CN102115595A - High electrical property and low corrosion flame retardant reinforcing nylon material and preparation method thereof - Google Patents

High electrical property and low corrosion flame retardant reinforcing nylon material and preparation method thereof Download PDF

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Publication number
CN102115595A
CN102115595A CN2010100192075A CN201010019207A CN102115595A CN 102115595 A CN102115595 A CN 102115595A CN 2010100192075 A CN2010100192075 A CN 2010100192075A CN 201010019207 A CN201010019207 A CN 201010019207A CN 102115595 A CN102115595 A CN 102115595A
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China
Prior art keywords
flame
retardant
nylon material
flame retardant
high electrical
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CN2010100192075A
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Chinese (zh)
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余徐南
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FOSHAN SHUNDE WHEELING PLASTIC Co Ltd
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FOSHAN SHUNDE WHEELING PLASTIC Co Ltd
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Priority to CN2010100192075A priority Critical patent/CN102115595A/en
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Abstract

The invention discloses a high electrical property and low corrosion flame retardant reinforcing nylon material and a preparation method thereof, aiming at solving the defects of low electrical property and high corrosion caused by red phosphorus based flame retardant added into flame retardant reinforcing nylon in the prior art. The invention adopts the technical scheme that the high electrical property and low corrosion flame retardant reinforcing nylon material disclosed by the invention has the formulation (by weight percent): (1) 40-65% of nylon 66 resin, (2) 10-20% of red phosphorus based flame retardant masterbatch, (3) 1-5% of compatilizer, (4) 3-10% of synergistic compound flame retardant system, (5) 0.5-5% of acid absorbent, (6) 0.1-0.5% of antioxidant, (7) 0.2-0.8% of lubricating agent and (8) 10-30% of glass fiber; and the reinforcing nylon material can be prepared by mixing all the components in a high-speed mixing machine for 1-2min and then putting into a twin-screw extruder for extrusion and pelleting. The flame retardant reinforcing nylon material is excellent in the electrical property, low in corrosion (extremely low in corrosion for equipment and a mould) as well as high in fluidity, heat resistance and cost performance, and is capable of meeting the requirements of electrical and electronic appliances such as a temperature controller, a contactor, a circuit breaker and the like as well as domestic appliance products.

