CN103382302B - A kind of red phosphorus flame-retardant nylon composite and preparation method thereof - Google Patents
A kind of red phosphorus flame-retardant nylon composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of red phosphorus flame-retardant nylon composite and preparation method thereof, red phosphorus flame-retardant nylon composite comprises following composition by weight percentage: nylon resin 55-75%; Glass fibre 15-35%; Red phosphorus combustion inhibitor 6-8%; Toughner 2-5%; Lubricant 0.2-1%; Oxidation inhibitor 0.2-1%.Red phosphorus flame-retardant nylon composite preparation method of the present invention comprises: put into after mixing machine mixes by dry nylon resin, red phosphorus combustion inhibitor, toughner, lubricant and oxidation inhibitor by above-mentioned weight percent, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, through melt extruding granulation, obtained nylon composite.The red phosphorus nylon composite that the present invention obtains has good glowing filament flame retardant properties and toughness, is applicable to electronic apparatus and communication field.
Description
Technical field
The present invention relates to polymeric material field, particularly relate to and a kind ofly improve red phosphorus flame-retardant nylon composite of nylon material glowing filament flame retardant properties and preparation method thereof.
Background technology
Nylon (polymeric amide) material is that in five large general engineering plastic, output is maximum, kind maximum, purposes this kind of material of a kind of base resin that is the widest, high comprehensive performance is widely used in every field.PA66 and PA6 is wherein most widely used two kinds, but PA66 and the PA6 flame retardant resistance of non-modified is poor, belong to inflammable material, to add after glass fibre more easy firing, the danger of the situation initiation fire due to electric leakage, short circuit, electric arc, electrical spark in live line work environment still exists, this shortcoming limits its range of application, especially in the field such as electronic apparatus and communication.Therefore, prepare a kind of can meet high electrical performance requirement, low cost fire-retardant nylon material to expand nylon fire retardant material range of application, promote that electronic apparatus and communications industry development etc. are of practical significance.
Publication number is that the Chinese patent of CN1935899 discloses a kind of environmental-protection fire-resistant nylon composition and preparation method thereof.The weight ratio of each component content is: nylon resin 18 ~ 100 parts, fire-retardant master granule 0 ~ 20 part, auxiliary flame retardant 0 ~ 10 part, 0 ~ 2 part, oxidation inhibitor, nucleator 0 ~ 5 part, internal lubricant 0 ~ 5 part, weighting material or reinforce 0 ~ 40 part.The red phosphorus flame-retardant masterbatch that this patent adopts is with Phosphorous Inorganic Flame Retardant and the composite use of the inorganic combustion inhibitor such as aluminium hydroxide, expansile graphite, with nylon matrix resin be carrier between organic and inorganic between environmental protection fire retarding agent.This fire retardant can not produce obnoxious flavour, and can resistance to 350 DEG C of high temperature, has excellent consistency with high temperature resistant nylon.This environmental-protection fire-resistant nylon has good flame retardant resistance and thermotolerance, and has good mechanical property, flowing property, precise forming and dimensional stability, is mainly used in field of electronics, also can be used for the fields such as Industrial materials, engineering materials and trolley part.
Publication number is that the Chinese patent of CN102924917A discloses a kind of proof voltage flame-resistant insulation reinforced PA66 engineering plastics.This project plastics are composed of the following components by weight percentage: PA66 resin 30-60%; PPO resin 1.5-9%; Compatilizer 2-5%; Red phosphorus combustion inhibitor master batch 10-20%; Proof voltage insulation modified filler particle 2-10%; Alkali-free short glass fiber 0.01-35%; Other auxiliary agents 1-2%.Described proof voltage insulation modified filler is at least one in calcined kaolin, mica, halloysite carbon nanotube three kinds of filler grains, other auxiliary agents described comprise amino silicane coupling agent, and described filler grain process accounts for the amino silicane coupling agent process of 5% of described filler grain weight.Nylon66 fiber engineering plastics prepared by the present invention have excellent proof voltage insulating property, also have good mechanical property and flame retardant properties simultaneously, can be applicable to prepare the electronic apparatus component having proof voltage and flame-retardancy requirements.
Summary of the invention
The invention provides a kind of red phosphorus flame-retardant nylon composite and preparation method thereof, it has good glowing filament flame retardant properties and toughness, is applicable to electronic apparatus and communication field.
