CN102952399A - Environment-friendly flame retardant glass fiber reinforced polyamide 66 (PA66) material with high comparative tracking index (CTI) value and high glow wire ignition temperature (GWIT) value and preparation method thereof - Google Patents
Environment-friendly flame retardant glass fiber reinforced polyamide 66 (PA66) material with high comparative tracking index (CTI) value and high glow wire ignition temperature (GWIT) value and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an environment-friendly flame retardant glass fiber reinforced polyamide 66 (PA66) material with high comparative tracking index (CTI) value and high glow wire ignition temperature (GWIT) value, which comprises the raw material components by weight percent: 45-68% of PA66, 6-20% of compound fire retardant, 3-15% of antimonous oxide, 20-30% of glass fiber, 2-10% of compatilizer, 0.1-1% of antioxidant and 0.1-1% of oxide, wherein the compound fire retardant comprises brominated polystyrene, magnesium hypophosphite and talcum powder. The invention also discloses a preparation method of the environment-friendly flame retardant glass fiber reinforced PA66 material with high CTI value and high GWIT value. The composite material is higher in GWIT value and CTI value, better in flame retardant effect, environment-friendly in material and balanced in combination properties, thus being widely applied to products in the field of electronic electric appliances such as a low-voltage electronic capacitor shell, a load break switch, a carbon brush bracket, a moulded case circuit breaker and the like.
Description
Technical field
The present invention relates to technical field of composite materials, specifically, is a kind of high CTI value, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material and preparation method thereof.
Background technology
Nylon (Nylon), the Chinese name polymeric amide, English name Polyamide(is called for short PA), be contain on the molecular backbone chain recurring amide radical group-[NHCO]-the thermoplastic resin general name.Its name is decided by the concrete carbonatoms of synthon, as: polycaprolactam (nylon 6, abbreviation PA6), polyhexamethylene adipamide (nylon 66, abbreviation PA66), poly-sebacic acid decamethylene diamine (nylon 1010, abbreviation PA1010), polyhexamethylene sebacamide (NYLON610 is called for short PA610), nylon 11 (（Fen Mo/Ke Li） Nylon11 in powder/granular form is called for short PA11), poly-lauramide (nylon 12, abbreviation PA12), nylon 46 (nylon 46 is called for short PA46).PA degree of crystallinity is high, and fusing point is obvious; Surface hardness is large, abrasion performance, and frictional coefficient is little; Self lubricity and noise reduction are arranged; Low-temperature performance is good, and certain thermotolerance (can use below 100 degree) is arranged; Nontoxic, odorless, mildew and rot self-extinguishing, good weatherability are arranged, but dyeability are poor.
21 century electronics, electric, communication, household electrical appliances, electromechanical equipment are to the high-performance micro development, and more and more higher to the requirement of flame-retardant PA 66 material, simultaneously, along with the understanding of the mankind to environmental protection, Green Product is subject to common concern.Therefore, flame-retardant PA 66 Materials direction is: performance function flame-retardant PA 66 material becomes main flow; The kind of environmental type flame-retardant PA 66 material and demand are more and more; The production of flame-retardant PA 66 material is to many variety series future development; The use of fire retardant is to diversification, compound development.Traditional bromide fire retardant can not satisfy the requirement of high standard product, the fire retardant compound system that some are traditional, for example glass fibre+TDE+antimonous oxide compound system, glass fibre+brominated Polystyrene+antimonous oxide compound system, the CTI value of these compound systems (comparative tracking index, the relative discharge tracking index) and GWIT value (glow-wire ignition temperature, glow-wire ignition temperature) not high, be not suitable for the power utilization environment of high request.
