Enhanced monomer casting nylon material and preparation method thereof

By adding glass fiber, resin particles, graphene powder, and antibacterial agents to the single lava material to form an enhanced nylon material, the problem of lack of corrosion and antibacteriality in the existing nylon material in an acidic environment has achieved it, and achieved it. Higher corrosion resistance, antibacteriality and overall performance.

CN119350844APending Publication Date: 2025-01-24JIANGSU YIYUAN NEW MATERIALS TECH CO LTD

Patent Information

Application Number
CN202411957904.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-01-24

AI Technical Summary

Technical Problem

The existing monomer cast nylon materials are insufficient in acidic environments to corrosion and antibacterial properties, and are susceptible to corrosion and bacterial adhesion, affecting their safety.

Method used

The enhanced monomer -lava material composed of ingenid, glass fiber, resin particles, graphene powder, and antibacterial agents is used to improve the density and antibacterial properties of the material through concentration reactions and modification treatment.

Benefits of technology

It improves the corrosion resistance and antibacteriality of nylon materials, enhances the density and antibacterial effect of the material, extends the duration of antibacterial effects, and improves the overall strength and wear resistance of the material.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses an enhanced monomer casting nylon material and a preparation method thereof, and relates to the technical field of high-molecular compounds, in particular to a high-molecular compound obtained by reaction except for carbon-carbon unsaturated bond, the nylon material comprises caprolactam, glass fiber, resin particles, graphene powder and an antibacterial agent, by utilizing the high strength of the glass fiber and the resin particles, the texture of the nylon material is tighter, an attachment site is provided for the antibacterial agent when the nylon material is combined with the caprolactam, the antibacterial agent and the caprolactam can have firmer combining capacity, the compact material structure can resist corrosion, and the service life of the antibacterial agent is prolonged. The corrosion resistance and the antibacterial property of the monomer casting nylon are improved, and the defect that the corrosion resistance and the antibacterial property are insufficient in the monomer casting nylon process is overcome; the silver ion antibacterial agent is tightly combined with the graphene, so that the release speed of the silver ion antibacterial agent can be slowed down, and a stable antibacterial effect can be realized.
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Description

Technical Field

[0001] The present invention relates to the technical field of polymer compounds, in particular to a polymer compound obtained by a reaction other than carbon-carbon unsaturated bonds, and in particular to an enhanced monomer casting nylon material and a preparation method thereof. Background Art

[0002] Monomer cast nylon, also known as MC nylon, is an engineering plastic made through a specific process. It uses base-catalyzed polymerization to polymerize caprolactam or other lactam monomers directly in the mold and solidify into a shape. This material has a series of excellent physical and mechanical properties and is widely used in many industrial fields.

[0003] However, when nylon materials are used in acidic environments, long-term contact between nylon materials and acidic liquids will damage the structure of the monomer cast nylon, reduce the corrosion resistance of the nylon materials, and make the nylon materials easy for bacteria to attach, which will not only reduce the safety of the use of nylon materials, but also further aggravate the corrosion of nylon materials.

[0004] Therefore, it is necessary to improve the monomer cast nylon material in the prior art to solve the above problems. Summary of the invention

[0005] The present invention overcomes the deficiencies of the prior art and provides a reinforced monomer cast nylon material and a preparation method thereof, aiming to solve the defects of the prior art that the monomer cast nylon has insufficient corrosion resistance and antibacterial properties in an acidic use environment.

[0006] To achieve the above object, the technical solution adopted by the present invention is: a reinforced monomer cast nylon material, characterized in that it is composed of component A, component B and component C, wherein: Component A is caprolactam; Component B is glass fiber, resin particles and graphene powder, and the mass ratio of the glass fiber, the resin particles and the graphene powder is 1-2:1-2:2-3; Component C is an antibacterial agent, an activator, a coupling agent and a catalyst, wherein the mass ratio of the antibacterial agent, the activator, the coupling agent and the catalyst is 5-7:0.2-0.4:0.5-0.8:0.3-0.5, the antibacterial agent includes a silver ion antibacterial agent and a quaternary ammonium salt antibacterial agent, and the mass ratio of the silver ion antibacterial agent to the quaternary ammonium salt antibacterial agent is 1:1-2; The mass ratio of the A component, the B component and the C component is 60-70:20-45:5-10.

[0007] In a preferred embodiment of the present invention, the fineness of the glass fiber is 6D-8D, and the length of the glass fiber is 60-80 μm.

