-white appearance limitations caused by the crystallization of traditional nylon materials, and it is widely used in fields with stringent requirements for visual clarity, such as precision optical instruments, electronic component packaging, food packaging, medical equipment, and the eyewear industry.

[0003] However, with the rapid development of high-tech industries, especially in fields such as electronic manufacturing, semiconductor packaging, and precision instrument transportation and storage, materials face increasingly complex challenges. In these applications, electrostatic accumulation has become a critical issue that cannot be ignored. Common polymer materials, including basic transparent nylon, are excellent insulators. This property makes them highly susceptible to generating and accumulating static charges during friction, contact, or separation.

[0004] Currently, the main methods for imparting antistatic properties to nylon include adding antistatic agents and copolymerization. CN103390497A achieves a light transmittance of 89%~90% and a surface resistivity ≤10 by adjusting the amount of antistatic agent (ethoxylauramide) to 2%. 11 CN115926153A discloses a method for preparing a bio-based transparent nylon material. Using a compound containing ether bonds and a diamine compound, under nitrogen protection, a one-pot method is used to prepare the bio-based transparent nylon material. This material exhibits high transparency, low haze, and excellent mechanical properties, with a light transmittance of 92% and a surface resistivity of 10⁻⁶. 9 Ω, suitable for eyeglass lenses.

[0005] CN114276679A discloses an antistatic transparent nylon material, comprising the following raw materials in parts by weight: transparent nylon: 700-800 parts; antistatic agent: 180-240 parts; light stabilizer: 2-10 parts; antioxidant: 1-3 parts; lubricant: 1-3 parts; nanowire-modified carbon nanotubes: 0.1-0.7 parts; and palladium-modified powder: 0.1-0.3 parts. This patent describes a high-performance antistatic material prepared by adding an antistatic agent and compounding alkyl sulfonate with nanowire-modified carbon nanotubes, achieving a surface resistivity of 8.5 × 10⁻⁶. 10 Ω-6.2×10 7 Ω, light transmittance 85%-90%, tensile strength 113-120MPa.

[0006] CN105330852B discloses a bio-based long-chain transparent nylon, which is copolymerized with isophthalic acid, decanediamine, adipic acid and polyesteramide, and the addition of a crystallization promoter (long-chain calcium carboxylate) and a molecular weight regulator (benzoic acid) improves the notched impact strength and antistatic ability of the copolymer. The material has a water absorption rate of less than 1%, a light transmittance of 90%, and a surface resistivity of 10. 9 Ω, heat distortion temperature 120℃.

[0007] CN111363349A discloses a flame-retardant and antistatic reinforced nylon composite material, the raw materials of which include the following components by weight: 60-90 parts nylon, 5-15 parts glass fiber, 3-10 parts carbon fiber, 0.5-10 parts carbon nanotubes, 10-15 parts red phosphorus, 0.3-2 parts borate alkylamine, 0-1.5 parts lubricant, and 0.3-3 parts composite additives. This patent improves the antistatic effect and mechanical properties of the composite material by compounding carbon nanotubes with borate alkylamine and adding an appropriate amount of carbon fiber. However, existing antistatic transparent nylon materials struggle to balance antistatic durability, high light transmittance, and good mechanical properties.

[0008] Therefore, developing an antistatic transparent nylon material with good mechanical properties and solvent resistance is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0009] In view of the shortcomings of the prior art, the purpose of this invention is to provide a transparent nylon material, its preparation method and application, wherein the transparent nylon material has excellent antistatic properties, good mechanical properties, high light transmittance and excellent solvent resistance.

[0010] To achieve this objective, the present invention adopts the following technical solution:

[0011] In a first aspect, the present invention provides a transparent nylon material, wherein the raw materials for preparing the transparent nylon material include the following components:

[0012] Transparent nylon prepolymer and polyetheramine;

[0013] The raw materials for preparing the transparent nylon prepolymer include the following components:

[0014] Dicarboxylic acid, diamine, and capping agent.

[0015] This invention prepares a transparent nylon prepolymer using a diacid, a diamine, and a capping agent, and then reacts it with a polyetheramine to prepare a transparent nylon material. The polyether segments in the polyetheramine are hydrophilic, capable of adsorbing moisture from the air. This moisture forms a continuous, thin water film on the surface of the transparent nylon material, creating a conductive pathway that allows accumulated static charge to be quickly discharged. The amino groups in the polyetheramine are polar and have a certain degree of conductivity, allowing them to interact with the electrostatic charges on the molecular chains of the transparent nylon material, thereby improving its antistatic properties. Simultaneously, the transparent nylon material also exhibits good mechanical properties, high light transmittance, and solvent resistance.