A kind of red phosphorus flame-retardant nylon composite, comprises following composition by weight percentage:
Nylon resin 55-75%;
Glass fibre 15-35%;
Red phosphorus combustion inhibitor 6-8%;
Toughner 2-5%;
Lubricant 0.2-1%;
Oxidation inhibitor 0.2-1%.
Described nylon resin is one or both in PA6, PA66.
Described glass fibre selects continuous long glass fiber by interface modifier process or short chopped glass fiber, is preferably Mount Taishan short fiber 435N or the long fine 988A of megalith.The fiber of the endless that this area is drawn with mechanical drawing process by platinum alloy plate, is called continuous long glass fiber, common name macrofiber; By the discontinuous fiber that roller or air-flow are made, be called staple glass fibre, common name staple fibre or short chopped glass fiber.
Described red phosphorus combustion inhibitor is red phosphor masterbatch, point of ignition >=320 DEG C, and outward appearance is red-purple particle, and red phosphorus content is 40-80%; The addition of described red phosphorus combustion inhibitor is with the Weight computation of pure red phosphorus, and as used the red phosphor masterbatch (red phosphorus content 40%) of 15%, then red phosphorus combustion inhibitor consumption is 6%.Described red phosphorus combustion inhibitor is preferably the red phosphor masterbatch of Sichuan morning twilight 440B.
Described toughner is maleic anhydride graft compatilizer, and maleic anhydride graft compatilizer is by introducing strong polar reaction group, and making material have high polarity and reactivity, is a kind of macromolecule interfacial coupling agent, compatilizer, dispersion enhancing agents.Described toughner is maleic anhydride graft PE(PE-g-MAH), maleic anhydride graft PP(PP-g-MAH), maleic anhydride graft POE(POE-g-MAH) or maleic anhydride graft EPDM(EPDM-g-MAH), adding of toughner, Reinforced Nylon is toughness reinforcing, fire-retardant toughened, improve the shock resistance of nylon, winter hardiness, forming process type, reduce water-intake rate.As preferably, described toughner is maleic anhydride graft POE, and the trade mark is the light N409 of energy.
Described lubricant is TAF or silicone powder.TAF is with ethylene bis-fatty acid amides (EBS) for base-material, under the effect of catalyzer, reacts form BAB type multipolymer containing polar group reactive monomer and EBS.This multipolymer had both maintained the lubricating property of EBS, had again the polar group structure that can combine with glass, inorganic filler surface segment polarity group.In the compound systems such as fiberglass reinforced PA 6, PA66, TAF defines similar anchoring node between glass fibre and matrix resin, improves the bond state of glass fibre and matrix resin, and then improves the dispersiveness of glass fibre in matrix resin.Meanwhile, lubricant TAF has lubricating property again, improves the processing fluidity of matrix material, improves the surface smoothness of matrix material.Described silicone powder is silicone powder GM-100, and it is made up of ultra-high molecular weight polysiloxane, and it easily disperses in resin, can improve plastic working mobility and release property, improve surface luster, promotes surperficial silk quality sense of touch, improves scraping and wiping resistance performance; Improve flame retardant resistance, reduce smoke density, improve fire retardant material shock strength and surface gloss; There is satisfactory stability and non-migratory.
Described oxidation inhibitor is one or more in antioxidant 1010, oxidation inhibitor 1098 or irgasfos 168.As preferably, described oxidation inhibitor is two kinds in antioxidant 1010, oxidation inhibitor 1098 or irgasfos 168.
As preferably, described red phosphorus flame-retardant nylon composite, comprises following composition by weight percentage:
Nylon resin 58-68%;
Glass fibre 20-30%;
Red phosphorus combustion inhibitor 6-8%;
Toughner 3-5%;
Lubricant 0.3-0.8%;
Oxidation inhibitor 0.4-0.6%.
The ratio control of nylon resin and glass fibre is the intensity being conducive to nylon material most in said ratio, in nylon resin, add too much glass fibre be unfavorable for glass fibre dispersiveness wherein, and glass fibre is very few can cause nylon material intensity difference.
More preferred, described red phosphorus flame-retardant nylon composite, comprises following composition by weight percentage:
Nylon resin 58-68%;
Glass fibre 20-30%;
Red phosphorus combustion inhibitor 6-8%;
Toughner 3%;
Lubricant 0.3-0.8%;
Oxidation inhibitor 0.4-0.6%.