[0008] In a preferred embodiment of the present invention, the resin particles are phenolic resin particles, and the diameter of the phenolic resin particles is 30-40 μm.

[0009] In a preferred embodiment of the present invention, the radial dimension of the graphene powder is 1-10 μm, and the thickness dimension is 20-50 nm.

[0010] In a preferred embodiment of the present invention, the activator, the coupling agent and the catalyst are N-acetyl caprolactam, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and potassium hydroxide, respectively.

[0011] In a preferred embodiment of the present invention, the silver ion antibacterial agent is one of silver nitrate, silver chloride and silver sulfide, and the quaternary ammonium salt antibacterial agent is one of dioctyldimethylammonium chloride and dodecyltrimethylammonium chloride.

[0012] To achieve the above object, the second technical solution adopted by the present invention is: a method for preparing a reinforced monomer cast nylon material, comprising the following steps: S1: placing caprolactam monomer in a reaction kettle, adding a catalyst and an activator, and performing copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min, and performing vacuum treatment during the reaction to obtain copolymerized caprolactam; S2: adding graphene powder to a silver ion antibacterial agent solution, wherein the concentration of the silver ion antibacterial agent solution is 10-30%, the immersion time is 30-60 min, and the mass ratio between the graphene powder and the silver ion antibacterial agent solution is 1:4-6, taking out and drying to obtain modified graphene powder; S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, the stirring process is 10-15 minutes, to obtain a mixed caprolactam; S4: adding glass fiber, resin particles, coupling agent and quaternary ammonium salt antibacterial agent to the mixed caprolactam in S3 in sequence and mixing them evenly, adjusting the temperature to 140-160° C. and mixing time to 20-40 min during the mixing process to obtain modified caprolactam; S5: preheating the mold, pouring the modified caprolactam in S4 into the mold, centrifuging the mold for 5-15 minutes, cooling to room temperature and demolding to obtain a reinforced monomer cast nylon material.

[0013] In a preferred embodiment of the present invention, the preheating temperature of the mold in S5 is 120-140°C.

[0014] In a preferred embodiment of the present invention, the rotation speed of the centrifugal treatment in S5 is 150-300 rpm.

[0015] In a preferred embodiment of the present invention, in S5, the modified caprolactam after demoulding is placed in an oil bath environment at 80-120° C. for 1-2 hours.

[0016] The present invention solves the defects existing in the background technology and has the following beneficial effects: (1) The present invention provides a reinforced monomer cast nylon material, comprising caprolactam, glass fiber, resin particles, graphene powder and an antibacterial agent. The high strength of the glass fiber and the resin particles is utilized to make the texture of the nylon material more compact, and an attachment site is provided for the antibacterial agent when combined with caprolactam. Compared with the monomer cast nylon material in the prior art, the antibacterial agent and caprolactam have a stronger bonding ability, and the dense material structure can resist corrosion, thereby improving the corrosion resistance and antibacterial properties of the monomer cast nylon, and solving the defects of insufficient corrosion resistance and antibacterial properties in the monomer cast nylon process in the prior art.

[0017] (2) In the present invention, graphene is immersed in a silver ion antibacterial agent solution. The silver ion antibacterial agent and graphene are tightly combined, which can slow down the release rate of the silver ion antibacterial agent. Compared with the prior art, a stable antibacterial effect can be achieved, and graphene can enhance the antibacterial effect of the silver ion antibacterial agent, so that the monomer cast nylon has a high-efficiency and long-lasting antibacterial effect.

[0018] (3) In the present invention, glass fibers and resin particles are used in combination with caprolactam to enhance the density of nylon materials. Compared with the prior art, glass fibers and resin particles can improve the resistance of nylon materials to chemical substances, reduce corrosion and chemical degradation, and form a physical barrier with nylon monomers to slow down the penetration of corrosive media and improve corrosion resistance.

[0019] (4) In the present invention, the modified caprolactam after demolding is placed in an oil bath environment, and the oil bath heating of the demolded product can reduce the residual stress in the material and form a microporous structure in the material. Compared with the prior art, the microporous structure provides more attachment points and distribution space for the antibacterial agent, and can slow down the penetration of the corrosive medium into the material, reduce the corrosion rate, and improve the antibacterial and corrosion resistance of the monomer cast nylon material.