[0016] The following are preferred technical solutions of the present invention, but are not intended to limit the technical solutions provided by the present invention. The purpose and beneficial effects of the present invention can be better achieved and realized through the following preferred technical solutions.

[0017] Preferably, the mass ratio of the transparent nylon prepolymer to the polyetheramine is 100:(5-25), such as 100:5, 100:7, 100:9, 100:11, 100:13, 100:15, 100:17, 100:19, 100:21, 100:23, or 100:25.

[0018] If the mass ratio of the two is too high, that is, if the amount of polyetheramine is too low, the antistatic properties of the transparent nylon material cannot be effectively improved; if the mass ratio of the two is too low, that is, if the amount of polyetheramine is too high, the tensile strength, tensile modulus, flexural strength and hardness of the transparent nylon material will decrease.

[0019] Preferably, the number average molecular weight of the polyetheramine is 500-5000 (e.g., 500, 1000, 1500, 2000, 2500, 3000, 3500, 4000, 4500 or 5000, etc.), more preferably 500-3000, and even more preferably 900-2000.

[0020] Preferably, the molar ratio of the dicarboxylic acid to the diamine is (0.9-1.1):1, for example, 0.9:1, 1:1 or 1.1:1.

[0021] Preferably, the dicarboxylic acid includes any one or a combination of at least two of isophthalic acid, terephthalic acid, adipic acid, sebacic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, or hexadecanoic acid.

[0022] Preferably, the diamine comprises any one or a combination of at least two of 4,4'-diaminodicyclohexylmethane, pentanediamine, hexanediamine, decacarbonylamine, undecanoic acid, dodecacarbonylamine, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, or hexadecanoic acid.

[0023] Preferably, at least one of the dicarboxylic acid and diamine is a combination of two or more types.

[0024] Preferably, the dicarboxylic acid includes at least isophthalic acid.

[0025] Preferably, when there are two or more dicarboxylic acids, the proportion of isophthalic acid is ≥20%, with the molar amount of dicarboxylic acid being 100%, for example, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, or 90%, etc.

[0026] Preferably, the capping agent comprises a dibasic acid and / or an anhydride.

[0027] Preferably, the dicarboxylic acid includes any one or a combination of at least two of adipic acid, sebacic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, or hexadecanoic acid.

[0028] Preferably, the acid anhydride includes any one or a combination of at least two of maleic anhydride, phthalic anhydride, succinic anhydride, or acetic anhydride.

[0029] Preferably, based on the mass of the transparent nylon prepolymer, the amount of the capping agent is 0.01-1%, such as 0.01%, 0.1%, 0.2%, 0.4%, 0.6%, 0.8%, or 1%.

[0030] Preferably, the raw materials for preparing the transparent nylon prepolymer further include a first catalyst.

[0031] Preferably, the first catalyst comprises any one or a combination of at least two of phosphoric acid, p-toluenesulfonic acid, zinc acetate, sodium hypophosphite, calcium hypophosphite, or manganese acetate.

[0032] Preferably, based on the mass of the transparent nylon prepolymer, the amount of the first catalyst is 0.01-0.1%, such as 0.01%, 0.03%, 0.05%, 0.07%, 0.09%, or 0.1%.

[0033] Preferably, the raw materials for preparing the transparent nylon material further include a second catalyst and / or an antioxidant.

[0034] Preferably, the second catalyst comprises any one or a combination of at least two of tetrabutyl titanate, stannous octoate, zinc acetate, or phosphorous acid.

[0035] Preferably, the antioxidant comprises any one or a combination of at least two of the following: N,N'-bis-(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl)hexamethylenediamine (antioxidant 1098), pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] (antioxidant 1010), octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate (antioxidant 1076), 4,4'-thiobis(6-tert-butyl-3-methylphenol) (antioxidant 330), or bis-stearyl thiodipropionate.

[0036] Preferably, the amount of antioxidant is 0.01-1% based on 100% of the mass of the transparent nylon prepolymer, such as 0.01%, 0.1%, 0.2%, 0.4%, 0.6%, 0.8% or 1%.

