Compression molding process of polyether sulfone flame-retardant composite material

Abstract

The invention discloses a compression molding process of a polyethersulfone flame-retardant composite material. The compression molding process comprises the following steps: S1, preparing raw materials in percentage by mass; s2, mixing the raw materials; step S3, preheating treatment; step S4, compression molding; step S5, cooling and shaping; step S6, carrying out post-treatment; by adding innovative components such as the phosphorus-nitrogen flame retardant, the nano silicon dioxide, the graphene and the nano-scale aluminum silicate fiber, the flame retardant property of the composite material is remarkably improved, and the composite material can meet higher fireproof requirements; due to the addition of the nanoscale aluminum silicate fibers, the tensile strength is improved while the density of the material is reduced, the mechanical property and the thermal stability of the composite material are further enhanced, and the application range of the composite material is widened; the compression molding process is simple, convenient to operate, high in production efficiency and suitable for large-scale industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of polymer material processing, and in particular relates to a compression molding process for a polyethersulfone flame-retardant composite material. Background Art

[0002] Polyethersulfone (PES) is a high-performance engineering plastic with excellent heat resistance, mechanical properties, and chemical stability. However, its poor flame retardancy limits its application in areas requiring high fire protection. While various methods have been developed to improve the flame retardancy of PES, these methods often suffer from poor flame retardancy, significant impact on material properties, or high costs. Therefore, the development of a flame-retardant composite material and its molding process that is efficient, environmentally friendly, and minimizes the impact on PES performance is of great significance.

[0003] Based on this, a compression molding process for polyethersulfone flame retardant composite materials was designed. Summary of the Invention

[0004] In view of the above situation, in order to overcome the defects of the prior art, the present invention provides a compression molding process for a polyethersulfone flame retardant composite material, which effectively solves the problems raised in the above background.

[0005] To achieve the above object, the present invention provides the following technical solution: a compression molding process for a polyethersulfone flame-retardant composite material, comprising the following steps:

[0006] Step S1: Prepare raw materials by mass percentage

[0007] Polyethersulfone: 40-60%;

[0008] Phosphorus and nitrogen flame retardants: 10-20%;

[0009] Nano-silicon dioxide: 5-15%;

[0010] Graphene: 3-8%;

[0011] Nano-scale aluminum silicate fiber: 2-6%;

[0012] Epoxy resin: 5-10%;

[0013] Antioxidant: 0.5-2%;

[0014] Lubricant: 0.5-2%;

[0015] Step S2: Mixing raw materials

[0016] Add polyethersulfone, phosphorus-nitrogen flame retardant, nano-silica, graphene, nano-aluminum silicate fiber, epoxy resin, antioxidant and lubricant into a high-speed mixer according to the above proportions, mix at a speed of 1000-1500 r / min for 5-10 minutes to ensure that all components are fully mixed and the temperature of the mixed material is maintained at 40-60°C;

[0017] Step S3: Preheating

[0018] Place the mixed material into a preheated mold at 200-250°C for 10-15 minutes. During this process, the epoxy resin in the material begins to partially solidify, forming a preliminary network structure, which helps improve fluidity and uniformity in the subsequent molding process.

[0019] Step S4: compression molding

[0020] The preheated material is quickly transferred to a molding machine. The mold temperature of the molding machine is 260-300°C, the pressure is 10-15 MPa, and the molding time is 10-15 minutes. During this process, the polyethersulfone is fully melted and fills the mold. At the same time, the phosphorus-nitrogen flame retardant, nano-silica, graphene, and nano-aluminum silicate fibers synergistically react with the polyethersulfone at high temperature to form a stable flame retardant system.

[0021] Step S5: Cooling and shaping

[0022] After compression molding, the mold is immediately removed from the molding machine and placed in a cooling device for cooling and shaping. The temperature of the cooling device is 20-40°C and the cooling time is 15-20 minutes. During the cooling process, the composite material gradually solidifies and forms a product with a certain shape and size.