Description

A kind of high electrical performance low-corrosiveness flame-retardant reinforced nylon material and preparation method thereof
Technical field
The present invention relates to a kind of technical field of polymer materials, especially a kind of high electrical performance low-corrosiveness flame-retardant reinforced nylon material and preparation method thereof.
Background technology
Flameproof polyamide (PA) is a kind of widely used fire-resistant engineering plastics, and it is used for electronics, electric, instrument, automobile and other industries, existing nearly 30 years history.The PA of industrial production has enhancement type to reach not enhancement type two classes, and the flame retardant products general requirement has the UL94V-0 flame retardant grade.The method of fire-retardant PA, great majority adopt additive flame retardant, also occur some in recent years with the fire-retardant PA of reactive flame retardant, for example, contain nylon 66 multipolymers of triaryl phosphine oxide on the main chain.Because the processing temperature of PA is higher, so the additive flame retardant that it adopts is the aromatic series bromide fire retardant, consider from balance various factors (efficient, processing, price, to effect of material performance etc.), can recommend main decabromodiphynly oxide (DBDPO), Brominated Polystyrene (BPS), polyacrylic acid pentabromo-benzyl ester (PPBBA), brominated epoxy resin (1BER) and ten tetrabromos, the two phenoxy group benzene (DBDPOB) etc. that use.
Regulation in " about banning use of the instruction of some objectionable impurities in the electronic electric equipment " that on February 13rd, 2003, European Union announced must not contain 6 kinds of objectionable impuritiess such as polybromodiphenyl ether and Polybrominated biphenyl in electronics and the electric installation.Therefore, efficient, the low toxicity of exploitation, not halogen-containing halogen-free reinforced nylon have been trend of the times.Using wider halogen-free flame retardants in the nylon is red phosphorus, but the iron level of red phosphorus master batch and the addition in prescription influence nylon material electrical property and corrodibility, and the red phosphorus flame-retardant Reinforced Nylon extrude and injection moulding process in, because the unstable of red phosphorus, can produce flame phenomenon and a large amount of dense smoke, the corrodibility of same phosphoric acid has a significant impact equipment and mould.
Summary of the invention
Shortcoming at above-mentioned prior art existence, the experience of this area work is engaged in inventor's accumulation for many years, through feasibility study repeatedly, get generation of the present invention eventually, the present invention discloses a kind of high electrical performance low-corrosiveness flame-retardant reinforced nylon material and preparation method thereof, solves prior art and causes the defective that electrical property is low, corrodibility is big at flame-retardant reinforced nylon Longli interpolation red phosphorus combustion inhibitor.
The technical solution used in the present invention is: a kind of high electrical performance disclosed by the invention, low corrosion flame-retardant reinforced nylon prescription (according to weight percent) are: (1) Nylon 66 40-65%, (2) red phosphorus flame-retardant master batch 10-20%, (3) compatilizer 1-5%, (4) synergistic compositional flame-retardant system 3-10%, (5) acid absorber 0.5-5%, (6) oxidation inhibitor 0.1-0.5%, (7) lubricant 0.2-0.8% (8) glass fibre 10-30% composition, each component mixed in high speed mixer after 1~2 minute puts into the twin screw extruder extruding pelletization promptly.
Wherein said high electrical performance low-corrosiveness flame-retardant reinforced nylon material, nylon resin system are single Nylon 66 or Nylon 66 and Nylon 6 compound system; Wherein Nylon 66 and Nylon 6 are medium-viscosity resin, relative viscosity 2.6-2.8PaS; The red phosphorus flame-retardant master batch is to be carrier with the nylon resin, and red phosphorus content is the master batch of 45-55%, and wherein red phosphorus is earlier through coating and the deironing processing; Compatilizer is the grafts of ethylene-acrylate copolymer or ethylene-octene copolymer grafted maleic anhydride and their compound; The synergistic compound flame retardant is that one or more fire retardants are composite forms by modified superfine magnesium hydroxide, modified superfine aluminium hydroxide, modified extrafine talc powder and anhydrous zinc borate etc.; Wherein modified superfine oxyhydroxide is surface treated, particle diameter 2000 order to 5000 orders; Wherein modified extrafine talc powder is surface treated, particle diameter 5000 order to 10000 orders; Acid absorber is one or more mixtures such as hydrotalcite, calcium stearate, Zinic stearas, extra light calcined magnesia; Oxidation inhibitor is four (β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester promptly 1010,4.4 '-two (α. α-Er Jiajibianji) pentanoic promptly 445, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester promptly 168, i.e. a kind of or multiple composite the forming such as 626 of two (2.4-di-tert-butyl-phenyl) pentaerythritol diphosphites; Lubricant is N, and N '-ethylene bis stearamide is EBS, and polyethylene wax ethene-acrylic acid multipolymer is 540A, one or more mixtures such as silicone powder or silicone master batch.