Chinese patent literature application number 200610028821.1, open day on January 16th, 2008, a kind of flame-proof enhancement PA 66 composition is disclosed, this flame-proof enhancement PA 66 composition is by the PA66 base resin, glass, main flame retardant (brominated epoxy resin of molecular weight more than 10000), the auxiliary flame retardant antimonous oxide, toughening agent maleic anhydride grafting POE, the stablizer hydrotalcite, lubricant stearic acid and oxidation inhibitor Hinered phenols and phosphorous acid esters form, the PA66 composition satisfactory mechanical property of preparation, flame retardant effect is better, but the total content of main flame retardant and auxiliary flame retardant is higher, and GWIT and the CTI situation of composition is not provided.Chinese patent literature application number 201110301621.X, open day on March 21st, 2012, announced a kind of halogen-free flame retarding strengthened PA 66 material and preparation method thereof, its composition of described PA66 material is by weight ratio: PA66 resin 34～41%, alkali-free long glass fibres 30～40%, the high red phosphorus master batch 15～18% of filling, CTI improving agent 1～3%, anticorrosion erosion resistant agent 3～5%, compatible toughening agents 3～5%, oxidation inhibitor 0.4～1%, lubricant 0.4～1%, owing to adopting the red phosphorus master batch as fire retardant, increase substantially the CTI value of PA66 and reduced it to corrosion of metal, the CTI value is up to 480V.But yet there are no report about the compound PA66 material that integrates the advantages such as high GWIT value, high CTI value, environmental protection, over-all properties equilibrium.
Summary of the invention
The objective of the invention is for deficiency of the prior art, a kind of high CTI value, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material are provided.This matrix material glow wire temperature is higher, environmental protection, and over-all properties is balanced, is applicable to the Low-voltage Electronic capacitor case, load break switch, carbon brush supports, the electronic applications such as breaker of plastic casing.
Again one purpose of the present invention is that a kind of high CTI value, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material preparation method are provided.
For achieving the above object, the technical scheme taked of the present invention is:
A kind of high CTI value, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material, described material comprises the feed composition of following weight percent content:
PA66 45%～68%，
Compound flame redundant 6%～20%,
Antimonous oxide 3%～15%,
Glass fibre 20%～30%,
Compatilizer 2%～10%,
Oxidation inhibitor 0.1%～1%,
Oxide compound 0.1%～1%,
Described compound flame redundant is comprised of brominated Polystyrene, magnesium hypophosphite and talcum powder.
Described PA66 is polyhexamethylene adipamide, and its limiting viscosity is 2.8 dl/g.
Described compound flame redundant is comprised of the feed composition of following weight percent content: brominated Polystyrene 50%, magnesium hypophosphite 25%, talcum powder 25%.
Described glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface.
Described compatilizer is maleic anhydride graft POE.
Described oxidation inhibitor is Hinered phenols antioxidant.
Described oxidation inhibitor is oxidation inhibitor 1330.
Described oxide compound is ferric oxide.
For realizing above-mentioned second purpose, the technical scheme that the present invention takes is:
A kind of high CTI value, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material preparation method comprise the steps:
(1) takes by weighing each raw material according to above-mentioned weight percent;
The various raw materials that (2) will weigh up are put into high mixer, mix 2～5 minutes, and then discharging uses the twin screw extruder extruding pelletization.
The processing temperature of described twin screw extruder is 220～255 ℃, and the screw rod revolution is 30～40Hz.
The invention has the advantages that:
1, the present invention adopts the BACN compound system, compares with traditional flame-retardant system, in the situation that the fire retardant percentage composition is identical, the novel built system can make the GWIT value of material improve 50 ℃ to 100 ℃, can pass through 850 ℃ of glowing filaments;
2, the adding of glass fibre can make the GWIT value of material obviously improve, and compatilizer can improve the impact property of material, improves the materials processing flowability, reduces frictional coefficient, improves slipping;
3, Hinered phenols antioxidant can improve matrix material in the antioxidant property of the course of processing and the ageing resistance in the use procedure, adopts oxide compound as the auxiliary agent of carrying high CTI value;
4, the present invention is under specific processing conditions, and raw material is better dispersed, and the residence time is short, adopts and shears slightly weak combination, prevents that fire retardant from decomposing, thereby has guaranteed the steady quality of material; GWIT value and the CTI value of the matrix material for preparing are higher, flame retardant effect is better, the matrix material environmental protection, over-all properties is balanced, can be widely used in the product of the field of electronics such as Low-voltage Electronic capacitor case, load break switch, carbon brush supports, breaker of plastic casing.