[0023] Step S6: Post-processing

[0024] After cooling and shaping, the composite material product is taken out of the mold, the surface is cleaned and the size is trimmed, and then the product is placed in an oven for post-processing at an oven temperature of 150-200°C for 2-3 hours to eliminate residual stress; post-processing can further improve the mechanical properties and flame retardant properties of the product.

[0025] Preferably, in step S1, the phosphorus-nitrogen flame retardant is a mixture of ammonium polyphosphate and melamine cyanurate, and the mass ratio of the two is 1:1-1:3.

[0026] Preferably, in step S1, the particle size of the nano-silicon dioxide is 10-50 nm.

[0027] Preferably, in step S1, the number of graphene layers is 3-10.

[0028] Preferably, in step S1, the diameter of the nano-scale aluminum silicate fiber is 10-50 nm and the length is 1-5 mm.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] 1. By adding innovative ingredients such as phosphorus-nitrogen flame retardants, nano-silica, graphene, and nano-aluminum silicate fibers, the flame retardant properties of the composite material are significantly improved, enabling it to meet higher fire protection requirements;

[0031] 2. The addition of nano-scale aluminum silicate fibers reduces material density while increasing tensile strength, further enhancing the mechanical properties and thermal stability of the composite material and broadening its application range;

[0032] 3. The compression molding process of the present invention is simple, easy to operate, and has high production efficiency, and is suitable for large-scale industrial production;

[0033] 4. The flame retardants and reinforcing materials used in this invention are environmentally friendly and do not contain harmful halogen compounds, meeting modern environmental requirements. In addition, the addition of nano-scale aluminum silicate fibers not only improves performance but also reduces dependence on traditional flame retardants, thereby reducing the environmental impact of the material.

[0034] 5. This process has little effect on the mechanical properties and processing properties of polyethersulfone. The prepared composite material has excellent comprehensive performance and has broad application prospects. DETAILED DESCRIPTION

[0035] The technical solutions of the present invention will be clearly and completely described below in conjunction with specific embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0036] The present invention provides a compression molding process for a polyethersulfone flame retardant composite material, comprising the following steps:

[0037] Step S1: Prepare raw materials by mass percentage

[0038] Polyethersulfone: 40-60%;

[0039] Phosphorus and nitrogen flame retardants: 10-20%;

[0040] Nano-silicon dioxide: 5-15%;

[0041] Graphene: 3-8%;

[0042] Nano-scale aluminum silicate fiber: 2-6%;

[0043] Epoxy resin: 5-10%;

[0044] Antioxidant: 0.5-2%;

[0045] Lubricant: 0.5-2%;

[0046] Step S2: Mixing raw materials

[0047] Add polyethersulfone, phosphorus-nitrogen flame retardant, nano-silica, graphene, nano-aluminum silicate fiber, epoxy resin, antioxidant and lubricant into a high-speed mixer according to the above proportions, mix at a speed of 1000-1500 r / min for 5-10 minutes to ensure that all components are fully mixed and the temperature of the mixed material is maintained at 40-60°C;

[0048] Step S3: Preheating

[0049] Place the mixed material into a preheated mold at 200-250°C for 10-15 minutes. During this process, the epoxy resin in the material begins to partially solidify, forming a preliminary network structure, which helps improve fluidity and uniformity in the subsequent molding process.

[0050] Step S4: compression molding

[0051] The preheated material is quickly transferred to a molding machine. The mold temperature of the molding machine is 260-300°C, the pressure is 10-15 MPa, and the molding time is 10-15 minutes. During this process, the polyethersulfone is fully melted and fills the mold. At the same time, the phosphorus-nitrogen flame retardant, nano-silica, graphene, and nano-aluminum silicate fibers synergistically react with the polyethersulfone at high temperature to form a stable flame retardant system.

