Reinforced flame-retardant PC composite material and preparation method thereof
By introducing a combination of end-hydroxyl hyperbranched polycarbonate, micro-crosslinker and hyperbranched tripolyphosphazene terpyridine CTP-TPY into PC composite materials, an interpenetrating network structure is formed, which solves the problems of insufficient mechanical properties, flame retardancy and weather resistance of PC composite materials and realizes the preparation of high-performance PC composite materials.
Patent Information
- Application Number
- CN202510988193.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-17
- Publication Date
- 2025-10-03
AI Technical Summary
Existing PC composite materials have deficiencies in mechanical properties, flame retardancy, impact toughness and weather resistance, and functional additives and fillers are unevenly dispersed, which affects the stability of material properties and increases production complexity and cost.
PC resin, end-hydroxy hyperbranched polycarbonate, micro-crosslinker, filler, hyperbranched tripolyphosphazene terpyridine CTP-TPY and other combinations are used for extrusion molding through a twin-screw extruder to form an interpenetrating network structure, thereby improving the mechanical properties, flame retardancy and weather resistance of the material.
The prepared reinforced flame-retardant PC composite material has excellent mechanical properties, good flame retardancy and impact toughness, excellent weather resistance, and the preparation process is simple, suitable for large-scale production, and has stable performance.
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of composite materials, and in particular to a reinforced flame-retardant PC composite material and a preparation method thereof. Background Art
[0002] Polycarbonate (PC) is a thermoplastic engineering plastic with excellent comprehensive properties, featuring superior electrical insulation, dimensional stability, creep resistance, and non-toxicity. It is widely used in electronics, packaging, medical devices, transportation, and other fields. However, unmodified PC still has many shortcomings, including insufficient processing fluidity, poor impact toughness, and the need for further improvement in flame retardancy, mechanical properties, and weather resistance. It is precisely in this context that PC composites have emerged, attracting widespread attention within the industry.
[0003] Existing PC composites often incorporate functional additives and fillers during production, leading to problems such as uneven dispersion of these additives and fillers and poor interfacial adhesion with the PC matrix. Over long-term use, these additives and fillers are prone to leakage, affecting the composite's performance stability. Furthermore, the addition of large amounts of these additives and fillers increases the complexity and cost of the production process.
[0004] To address the above-mentioned issues, a Chinese invention patent with authorization announcement number CN115449207B discloses a halogen-free flame-retardant reinforced PC composite material, its preparation method, and application. The halogen-free flame-retardant reinforced PC composite material provided by the invention comprises: polycarbonate, glass fiber, a halogen-free flame retardant, a CTI improver, and an aging-resistant agent; wherein: the mass ratio of the halogen-free flame retardant, CTI improver, and aging-resistant agent is (5-10):(6-12):(8-12). The invention also provides a method for preparing a high-CTI, aging-resistant, halogen-free flame-retardant reinforced PC composite material for connectors. The PC composite material obtained by the invention has excellent comprehensive properties, with a CTI value increased to 400V, strong aging resistance, and flame retardancy reaching UL94 V-0 level. However, its toughness and weather resistance still need to be further improved.
[0005] It can be seen that the present invention still needs a reinforced flame-retardant PC composite material with good mechanical properties, excellent flame retardancy, impact toughness and weather resistance and a preparation method thereof. Summary of the Invention
[0006] The purpose of the present invention is to overcome the deficiencies of the prior art and to provide a reinforced flame-retardant PC composite material having good mechanical properties, excellent flame retardancy, impact toughness and weather resistance and a preparation method thereof.