[0037] In a second aspect, the present invention provides a method for preparing a transparent nylon material as described in the first aspect, the method comprising the following steps:

[0038] (1) A diacid, a diamine and a capping agent are mixed and reacted to obtain the transparent nylon prepolymer;

[0039] (2) Mix the transparent nylon prepolymer and polyetheramine and react to obtain the transparent nylon material.

[0040] Preferably, in step (1), the mixed components further include a first catalyst.

[0041] Preferably, in step (1), the reaction includes a salt formation reaction and a prepolymerization reaction.

[0042] Preferably, the temperature of the salt formation reaction is 75-100℃, such as 75℃, 76℃, 78℃, 80℃, 82℃, 84℃, 86℃, 88℃, 90℃, 92℃, 94℃, 96℃, 98℃ or 100℃.

[0043] Preferably, the salt formation reaction time is 30-60 min, for example, 30 min, 35 min, 40 min, 45 min, 50 min, 55 min or 60 min.

[0044] Preferably, the salt-forming reaction is carried out under normal pressure.

[0045] Preferably, in step (2), the mixed components further include a second catalyst and / or an antioxidant.

[0046] Preferably, in step (2), the reaction temperature is 220-270℃, such as 220℃, 225℃, 230℃, 235℃, 240℃, 245℃, 250℃, 255℃, 260℃, 265℃ or 270℃.

[0047] Preferably, in step (2), the reaction is carried out first at atmospheric pressure and then under vacuum.

[0048] Preferably, the pressure of the vacuum is -1.5 to -1 bar, such as -1.5 bar, -1.4 bar, -1.3 bar, -1.2 bar, -1.1 bar, or -1 bar.

[0049] Preferably, the preparation method specifically includes the following steps:

[0050] (1) Mix the diacid, diamine and end-capping agent, control the stirring speed at 100-150 rpm, and carry out the salt formation reaction at 75-100℃ and normal pressure for 30-60 min; control the temperature at 240-245℃ until the pressure rises to 16-20 bar, raise the temperature to 260-276℃ at 10℃ / 10 min, stir at 50-150 rpm, open the pressure holding valve, and carry out the prepolymerization reaction; when the temperature reaches 245-256℃, start to reduce the pressure at a rate of 1.5-2.5 bar / 10 min and a time of 80-100 min until the pressure drops to 0 bar; then evacuate and react for 10-40 min at a pressure of -1.0~-0.8 bar, a stirring speed of 80-120 rpm and a temperature of 245-256℃ to obtain the transparent nylon prepolymer;

[0051] (2) The transparent nylon prepolymer, polyetheramine, second catalyst and antioxidant are mixed and stirred at 220-270℃ and normal pressure for 30-60 min. Then the pressure is controlled at -1.5~-1 bar and the reaction is carried out for 0.5-2 h. The mixture is then extruded, cooled and granulated to obtain the transparent nylon material.

[0052] Thirdly, the present invention provides the application of the transparent nylon material as described in the first aspect in precision optical instruments, electronic component packaging, food packaging, medical devices, or eyeglasses.

[0053] Compared with the prior art, the present invention has the following beneficial effects:

[0054] The transparent nylon material prepared by this invention possesses excellent antistatic properties, good mechanical properties, high light transmittance, and excellent solvent resistance. Specifically, its tensile strength is above 61 MPa, tensile modulus is above 2000 MPa, elongation at break is above 65%, flexural strength is above 65 MPa, Shore hardness is between 55 and 80 HD, light transmittance is above 85%, haze is below 4%, it is resistant to ethanol and gasoline, and its surface resistivity is (0.9-9) × 10⁻⁶. 10 Ω. Detailed Implementation

[0055] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0056] The source information of some raw materials used in the embodiments and comparative examples of this invention is as follows:

[0057] Polyetheramine: Huntsman, ED900.

