TWI757885B - A high performance halogen-free flame retardant pc/cf composite and products thereof - Google Patents
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本發明涉及複合材料技術領域,尤其是一種高性能無鹵阻燃PC/CF複合材料及其製品。 The invention relates to the technical field of composite materials, in particular to a high-performance halogen-free flame-retardant PC/CF composite material and its products.
在電子電器、汽車等領域,產品的輕量化逐漸成為現代產品的趨勢,聚碳酸酯(Polycarbonate,PC)和碳纖維(Carbon Fiber,CF)的複合材料因其具有強度高,且與其他增強材料相比比重小的優點,而越來越受歡迎。 In the fields of electronic appliances, automobiles, etc., the lightweight of products has gradually become the trend of modern products. The composite materials of polycarbonate (PC) and carbon fiber (CF) have high strength and are compatible with other reinforcing materials. It is more and more popular because of its small specific gravity.
在電子電工產品中,由於PC/CF複合材料對阻燃的要求較高,因此會在複合材料中加入較多的阻燃劑,然而當碳纖維的直徑在微米級,燃燒時存在嚴重的「燈芯效應」,過多的阻燃劑不僅使物性降低,而且會使材料的熱變形溫度(Heat Deflection Temperature,HDT)降低到90℃以下。 In electronic and electrical products, PC/CF composites have higher requirements for flame retardancy, so more flame retardants are added to the composite materials. However, when the diameter of carbon fibers is in the micron level, there is a serious "wick" when burning. Excessive flame retardant not only reduces the physical properties, but also reduces the Heat Deflection Temperature (HDT) of the material to below 90°C.
因此,有必要對現有的技術進行改進。 Therefore, it is necessary to improve the existing technology.
本發明要解決的技術問題是:為了解決現有技術中的PC/CF複合材料中因加入了較多的阻燃劑,而使得材料的HDT降低的問 題。本發明提供了一種高性能無鹵阻燃PC/CF複合材料及其製品來解決上述問題。 The technical problem to be solved by the present invention is: in order to solve the problem of reducing the HDT of the material due to the addition of more flame retardants in the PC/CF composite material in the prior art question. The present invention provides a high-performance halogen-free flame-retardant PC/CF composite material and its products to solve the above problems.
本發明解決其技術問題的方案是:一種高性能無鹵阻燃PC/CF複合材料,包括以下重量份的組分:PC,60~75份;碳纖維,10~30份;及阻燃劑,4.5~10份;其中阻燃劑由磷氮烯阻燃劑和有機矽阻燃劑複配。 The solution of the present invention to solve the technical problem is: a high-performance halogen-free flame retardant PC/CF composite material, comprising the following components in parts by weight: PC, 60-75 parts; carbon fiber, 10-30 parts; and a flame retardant, 4.5~10 parts; the flame retardant is compounded by phosphazene flame retardant and organosilicon flame retardant.
較佳地,PC為雙酚A型聚碳酸酯、聚酯型聚碳酸酯、有機矽-聚碳酸酯(共聚)、環己烷雙酚A型聚碳酸酯、以及雙酚TMC(1,1-Bis(4-hydroyphenyl)-3,3,5-trimethyl-cyclohexane)合成的耐高溫聚碳酸酯的一種或多種複配。 Preferably, PC is bisphenol A polycarbonate, polyester polycarbonate, silicone-polycarbonate (copolymerization), cyclohexane bisphenol A polycarbonate, and bisphenol TMC (1,1 -One or more compounds of high temperature resistant polycarbonate synthesized by Bis(4-hydroyphenyl)-3,3,5-trimethyl-cyclohexane).
較佳地,PC的重均分子量在20000~50000之間,分子量分布在1~2.5之間。 Preferably, the weight average molecular weight of PC is between 20,000 and 50,000, and the molecular weight distribution is between 1 and 2.5.
較佳地,在溫度為300℃、負荷重量為1.2kg下,所述PC的熔體質量流動速率為(3~70)g/10min。 Preferably, when the temperature is 300° C. and the load weight is 1.2 kg, the melt mass flow rate of the PC is (3~70) g/10min.