[0007] To achieve the above object, the technical solution adopted by the present invention is: a reinforced flame-retardant PC composite material, comprising the following raw materials in parts by weight: 80 parts of PC resin, 10-20 parts of terminal hydroxyl hyperbranched polycarbonate, 5-8 parts of micro-crosslinking agent, 3-5 parts of coupling agent, 25-35 parts of filler, 5-8 parts of hyperbranched tripolyphosphazene terpyridine CTP-TPY, 2-4 parts of compatibilizer, 0.3-0.6 parts of antioxidant, 0.3-0.6 parts of lubricant, 0.8-1.2 parts of initiator, 2-4 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1-3 parts of octaphenylcyclotetrasiloxane, 4-6 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 0.8-1.2 parts of catalyst.
[0008] Preferably, the PC resin is Lexan PC 121.
[0009] Preferably, the hydroxyl-terminated hyperbranched polycarbonate is prepared according to the method of Example 5 of Chinese invention patent with authorization publication number CN107151316B.
[0010] Preferably, the micro-crosslinking agent is at least one of polyethylene glycol methacrylate and perfluoroalkyl acrylate FC-14.
[0011] Preferably, the polyethylene glycol methacrylate has an average molecular weight of 475 and is provided by Changsha Jingkang New Materials Technology Co., Ltd.; the perfluoroalkyl acrylate FC-14 is provided by Taipuda New Materials.
[0012] Preferably, the coupling agent is at least one of silane coupling agent KH550, silane coupling agent KH560, and silane coupling agent KH570.
[0013] Preferably, the filler is a mixture of metal powder, nano-boron fiber, and graphene oxide in a mass ratio of 1:(1-2):(0.8-1.2).
[0014] Preferably, the metal powder is nano copper powder with an average particle size of 10-100 nm.
[0015] Preferably, the average diameter of the nano-boron fiber is 300-500 nm, and the aspect ratio is (15-25):1.
[0016] Preferably, the graphene oxide is a single-layer graphene oxide with a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, numbered XF002-2, CAS number 7440-44-0, and provided by Jiangsu Xianfeng Nanomaterial Technology Co., Ltd.
[0017] Preferably, there is no special requirement for the source of the hyperbranched tripolyphosphazene terpyridine CTP-TPY. In one embodiment of the present invention, the hyperbranched tripolyphosphazene terpyridine CTP-TPY is prepared according to the method of Example 2 of the Chinese invention patent with authorization announcement number CN106432341B.
[0018] Preferably, the compatibilizer is maleic anhydride grafted polypropylene, selected from MAH-g-PP with the brand name EXXELOR PO1020 provided by Exxon in the United States.
[0019] Preferably, the antioxidant is at least one of antioxidant 1010, antioxidant 168, and antioxidant 1076.
[0020] Preferably, the lubricant is at least one of pentaerythritol stearate, zinc stearate, and ethylene bisstearamide.
[0021] Preferably, the initiator is at least one of bis(tert-butylperoxyisopropyl)benzene, 2,5-dimethyl-2,5-di-tert-butylperoxyhexane, diisopropylbenzene peroxide, and di-tert-butyl peroxide.
[0022] Preferably, the catalyst is a mixture of phosphorus pentoxide and polyphosphoric acid in a mass ratio of (1-2):1.
[0023] Another object of the present invention is to provide a method for preparing the reinforced flame-retardant PC composite material, comprising the steps of: uniformly mixing the raw materials in parts by weight to obtain a mixture, adding the mixture to a twin-screw extruder for extrusion molding to obtain a reinforced flame-retardant PC composite material.
[0024] Preferably, the extrusion temperature of the twin-screw extruder is 280-320° C., and the screw speed is 300-350 r / min.
[0025] Due to the application of the above technical solution, the present invention has the following beneficial effects:
[0026] (1) The preparation method of the reinforced flame-retardant PC composite material disclosed in the present invention has a simple preparation process, high efficiency, stable performance of the prepared product, is suitable for large-scale production, does not require special equipment, requires little capital investment, and has high promotion and application value.