[0052] Step S5: Cooling and shaping

[0053] After compression molding, the mold is immediately removed from the molding machine and placed in a cooling device for cooling and shaping. The temperature of the cooling device is 20-40°C and the cooling time is 15-20 minutes. During the cooling process, the composite material gradually solidifies and forms a product with a certain shape and size.

[0054] Step S6: Post-processing

[0055] After cooling and shaping, the composite material product is taken out of the mold, the surface is cleaned and the size is trimmed, and then the product is placed in an oven for post-processing at an oven temperature of 150-200°C for 2-3 hours to eliminate residual stress; post-processing can further improve the mechanical properties and flame retardant properties of the product.

[0056] In step S1 of this embodiment, the phosphorus-nitrogen flame retardant is a mixture of ammonium polyphosphate and melamine cyanurate, and the mass ratio of the two is 1:1-1:3.

[0057] In step S1 of this embodiment, the particle size of the nano-silicon dioxide is 10-50 nm.

[0058] In step S1 of this embodiment, the number of graphene layers is 3-10.

[0059] In step S1 of this embodiment, the diameter of the nano-scale aluminum silicate fibers is 10-50 nm and the length is 1-5 mm.

[0060] Example 1:

[0061] A compression molding process for a polyethersulfone flame-retardant composite material comprises the following steps:

[0062] Step S1: Prepare raw materials by mass percentage

[0063] Polyethersulfone: 40%;

[0064] Phosphorus and nitrogen flame retardant: 10%;

[0065] Nano-silicon dioxide: 5%;

[0066] Graphene: 3%;

[0067] Nano-scale aluminum silicate fiber: 2%;

[0068] Epoxy resin: 5%;

[0069] Antioxidant: 0.5%;

[0070] Lubricant: 0.5%;

[0071] Step S2: Mixing raw materials

[0072] Add polyethersulfone, phosphorus-nitrogen flame retardant, nano-silica, graphene, nano-aluminum silicate fiber, epoxy resin, antioxidant and lubricant into a high-speed mixer according to the above proportions, mix at a speed of 1000 r / min for 5 minutes to ensure that all components are fully mixed and the temperature of the mixed material is maintained at 40°C;

[0073] Step S3: Preheating

[0074] The mixed material is placed in a preheated mold at 200°C for 10 minutes. During this process, the epoxy resin in the material begins to partially solidify, forming a preliminary network structure, which helps improve fluidity and uniformity in the subsequent molding process.

[0075] Step S4: compression molding

[0076] The preheated material is quickly transferred to a molding press, where the mold temperature is 260°C, the pressure is 10 MPa, and the molding time is 10 minutes. During this process, the polyethersulfone fully melts and fills the mold, while the phosphorus-nitrogen flame retardant, nano-silica, graphene, and nano-aluminum silicate fibers synergistically react with the polyethersulfone at high temperature to form a stable flame retardant system.

[0077] Step S5: Cooling and shaping

[0078] After compression molding, the mold is immediately removed from the molding machine and placed in a cooling device for cooling and shaping. The temperature of the cooling device is 20°C and the cooling time is 15 minutes. During the cooling process, the composite material gradually solidifies and forms a product with a certain shape and size.

[0079] Step S6: Post-processing

[0080] After cooling and shaping, the composite material product is taken out of the mold, the surface is cleaned and the size is trimmed, and then the product is placed in an oven for post-processing at an oven temperature of 150°C for 2 hours to eliminate residual stress; post-processing can further improve the mechanical properties and flame retardant properties of the product.

[0081] In step S1 of this embodiment, the phosphorus-nitrogen flame retardant is a mixture of ammonium polyphosphate and melamine cyanurate, with a mass ratio of 1:1.

[0082] In step S1 of this embodiment, the particle size of the nano-silicon dioxide is 10 nm.

[0083] In step S1 of this embodiment, the number of graphene layers is 3.