較佳地,磷氮烯阻燃劑為苯氧基環磷腈(phenoxy cyclophosphazene),苯氧基環磷腈的磷含量大於13%、氮含量含量大於5.8%、雜離子濃度小於0.01%、重均分子量693以及純度大於98.5%。 Preferably, the phosphazene flame retardant is phenoxy cyclophosphazene, and the phosphorus content of phenoxy cyclophosphazene is greater than 13%, the nitrogen content is greater than 5.8%, the concentration of hetero ions is less than 0.01%, and the weight is less than 0.01%. The average molecular weight is 693 and the purity is greater than 98.5%.
較佳地,有機矽阻燃劑為乙烯基-苯基矽烷,乙烯基-苯基矽烷的矽含量在50%~70%,矽烷重均分子量在2000~4000之間。 Preferably, the silicone flame retardant is vinyl-phenylsilane, the silicon content of vinyl-phenylsilane is 50%-70%, and the weight average molecular weight of the silane is between 2000-4000.
較佳地,碳纖維的絲數在40K~60K之間,單絲直徑在5~15μm以及短切長度為1~15mm。 Preferably, the number of filaments of the carbon fiber is between 40K and 60K, the diameter of the single filament is between 5 and 15 μm and the chopped length is between 1 and 15 mm.
較佳地,碳纖維的表面處理劑為氨基甲酸酯,氨基甲酸酯 分子量在200~500之間。 Preferably, the surface treatment agent of carbon fiber is carbamate, carbamate The molecular weight is between 200 and 500.
較佳地,還包括塑料抗滴落劑0.1~1份。 Preferably, 0.1-1 part of a plastic anti-drip agent is also included.
本發明還提供了一種製品,製品採用上述的高性能無鹵阻燃PC/CF複合材料製得。 The present invention also provides a product, which is prepared by using the above-mentioned high-performance halogen-free flame-retardant PC/CF composite material.
本發明的有益效果是,相對於現有技術中在PC/CF複合材料加入較多的阻燃劑來說,這種高性能無鹵阻燃PC/CF複合材料藉由在PC/CF複合材料加入由磷氮烯阻燃劑和有機矽阻燃劑複配的阻燃劑,不僅減少了阻燃劑的用量,而且能夠使得PC/CF複合材料在保持0.8mmV-0的阻燃等級的同時,提高其HDT。 The beneficial effect of the present invention is that, compared with the prior art that adds more flame retardants to the PC/CF composite material, the high performance halogen-free flame retardant PC/CF composite material can be obtained by adding more flame retardants to the PC/CF composite material. The flame retardant compounded by phosphazene flame retardant and silicone flame retardant not only reduces the amount of flame retardant, but also enables PC/CF composite materials to maintain the flame retardant grade of 0.8mmV-0, Raise its HDT.
本發明提供了一種高性能無鹵阻燃PC/CF複合材料,包括以下重量份的組分:PC,60~75份;碳纖維,10~30份;以及阻燃劑,4.5~10份,其中阻燃劑由磷氮烯阻燃劑和有機矽阻燃劑複配,並且磷氮烯阻燃劑為4~8份,有機矽阻燃劑為0.5~2份。 The invention provides a high-performance halogen-free flame-retardant PC/CF composite material, comprising the following components in parts by weight: PC, 60-75 parts; carbon fiber, 10-30 parts; and flame retardant, 4.5-10 parts, wherein The flame retardant is compounded by phosphazene flame retardant and organosilicon flame retardant, and the phosphazene flame retardant is 4~8 parts, and the organosilicon flame retardant is 0.5~2 parts.