[0027] (2) The reinforced flame-retardant PC composite material disclosed in the present invention is made of the following raw materials in parts by weight: 80 parts of PC resin, 10-20 parts of terminal hydroxyl hyperbranched polycarbonate, 5-8 parts of micro-crosslinking agent, 3-5 parts of coupling agent, 25-35 parts of filler, 5-8 parts of hyperbranched tripolyphosphazene terpyridine CTP-TPY, 2-4 parts of compatibilizer, 0.3-0.6 parts of antioxidant, 0.3-0.6 parts of lubricant, 0.8-1.2 parts of initiator, 2-4 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1-3 parts of octaphenylcyclotetrasiloxane, 4-6 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 0.8-1.2 parts of catalyst. Through the mutual coordination and joint action of the raw materials, the prepared PC composite material has good mechanical properties, excellent flame retardancy, impact toughness and weather resistance. At the same time, the hyperbranched tripolyphosphazene terpyridine, terminal hydroxyl hyperbranched polycarbonate, phosphaphenanthrene, and octaphenylcyclotetrasiloxane structures introduced, under the multiple effects of electronic effects, steric effects, and conjugated effects, make the manufactured products have better mechanical properties, better flame retardancy and impact properties, and better weather resistance.
[0028] (3) The reinforced flame-retardant PC composite material disclosed in the present invention comprises a filler comprising metal powder, nano-boron fiber, and graphene oxide mixed in a mass ratio of 1:(1-2):(0.8-1.2). The addition of metal powder can increase the specific gravity and antistatic properties of the material; in combination with nano-boron fiber and graphene oxide, it can also effectively improve the mechanical properties and flame retardant properties; the addition of graphene oxide is beneficial for improving the dispersion uniformity of the filler and its compatibility with the substrate; the addition of a micro-crosslinking agent can produce an ester exchange reaction with polycarbonate; at the same time, the raw materials containing unsaturated olefinic bonds can undergo an addition polymerization reaction, and the raw materials containing sulfonic acid groups can also interact with the raw materials containing benzene rings, thereby achieving good compatibility between the raw materials, cooperating with each other to form an interpenetrating network structure, and effectively improving the mechanical properties, flame retardancy, impact toughness, and weather resistance of the material.
[0029] (4) The enhanced flame-retardant PC composite material disclosed in the present invention has good compatibility with PC resin because the end-hydroxyl hyperbranched polycarbonate contains a polycarbonate structure. At the same time, the introduction of the hyperbranched structure can improve the impact toughness. The hydroxyl groups introduced thereon can improve the compatibility between the various raw materials. In addition, it can form a dense organic layer on the surface of the filler in combination with the hyperbranched tripolyphosphazene terpyridine, so that the bonding force between the filler and the PC substrate is stronger. The resulting material has better mechanical properties, flame retardancy, impact toughness and weather resistance, higher performance stability and longer service life. DETAILED DESCRIPTION
[0030] The following description is intended to disclose the present invention so that those skilled in the art can implement the present invention. The preferred embodiments described below are merely examples, and those skilled in the art may conceive of other obvious variations.
[0031] Example 1
[0032] A reinforced flame-retardant PC composite material comprises the following raw materials in parts by weight: 80 parts of PC resin, 10 parts of hydroxyl-terminated hyperbranched polycarbonate, 5 parts of a micro-crosslinking agent, 3 parts of a coupling agent, 25 parts of a filler, 5 parts of hyperbranched tripolyphosphazene terpyridine (CTP-TPY), 2 parts of a compatibilizer, 0.3 parts of an antioxidant, 0.3 parts of a lubricant, 0.8 parts of an initiator, 2 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1 part of octaphenylcyclotetrasiloxane, 4 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 0.8 parts of a catalyst.