In described nylon resin, add red phosphorus combustion inhibitor is for improving the flame retardant properties of said composition, make it have good glowing filament flame retardant properties, and to add toughner be wherein for ensureing the toughness of nylon material, but add due to toughner the flame retardant resistance affecting nylon material to a certain extent, the content of red phosphorus combustion inhibitor, toughner and nylon resin is controlled under aforementioned proportion, nylon material can be made still to have very high toughness having under good glowing filament flame retardant properties, meet need of production.
A preparation method for red phosphorus flame-retardant nylon composite, comprises the following steps:
By dry 55-75% nylon resin by weight percentage; 6-8% red phosphorus combustion inhibitor; 2-5% toughner; 0.2-1% lubricant; 0.2-1% oxidation inhibitor is put into after mixing machine mixes, and is placed in the hopper of twin screw extruder, and is fed from side by the glass fibre of 20-35% and add, through melt extruding granulation, and obtained described nylon composite.
Described twin screw extruder each district temperature controls respectively at 180-280 DEG C.
Compared with prior art, the present invention has following beneficial effect:
The present invention adds glass fibre, toughner control the content of nylon resin, glass fibre and toughner in nylon resin, make the red phosphorus flame-retardant nylon composite obtained can obtain good toughness while having high-glowing-filament-temperature flame-retardancy performance, be highly suitable for electronic apparatus and communication field.
Nylon composite preparation method of the present invention is simple, without the need to specific installation, is suitable for suitability for industrialized production.
Embodiment
Below by specific embodiment, the present invention is described in further detail, but does not therefore limit the present invention in described scope of embodiments.
Embodiment 1:
Dry nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor are taken as following weight percent and puts into after mixing machine mixes, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, twin screw extruder each district temperature controls respectively at 180-280 DEG C, through melt extruding granulation, prepare nylon composite.
Wherein, the proportioning by weight percentage such as nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor is:
Nylon resin 64%;
Glass fibre 25%;
Red phosphorus combustion inhibitor 7%;
Toughner 3%;
Lubricant 0.5%;
Oxidation inhibitor 0.5%.
Raw material sources:
Nylon resin adopts PA6, and it is the trade mark is the PA612400 that newly meeting U.S.A reaches; Glass fibre adopts the trade mark to be Mount Taishan short fiber 435N; Red phosphorus combustion inhibitor adopts Sichuan morning twilight 440B; Toughner adopts Du Pont 493D(maleic anhydride graft POE); Lubricant adopts trade mark TAF; Oxidation inhibitor is antioxidant 1010.
Embodiment 2:
Dry nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor are taken as following weight percent and puts into after mixing machine mixes, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, twin screw extruder each district temperature controls respectively at 180-280 DEG C, through melt extruding granulation, prepare nylon composite.
Wherein, the proportioning by weight percentage such as nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor is:
Nylon resin 66.1%;
Glass fibre 20%;
Red phosphorus combustion inhibitor 8%;
Toughner 5%;
Lubricant 0.3%;
Oxidation inhibitor 0.6%.
Raw material sources:
Nylon resin adopts PA66, and it is the PA66EPR27 of trade mark god horse; Glass fibre adopts the long fine 988A of trade mark megalith; Red phosphorus combustion inhibitor adopts Anhui Tongchen to believe to obtain FR4140R; Toughner is grafting EPDM, adopts the liter 9802 of day; Lubricant adopts trade mark TAF; Oxidation inhibitor adopts the mixture of oxidation inhibitor 1098 and irgasfos 168, and both weight ratios are 1:1.
Embodiment 3:
Dry nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor are taken as following weight percent and puts into after mixing machine mixes, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, twin screw extruder each district temperature controls respectively at 180-280 DEG C, through melt extruding granulation, prepare nylon composite.
Wherein, the proportioning by weight percentage such as nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor is:
Nylon resin 59.8%;
Glass fibre 30%;
Red phosphorus combustion inhibitor 6%;
Toughner 3%;
Lubricant 0.8%;
Oxidation inhibitor 0.4%.