[0020] (5) In the present invention, the resin particles can improve the interfacial bonding force between the nylon matrix and the glass fiber and graphene powder, so that the load can be more effectively transferred from the matrix to the glass fiber and graphene powder. Compared with the prior art, stress concentration is reduced, thereby improving the overall strength of the material and having a reinforcing function for the nylon material.

[0021] (6) In the present invention, the microporous structure can better absorb and dissipate energy when subjected to impact loads. The microporous structure can improve the dispersion of reinforcing fillers in the nylon matrix and reduce filler agglomeration, thereby more effectively transmitting stress. Compared with the prior art, the microporous structure can improve the fracture toughness and surface hardness of the nylon material, and improve the wear resistance of the nylon material while enhancing the strength of the nylon material, thereby enhancing the function of the nylon material. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art are briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative work. Figure 1 It is a method step diagram of a preferred embodiment of the present invention. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein. Therefore, the protection scope of the present invention is not limited to the specific embodiments disclosed below.

[0025] A reinforced monomer cast nylon material, characterized in that it consists of component A, component B and component C, wherein: Component A is caprolactam; Component B is glass fiber, resin particles and graphene powder, and the mass ratio of glass fiber, resin particles and graphene powder is 1-2:1-2:2-3; Component C includes an antibacterial agent, an activator, a coupling agent and a catalyst, wherein the mass ratio of the antibacterial agent, the activator, the coupling agent and the catalyst is 5-7:0.2-0.4:0.5-0.8:0.3-0.5, and the antibacterial agent includes a silver ion antibacterial agent and a quaternary ammonium salt antibacterial agent, wherein the mass ratio of the silver ion antibacterial agent to the quaternary ammonium salt antibacterial agent is 1:1-2; The mass ratio of component A, component B and component C is 60-70:20-45:5-10.

[0026] The invention comprises caprolactam, glass fiber, resin particles, graphene powder and antibacterial agent. The high strength of glass fiber and resin particles is utilized to make the texture of nylon material more compact, and an attachment site is provided for the antibacterial agent when combined with caprolactam, so that the antibacterial agent and caprolactam have a stronger bonding ability. The dense material structure can resist corrosion, so that the corrosion resistance and antibacterial property of the monomer casting nylon are improved, and the defects of insufficient corrosion resistance and antibacterial property in the monomer casting nylon process in the prior art are solved.

[0027] The fineness of glass fiber is 6D-8D, and the length of glass fiber is 60-80μm. The lower fineness of glass fiber means that the fiber is thinner, which can increase the surface area of ​​the fiber, thereby providing more contact points and better mechanical locking in the nylon matrix, improving the strength and stiffness of the composite material, and the increase in strength and stiffness can ensure that the nylon material is dense enough.

[0028] The resin particles are phenolic resin particles, and the diameter of the phenolic resin particles is 30-40μm. The addition of phenolic resin particles can improve the tensile strength, compressive strength and hardness of nylon materials, because the resin particles can serve as a dispersion point for stress concentration and improve the material's bearing capacity. Phenolic resin particles can improve the chemical stability of the material and resist chemical corrosion. The radial size of graphene powder is 1-10μm and the thickness is 20-50nm. The thickness of graphene is very thin, only 20-50nm, which provides it with a very high specific surface area, which helps to increase the contact area with the nylon matrix, thereby enhancing the interface bonding force. Graphene has good chemical stability and can improve the corrosion resistance and chemical resistance of nylon materials.

[0029] The activator, coupling agent and catalyst are N-acetyl caprolactam, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and potassium hydroxide respectively. As an activator, N-acetyl caprolactam can increase the activity of the reactants, promote the copolymerization reaction, and improve the reaction rate and efficiency. As a coupling agent, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane can form chemical bonds with inorganic fillers and nylon matrix, improve the interface bonding between them, and improve the mechanical properties of the composite material. In the preparation process of the antibacterial agent, the use of the activator and the catalyst can improve the dispersibility and activity of the antibacterial agent, thereby enhancing the antibacterial properties of the material.