[0084] In step S1 of this embodiment, the diameter of the nano-scale aluminum silicate fiber is 10 nm and the length is 1 mm.

[0085] Example 2:

[0086] A compression molding process for a polyethersulfone flame-retardant composite material comprises the following steps:

[0087] Step S1: Prepare raw materials by mass percentage

[0088] Polyethersulfone: 60%;

[0089] Phosphorus and nitrogen flame retardant: 20%;

[0090] Nano-silicon dioxide: 15%;

[0091] Graphene: 8%;

[0092] Nano-scale aluminum silicate fiber: 6%;

[0093] Epoxy resin: 10%;

[0094] Antioxidant: 2%;

[0095] Lubricant: 2%;

[0096] Step S2: Mixing raw materials

[0097] Add polyethersulfone, phosphorus-nitrogen flame retardant, nano-silica, graphene, nano-aluminum silicate fiber, epoxy resin, antioxidant and lubricant into a high-speed mixer according to the above proportions, mix at a speed of 1500 r / min for 10 minutes to ensure that all components are fully mixed and the temperature of the mixed material is maintained at 60°C;

[0098] Step S3: Preheating

[0099] The mixed material is placed in a preheated mold at 250°C for 15 minutes. During this process, the epoxy resin in the material begins to partially solidify, forming a preliminary network structure, which helps improve fluidity and uniformity in the subsequent molding process.

[0100] Step S4: compression molding

[0101] The preheated material is quickly transferred to a molding press, where the mold temperature is 300°C, the pressure is 15 MPa, and the molding time is 15 minutes. During this process, the polyethersulfone fully melts and fills the mold. Simultaneously, the phosphorus-nitrogen flame retardant, nano-silica, graphene, and nano-aluminum silicate fibers synergistically react with the polyethersulfone at high temperature to form a stable flame retardant system.

[0102] Step S5: Cooling and shaping

[0103] After compression molding, the mold is immediately removed from the molding machine and placed in a cooling device for cooling and shaping. The temperature of the cooling device is 40°C and the cooling time is 20 minutes. During the cooling process, the composite material gradually solidifies and forms a product with a certain shape and size.

[0104] Step S6: Post-processing

[0105] After cooling and shaping, the composite material product is taken out of the mold, the surface is cleaned and the size is trimmed, and then the product is placed in an oven for post-processing at an oven temperature of 200°C for 3 hours to eliminate residual stress; post-processing can further improve the mechanical properties and flame retardant properties of the product.

[0106] In step S1 of this embodiment, the phosphorus-nitrogen flame retardant is a mixture of ammonium polyphosphate and melamine cyanurate, with a mass ratio of 1:3.

[0107] In step S1 of this embodiment, the particle size of the nano-silicon dioxide is 50 nm.

[0108] In step S1 of this embodiment, the number of graphene layers is 10.

[0109] In step S1 of this embodiment, the diameter of the nano-scale aluminum silicate fiber is 50 nm and the length is 5 mm.

[0110] Example 3:

[0111] A compression molding process for a polyethersulfone flame-retardant composite material comprises the following steps:

[0112] Step S1: Prepare raw materials by mass percentage

[0113] Polyethersulfone: 50%;

[0114] Phosphorus and nitrogen flame retardant: 15%;

[0115] Nano-silicon dioxide: 10%;

[0116] Graphene: 5.5%;

[0117] Nano-scale aluminum silicate fiber: 4%;

[0118] Epoxy resin: 7.5%;

[0119] Antioxidant: 1.3%;

[0120] Lubricant: 1.3%;

[0121] Step S2: Mixing raw materials

[0122] Add polyethersulfone, phosphorus-nitrogen flame retardant, nano-silica, graphene, nano-aluminum silicate fiber, epoxy resin, antioxidant and lubricant into a high-speed mixer in the above proportions, mix at a speed of 1250 r / min for 8 minutes to ensure that all components are fully mixed and the temperature of the mixed material is maintained at 50°C;

[0123] Step S3: Preheating

[0124] The mixed material is placed in a preheated mold at 225°C for 13 minutes. During this process, the epoxy resin in the material begins to partially solidify, forming a preliminary network structure, which helps improve fluidity and uniformity in the subsequent molding process.