具體地,該高性能無鹵阻燃PC/CF複合材料中,PC為雙酚A型聚碳酸酯、聚酯型聚碳酸酯、有機矽-聚碳酸酯(共聚)、環己烷雙酚A型聚碳酸酯、以及雙酚TMC合成的耐高溫聚碳酸酯的一種或多種複配。PC的重均分子量在20000~50000之間,分子量分布在1~2.5之間。在溫度為300℃,負荷重量為1.2kg下,PC的熔體質量流動速率為(3~70)g/10min。 Specifically, in the high-performance halogen-free flame retardant PC/CF composite material, PC is bisphenol A polycarbonate, polyester polycarbonate, organosilicon-polycarbonate (copolymerization), cyclohexane bisphenol A One or more compounds of high temperature resistant polycarbonate synthesized from bisphenol TMC and bisphenol TMC. The weight average molecular weight of PC is between 20,000 and 50,000, and the molecular weight distribution is between 1 and 2.5. Under the temperature of 300℃ and the load weight of 1.2kg, the melt mass flow rate of PC is (3~70)g/10min.
該高性能無鹵阻燃PC/CF複合材料中,磷氮烯阻燃劑為苯氧基環磷腈,苯氧基環磷腈的磷含量大於13%、氮含量大於5.8%、雜離子濃度小於0.01%、重均分子量693以及純度大於98.5%。 In the high performance halogen-free flame retardant PC/CF composite material, the phosphazene flame retardant is phenoxy cyclophosphazene, and the phosphorus content of phenoxy cyclophosphazene is greater than 13%, the nitrogen content is greater than 5.8%, and the concentration of hetero ions Less than 0.01%, weight average molecular weight 693 and purity greater than 98.5%.
該高性能無鹵阻燃PC/CF複合材料中,有機矽阻燃劑為乙烯基-苯基矽烷,乙烯基-苯基矽烷的矽含量在50%~70%,矽烷重均分子量在2000~4000之間。 In this high-performance halogen-free flame retardant PC/CF composite material, the silicone flame retardant is vinyl-phenylsilane, the silicon content of vinyl-phenylsilane is 50%~70%, and the silane weight average molecular weight is 2000~ between 4000.
該高性能無鹵阻燃PC/CF複合材料中,碳纖維的絲數在40K~60K之間,單絲直徑在5~15μm以及短切長度為1~15mm。碳纖維的表面處理劑為氨基甲酸酯,氨基甲酸酯分子量在200~500之間。 In the high-performance halogen-free flame-retardant PC/CF composite material, the number of carbon fibers is between 40K and 60K, the diameter of the single fiber is 5-15μm and the chopped length is 1-15mm. The surface treatment agent of carbon fiber is carbamate, and the molecular weight of carbamate is between 200 and 500.
該高性能無鹵阻燃PC/CF複合材料中,還包括塑料抗滴落劑0.1~1份。塑料抗滴落劑使PC材料在塑料加工中纖維化,具有受熱收縮的特點及達到阻燃和防滴落的作用。 The high-performance halogen-free flame-retardant PC/CF composite material also includes 0.1 to 1 part of a plastic anti-drip agent. The plastic anti-drip agent makes the PC material fibrillated in the plastic processing, has the characteristics of thermal shrinkage, and achieves the effect of flame retardant and anti-drip.
下面藉由具體實施方式來進一步說明本發明的技術方案。 The technical solutions of the present invention are further described below by means of specific embodiments.
實施例1 Example 1
一種高性能無鹵阻燃PC/CF複合材料,包括以下重量份的組分:72.7份的PC、20份的碳纖維、7份的阻燃劑以及0.3份的塑料抗滴落劑。 A high-performance halogen-free flame retardant PC/CF composite material comprises the following components in parts by weight: 72.7 parts of PC, 20 parts of carbon fiber, 7 parts of flame retardant and 0.3 part of plastic anti-drip agent.
具體地,PC為雙酚A型聚碳酸酯。在溫度為300℃,負荷重量為1.2kg下,PC的熔體質量流動速率為40g/10min。 Specifically, PC is bisphenol A polycarbonate. At a temperature of 300°C and a load weight of 1.2kg, the melt mass flow rate of PC was 40g/10min.
碳纖維的絲數在40K~60K之間,單絲直徑在5~15μm以及短切長度為1~15mm。碳纖維的表面處理劑為氨基甲酸酯,氨基甲酸酯分子量在200~500之間。 The number of filaments of carbon fiber is between 40K~60K, the diameter of the single filament is 5~15μm and the chopped length is 1~15mm. The surface treatment agent of carbon fiber is carbamate, and the molecular weight of carbamate is between 200 and 500.