Flame-retardant reinforced nylon superior electrical property of the present invention, low-corrosiveness (minimum to equipment and mould corrodibility), high workability, high heat resistance, high performance-price ratio can satisfy the requirement of electronic apparatuss such as temperature controller, contactor, isolating switch and household electronic products.
Embodiment
Specify the present invention below in conjunction with embodiment.
Embodiment 1
Elder generation dries by the fire the nylon resin of 52.4% weight 3 hours down at 85 ℃, and the red phosphorus flame-retardant master batch of crossing 15% weight of strong magnetic was dried by the fire 3 hours down at 120 ℃, and control moisture is below 0.15%; Subsequently with the ethylene-octene copolymer grafted maleic anhydride of 3% weight, the synergistic compositional flame-retardant system of 8% weight, the acid absorber calcium stearate of 0.7% weight, primary antioxidant four (the β-(3 of 0.2% weight, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester (1010) and 0.1% auxiliary antioxidant three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester (168), starting material such as the lubricant silicone powder of 0.6% weight enter twin screw extruder plasticizing from the metering feeding device by the high speed mixer mixing after 2 minutes, fusion, the alkali free glass fibre that adds 20% weight simultaneously at twin screw extruder is again through extruding, cooling, cross strong magnetic, be packaged to be product;
Embodiment 2
Elder generation dries by the fire the nylon resin of 46.4% weight 3 hours down at 85 ℃, and the red phosphorus flame-retardant master batch of crossing 12% weight of strong magnetic was dried by the fire 3 hours down at 120 ℃, and control moisture is below 0.15%; Subsequently with the ethylene-octene copolymer grafted maleic anhydride of 2% weight, the synergistic compositional flame-retardant system of 8% weight, the acid absorber calcium stearate of 0.5% weight, primary antioxidant four (the β-(3 of 0.2% weight, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester (1010) and 0.1% auxiliary antioxidant three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester (168), starting material such as the lubricant silicone powder of 0.8% weight enter twin screw extruder plasticizing from the metering feeding device by the high speed mixer mixing after 2 minutes, fusion, the alkali free glass fibre that adds 30% weight simultaneously at twin screw extruder is again through extruding, cooling, cross strong magnetic, be packaged to be product;
Wherein synergistic compositional flame-retardant system is: the superfine talcum powder of the modified superfine magnesium hydroxide of 70% weight, the anhydrous zinc borate of 20% weight and 10% weight.
Preparation method and the technology of embodiment are as follows:
(1) raw-material processing and mixing
Nylon resin dried by the fire 3 hours down at 85 ℃, and the red phosphorus flame-retardant master batch dried by the fire 3 hours down at 120 ℃, and control moisture is below 0.15%;
The red phosphorus flame-retardant master batch is crossed strong magnetic treatment earlier; Major ingredient and compatilizer, synergistic compound flame retardant, acid absorber, oxidation inhibitor, lubricant etc. were mixed 2 minutes in high speed mixer, make the abundant dispersed with stirring of each component even;
(2) melt extrude
The material that mixes is added in the twin screw extruder, when melt extruding, introduce alkali free glass fibre at the 5th joint barrel and melt extrude, melt extrude temperature between 220-280 ℃, screw speed is 430 rev/mins;
(3) granulation and aftertreatment
The material of extruding is cooled off, air-dry, pelletizing, crosses strong magnetic, is packaged to be finished product;
Performance to a kind of high electrical performance low-corrosiveness flame-retardant reinforced nylon material of embodiment 1 and embodiment 2 gained is as follows
Test event Testing standard Test condition Embodiment 1 Embodiment 2
Ash content (%) GB?9345 750 ℃ of calcinations 23.3 32.5
Proportion (g/cm3) GB?1033 23℃ 1.312 1.383
Tensile strength (Mpa) GB?1040 50mm/min 110.2 140.2
Flexural strength (Mpa) GB?9341 2mm/min 168.1 202.8
Modulus in flexure (Mpa) GB?9341 2mm/min 6332 7534
Socle girder notched Izod impact strength (KJ/m 2) GB?1843 3.2mm,23℃ 7.5 11.2
Heat-drawn wire (℃) GB?1634 1.8Mpa,6.4m m 227.3 243.5
Flame retardant resistance (Class) UL94 2.5mm V-0 V-0
CTI(V) GB T4207 2.5mm 550 550
Corrodibility Minimum Minimum
Remarks: corrosive testing method is 155 ℃, its corrosion situation to the red copper electrode surface of range estimation after 21 days;
In sum, be preferred embodiment of the present invention, all changes of having done according to technical solution of the present invention when the function that is produced fails to exceed the scope of technical solution of the present invention, all belong to protection scope of the present invention.