[0033] The PC resin is Lexan PC 121; the hydroxyl-terminated hyperbranched polycarbonate is prepared according to the method of Example 5 of the Chinese invention patent with the authorization publication number CN107151316B; the micro-crosslinking agent is polyethylene glycol methacrylate; the average molecular weight of the polyethylene glycol methacrylate is 475, and it is produced by Changsha Jingkang New Materials Technology Co., Ltd.; the coupling agent is silane coupling agent KH550; the filler is a mixture of metal powder, nano boron fiber, and graphene oxide in a mass ratio of 1:1:0.8; the metal powder is nano copper powder with an average particle size of 1.5-1.0; The diameter is 10 nm; the average diameter of the nano-boron fiber is 300 nm, and the aspect ratio is 15:1; the graphene oxide is a single-layer graphene oxide with a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, numbered XF002-2, CAS number 7440-44-0, and provided by Jiangsu Xianfeng Nanomaterial Technology Co., Ltd.; the hyperbranched tripolyphosphazene terpyridine CTP-TPY is prepared according to the method of Example 2 of the Chinese invention patent with authorization announcement number CN106432341B.
[0034] The compatibilizer is maleic anhydride grafted polypropylene, selected from MAH-g-PP with the brand EXXELORPO1020 provided by Exxon in the United States; the antioxidant is antioxidant 1010; the lubricant is pentaerythritol stearate; the initiator is bis(tert-butyl peroxide isopropyl)benzene; and the catalyst is a mixture of phosphorus pentoxide and polyphosphoric acid in a mass ratio of 1:1.
[0035] A method for preparing the reinforced flame-retardant PC composite material comprises the following steps: uniformly mixing the raw materials according to parts by weight to obtain a mixture, adding the mixture into a twin-screw extruder for extrusion molding to obtain a reinforced flame-retardant PC composite material; the extrusion temperature of the twin-screw extruder is 280°C and the screw speed is 300 r / min.
[0036] Example 2
[0037] A reinforced flame-retardant PC composite material comprises the following raw materials in parts by weight: 80 parts of PC resin, 13 parts of hydroxyl-terminated hyperbranched polycarbonate, 6 parts of a micro-crosslinking agent, 3.5 parts of a coupling agent, 27 parts of a filler, 6 parts of hyperbranched tripolyphosphazene terpyridine (CTP-TPY), 2.5 parts of a compatibilizer, 0.4 parts of an antioxidant, 0.4 parts of a lubricant, 0.9 parts of an initiator, 2.5 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.5 parts of octaphenylcyclotetrasiloxane, 4.5 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 0.9 parts of a catalyst.
[0038] The PC resin is Lexan PC 121; the hydroxyl-terminated hyperbranched polycarbonate is prepared according to the method of Example 5 of the Chinese invention patent with the authorization publication number CN107151316B; the micro-crosslinking agent is perfluoroalkyl acrylate FC-14; the perfluoroalkyl acrylate FC-14 is provided by Taipuda New Materials; the coupling agent is silane coupling agent KH560; the filler is a mixture of metal powder, nano-boron fiber, and graphene oxide in a mass ratio of 1:1.3:0.9; the metal powder is nano-copper powder with an average particle size of 30 nm; the average diameter of the nano-boron fiber is 350 nm, and the aspect ratio is 17:1; the graphene oxide is a single-layer graphene oxide with a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, numbered XF002-2, CAS number 7440-44-0, and provided by Jiangsu Xianfeng Nanomaterial Technology Co., Ltd.; the hyperbranched tripolyphosphazene terpyridine CTP-TPY is according to the method of Example 2 of the Chinese invention patent with authorization announcement number CN106432341B.
[0039] The compatibilizer is maleic anhydride grafted polypropylene, selected from MAH-g-PP with the brand EXXELORPO1020 provided by Exxon in the United States; the antioxidant is antioxidant 168; the lubricant is zinc stearate; the initiator is 2,5-dimethyl-2,5-di-tert-butyl peroxide hexane; and the catalyst is a mixture of phosphorus pentoxide and polyphosphoric acid in a mass ratio of 1.3:1.