[0058] Example 1

[0059] This embodiment provides a transparent nylon material and its preparation method, the preparation method including the following steps:

[0060] (1) 464.95g adipic acid, 880.92g terephthalic acid, 381.49g isophthalic acid, 739.43g hexamethylenediamine, and 892.32g... 4,4'-Diaminodicyclohexylmethane, 14.0 g sebacic acid, and 3.0 g p-toluenesulfonic acid were added to a polymerization reactor. The oil temperature was set at 80°C, the stirring speed at 120 rpm, and the salt formation reaction was carried out at atmospheric pressure for 40 min. The oil temperature was then set to 240°C until the pressure reached 17 bar. The oil temperature was then increased to 265°C at a rate of 10°C / 10 min, with the stirring speed at 100 rpm. The pressure holding valve was opened, and the pressure inside the reactor was controlled at 17 bar to carry out the prepolymerization reaction. When the material temperature reached 250°C, the pressure was reduced at a rate of 2 bar / 10 min for 90 min until the pressure dropped to 0 bar. Then, a vacuum was applied, and the reaction was carried out at a vacuum of -0.9 bar, a stirring speed of 100 rpm, and a temperature of 250°C for 25 min to obtain the transparent nylon prepolymer.

[0061] (2) The transparent nylon prepolymer, 175.3g of polyetheramine (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:5.3), 1.9g of tetrabutyl titanate and 2.8g of antioxidant 1010 were added to the reactor and stirred at normal pressure for 30min. The reaction was carried out at a pressure of -1.2bar and 250℃ for 1h. Finally, the mixture was extruded, cooled, and granulated using a pelletizer to obtain the transparent nylon material.

[0062] Example 2

[0063] This embodiment provides a transparent nylon material and its preparation method, the preparation method including the following steps:

[0064] (1) 464.95g adipic acid, 880.92g terephthalic acid, 413.84g isophthalic acid, 739.43g hexamethylenediamine, and 892.32g... 4,4'-Diaminodicyclohexylmethane, 12.5g maleic anhydride, and 2.8g phosphoric acid were added to a polymerization reactor. The oil temperature was set at 75℃, the stirring speed at 150rpm, and the salt formation reaction was carried out at atmospheric pressure for 60min. The oil temperature was then set to 240℃ until the pressure reached 18bar. The oil temperature was then increased to 275℃ at a rate of 10℃ / 10min, with a stirring speed of 70rpm. The pressure-holding valve was opened, and the pressure inside the reactor was controlled at 18bar to carry out the prepolymerization reaction. When the material temperature reached 245℃, the pressure was reduced at a rate of 1.5bar / 10min for 100min until the pressure dropped to 0bar. Then, a vacuum was applied, and the reaction was carried out at a vacuum of -0.8bar, a stirring speed of 80rpm, and a temperature of 245℃ for 40min to obtain the transparent nylon prepolymer.

[0065] (2) The transparent nylon prepolymer, 370g of polyetheramine (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:11.1), 2.2g of tetrabutyl titanate and 2.3g of antioxidant 1076 were added to the reactor and stirred at normal pressure for 50min. The reaction was carried out at a pressure of -1.5bar and 270℃ for 0.5h. Finally, the mixture was extruded, cooled, and granulated using a pelletizer to obtain the transparent nylon material.

[0066] Example 3

[0067] This embodiment provides a transparent nylon material and its preparation method, the preparation method including the following steps:

[0068] (1) 464.95g adipic acid, 880.92g terephthalic acid, 449.99g isophthalic acid, 739.43g hexamethylenediamine, and 892.32g... 4,4'-Diaminodicyclohexylmethane, 5.3g undecanoic acid, and 1.9g sodium hypophosphite were added to a polymerization reactor. The oil temperature was set to 100℃, the stirring speed to 100rpm, and the salt formation reaction was carried out at atmospheric pressure for 30min. The oil temperature was then set to 240℃ until the pressure reached 16bar. The oil temperature was then increased to 255℃ at a rate of 10℃ / 10min, with a stirring speed of 150rpm. The pressure-holding valve was opened, and the pressure inside the reactor was controlled at 16bar to carry out the prepolymerization reaction. When the material temperature reached 250℃, the pressure was reduced at a rate of 2.5bar / 10min for 80min until the pressure dropped to 0bar. Then, a vacuum was applied, and the reaction was carried out at a vacuum of -1.0bar, a stirring speed of 120rpm, and a temperature of 250℃ for 10min to obtain the transparent nylon prepolymer.

[0069] (2) The transparent nylon prepolymer, 587.6g of polyetheramine (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:17.6), 2.8g of stannous octoate and 1.6g of antioxidant 330 were added to the reactor and stirred at normal pressure for 30min. The reaction was carried out at a pressure of -1bar and 220℃ for 2h. Finally, the mixture was extruded, cooled, and granulated using a pelletizer to obtain the transparent nylon material.