Claims (9)

1. high electrical performance low-corrosiveness flame-retardant reinforced nylon material is characterized in that composed of the following components by weight percentage:
Nylon resin 40-65%
Red phosphorus flame-retardant master batch 10-20%
Compatilizer 1-5%
Synergistic compound flame retardant 3-10%
Acid absorber 0.5-5%
Oxidation inhibitor 0.1-0.5%
Lubricant 0.2-0.8%
Alkali free glass fibre 10-30%
2. high electrical performance low-corrosiveness flame-retardant reinforced nylon material according to claim 1, wherein the nylon resin system is single Nylon 66 or Nylon 66 and Nylon 6 compound system; Wherein Nylon 66 and Nylon 6 are medium-viscosity resin, relative viscosity 2.6-2.8PaS.
3. high electrical performance low-corrosiveness flame-retardant reinforced nylon material according to claim 1 is characterized in that: the red phosphorus flame-retardant master batch is to be carrier with the nylon resin, and red phosphorus content is the master batch of 45-55%; Wherein red phosphorus is earlier through coating and the deironing processing.
4. high electrical performance low-corrosiveness flame-retardant reinforced nylon material according to claim 1 is characterized in that: compatilizer is ethene-acrylate copolymer or the grafts of ethene-octene copolymer grafted maleic anhydride and their compound.
5. high electrical performance low-corrosiveness flame-retardant reinforced nylon material according to claim 1 is characterized in that: the synergistic compound flame retardant is that one or more fire retardants are composite forms by modified superfine magnesium hydroxide, modified superfine aluminium hydroxide, modified extrafine talc powder and anhydrous zinc borate etc.; Wherein modified superfine oxyhydroxide is surface treated, particle diameter 2000 order to 5000 orders; Wherein modified extrafine talc powder is surface treated, particle diameter 5000 order to 10000 orders.
6. high electrical performance low-corrosiveness flame-retardant reinforced nylon material according to claim 1 is characterized in that: acid absorber is one or more mixtures such as hydrotalcite, calcium stearate, Zinic stearas, extra light calcined magnesia;
7. high electrical performance low-corrosiveness flame-retardant reinforced nylon material according to claim 1, it is characterized in that: oxidation inhibitor is four (β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester promptly 1010,4.4 '-two (α. α-Er Jiajibianji) pentanoic promptly 445, three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester promptly 168, i.e. a kind of or multiple composite the forming such as 626 of two (2.4-di-tert-butyl-phenyl) pentaerythritol diphosphites.
8. flame-retardant reinforced nylon material according to claim 1 is characterized in that: lubricant is N, and N '-ethylene bis stearamide is EBS, and polyethylene wax ethene-acrylic acid multipolymer is 540A, one or more mixtures such as silicone powder or silicone master batch.
9. the preparation method of high electrical performance low-corrosiveness flame-retardant reinforced nylon material according to claim 1, it is characterized in that: may further comprise the steps: the nylon resin with 40-65% weight dried by the fire 2-5 hour down at 85-90 ℃ earlier, the red phosphorus flame-retardant master batch of 10-20% weight was dried 2-5 hour down at 110-125 ℃, and control moisture is below 0.15%; From metering feeding device enter twin screw extruder plasticizing, fusion by the high speed mixer mixing after 1-2 minute with the compatilizer of 1-5% weight, the synergistic compositional flame-retardant system of 3-10% weight, the acid absorber of 0.5-5% weight, the oxidation inhibitor of 0.1-0.5% weight, the starting material such as lubricant of 0.2-0.8% weight subsequently, the alkali free glass fibre that adds 10-30% weight simultaneously at twin screw extruder is again through extruding, cool off, cross strong magnetic, being packaged to be product; Wherein the rotating speed of twin screw extruder is 200-600 rev/min, and extrusion temperature is 220-280 ℃.
Performance to a kind of high electrical performance low-corrosiveness flame-retardant reinforced nylon material of embodiment in the specification sheets 1 and embodiment 2 gained is as follows
Test event Testing standard Test condition Embodiment 1 Embodiment 2 Ash content (%) ?GB?9345 750 ℃ of calcinations 23.3 32.5 Proportion (g/cm3) ?GB?1033 23℃ 1.312 1.383
Tensile strength (Mpa) GB?1040 50mm/min 110.2 140.2 Flexural strength (Mpa) GB?9341 2mm/min 168.1 202.8 Modulus in flexure (Mpa) GB?9341 2mm/min 6332 7534 The socle girder notched Izod impact strength GB?1843 3.2mm,23℃ 7.5 11.2 Heat-drawn wire (℃) GB?1634 1.8Mpa,6.4m m 227.3 243.5 Flame retardant resistance (Class) UL94 2.5mm V-0 V-0 CTI(V) GB T4207 2.5mm 550 550 Corrodibility ? ? Minimum Minimum
Remarks: corrosive testing method is 155 ℃, its corrosion situation to the red copper electrode surface of range estimation after 21 days.
CN2010100192075A 2010-01-04 2010-01-04 High electrical property and low corrosion flame retardant reinforcing nylon material and preparation method thereof Pending CN102115595A (en)

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CN102382464A (en) * 2011-09-07 2012-03-21 上海日之升新技术发展有限公司 High-CTI (comparative tracking index) value and low-corrosivity red phosphorus flame-retarding glass fiber reinforced PA66 (polyamide 66) material and preparation method thereof
CN102382460A (en) * 2011-10-24 2012-03-21 浙江俊尔新材料有限公司 Low-acid-separation red phosphorus inflaming retarding reinforced polyamide material as well as preparation method and application thereof
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CN102382464A (en) * 2011-09-07 2012-03-21 上海日之升新技术发展有限公司 High-CTI (comparative tracking index) value and low-corrosivity red phosphorus flame-retarding glass fiber reinforced PA66 (polyamide 66) material and preparation method thereof
CN102382460A (en) * 2011-10-24 2012-03-21 浙江俊尔新材料有限公司 Low-acid-separation red phosphorus inflaming retarding reinforced polyamide material as well as preparation method and application thereof
CN102558839A (en) * 2011-12-21 2012-07-11 上海普利特复合材料股份有限公司 Low odor, anti-static electricity, red phosphorus flame retardant thermoplastic composition and preparation method thereof
CN102604380A (en) * 2012-03-26 2012-07-25 横店集团得邦工程塑料有限公司 High-heat-resistance and high-CTI (Comparative Tracking Index) inflaming retarding polyamide composite material and production process thereof
CN102634200A (en) * 2012-04-27 2012-08-15 常熟市发东塑业有限公司 Flame-retarding modified nylon composite material
CN102643540A (en) * 2012-04-27 2012-08-22 常熟市发东塑业有限公司 Method for preparing flame-retardant modified nylon composite
CN102732021A (en) * 2012-07-17 2012-10-17 上海日之升新技术发展有限公司 High CTI (Comparative Tracking Index) flame retardant glass fiber reinforced PA66 (Polyamide 66)/PE (Polyethylene) alloy composite and preparation method thereof
CN102775782A (en) * 2012-07-17 2012-11-14 上海日之升新技术发展有限公司 Flame-retardant glass fiber reinforced PA (polyamide) 66/PP (propene polymer) alloy composition and preparation method thereof
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Application publication date: 20110706