[0030] Silver ion antibacterial agent is one of silver nitrate, silver chloride and silver sulfide, and quaternary ammonium salt antibacterial agent is one of dioctyl dimethyl ammonium chloride and dodecyl trimethyl ammonium chloride. Silver ions have broad-spectrum antibacterial properties and can kill more than 650 kinds of viruses and bacteria. The antibacterial principle of silver ions is mainly to destroy the DNA structure of bacteria, electrostatically interact with the negative charge of the cell wall, destroy the cell wall, and then penetrate into the bacterial cells, coordinate with the sulfhydryl or amino group in the protease, so that the protease loses its activity and causes the death of bacteria. The antibacterial effect of silver ions is long-lasting, and it can repeatedly contact with different colonies and kill bacteria. The antibacterial mechanism of quaternary ammonium salts is mainly through adsorption to the surface of bacteria, penetrating the cell wall, combining with the cell membrane, disrupting the composition of the cell membrane, causing leakage of intracellular substances, and ultimately causing the death of bacteria.

[0031] like Figure 1 As shown, in order to achieve the above-mentioned purpose, the second set of technical solutions adopted by the present invention is: a method for preparing a reinforced monomer cast nylon material, comprising the following steps: S1: placing caprolactam monomer in a reaction kettle, adding a catalyst and an activator, and performing copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min, and performing vacuum treatment during the reaction to obtain copolymerized caprolactam; S2: adding graphene powder to a silver ion antibacterial agent solution, wherein the concentration of the silver ion antibacterial agent solution is 10-30%, the immersion time is 30-60 min, and the mass ratio between the graphene powder and the silver ion antibacterial agent solution is 1:4-6, taking out and drying to obtain modified graphene powder; S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, the stirring process is 10-15 minutes, to obtain a mixed caprolactam; S4: adding glass fiber, resin particles, coupling agent and quaternary ammonium salt antibacterial agent to the mixed caprolactam in S3 in sequence and mixing them evenly, adjusting the temperature to 140-160° C. and mixing time to 20-40 min during the mixing process to obtain modified caprolactam; S5: preheating the mold, pouring the modified caprolactam in S4 into the mold, centrifuging the mold for 5-15 minutes, cooling to room temperature and demolding to obtain a reinforced monomer cast nylon material.

[0032] The preheating temperature of the mold in S5 is 120-140℃. Preheating can improve the fluidity of the modified caprolactam, making it easier to fill the complex shapes and detailed parts of the mold. Uniform heating of the mold helps the material to solidify evenly in the mold, reducing internal stress and deformation.

[0033] The centrifugal treatment in S5 is performed at a speed of 150-300 rpm. The lower centrifugal speed helps to expel air and other gases during the material filling process and reduce bubbles in the final product. The centrifugal force helps to strengthen the interface bonding between different components in the material and improve the overall performance of the composite material.

[0034] In S5, the modified caprolactam after demoulding is placed in an oil bath environment at 80-120°C for 1-2 hours. By controlling the heating process, the internal stress generated by the material during the curing process can be gradually released, reducing the risk of deformation and cracking of the material. Oil bath heating helps to optimize the microstructure of the material, forming a more uniform and denser structure and improving the overall performance of the material.

[0035] Preheating the mold to 120-140°C and placing the demoulded modified caprolactam in an oil bath environment at 80-120°C for 1-2 hours can promote the crystallization and shrinkage of the polymer, thereby forming a microporous structure in the nylon material. The microporous structure provides more attachment points and distribution space for the antimicrobial agent, allowing the antimicrobial agent to be more evenly dispersed in the material. The micropores can serve as a reservoir for the antimicrobial agent, slowly releasing the antimicrobial ingredients and prolonging the duration of the antimicrobial effect. The microporous structure may slow down the penetration of the corrosive medium into the material and reduce the corrosion rate. In some cases, the microporous structure may contribute to the self-repair of the material. When the surface is damaged, the material in the micropores can migrate to the damaged area to help repair it. Embodiment 1

[0036] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0037] S2: adding 8 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0038] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 10 parts of glass fibers with a fineness of 8D and a length of 60 μm, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment of 80°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 2

[0039] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0040] S2: adding 10 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0041] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 10 parts of glass fibers with a fineness of 8D and a length of 60 μm, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment of 80°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 3

[0042] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0043] S2: adding 8 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0044] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 12.5 parts of glass fiber with a fineness and length of 8D and 60 μm respectively, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment of 80°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 4

[0045] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0046] S2: adding 15 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0047] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 10 parts of glass fibers with a fineness of 8D and a length of 60 μm, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment of 80°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 5

[0048] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0049] S2: adding 17 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0050] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 10 parts of glass fibers with a fineness of 8D and a length of 60 μm, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment of 80°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 6

[0051] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0052] S2: adding 8 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0053] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 12.5 parts of glass fiber with a fineness and length of 8D and 60 μm respectively, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment at 60°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 7