[0070] Example 4

[0071] This embodiment provides a transparent nylon material and its preparation method, the preparation method including the following steps:

[0072] (1) 464.95g adipic acid, 880.92g terephthalic acid, 490.67g isophthalic acid, 739.43g hexamethylenediamine, and 892.32g... 4,4'-Diaminodicyclohexylmethane, 14.0 g sebacic acid, and 3.0 g p-toluenesulfonic acid were added to a polymerization reactor. The oil temperature was set at 80°C, the stirring speed at 120 rpm, and the salt formation reaction was carried out at atmospheric pressure for 40 min. The oil temperature was then set to 240°C until the pressure reached 17 bar. The oil temperature was then increased to 265°C at a rate of 10°C / 10 min, with the stirring speed at 100 rpm. The pressure holding valve was opened, and the pressure inside the reactor was controlled at 17 bar to carry out the prepolymerization reaction. When the material temperature reached 250°C, the pressure was reduced at a rate of 2 bar / 10 min for 90 min until the pressure dropped to 0 bar. Then, a vacuum was applied, and the reaction was carried out at a vacuum of -0.9 bar, a stirring speed of 100 rpm, and a temperature of 250°C for 25 min to obtain the transparent nylon prepolymer.

[0073] (2) The transparent nylon prepolymer, 832.5g of polyetheramine (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:25), 1.2g of stannous octoate and 2.8g of antioxidant 1010 are added to the reactor and stirred at normal pressure for 50min. The reaction is carried out at a pressure of -1.2bar and 250℃ for 1h. Finally, the mixture is extruded, cooled, and granulated using a pelletizer to obtain the transparent nylon material.

[0074] Example 5

[0075] The difference from Example 1 is that the dicarboxylic acid used is 587.81g of terephthalic acid and 1044.62g of isophthalic acid; the diamine used is 1370.58g of hexamethylenediamine and 175.3g of polyetheramine (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:5.3). The amounts of other components and the preparation methods are the same as in Example 1.

[0076] Example 6

[0077] The difference from Example 1 is that the dicarboxylic acid used is 587.81g of terephthalic acid and 1432.97g of isophthalic acid; the diamine used is 1370.58g of hexamethylenediamine; and the polyetheramine is 370g (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:11.1). The amounts of the remaining components and the preparation methods are the same as in Example 1.

[0078] Example 7

[0079] The difference from Example 1 is that the dicarboxylic acid used is 587.81g of terephthalic acid and 1469.11g of isophthalic acid; the diamine used is 1370.58g of hexamethylenediamine; and the polyetheramine is 587.6g (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:17.6). The amounts of the remaining components and the preparation methods are the same as in Example 1.

[0080] Example 8

[0081] The difference from Example 1 is that the dicarboxylic acid used is 587.81g of terephthalic acid and 1509.8g of isophthalic acid; the diamine used is 1370.58g of hexamethylenediamine; and the polyetheramine is 832.5g (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:25). The amounts of the remaining components and the preparation methods are the same as in Example 1.

[0082] Example 9

[0083] The difference from Example 1 is that the dicarboxylic acid used is 691.53g of terephthalic acid and 1066.42g of isophthalic acid; the diamine used is 725.57g of hexamethylenediamine and 875.6g of 4,4'-diaminodicyclohexylmethane (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:5.3), and the amounts and preparation methods of the remaining components are the same as in Example 1.

[0084] Example 10

[0085] The difference from Example 1 is that the dicarboxylic acid used is 691.53g of terephthalic acid and 1098.76g of isophthalic acid; the diamine used is 725.57g of hexamethylenediamine and 875.6g of 4,4'-diaminodicyclohexylmethane; and the polyetheramine is 370g (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:11.1). The amounts of the remaining components and the preparation methods are the same as in Example 1.

[0086] Example 11

[0087] The difference from Example 1 is that: the dicarboxylic acid used is 691.53g of terephthalic acid and 1134.91g of isophthalic acid; the diamine used is 725.57g of hexamethylenediamine and 875.6g of 4,4'-diaminodicyclohexylmethane; and the polyetheramine is 587.6g (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:17.6). The amounts of the remaining components and the preparation methods are the same as in Example 1.