[0040] A method for preparing the reinforced flame-retardant PC composite material comprises the following steps: uniformly mixing the raw materials according to parts by weight to obtain a mixture, adding the mixture into a twin-screw extruder for extrusion molding to obtain a reinforced flame-retardant PC composite material; the extrusion temperature of the twin-screw extruder is 285°C and the screw speed is 310 r / min.
[0041] Example 3
[0042] A reinforced flame-retardant PC composite material comprises the following raw materials in parts by weight: 80 parts of PC resin, 15 parts of hydroxyl-terminated hyperbranched polycarbonate, 6.5 parts of a micro-crosslinking agent, 4 parts of a coupling agent, 30 parts of a filler, 6.5 parts of hyperbranched tripolyphosphazene terpyridine (CTP-TPY), 3 parts of a compatibilizer, 0.45 parts of an antioxidant, 0.45 parts of a lubricant, 1 part of an initiator, 3 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2 parts of octaphenylcyclotetrasiloxane, 5 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 1 part of a catalyst.
[0043] The PC resin is Lexan PC 121; the hydroxyl-terminated hyperbranched polycarbonate is prepared according to the method of Example 5 of the Chinese invention patent with the authorization publication number CN107151316B; the micro-crosslinking agent is a mixture of polyethylene glycol methacrylate and perfluoroalkyl acrylate FC-14 in a mass ratio of 3:5; the average molecular weight of the polyethylene glycol methacrylate is 475 and is provided by Changsha Jingkang New Materials Technology Co., Ltd.; the perfluoroalkyl acrylate FC-14 is provided by Taipuda New Materials; the coupling agent is silane coupling agent KH570; the filler is metal powder, nano-boron fiber, and graphene oxide in a mass ratio of 1:1. :1.5:1; the metal powder is nano copper powder with an average particle size of 60 nm; the nano boron fiber has an average diameter of 400 nm and an aspect ratio of 20:1; the graphene oxide is a single-layer graphene oxide with a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, numbered XF002-2, CAS number 7440-44-0, provided by Jiangsu Xianfeng Nanomaterial Technology Co., Ltd.; the hyperbranched tripolyphosphazene terpyridine CTP-TPY is prepared according to the method of Example 2 of the Chinese invention patent with authorization announcement number CN106432341B.
[0044] The compatibilizer is maleic anhydride grafted polypropylene, selected from MAH-g-PP with the brand EXXELORPO1020 provided by Exxon in the United States; the antioxidant is antioxidant 1076; the lubricant is ethylene bisstearamide; the initiator is dicumyl peroxide; and the catalyst is a mixture of phosphorus pentoxide and polyphosphoric acid in a mass ratio of 1.5:1.
[0045] A method for preparing the reinforced flame-retardant PC composite material comprises the following steps: uniformly mixing the raw materials according to parts by weight to obtain a mixture, adding the mixture into a twin-screw extruder for extrusion molding to obtain a reinforced flame-retardant PC composite material; the extrusion temperature of the twin-screw extruder is 290°C and the screw speed is 320 r / min.
[0046] Example 4
[0047] A reinforced flame-retardant PC composite material comprises the following raw materials in parts by weight: 80 parts of PC resin, 18 parts of hydroxyl-terminated hyperbranched polycarbonate, 7 parts of a micro-crosslinking agent, 4.5 parts of a coupling agent, 33 parts of a filler, 7.5 parts of hyperbranched tripolyphosphazene terpyridine (CTP-TPY), 3.5 parts of a compatibilizer, 0.55 parts of an antioxidant, 0.55 parts of a lubricant, 1.1 parts of an initiator, 3.5 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 2.5 parts of octaphenylcyclotetrasiloxane, 5.5 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 1.1 parts of a catalyst.
