CN101914271B - Environment-friendly flame retardant PBT/PC composite material and preparation method thereof - Google Patents
Environment-friendly flame retardant PBT/PC composite material and preparation method thereof Download PDFInfo
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- CN101914271B CN101914271B CN 201010270894 CN201010270894A CN101914271B CN 101914271 B CN101914271 B CN 101914271B CN 201010270894 CN201010270894 CN 201010270894 CN 201010270894 A CN201010270894 A CN 201010270894A CN 101914271 B CN101914271 B CN 101914271B
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Abstract
The invention provides an environment-friendly flame retardant PBT/PC composite material which comprises the following components in percentage by weight: 30-60% of PBT, 10-50% of PC, 0.1-1% of ester exchange inhibitor, 5-25% of fire retardant, 0-5% of flame retardant assistant, 1-10% of toughening compatilizer, 20-50% of glass fiber and 1-5% of processing additive. The invention also provides a preparation method of the composite material. The environment-friendly flame retardant PBT/PC composite material prepared by the invention has excellent mechanical property and flame retardant property, does not endanger the environment and human health, meets the requirements of EU ROHS instructions, has good liquidity and de-molding performance, improves the processing degree of freedom and production forming efficiency, has superior heat-resistant property and a heat-deformation temperature of 210 DEG C, has small shrinkage and good dimensional stability, prevents buckling deformation, and has high surface gloss and good appearance.
Description
Technical field
The present invention relates to a kind of electronic connector with environment-friendly flame retardant PBT/PC matrix material and preparation method thereof, especially environment-friendly flame retardant PBT/PC matrix material and preparation method thereof.
Technical background
Polybutylene terephthalate (PBT) is the fast thermoplasticity engineering materials of a kind of crystallization velocity; Be easy to realize high-speed molding; It has characteristics such as excellent mechanics, electricity, resistance to chemical attack, easy-formation and rate of moisture absorption are low; Be a kind of thermoplastic engineering plastic of high comprehensive performance, be widely used in automobile, the electronic apparatus production, be used for part of higher part of manufacturing machine requirement of strength and heat-resisting, shock-resistant, wear-resisting wiping etc.; Become important a member in the five large-engineering plastics, fiber glass reinforced PBT can increase substantially the shock strength and the heat-drawn wire of material.
The second-order transition temperature of PBT is low; The product molding shrinking percentage is bigger; It is low to exist notched Izod impact strength, shortcoming such as rigidity deficiency under the high temperature. therefore with PBT and PC blending and modifying, can realize mutual supplement with each other's advantages; Overcome deficiencies such as the PC chemical proofing is poor, forming process difficulty, remedied shortcomings such as PBT poor heat resistance, impact property are not high, molding shrinkage is big again.PBT is a crystalline polymer, and PC is an amorphous polymer, so PBT/PC belongs to typical crystallization and amorphous polymer co-mixing system, its interface imperfect bonding, and shock strength is low, can add the 3rd component and improve consistency, to improve the mechanical property of blend.
Flame-retardant PBT/PC matrix material is used very extensive in electric field; The enhancing day by day of Along with people's environmental protection, safety, health perception; Countries in the world begin the emphasis of environment friendly flame retardant as research and development and application; Some traditional bromide fire retardants force the user to seek the surrogate of bromine flame retardant owing to receive the pressure of increasingly stringent environmental requirement, have promoted the appearance of new flame-retardant system simultaneously.The atrophy in traditional bromide fire retardant such as polybromodiphenyl ether market is for environmentally friendly bromide fire retardant products such as brominated epoxy resin, TDE provide the market space.
Summary of the invention
The objective of the invention is to overcome the bad problem of bonding interface of PBT and PC; A kind of high efficiency flame retardance that has is provided; Good comprehensive mechanical property satisfies the environment-friendly flame retardant PBT/PC matrix material of ROHS command request simultaneously, and being mainly used in electronic connector is the electric field of representative.
Another object of the present invention provides the preparation method of above-mentioned environment-friendly flame retardant PBT/PC matrix material.
For realizing above purpose, technical scheme of the present invention is:
A kind of environment-friendly flame retardant PBT/PC matrix material, percentage ratio meter by weight, proportioning consists of:
PBT 30 to 60%
PC 10 to 50%
Ester exchange inhibitor 0.1 to 1%
Fire retardant 5 to 25%
Fire-retardant auxiliary 0 to 5%
Toughness reinforcing compatilizer 1 to 10%
Spun glass 20 to 50%
Processing aid 1 to 5%.
Described PBT is a polybutylene terephthalate, and specific density is 1.28 to 1.35g/cm
3, limiting viscosity is 0.8 to 1.5Pa.S, melt temperature is 220 to 235 ℃.
Described PC is a bisphenol-a polycarbonate, specific density 1.20 to 1.43,146 to 152 ℃ of second-order transition temperatures.
Described ester exchange inhibitor is one or more in triphenyl phosphite (TPPi), Sodium Acid Pyrophosphate (DSDP), SODIUM PHOSPHATE, MONOBASIC and the ammonium di-hydrogen phosphate.