[0088] Example 12

[0089] The difference from Example 1 is that the dicarboxylic acid used is 691.53g of terephthalic acid and 1175.60g of isophthalic acid; the diamine used is 725.57g of hexamethylenediamine and 875.6g of 4,4'-diaminodicyclohexylmethane; and 832.5g of polyetheramine (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:25). The amounts and preparation methods of the remaining components are the same as in Example 1.

[0090] Example 13

[0091] The difference from Example 1 is that the amount of polyetheramine used is 99.2g (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:3), while the amount of other components and the preparation method are the same as in Example 1.

[0092] Example 14

[0093] The difference from Example 1 is that the amount of polyetheramine used is 992g (the mass ratio of transparent nylon prepolymer to polyetheramine is 100:30), while the amount of other components and the preparation method are the same as in Example 1.

[0094] Comparative Example 1

[0095] The difference from Example 1 is that in step (1), in the final condensation vacuum stage, under the conditions of vacuum degree of -0.9 bar, stirring rate of 100 rpm and temperature of 250°C, the reaction continues for 70 min to obtain transparent nylon material.

[0096] Performance testing:

[0097] (1) Tensile strength: Tested in accordance with ISO 527-1.

[0098] (2) Stretch film weight: Tested in accordance with ISO 527-1.

[0099] (3) Elongation at break: Tested in accordance with ISO 527-1.

[0100] (4) Bending strength: Tested in accordance with ISO 178.

[0101] (5) Shore hardness: tested according to ISO 2039-2 Shore hardness tester.

[0102] (6) Light transmittance: Tested according to ISO 13468.

[0103] (7) Haze: Tested according to ISO 14782.

[0104] (8) Ethanol resistance: Immerse the material in ethanol for 72 h and judge whether there is swelling.

[0105] (9) Gasoline resistance: Immerse the material in gasoline for 72 hours and judge whether there is swelling.

[0106] (10) Surface resistivity: Tested in accordance with ISO 3915.

[0107] The performance of the transparent nylon materials provided in the examples and comparative examples was tested, and the results are shown in Tables 1-2:

[0108] Table 1

[0109]

[0110] Table 2

[0111]

[0112] As shown in Tables 1-2, the transparent nylon materials prepared in Examples 1-12 of this invention possess excellent antistatic properties, good mechanical properties, high light transmittance, and excellent solvent resistance. Specifically, their tensile strength is above 61 MPa, tensile modulus is above 2000 MPa, elongation at break is above 65%, flexural strength is above 65 MPa, Shore hardness is between 55 and 80 HD, light transmittance is above 85%, haze is below 4%, they are resistant to ethanol and gasoline, and their surface resistivity is (0.9-9) × 10⁻⁶. 10 Ω.

[0113] The comparison between Examples 1 and Examples 13-14 shows that if the amount of polyetheramine is small, the antistatic properties of the transparent nylon material will decrease significantly; if the amount of polyetheramine is large, the tensile strength, tensile modulus, flexural strength and hardness of the transparent nylon material will decrease.

[0114] A comparison between Example 1 and Comparative Example 1 shows that the surface resistivity of the transparent nylon material in Comparative Example 1 is as high as 20000 × 10⁻⁶. 10 Ω indicates that polyetheramine can significantly improve the antistatic properties of transparent nylon materials.

[0115] The above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A transparent nylon material, characterized by, The raw material for preparing the transparent nylon material comprises the following components: a transparent nylon prepolymer and a polyether amine; The raw material for preparing the transparent nylon prepolymer comprises the following components: a dibasic acid, a dibasic amine and a capping agent.

2. The transparent nylon material of claim 1, wherein, The mass ratio of the transparent nylon prepolymer and the polyether amine is 100:(5-25); Preferably, the number average molecular weight of the polyether amine is 500-5000, further preferably 500-3000, and still further preferably 900-2000; Preferably, the molar ratio of the dibasic acid and the dibasic amine is (0.9-1.1):1; Preferably, the dibasic acid comprises any one or a combination of at least two of isophthalic acid, terephthalic acid, adipic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid or hexadecanedioic acid; Preferably, the dibasic amine comprises any one or a combination of at least two of 4,4'-diaminodicyclohexyl methane, pentanediamine, hexanediamine, decanediamine, undecanediamine, dodecanediamine, tridecanediamine, tetradecanediamine, pentadecanediamine or hexadecanediamine; Preferably, at least one of the dibasic acid and the dibasic amine is a combination of two or more; Preferably, the dibasic acid comprises at least isophthalic acid; Preferably, when the dibasic acid is two or more, the proportion of isophthalic acid is ≥20% based on 100% of the molar amount of the dibasic acid.