阻燃劑為6份的苯氧基環磷腈和1份的乙烯基-苯基矽烷複配。苯氧基環磷腈的磷含量大於13%、氮含量大於5.8%、雜離子濃度小於0.01%、重均分子量693以及純度大於98.5%。乙烯基-苯基矽烷的矽含量在50%~70%、矽烷重均分子量在2000~4000之間。 The flame retardant is a compound of 6 parts of phenoxycyclophosphazene and 1 part of vinyl-phenylsilane. The phosphorus content of phenoxycyclophosphazene is more than 13%, the nitrogen content is more than 5.8%, the concentration of hetero ions is less than 0.01%, the weight average molecular weight is 693, and the purity is more than 98.5%. The silicon content of vinyl-phenylsilane is 50%~70%, and the silane weight average molecular weight is between 2000~4000.
塑料抗滴落劑為聚四氟乙烯。 The plastic anti-drip agent is polytetrafluoroethylene.
製備該高性能無鹵阻燃PC/CF複合材料時,按照上述配比稱取相應重量份的組分,將各組分混合均勻後熔融擠出造粒。 When preparing the high-performance halogen-free flame-retardant PC/CF composite material, the components in the corresponding parts by weight are weighed according to the above ratio, and the components are uniformly mixed and then melted, extruded and pelletized.
對比例1 Comparative Example 1
一種PC/CF複合材料,包括以下重量份的組分:66.7份的PC、20份的碳纖維、13份的阻燃劑以及0.3份的塑料抗滴落劑。 A PC/CF composite material comprises the following components in parts by weight: 66.7 parts of PC, 20 parts of carbon fiber, 13 parts of flame retardant and 0.3 part of plastic anti-drip agent.
具體地,PC為雙酚A型聚碳酸酯,阻燃劑為磷酸酯阻燃劑(Bisphenol-A Bis(Diphenyl Phosphate),BDP),塑料抗滴落劑為聚四氟乙烯。 Specifically, the PC is bisphenol A polycarbonate, the flame retardant is a phosphate ester flame retardant (Bisphenol-A Bis (Diphenyl Phosphate), BDP), and the plastic anti-drip agent is polytetrafluoroethylene.
該複合材料的製備方法與實施例1相同。 The preparation method of the composite material is the same as that of Example 1.
實施例2 Example 2
一種高性能無鹵阻燃PC/CF複合材料,包括以下重量份的組分:65.7份的PC、25份的碳纖維、9份的阻燃劑以及0.3份的塑料抗滴落劑。 A high-performance halogen-free flame-retardant PC/CF composite material comprises the following components in parts by weight: 65.7 parts of PC, 25 parts of carbon fiber, 9 parts of flame retardant and 0.3 part of plastic anti-drip agent.
具體地,PC為雙酚A型聚碳酸酯。在溫度為300℃,負荷重量為1.2kg下,PC的熔體質量流動速率為40g/10min。 Specifically, PC is bisphenol A polycarbonate. At a temperature of 300°C and a load weight of 1.2kg, the melt mass flow rate of PC was 40g/10min.
碳纖維的絲數在40K~60K之間,單絲直徑在5~15μm以及短切長度為1~15mm。碳纖維的表面處理劑為氨基甲酸酯,氨基甲酸 酯分子量在200~500之間。 The number of filaments of carbon fiber is between 40K~60K, the diameter of the single filament is 5~15μm and the chopped length is 1~15mm. The surface treatment agent of carbon fiber is urethane, urethane The molecular weight of the ester is between 200 and 500.
阻燃劑為8份的苯氧基環磷腈和1份的乙烯基-苯基矽烷複配。苯氧基環磷腈的磷含量大於13%、氮含量大於5.8%、雜離子濃度小於0.01%、重均分子量693以及純度大於98.5%。乙烯基-苯基矽烷的矽含量在50%~70%,矽烷重均分子量在2000~4000之間。 The flame retardant is compounded by 8 parts of phenoxy cyclophosphazene and 1 part of vinyl-phenyl silane. The phosphorus content of phenoxycyclophosphazene is more than 13%, the nitrogen content is more than 5.8%, the concentration of hetero ions is less than 0.01%, the weight average molecular weight is 693, and the purity is more than 98.5%. The silicon content of vinyl-phenylsilane is 50%~70%, and the weight average molecular weight of the silane is between 2000~4000.