[0048] The PC resin is Lexan PC 121; the terminal hydroxyl hyperbranched polycarbonate is prepared according to the method of Example 5 of the Chinese invention patent with the authorization publication number CN107151316B; the micro-crosslinking agent is polyethylene glycol methacrylate; the average molecular weight of the polyethylene glycol methacrylate is 475, and it is produced by Changsha Jingkang New Material Technology Co., Ltd.; the coupling agent is a mixture of silane coupling agent KH550, silane coupling agent KH560, and silane coupling agent KH570 in a mass ratio of 1:1:1; the filler is a mixture of metal powder, nano-boron fiber, and graphene oxide in a mass ratio of 1:1.8:1.1. The metal powder is nano copper powder with an average particle size of 90 nm; the average diameter of the nano boron fiber is 450 nm, and the aspect ratio is 23:1; the graphene oxide is a single-layer graphene oxide with a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, numbered XF002-2, CAS number 7440-44-0, provided by Jiangsu Xianfeng Nanomaterial Technology Co., Ltd.; the hyperbranched tripolyphosphazene terpyridine CTP-TPY is prepared according to the method of Example 2 of the Chinese invention patent with authorization announcement number CN106432341B.
[0049] The compatibilizer is maleic anhydride grafted polypropylene, selected from MAH-g-PP with the brand EXXELORPO1020 provided by Exxon in the United States; the antioxidant is a mixture of antioxidant 1010, antioxidant 168, and antioxidant 1076 in a mass ratio of 1:1:2; the lubricant is a mixture of pentaerythritol stearate, zinc stearate, and ethylene bisstearamide in a mass ratio of 1:2:3; the initiator is a mixture of bis(tert-butylperoxyisopropyl)benzene, 2,5-dimethyl-2,5-di-tert-butylperoxide hexane, diisopropylbenzene peroxide, and di-tert-butyl peroxide in a mass ratio of 1:2:1:1; and the catalyst is a mixture of phosphorus pentoxide and polyphosphoric acid in a mass ratio of 1.8:1.
[0050] A method for preparing the reinforced flame-retardant PC composite material comprises the following steps: uniformly mixing the raw materials according to parts by weight to obtain a mixture, adding the mixture into a twin-screw extruder for extrusion molding to obtain a reinforced flame-retardant PC composite material; the extrusion temperature of the twin-screw extruder is 300°C and the screw speed is 330 r / min.
[0051] Example 5
[0052] A reinforced flame-retardant PC composite material comprises the following raw materials in parts by weight: 80 parts of PC resin, 20 parts of hydroxyl-terminated hyperbranched polycarbonate, 8 parts of a micro-crosslinking agent, 5 parts of a coupling agent, 35 parts of a filler, 8 parts of hyperbranched tripolyphosphazene terpyridine (CTP-TPY), 4 parts of a compatibilizer, 0.6 parts of an antioxidant, 0.6 parts of a lubricant, 1.2 parts of an initiator, 4 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3 parts of octaphenylcyclotetrasiloxane, 6 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 1.2 parts of a catalyst.
[0053] The PC resin is Lexan PC 121; the hydroxyl-terminated hyperbranched polycarbonate is prepared according to the method of Example 5 of the Chinese invention patent with the authorization publication number CN107151316B; the micro-crosslinking agent is perfluoroalkyl acrylate FC-14; the perfluoroalkyl acrylate FC-14 is provided by Taipuda New Materials; the coupling agent is silane coupling agent KH550; the filler is a mixture of metal powder, nano-boron fiber, and graphene oxide in a mass ratio of 1:2:1.2; the metal powder is nano-copper powder with an average particle size of 100 nm. m; the average diameter of the nano-boron fiber is 500 nm, and the aspect ratio is 25:1; the graphene oxide is a single-layer graphene oxide with a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, numbered XF002-2, CAS number 7440-44-0, and provided by Jiangsu Xianfeng Nanomaterial Technology Co., Ltd.; the hyperbranched tripolyphosphazene terpyridine CTP-TPY is according to the method of Example 2 of the Chinese invention patent with authorization announcement number CN106432341B.