Embodiment
The below elaborates to embodiment provided by the invention.
High CTI value of the present invention, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material, described PA66 is commercially available polyhexamethylene adipamide, its limiting viscosity is preferably 2.8 dl/g, also can be other value of 2.0～3.2 dl/g scopes; Described compound flame redundant is comprised of brominated Polystyrene (being called for short BPS), magnesium hypophosphite and talcum powder, and weight percent content is preferably BPS 50%, magnesium hypophosphite 25%, talcum powder 25%, the GWIT value of this fire retardant energy Effective Raise matrix material; Described glass fibre is preferably the alkali free glass fibre that process through silane coupling agent on the surface, and glass fibre is added in the silane coupling agent, and its surface is processed through silane coupling agent, and it can make the GWIT value of material obviously improve; Described compatilizer can improve the impact property of material, can be maleic anhydride grafted polystyrene, imide-modified vinylformic acid, maleic anhydride graft PPO etc., is preferably maleic anhydride graft POE; Described oxidation inhibitor is preferably the oxidation inhibitor 1330 in the Hinered phenols antioxidant, can also be antioxidant 1010, antioxidant 300, thio-2 acid dibasic acid esters etc., all can block, suppress or delay polymkeric substance oxidation or autoxidation process, can improve matrix material in the course of processing antioxidant property and the ageing resistance in the use procedure; Described oxide compound is as the auxiliary agent of carrying high CTI value, can be aluminum oxide, magnesium oxide etc., is preferably ferric oxide.
In the PA66 composite manufacture process of the present invention, the various raw materials that weigh up are put into high mixer, mixed 2～5 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 30～40Hz.
Embodiment 1 PA66 composite manufacture ()
The limiting viscosity of PA66 is 2.8 dl/g, compound flame redundant is that the raw material of BPS 50%, magnesium hypophosphite 25% and talcum powder 25% forms by weight percent content, glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface, compatilizer is maleic anhydride graft POE, oxidation inhibitor is oxidation inhibitor 1330, and oxide compound is ferric oxide.
Take by weighing each feed composition: PA66 45% by following weight percent content, compound flame redundant 20%, antimonous oxide 4%, glass fibre 20%, compatilizer 10%, oxidation inhibitor 0.1%, oxide compound 0.9%.Each raw material that weighs up is put into high mixer, mixed 2 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 30Hz.
Embodiment 2 PA66 composite manufactures (two)
The limiting viscosity of PA66 is 2.8 dl/g, compound flame redundant is that the raw material of BPS 50%, magnesium hypophosphite 25% and talcum powder 25% forms by weight percent content, glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface, compatilizer is maleic anhydride graft POE, oxidation inhibitor is antioxidant 1010, and oxide compound is ferric oxide.
Take by weighing each feed composition: PA66 55% by following weight percent content, compound flame redundant 8%, antimonous oxide 3%, glass fibre 30%, compatilizer 2%, oxidation inhibitor 1%, oxide compound 1%.Each raw material that weighs up is put into high mixer, mixed 5 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 35Hz.
Embodiment 3 PA66 composite manufactures (three)
The limiting viscosity of PA66 is 2.0 dl/g, and compound flame redundant is that the raw material of BPS 45%, magnesium hypophosphite 30% and talcum powder 25% forms by weight percent content, and compatilizer is maleic anhydride graft PPO, and oxidation inhibitor is oxidation inhibitor 1330, and oxide compound is aluminum oxide.
Take by weighing each feed composition: PA66 50% by following weight percent content, compound flame redundant 13%, antimonous oxide 3%, glass fibre 25%, compatilizer 8%, oxidation inhibitor 0.5%, oxide compound 0.5%.Each raw material that weighs up is put into high mixer, mixed 3 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 40Hz.