[0125] Step S4: compression molding

[0126] The preheated material is quickly transferred to a molding press, where the mold temperature is 280°C, the pressure is 13 MPa, and the molding time is 13 minutes. During this process, the polyethersulfone fully melts and fills the mold. Simultaneously, the phosphorus-nitrogen flame retardant, nano-silica, graphene, and nano-aluminum silicate fibers synergistically react with the polyethersulfone at high temperature to form a stable flame retardant system.

[0127] Step S5: Cooling and shaping

[0128] After compression molding, the mold is immediately removed from the molding machine and placed in a cooling device for cooling and shaping. The temperature of the cooling device is 30°C and the cooling time is 18 minutes. During the cooling process, the composite material gradually solidifies and forms a product with a certain shape and size.

[0129] Step S6: Post-processing

[0130] After cooling and shaping, the composite material product is taken out of the mold, the surface is cleaned and the size is trimmed, and then the product is placed in an oven for post-processing at an oven temperature of 175°C for 2.5 hours to eliminate residual stress; post-processing can further improve the mechanical properties and flame retardant properties of the product.

[0131] In step S1 of this embodiment, the phosphorus-nitrogen flame retardant is a mixture of ammonium polyphosphate and melamine cyanurate, with a mass ratio of 1:2.

[0132] In step S1 of this embodiment, the particle size of the nano-silicon dioxide is 30 nm.

[0133] In step S1 of this embodiment, the number of graphene layers is 7.

[0134] In step S1 of this embodiment, the diameter of the nano-scale aluminum silicate fiber is 30 nm and the length is 3 mm.

[0135] Example 4:

[0136] A compression molding process for a polyethersulfone flame-retardant composite material comprises the following steps:

[0137] Step S1: Prepare raw materials by mass percentage

[0138] Polyethersulfone: 45%;

[0139] Phosphorus and nitrogen flame retardant: 12%;

[0140] Nano-silicon dioxide: 7%;

[0141] Graphene: 4%;

[0142] Nano-scale aluminum silicate fiber: 3%;

[0143] Epoxy resin: 6%;

[0144] Antioxidant: 1%;

[0145] Lubricant: 1%;

[0146] Step S2: Mixing raw materials

[0147] Add polyethersulfone, phosphorus-nitrogen flame retardant, nano-silica, graphene, nano-aluminum silicate fiber, epoxy resin, antioxidant and lubricant into a high-speed mixer in the above proportions and mix at a speed of 1100 r / min for 6 minutes to ensure that all components are fully mixed. The temperature of the mixed material is maintained at 45°C;

[0148] Step S3: Preheating

[0149] The mixed material is placed in a preheated mold at 220°C for 12 minutes. During this process, the epoxy resin in the material begins to partially solidify, forming a preliminary network structure, which helps improve fluidity and uniformity in the subsequent molding process.

[0150] Step S4: compression molding

[0151] The preheated material is quickly transferred to a molding press, where the mold temperature is 270°C, the pressure is 11 MPa, and the molding time is 12 minutes. During this process, the polyethersulfone fully melts and fills the mold. Simultaneously, the phosphorus-nitrogen flame retardant, nano-silica, graphene, and nano-aluminum silicate fibers synergistically react with the polyethersulfone at high temperature to form a stable flame retardant system.

[0152] Step S5: Cooling and shaping

[0153] After compression molding, the mold is immediately removed from the molding machine and placed in a cooling device for cooling and shaping. The temperature of the cooling device is 25°C and the cooling time is 16 minutes. During the cooling process, the composite material gradually solidifies and forms a product with a certain shape and size.