[0054] The compatibilizer is maleic anhydride grafted polypropylene, selected from MAH-g-PP with the brand EXXELORPO1020 provided by Exxon in the United States; the antioxidant is antioxidant 1010; the lubricant is pentaerythritol stearate; the initiator is bis(tert-butyl peroxyisopropyl)benzene; and the catalyst is a mixture of phosphorus pentoxide and polyphosphoric acid in a mass ratio of 2:1.
[0055] A method for preparing the reinforced flame-retardant PC composite material comprises the following steps: uniformly mixing the raw materials according to parts by weight to obtain a mixture, adding the mixture into a twin-screw extruder for extrusion molding to obtain a reinforced flame-retardant PC composite material; the extrusion temperature of the twin-screw extruder is 305°C and the screw speed is 340r / min.
[0056] Comparative Example 1
[0057] This example provides a reinforced flame-retardant PC composite material, which is basically the same as Example 1, except that an equal amount of PC resin is used to replace the terminal hydroxyl hyperbranched polycarbonate and the hyperbranched tripolyphosphazene terpyridine CTP-TPY.
[0058] Comparative Example 2
[0059] This example provides a reinforced flame-retardant PC composite material, which is basically the same as Example 1, except that 2-acrylamido-2-methylpropanesulfonic acid is not added, and an equal amount of octaphenylcyclotetrasiloxane is used instead of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.
[0060] In order to further illustrate the beneficial technical effects of the reinforced flame-retardant PC composite materials involved in each embodiment of the present invention, relevant performance tests were conducted on the reinforced flame-retardant PC composite materials involved in Examples 1-5 and Comparative Examples 1-2; the test methods are as follows:
[0061] (1) Tensile properties: The tensile strength test was performed according to GB / T 1040.1-2018 at a tensile speed of 5 mm / s.
[0062] (2) Notched impact strength: tested in accordance with GB / T1843-2008 standard, with specimen dimensions of (80±2) mm × (10±0.2) mm × (4±0.2) mm, notch bottom radius of 0.25±0.05 mm, and notch retention thickness of 8.0±0.2 mm.
[0063] (3) Weather resistance: Each example of reinforced flame retardant PC composite material was subjected to a carbon arc lamp aging test according to GB / T16422.4-1996, using a continuous 720-h illumination test, a blackboard temperature of (65±3)°C, a relative humidity of (50±5)%, and then cooled to room temperature to measure the tensile strength retention rate of the product. Tensile strength retention rate = tensile strength after aging / tensile strength before aging × 100%. The greater the tensile strength retention rate, the better the weather resistance. The tensile strength test refers to (1) the test method of tensile properties.
[0064] (4) Flame retardancy: tested according to UL94 standard.
[0065] As can be seen from Table 1, the reinforced flame-retardant PC composite materials involved in each embodiment of the present invention have higher mechanical properties and notched impact strength, more excellent flame retardancy and weather resistance. The combined addition of terminal hydroxyl hyperbranched polycarbonate, hyperbranched tripolyphosphazene terpyridine CTP-TPY, 2-acrylamido-2-methylpropanesulfonic acid, octaphenylcyclotetrasiloxane, and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is beneficial to improving the above properties.
[0066] Table 1 Test results of properties of reinforced flame retardant PC composite materials
[0067] project tensile strength Notched impact strength Weather resistance flame retardancy unit MPa <![CDATA[KJ / m 2 ]]> % class Example 1 96.8 85.3 98.68 V-0 Example 2 99.0 86.5 98.99 V-0 Example 3 101.5 87.0 99.46 V-0 Example 4 104.5 88.0 99.70 V-0 Example 5 106.0 88.7 99.97 V-0 Comparative Example 1 88.6 73.2 97.93 V-2 Comparative Example 2 79.7 80.4 95.45 V-2
[0068] The above embodiments are only for illustrating the technical concept and features of the present invention. Their purpose is to enable people familiar with this technology to understand the content of the present invention and implement it accordingly. They are not intended to limit the scope of protection of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of protection of the present invention.