Embodiment 4 PA66 composite manufactures (four)
The limiting viscosity of PA66 is 2.8 dl/g, compound flame redundant is that the raw material of BPS 50%, magnesium hypophosphite 25% and talcum powder 25% forms by weight percent content, glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface, compatilizer is maleic anhydride graft POE, oxidation inhibitor is oxidation inhibitor 1330, and oxide compound is ferric oxide.
Take by weighing each feed composition: PA66 68% by following weight percent content, compound flame redundant 6%, antimonous oxide 3%, glass fibre 20%, compatilizer 2%, oxidation inhibitor 0.9%, oxide compound 0.1%.Each raw material that weighs up is put into high mixer, mixed 4 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 38Hz.
Embodiment 5 PA66 composite manufactures (five)
The limiting viscosity of PA66 is 3.2 dl/g, compound flame redundant is that the raw material of BPS 50%, magnesium hypophosphite 25% and talcum powder 25% forms by weight percent content, glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface, compatilizer is maleic anhydride graft POE, oxidation inhibitor is antioxidant 300, and oxide compound is ferric oxide.
Take by weighing each feed composition: PA66 45% by following weight percent content, compound flame redundant 10%, antimonous oxide 15%, glass fibre 24%, compatilizer 5%, oxidation inhibitor 0.4%, oxide compound 0.6%.Each raw material that weighs up is put into high mixer, mixed 5 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 30Hz.
Embodiment 6 PA66 composite manufactures (six)
The limiting viscosity of PA66 is 2.5 dl/g, compound flame redundant is that the raw material of BPS 60%, magnesium hypophosphite 20% and talcum powder 20% forms by weight percent content, compatilizer is maleic anhydride grafted polystyrene, and oxidation inhibitor is oxidation inhibitor 1330, and oxide compound is ferric oxide.
Take by weighing each feed composition: PA66 47% by following weight percent content, compound flame redundant 16%, antimonous oxide 10%, glass fibre 22%, compatilizer 4%, oxidation inhibitor 0.7%, oxide compound 0.3%.Each raw material that weighs up is put into high mixer, mixed 4 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 40Hz.
Embodiment 7 PA66 composite manufactures (seven)
The limiting viscosity of PA66 is 2.8 dl/g, compound flame redundant is that the raw material of BPS 50%, magnesium hypophosphite 25% and talcum powder 25% forms by weight percent content, glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface, compatilizer is maleic anhydride graft POE, oxidation inhibitor is oxidation inhibitor 1330, and oxide compound is magnesium oxide.
Take by weighing each feed composition: PA66 60% by following weight percent content, compound flame redundant 7%, antimonous oxide 6%, glass fibre 23%, compatilizer 3%, oxidation inhibitor 0.6%, oxide compound 0.4%.Each raw material that weighs up is put into high mixer, mixed 3 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, and two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw rod revolution is 35Hz.
Need to prove, the glass fiber reinforced PA66 matrix material that embodiment 1-7 is obtained carries out performance test, adopt the ASTM standard, test result shows: the PA66 matrix material of preparation has higher GWIT value and CTI value, and the flame retardant resistance of matrix material, tensile strength and flexural strength all meet the requirements.
Embodiment 8～9 and Comparative Examples 1～7
The limiting viscosity of PA66 is 2.8 dl/g; Compound flame redundant is that the raw material of BPS 50%, magnesium hypophosphite 25% and talcum powder 25% forms by weight percent content; Common fire retardant can be triphenylphosphate, TDE, decabromodiphynly oxide, magnesium hydroxide, red phosphorus etc., and the present invention all adopts TDE; Glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface; Compatilizer is maleic anhydride graft POE; Oxidation inhibitor is oxidation inhibitor 1330; Oxide compound is ferric oxide.
(%) takes by weighing each feed composition by the weight percent content shown in the table 1.Each raw material that weighs up is put into high mixer, mixed 5 minutes, then discharging uses the twin screw extruder extruding pelletization; The processing temperature of described twin screw extruder is 220～255 ℃, and forcing machine comprises nine warm areas, wherein one section 220 ℃, two sections 250 ℃, three sections 255 ℃, four sections 255 ℃, five sections 255 ℃, six sections 240 ℃, seven sections 230 ℃, eight sections 230 ℃, nine sections 230 ℃, the screw host revolution is 35Hz, and the feeding revolution is 13 Hz.