[0054] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0055] S2: adding 8 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0056] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 12.5 parts of glass fiber with a fineness and length of 8D and 60 μm respectively, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment at 100°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 8

[0057] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0058] S2: adding 8 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0059] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 12.5 parts of glass fiber with a fineness and length of 8D and 60 μm respectively, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 minutes, demolding it after cooling to room temperature, and placing it in an oil bath environment at 120°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material. Embodiment 9

[0060] This embodiment prepares a reinforced monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, and 0.3 parts of potassium hydroxide and 0.2 parts of N-acetyl caprolactam are added to carry out copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min. During the reaction, vacuum treatment is carried out to obtain copolymerized caprolactam.

[0061] S2: adding 8 parts of graphene powder into 40 parts of silver chloride solution, wherein the concentration of the silver chloride solution is 10%, the immersion time is 45 minutes, taking out and drying to obtain modified graphene powder.

[0062] S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, maintaining the temperature at 100° C. during the stirring process, and stirring for 10 minutes to obtain mixed caprolactam; S4: 12.5 parts of glass fiber with a fineness and length of 8D and 60 μm respectively, 5 parts of phenolic resin particles with a particle diameter of 30 μm, 0.5 parts of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3 parts of dioctyldimethylammonium chloride are sequentially added to the mixed caprolactam in S3, and mixed evenly. During the mixing process, the temperature is adjusted to 160° C. and the mixing time is 20 min to obtain modified caprolactam; S5: preheating the mold so that the mold temperature is 130°C, pouring the modified caprolactam in S4 into the mold, centrifuging it after pouring, the speed of centrifugation is 200 rpm, the centrifugation time is 10 min, demolding it after cooling to room temperature, and placing it in an oil bath environment at 140°C for 1 hour after demolding to obtain a reinforced monomer cast nylon material.

[0063] Comparative Example 1 This comparative example provides a monomer cast nylon material, and the preparation method is as follows: S1: 60 parts of caprolactam monomer are placed in a reaction kettle, 0.3 parts of a catalyst and 0.2 parts of an activator are added, and copolymerization is carried out at a reaction temperature of 80-120° C. and a reaction time of 20-40 min. Vacuum treatment is carried out during the reaction to obtain copolymerized caprolactam.

[0064] S2: pouring the copolymerized caprolactam in S1 into a mold, centrifuging the mold at a speed of 200 rpm for 10 min, and demolding the mold after cooling to room temperature to obtain a monomer cast nylon material.

[0065] Take samples of equal weight from the nylon materials in Examples 1 to 9 and Comparative Example 1, and test the antibacterial rate of the samples according to the national standard GB / T20944.3-2008. After the samples are immersed in dilute hydrochloric acid with a pH of 3 for 500 hours, the tensile strength of the samples is measured according to the national standard GB / T 1040.2-2022, and the tensile strength retention rate is calculated.

[0066] Table 1 Experimental data of antibacterial and corrosion resistance of samples in Examples 1 to 9 and Comparative Example 1

[0067] It can be seen from Table 1 that the antibacterial rate and tensile strength in Examples 1 to 9 are greater than those in the comparative example, and the reinforced monomer cast nylon material of the present invention has good antibacterial and corrosion resistance.

[0068] In Examples 1 to 5, as the proportion of graphene in the nylon material gradually increases, the antibacterial and corrosion resistance first increase and then decrease. This is because an appropriate amount of graphene can enhance interface bonding, enhance antibacterial and corrosion resistance, but excessive graphene may cause uneven distribution of the antibacterial agent, affecting the antibacterial effect. When the graphene content is too high, too many microcracks and defects will be formed, resulting in reduced density of the nylon material and reduced corrosion resistance. The best embodiment is Example 3.

[0069] In Example 3 and Examples 6 to 9, as the temperature of the oil bath environment gradually increases, the antibacterial and corrosion resistance first increase and then decrease. This is because the appropriate temperature increase can reduce the stress inside the material, help release the internal stress generated during the processing, form a microporous structure, and improve the antibacterial and corrosion resistance of the material. Too high an oil bath temperature causes too many and too large pores to form on the surface or inside the material, providing a penetration path for microorganisms and corrosive media, reducing the density of the material, and reducing the antibacterial and corrosion resistance. The best embodiment is Example 7.