Claims
1. A reinforced flame retardant PC composite material, characterized in that: The invention comprises the following raw materials in parts by weight: 80 parts of PC resin, 10-20 parts of terminal hydroxyl hyperbranched polycarbonate, 5-8 parts of micro-crosslinking agent, 3-5 parts of coupling agent, 25-35 parts of filler, 5-8 parts of hyperbranched tripolyphosphazene terpyridine CTP-TPY, 2-4 parts of compatibilizer, 0.3-0.6 parts of antioxidant, 0.3-0.6 parts of lubricant, 0.8-1.2 parts of initiator, 2-4 parts of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1-3 parts of octaphenylcyclotetrasiloxane, 4-6 parts of 2-acrylamido-2-methylpropanesulfonic acid, and 0.8-1.2 parts of catalyst.
2. The reinforced flame retardant PC composite material according to claim 1, characterized in that: The PC resin is Lexan PC121.
3. The reinforced flame retardant PC composite material according to claim 1, characterized in that: The micro-crosslinking agent is at least one of polyethylene glycol methacrylate and perfluoroalkyl acrylate FC-14.
4. The reinforced flame retardant PC composite material according to claim 3, characterized in that: The average molecular weight of the polyethylene glycol methacrylate is 475.
5. The reinforced flame retardant PC composite material according to claim 1, characterized in that: The coupling agent is at least one of silane coupling agent KH550, silane coupling agent KH560, and silane coupling agent KH570.
6. The reinforced flame retardant PC composite material according to claim 1, characterized in that: The filler is a mixture of metal powder, nano-boron fiber, and graphene oxide in a mass ratio of 1:(1-2):(0.8-1.2); the metal powder is nano-copper powder with an average particle size of 10-100 nm; the nano-boron fiber has an average diameter of 300-500 nm and an aspect ratio of (15-25):1; the graphene oxide is a single-layer graphene oxide with a sheet diameter of 0.5-5 μm and a thickness of 0.8-1.2 nm, and is numbered XF002-2.
7. The reinforced flame retardant PC composite material according to claim 1, characterized in that: The compatibilizer is maleic anhydride grafted polypropylene, selected from MAH-g-PP with the brand name EXXELOR PO1020 provided by Exxon in the United States; the antioxidant is at least one of antioxidant 1010, antioxidant 168, and antioxidant 1076.
8. The reinforced flame-retardant PC composite material according to claim 1, characterized in that: The lubricant is at least one of pentaerythritol stearate, zinc stearate, and ethylene bisstearamide; the initiator is at least one of bis(tert-butylperoxyisopropyl)benzene, 2,5-dimethyl-2,5-di-tert-butylperoxyhexane, diisopropylbenzene peroxide, and di-tert-butyl peroxide; and the catalyst is a mixture of phosphorus pentoxide and polyphosphoric acid in a mass ratio of (1-2):
1.
9. A method for preparing the reinforced flame-retardant PC composite material according to any one of claims 1 to 8, characterized in that: The method comprises the following steps: uniformly mixing raw materials according to parts by weight to obtain a mixture, adding the mixture into a twin-screw extruder for extrusion molding, and obtaining a reinforced flame-retardant PC composite material.
10. The method for preparing the reinforced flame-retardant PC composite material according to claim 9, characterized in that: The extrusion temperature of the twin-screw extruder is 280-320° C., and the screw speed is 300-350 r / min.
Citation Information
Patent Citations
Hyperbranched polyphosphazene flame retardant charring agent and preparing method thereof
CN103992481A
Flame-retardant PC composition and preparation method thereof
CN113773628A
Modified polycarbonate material as well as preparation method and application thereof
CN114634697A
Protection material for power battery of new energy automobile and preparation method of protection material
CN115304861A
High-transparency polyester material and preparation method thereof
CN119019823A
Cited By
A high toughness polycarbonate composite
CN122541978A