Described fire retardant be Halogen phosphorus flame retardant ammonium polyphosphate (APP), primary ammonium phosphate, Secondary ammonium phosphate, SULPHOSUCCINIC ACID ESTER and environmental protection type bromide fire retardant tetrabromo-bisphenol, decabromodiphynly oxide, gather in dibromobenzene aether, pentabromotoluene and the hexabromocyclododecane one or more.
Described fire-retardant auxiliary is one or more of antimony type oxide and metaantimmonic acid salt.
Described toughness reinforcing compatilizer is ethylene-acrylate class-glycidyl methacrylate copolymer, one or more in the polyolefine of the elastomerics of " nuclear-shell " structure, the elastomerics of glycidyl methacrylate graft, glycidyl methacrylate graft.The elastomer core of described " nuclear-shell " structure is the acrylic ester elastomer of lower crosslink density, TEB 3K in the outer grafting.
Described processing aid is one or more mixtures in lipid acid, calcium stearate, silicone powder, silicone master batch, modification ethylene bis-fatty acid amides (TAF), the ethylene bis stearamide (EBS).
Described electronic connector is with environment-friendly flame retardant PBT/PC matrix material; Its preparation method is: with PBT, PC, ester exchange inhibitor, fire retardant, toughness reinforcing compatilizer, processing aid in proportion after the high-speed mixer dispersing and mixing; The side feeding adds spun glass, through the twin screw extruder fusion, mixing, extrude, cooling, pelletizing, drying and pack.It is 30 to 60: 1 that twin screw is extruded length-to-diameter ratio, and each section extruder temperature is 200 to 280 ℃, and screw speed is 250 to 450rpm.
Environment-friendly flame retardant PBT of the present invention/PC matrix material is suitable for that injection moulding is various to have the electronic connector of environmental protection flame retardant requirement and an electronic and electric components of sophisticated, has following characteristics:
1) mechanical property and the flame retardant properties of excellence;
2) do not endanger environment and HUMAN HEALTH, satisfy the ROHS of European Union command request;
3) flowability and release property are good, improve the processing degree of freedom and produce shaping efficiency;
4) fine heat-resisting performance, 210 ℃ of heat-drawn wires;
5) shrinking percentage is little, and dimensional stability is good, prevents buckling deformation;
6) surface gloss is high, and outward appearance is good.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.These embodiment only are used to the present invention is described and do not limit the scope of the invention.
Embodiment 1 to 10
In proportion after the high-speed mixer dispersing and mixing, the side feeding adds spun glass with PBT, PC, ester exchange inhibitor, fire retardant, toughness reinforcing compatilizer, processing aid, through the twin screw extruder fusion, mixing, extrude, cooling, pelletizing, drying and pack.It is 40: 1 that twin screw is extruded length-to-diameter ratio, and each section extruder temperature is 240 to 270 ℃, and screw speed is 400rpm.Each embodiment prepared composite material is injection molded into test bars by standard size, and mechanical property is tested by the SIO international standard respectively, and flame retardant properties is tested by the UL94 standard.
Embodiment 1 to 3 has verified different PBT/PC ratios, and proportioning and test data result see table 1 in detail.Embodiment 4 to 6 has verified the consumption of impact modifying agent, and other components change, and proportioning and test data result see table 2 in detail.Embodiment 7 to 10 has verified different flame retardant kind and consumption, and proportioning and test data result see table 3 in detail.Wherein, DSDP is an ester exchange inhibitor: Sodium Acid Pyrophosphate; 2100 is bromide fire retardant: TDE; ST-FR-B01 is a bromide fire retardant: brominated epoxy resin, ST-EPFR-300A are Halogen phosphorus, nitrogen flame retardant, and AX 8900 is toughness reinforcing compatilizer: ethylene-acrylate class-glycidyl methacrylate copolymer.
Table 1, Example formulations table and composite property test result
Table 2, Example formulations table and composite property test result
Table 3, Example formulations table and composite property test result
Claims (7)
1. environment-friendly flame retardant PBT/PC matrix material is characterized in that percentage ratio meter by weight, and proportioning consists of:
Described fire retardant be Halogen phosphorus flame retardant ammonium polyphosphate, primary ammonium phosphate, Secondary ammonium phosphate, SULPHOSUCCINIC ACID ESTER and environmental protection type bromide fire retardant tetrabromo-bisphenol, decabromodiphynly oxide, gather in dibromobenzene aether, pentabromotoluene and the hexabromocyclododecane one or more.
2. environment-friendly flame retardant PBT according to claim 1/PC matrix material is characterized in that: described ester exchange inhibitor is one or more in triphenyl phosphite, Sodium Acid Pyrophosphate, SODIUM PHOSPHATE, MONOBASIC and the ammonium di-hydrogen phosphate.
3. environment-friendly flame retardant PBT according to claim 1/PC matrix material is characterized in that: described fire-retardant auxiliary is one or more of antimony type oxide and metaantimmonic acid salt.