Each composition of raw materials in table 1 embodiment 8～9 and the Comparative Examples 1～7
Embodiment 10 performance tests
Adopt the ASTM standard, the PA66 matrix material that embodiment 8～9, Comparative Examples 1～7 are prepared carries out performance test, and test result is as shown in table 2.
The performance test results of table 2 matrix material
Associative list 1 and table 2, as can be known, the present invention adopts the BACN compound system from table, compares the GWIT value of novel built fire retardant energy Effective Raise material with traditional common fire retardant; The adding of alkali free glass fibre can make the GWIT value of matrix material obviously improve, and compatilizer can improve the impact property of material; Ferric oxide has considerable influence to carrying high CTI value.
GWIT value and the CTI value of matrix material of the present invention are higher, flame retardant effect is better, the matrix material environmental protection, over-all properties is balanced, can be widely used in the product of the field of electronics such as Low-voltage Electronic capacitor case, load break switch, carbon brush supports, breaker of plastic casing.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the inventive method; can also make some improvement and replenish, these improvement and replenish and also should be considered as protection scope of the present invention.
Claims (10)
1. a high CTI value, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material is characterized in that, described material comprises the feed composition of following weight percent content:
PA66 45%～68%，
Compound flame redundant 6%～20%,
Antimonous oxide 3%～15%,
Glass fibre 20%～30%,
Compatilizer 2%～10%,
Oxidation inhibitor 0.1%～1%,
Oxide compound 0.1%～1%,
Described compound flame redundant is comprised of brominated Polystyrene, magnesium hypophosphite and talcum powder.
2. high CTI value according to claim 1, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material is characterized in that, described PA66 is polyhexamethylene adipamide, and its limiting viscosity is 2.8 dl/g.
3. high CTI value according to claim 1, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material, it is characterized in that, described compound flame redundant is comprised of the feed composition of following weight percent content: brominated Polystyrene 50%, magnesium hypophosphite 25%, talcum powder 25%.
4. high CTI value according to claim 1, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material is characterized in that, described glass fibre is the alkali free glass fibre that process through silane coupling agent on the surface.
5. high CTI value according to claim 1, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material is characterized in that, described compatilizer is maleic anhydride graft POE.
6. high CTI value according to claim 1, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material is characterized in that, described oxidation inhibitor is Hinered phenols antioxidant.
7. high CTI value according to claim 6, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material is characterized in that, described oxidation inhibitor is oxidation inhibitor 1330.
8. high CTI value according to claim 1, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material is characterized in that, described oxide compound is ferric oxide.
9. a high CTI value, high GWIT value environment-protection flame-proof fiberglass reinforced plastic PA66 material preparation method is characterized in that, comprise the steps:
(1) takes by weighing each raw material according to weight percent claimed in claim 1;
The various raw materials that (2) will weigh up are put into high mixer, mix 2～5 minutes, and then discharging uses the twin screw extruder extruding pelletization.
10. preparation method according to claim 9 is characterized in that, the processing temperature of described twin screw extruder is 220～255 ℃, and the screw rod revolution is 30～40Hz.
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| CN104072981A (en) * | 2014-07-14 | 2014-10-01 | 苏州创佳塑胶有限公司 | Halogen-free flame retardant polyamide material and preparation method thereof |
| CN104974516A (en) * | 2015-06-25 | 2015-10-14 | 东莞市众一新材料科技有限公司 | High glow-wire halogen-free flame retardant composite material and preparation method thereof |
| CN108047705A (en) * | 2017-12-12 | 2018-05-18 | 天津金发新材料有限公司 | A kind of flame-retardant polyamide composition and preparation method thereof |
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| CN113388248A (en) * | 2021-07-21 | 2021-09-14 | 合诚技术股份有限公司 | high-CTI brominated flame-retardant reinforced polyamide composite material and preparation method and application thereof |
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