塑料抗滴落劑為聚四氟乙烯。 The plastic anti-drip agent is polytetrafluoroethylene.
製備該高性能無鹵阻燃PC/CF複合材料時,按照上述配比稱取相應重量份的組分,將各組分混合均勻後熔融擠出造粒。 When preparing the high-performance halogen-free flame-retardant PC/CF composite material, the components in the corresponding parts by weight are weighed according to the above ratio, and the components are uniformly mixed and then melted, extruded and pelletized.
對比例2 Comparative Example 2
一種PC/CF複合材料,包括以下重量份的組分:60.7份的PC、25份的碳纖維、14份的阻燃劑以及0.3份的塑料抗滴落劑。 A PC/CF composite material comprises the following components in parts by weight: 60.7 parts of PC, 25 parts of carbon fiber, 14 parts of flame retardant and 0.3 part of plastic anti-drip agent.
具體地,PC為雙酚A型聚碳酸酯,阻燃劑為磷酸酯阻燃劑(BDP),塑料抗滴落劑為聚四氟乙烯。 Specifically, the PC is bisphenol A polycarbonate, the flame retardant is a phosphate ester flame retardant (BDP), and the plastic anti-drip agent is polytetrafluoroethylene.
該複合材料的製備方法與實施例2相同。 The preparation method of the composite material is the same as that of Example 2.
以上實施例1、對比例1、實施例2及對比例2熔融擠出造粒後,然後將各實施例中的粒子在注塑機上注塑成型標準測試樣條,按標準測試所得材料的機械性能,測試結果如表1所示:
從實施例1、對比例1、實施例2以及對比例2的測試結果可知:相對於現有技術中在PC/CF複合材料加入較多的阻燃劑來說,本發明藉由在PC/CF複合材料加入由磷氮烯阻燃劑和有機矽阻燃劑複配的阻燃劑,不僅減少了阻燃劑的用量,而且能夠使得PC/CF複合材料在保持0.8mm V-0的阻燃等級的同時,提高其HDT。 From the test results of Example 1, Comparative Example 1, Example 2 and Comparative Example 2, it can be known that: compared with the prior art that adds more flame retardants to the PC/CF composite material, the present invention is The addition of a flame retardant compounded by phosphazene flame retardant and organosilicon flame retardant to the composite material not only reduces the amount of flame retardant, but also enables the PC/CF composite material to maintain a flame retardant of 0.8mm V-0. While leveling, increase its HDT.
本發明還提供了一種製品,其採用上述的高性能無鹵阻燃PC/CF複合材料製得,具有高阻燃性以及高的HDT,可廣泛應用在對阻燃等級要求高的電子電工產品中。 The present invention also provides a product, which is made of the above-mentioned high-performance halogen-free flame-retardant PC/CF composite material, has high flame retardancy and high HDT, and can be widely used in electronic and electrical products that require high flame retardant grades middle.
需指出的是,本發明不限於上述實施方式,任何熟悉本專業的技術人員基於本發明技術方案對上述實施例所作的任何簡單修改、等同變化與修飾,都落入本發明的保護範圍內。 It should be pointed out that the present invention is not limited to the above-mentioned embodiments, and any simple modifications, equivalent changes and modifications made to the above-mentioned embodiments by any person skilled in the art based on the technical solutions of the present invention all fall within the protection scope of the present invention.
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CN108779593A (en) * | 2016-03-08 | 2018-11-09 | 日立化成株式会社 | Carbon fiber nonwoven fabric, the manufacturing method of carbon fiber nonwoven fabric, carbon fiber multilayer cloth and composite material |
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CN109423024A (en) * | 2017-09-01 | 2019-03-05 | 汉达精密电子(昆山)有限公司 | Halogen-free flame retardant PC/CF anti-static material and products thereof |
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