4. environment-friendly flame retardant PBT according to claim 1/PC matrix material; It is characterized in that: described toughness reinforcing compatilizer is ethylene-acrylate class-glycidyl methacrylate copolymer; In the polyolefine of the elastomerics of " nuclear-shell " structure, the elastomerics of glycidyl methacrylate graft, glycidyl methacrylate graft one or more; The elastomer core of described " nuclear-shell " structure is the acrylic ester elastomer of lower crosslink density, TEB 3K in the outer grafting.
5. environment-friendly flame retardant PBT according to claim 1/PC matrix material is characterized in that: described processing aid is one or more in lipid acid, calcium stearate, silicone powder, silicone master batch, modification ethylene bis-fatty acid amides, the ethylene bis stearamide.
6. the preparation method of the described environment-friendly flame retardant PBT of the arbitrary claim of claim 1 to 5/PC matrix material; It is characterized in that: with PBT, PC, ester exchange inhibitor, fire retardant, toughness reinforcing compatilizer, processing aid in proportion after the high-speed mixer dispersing and mixing; The side feeding adds spun glass; Through the twin screw extruder fusion, mixing, extrude, cooling, pelletizing, drying, promptly make environment-friendly flame retardant PBT/PC matrix material.
7. the preparation method of environment-friendly flame retardant PBT according to claim 6/PC matrix material is characterized in that: it is 30 to 60: 1 that described twin screw extruder is extruded length-to-diameter ratio, and each section extruder temperature is 200 to 280 ℃, and screw speed is 250 to 450rpm.
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| CN102181139B (en) * | 2011-01-27 | 2013-12-11 | 上海锦湖日丽塑料有限公司 | Glass fiber reinforcement polycarbonate resin and preparation method thereof |
| CN102492170B (en) * | 2011-12-20 | 2014-01-29 | 广州市聚赛龙工程塑料有限公司 | Preparation method of antimony trioxide master batch |
| CN103525051B (en) * | 2013-09-27 | 2015-10-14 | 惠州市昌亿新材料有限公司 | A kind of high-strength toughness reinforcing PC/PBT alloy material and its preparation method and application |
| CN103525050B (en) * | 2013-09-27 | 2015-09-30 | 惠州市昌亿科技股份有限公司 | A kind of high shading PC polymkeric substance and its preparation method and application |
| CN103613914B (en) * | 2013-11-13 | 2016-01-20 | 广东聚石化学股份有限公司 | A kind of high glowing filament ignition temperature environment-friendly flame retardant PBT matrix material and preparation method thereof |
| CN104356623B (en) * | 2014-09-30 | 2017-01-11 | 广东天保新材料有限责任公司 | Warping deformation-free PC/PBT alloy material and preparation method thereof |
| CN105623029B (en) * | 2014-10-27 | 2018-12-28 | 中国石油化工股份有限公司 | Composite reinforcing agent, PC/PBT alloy and application |
| CN104559105B (en) * | 2014-12-09 | 2016-09-21 | 惠州市昌亿科技股份有限公司 | A kind of low-shrinkage and high-strength degree PBT/PC alloy material for 3D printing and its preparation method and application |
| CN104693767A (en) * | 2014-12-15 | 2015-06-10 | 深圳市富恒新材料股份有限公司 | Glass fiber reinforced PC alloy material and preparation method thereof |
| CN104559114A (en) * | 2014-12-31 | 2015-04-29 | 上海锦湖日丽塑料有限公司 | Reactive thermoplastic resin combination and preparation method thereof |
| CN105086385B (en) * | 2015-08-25 | 2017-03-22 | 惠州市沃特新材料有限公司 | High-impact flame-retardant PBT/PC (polybutylene terephthalate/poly carbonate) alloy material and preparation method thereof |
| CN105316791B (en) * | 2015-11-26 | 2018-01-09 | 常州灵达特种纤维有限公司 | A kind of preparation method of soft wear resistant type polyester bulk filament |
| CN105713355A (en) * | 2015-12-25 | 2016-06-29 | 上海胜南复合材料有限公司 | High-performance warping-proof glass fiber reinforced PBT (polybutylene terephthalate)/PC (polycarbonate) alloy material |
| CN106519627B (en) * | 2016-05-08 | 2019-05-31 | 宁波泰甬汽车零部件有限公司 | Antistatic PC-PBT intermingling material and its preparation method and application |
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| CN107746558A (en) * | 2017-12-01 | 2018-03-02 | 上海金发科技发展有限公司 | One kind imitates ceramic PBT/PC resin combinations and preparation method thereof |
| CN107841098A (en) * | 2017-12-01 | 2018-03-27 | 上海金发科技发展有限公司 | A kind of imitative ceramic flame-proof PBT/PC resin combinations and preparation method thereof |
| CN108504068B (en) * | 2018-04-25 | 2020-06-23 | 横店集团得邦工程塑料有限公司 | High-fatigue-resistance flame-retardant PC/PBT alloy material and preparation method thereof |
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