[0154] Step S6: Post-processing

[0155] After cooling and shaping, the composite material product is taken out of the mold, the surface is cleaned and the size is trimmed, and then the product is placed in an oven for post-processing at an oven temperature of 160°C and a processing time of 2.2 hours to eliminate residual stress; post-processing can further improve the mechanical properties and flame retardant properties of the product.

[0156] In step S1 of this embodiment, the phosphorus-nitrogen flame retardant is a mixture of ammonium polyphosphate and melamine cyanurate, with a mass ratio of 1:1.

[0157] In step S1 of this embodiment, the particle size of the nano-silicon dioxide is 20 nm.

[0158] In step S1 of this embodiment, the number of graphene layers is 5.

[0159] In step S1 of this embodiment, the diameter of the nano-scale aluminum silicate fiber is 20 nm and the length is 2 mm.

[0160] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0161] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. A compression molding process for a polyethersulfone flame retardant composite material, characterized in that: The following steps are involved: Step S1: Prepare raw materials by mass percentage Polyethersulfone: 40-60%; Phosphorus and nitrogen flame retardants: 10-20%; Nano-silicon dioxide: 5-15%; Graphene: 3-8%; Nano-scale aluminum silicate fiber: 2-6%; Epoxy resin: 5-10%; Antioxidant: 0.5-2%; Lubricant: 0.5-2%; Step S2: Mixing raw materials Add polyethersulfone, phosphorus-nitrogen flame retardant, nano-silica, graphene, nano-aluminum silicate fiber, epoxy resin, antioxidant and lubricant into a high-speed mixer according to the above proportions, mix at a speed of 1000-1500 r / min for 5-10 minutes to ensure that all components are fully mixed and the temperature of the mixed material is maintained at 40-60°C; Step S3: Preheating Place the mixed material into a preheated mold at 200-250°C for 10-15 minutes. During this process, the epoxy resin in the material begins to partially solidify, forming a preliminary network structure, which helps improve fluidity and uniformity in the subsequent molding process. Step S4: compression molding The preheated material is quickly transferred to a molding machine. The mold temperature of the molding machine is 260-300°C, the pressure is 10-15 MPa, and the molding time is 10-15 minutes. During this process, the polyethersulfone is fully melted and fills the mold. At the same time, the phosphorus-nitrogen flame retardant, nano-silica, graphene, and nano-aluminum silicate fibers synergistically react with the polyethersulfone at high temperature to form a stable flame retardant system. Step S5: Cooling and shaping After compression molding, the mold is immediately removed from the molding machine and placed in a cooling device for cooling and shaping. The temperature of the cooling device is 20-40°C and the cooling time is 15-20 minutes. During the cooling process, the composite material gradually solidifies and forms a product with a certain shape and size. Step S6: Post-processing After cooling and shaping, the composite material product is taken out of the mold, the surface is cleaned and the size is trimmed, and then the product is placed in an oven for post-processing at an oven temperature of 150-200°C for 2-3 hours to eliminate residual stress; post-processing can further improve the mechanical properties and flame retardant properties of the product.

2. The compression molding process of a polyethersulfone flame retardant composite material according to claim 1, characterized in that: In step S1, the phosphorus-nitrogen flame retardant is a mixture of ammonium polyphosphate and melamine cyanurate, with a mass ratio of the two being 1:1-1:

3.

3. The compression molding process of a polyethersulfone flame retardant composite material according to claim 1, characterized in that: In the step S1, the particle size of the nano-silicon dioxide is 10-50 nm.

4. The compression molding process of a polyethersulfone flame retardant composite material according to claim 1, characterized in that: In step S1, the number of graphene layers is 3-10.

5. The compression molding process of a polyethersulfone flame retardant composite material according to claim 1, characterized in that: In step S1, the diameter of the nano-scale aluminum silicate fiber is 10-50 nm and the length is 1-5 mm.