[0070] The above is based on the ideal embodiment of the present invention. Through the above description, relevant personnel can make various changes and modifications without departing from the technical concept of the present invention. The technical scope of the present invention is not limited to the content in the specification, and the technical scope must be determined according to the scope of the claims.

Claims

1. A reinforced monomer cast nylon material, characterized in that: It consists of component A, component B and component C, wherein: Component A is caprolactam; Component B is glass fiber, resin particles and graphene powder, and the mass ratio of the glass fiber, the resin particles and the graphene powder is 1-2:1-2:2-3; Component C is an antibacterial agent, an activator, a coupling agent and a catalyst, wherein the mass ratio of the antibacterial agent, the activator, the coupling agent and the catalyst is 5-7:0.2-0.4:0.5-0.8:0.3-0.5, the antibacterial agent includes a silver ion antibacterial agent and a quaternary ammonium salt antibacterial agent, and the mass ratio of the silver ion antibacterial agent to the quaternary ammonium salt antibacterial agent is 1:1-2; The mass ratio of the A component, the B component and the C component is 60-70:20-45:5-10.

2. The reinforced monomer cast nylon material according to claim 1, characterized in that: The glass fiber has a fineness of 6D-8D and a length of 60-80 μm.

3. The reinforced monomer cast nylon material according to claim 1, characterized in that: The resin particles are phenolic resin particles, and the diameter of the phenolic resin particles is 30-40 μm.

4. The reinforced monomer cast nylon material according to claim 1, characterized in that: The radial dimension of the graphene powder is 1-10 μm, and the thickness dimension is 20-50 nm.

5. The reinforced monomer cast nylon material according to claim 1, characterized in that: The activator, the coupling agent and the catalyst are N-acetyl caprolactam, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and potassium hydroxide respectively.

6. The reinforced monomer cast nylon material according to claim 1, characterized in that: The silver ion antibacterial agent is one of silver nitrate, silver chloride and silver sulfide, and the quaternary ammonium salt antibacterial agent is one of dioctyl dimethyl ammonium chloride and dodecyl trimethyl ammonium chloride.

7. A method for preparing a reinforced monomer cast nylon material, based on the reinforced monomer cast nylon material according to any one of claims 1 to 6, characterized in that: The following steps are involved: S1: placing caprolactam monomer in a reaction kettle, adding a catalyst and an activator, and performing copolymerization reaction at a reaction temperature of 80-120° C. for a reaction time of 20-40 min, and performing vacuum treatment during the reaction to obtain copolymerized caprolactam; S2: adding graphene powder to a silver ion antibacterial agent solution, wherein the concentration of the silver ion antibacterial agent solution is 10-30%, the immersion time is 30-60 min, and the mass ratio between the graphene powder and the silver ion antibacterial agent solution is 1:4-6, taking out and drying to obtain modified graphene powder; S3: adding the modified graphene powder in S2 to the copolymerized caprolactam in S1, stirring during the adding process, the stirring process is 10-15 minutes, to obtain mixed caprolactam; S4: adding glass fiber, resin particles, coupling agent and quaternary ammonium salt antibacterial agent to the mixed caprolactam in S3 in sequence and mixing them evenly, adjusting the temperature to 140-160° C. and mixing time to 20-40 min during the mixing process to obtain modified caprolactam; S5: preheating the mold, pouring the modified caprolactam in S4 into the mold, centrifuging the mold for 5-15 minutes, cooling to room temperature and demolding to obtain a reinforced monomer cast nylon material.

8. The method for preparing a reinforced monomer cast nylon material according to claim 7, characterized in that: The preheating temperature of the mold in S5 is 120-140°C.

9. The method for preparing a reinforced monomer cast nylon material according to claim 7, characterized in that: The rotation speed of the centrifugal treatment in S5 is 150-300 rpm.

10. The method for preparing a reinforced monomer cast nylon material according to claim 7, characterized in that: In S5, the demoulded modified caprolactam is placed in an oil bath environment at 80-120° C. for 1-2 hours.

Citation Information

Patent Citations

  • Phenolic resin / MC nylon composite material, and preparation method thereof

    CN103570937A

  • Casting nylon / graphene nanocomposite material and preparation method thereof

    CN105622929A

  • Antibacterial MC (monomer casting) nylon composite material and preparation method thereof

    CN106380593A

  • Monomer casting nylon and preparation method thereof

    CN109467693A

  • Antibacterial modified graphene polyamide 6 composite material and preparation method thereof

    CN116144018A

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