3. The transparent nylon material according to claim 1 or 2, characterized in that, The capping agent comprises a dibasic acid and / or an anhydride; Preferably, the dibasic acid comprises any one or a combination of at least two of adipic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid or hexadecanedioic acid; Preferably, the anhydride comprises any one or a combination of at least two of maleic anhydride, phthalic anhydride, succinic anhydride or acetic anhydride; Preferably, the amount of the capping agent is 0.01-1% based on 100% of the mass of the transparent nylon prepolymer.

4. The transparent nylon material according to any one of claims 1-3, wherein, The raw material for preparing the transparent nylon material further comprises a first catalyst; Preferably, the first catalyst comprises any one or a combination of at least two of phosphoric acid, p-toluenesulfonic acid, zinc acetate, sodium hypophosphite, calcium hypophosphite or manganese acetate; Preferably, the amount of the first catalyst is 0.01-0.1% based on 100% of the mass of the transparent nylon prepolymer.

5. The transparent nylon material according to any one of claims 1-4, wherein, The raw material for preparing the transparent nylon material further comprises a second catalyst and / or an antioxidant; Preferably, the second catalyst comprises any one or a combination of at least two of tetrabutyl titanate, stannous octoate, zinc acetate or phosphorous acid; Preferably, the antioxidant comprises any one or a combination of at least two of N,N'-bis-(3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl)hexanediamine, tetra[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid]pentaerythritol ester, β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid n-octadecyl ester, 4,4'-thiobis(6-tert-butyl-3-methylphenol) or distearyl thiodipropionate. Preferably, the antioxidant is used in an amount of 0.01-1% based on 100% of the mass of the transparent nylon prepolymer.

6. The method of making a transparent nylon material according to any one of claims 1-5, wherein, The preparation method comprises the following steps: (1) mixing, reacting diacid, diamine and end-capping agent to obtain the transparent nylon prepolymer; (2) mixing, reacting the transparent nylon prepolymer and polyetheramine to obtain the transparent nylon material.

7. The production method according to claim 6, wherein In step (1), the mixed components further comprise a first catalyst; Preferably, in step (1), the reaction comprises a salt formation reaction and a prepolymerization reaction; Preferably, the salt formation reaction is carried out at a temperature of 75-100℃; Preferably, the salt formation reaction is carried out for 30-60 min; Preferably, the salt formation reaction is carried out under normal pressure.

8. The production method according to claim 6 or 7, characterized by, In step (2), the mixed components further comprise a second catalyst and / or an antioxidant; Preferably, in step (2), the reaction is carried out at a temperature of 220-270℃; Preferably, in step (2), the reaction is carried out first under normal pressure and then under vacuum; Preferably, the pressure of the vacuum is -1.5~-1 bar.

9. The method of any one of claims 6-8, wherein, The preparation method specifically comprises the following steps: (1) mixing diacid, diamine and end-capping agent, controlling the stirring rate to be 100-150 rpm, carrying out a salt formation reaction at 75-100℃ under normal pressure for 30-60 min, controlling the temperature to be 240-245℃ until the pressure rises to 16-20 bar, raising the temperature to 260-276℃ at a rate of 10℃ / 10 min, controlling the stirring rate to be 50-150 rpm, opening the pressure retaining valve, carrying out a prepolymerization reaction, when the temperature reaches 245-256℃, starting to reduce the pressure at a rate of 1.5-2.5 bar / 10 min for 80-100 min until the pressure is reduced to 0 bar, then vacuumizing, reacting for 10-40 min under the conditions of a pressure of -1.0~-0.8 bar, a stirring rate of 80-120 rpm and a temperature of 245-256℃ to obtain the transparent nylon prepolymer; (2) mixing the transparent nylon prepolymer, polyetheramine, second catalyst and antioxidant, stirring at 220-270℃ under normal pressure for 30-60 min, then controlling the pressure to be -1.5~-1 bar, reacting for 0.5-2 h, punch extruding, cooling, granulating to obtain the transparent nylon material.

10. Use of the transparent nylon material according to any one of claims 1-5 in precision optical instruments, electronic component packaging, food packaging, medical devices or spectacles.

Citation Information

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