Raw material sources:
Nylon resin adopts PA66, and it is the PA66EPR27 of trade mark god horse; Glass fibre adopts the long fine 988A of trade mark megalith; Red phosphorus combustion inhibitor adopts Sichuan morning twilight 440B; Toughner is POE-g-MAH, adopts the light N409 of energy; Lubricant adopts trade mark silicone powder GM100; Oxidation inhibitor adopts the mixture of antioxidant 1010 and irgasfos 168, and both weight ratios are 1:1.
Comparative example 1:
Dry nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor are taken as following weight percent and puts into after mixing machine mixes, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, twin screw extruder each district temperature controls respectively at 180-280 DEG C, through melt extruding granulation, prepare nylon composite.
Wherein, the proportioning by weight percentage such as nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor is:
Nylon resin 67%;
Glass fibre 25%;
Red phosphorus combustion inhibitor 7%;
Toughner 0%;
Lubricant 0.5%;
Oxidation inhibitor 0.5%.
Raw material sources:
Nylon resin adopts PA6, and it is the trade mark is the PA612400 that newly meeting U.S.A reaches; Glass fibre adopts the trade mark to be Mount Taishan short fiber 435N; Red phosphorus combustion inhibitor adopts Sichuan morning twilight 440B; Toughner adopts Du Pont 493D(maleic anhydride graft POE); Lubricant adopts trade mark TAF; Oxidation inhibitor is antioxidant 1010.
Comparative example 2:
Dry nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor are taken as following weight percent and puts into after mixing machine mixes, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, twin screw extruder each district temperature controls respectively at 180-280 DEG C, through melt extruding granulation, prepare nylon composite.
Wherein, the proportioning by weight percentage such as nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor is:
Nylon resin 71.1%;
Glass fibre 20%;
Red phosphorus combustion inhibitor 8%;
Toughner 0%;
Lubricant 0.3%;
Oxidation inhibitor 0.6%.
Raw material sources:
Nylon resin adopts PA66, and it is the PA66EPR27 of trade mark god horse; Glass fibre adopts the long fine 988A of trade mark megalith; Red phosphorus combustion inhibitor adopts Anhui Tongchen to believe to obtain FR4140R; Toughner is grafting EPDM, adopts the liter 9802 of day; Lubricant adopts trade mark TAF; Oxidation inhibitor is the mixture of oxidation inhibitor 1098 and irgasfos 168, and both weight ratios are 1:1.
Comparative example 3:
Dry nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor are taken as following weight percent and puts into after mixing machine mixes, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, twin screw extruder each district temperature controls respectively at 180-280 DEG C, through melt extruding granulation, prepare nylon composite.
Wherein, the proportioning by weight percentage such as nylon resin, red phosphorus combustion inhibitor, lubricant and oxidation inhibitor is:
Nylon resin 62.8%;
Glass fibre 30%;
Red phosphorus combustion inhibitor 6%;
Toughner 0%;
Lubricant 0.8%;
Oxidation inhibitor 0.4%.
Raw material sources:
Nylon resin adopts PA66, and it is the PA66EPR27 of trade mark god horse; Glass fibre adopts the long fine 988A of trade mark megalith; Red phosphorus combustion inhibitor adopts Sichuan morning twilight 440B; Toughner is POE-g-MAH, adopts the light N409 of energy; Lubricant adopts trade mark silicone powder GM100; Oxidation inhibitor is the mixture of antioxidant 1010 and irgasfos 168, and both weight ratios are 1:1.
Performance test
The nylon composite prepared in embodiment 1-3 and comparative example 1-3 under 100-120 DEG C of condition after dry 4-6 hour, is injection molded into mechanics, flame retardant properties standard testing batten and print through injection moulding machine, tests by relevant criterion in convection oven.Performance test data is as following table 1:
Table 1 test result
Tensile strength is tested by GB/T1040.2-2006 standard;
Flexural strength and modulus in flexure are tested by GB/T9341-2008 standard;
Simple beam impact strength is tested by GB/T1043.1-2008 standard:
Glowing filament flame retardant properties is tested by GB/T5169.11-2006 standard, and print is disk, and print is of a size of: diameter 100 ± 2mm, thick 1.6 ± 0.1mm.
Can as apparent from the detected result of table 1, do not add the nylon composite of the comparative example 1,2,3 of toughner not by 850 DEG C of glowing filament flame retardant tests, and namely embodiment 1,2,3 can pass through 850 DEG C of glowing filament flame retardant tests after interpolation toughner, and shock strength has part to improve, illustrate and add the glowing filament flame retardant properties that toughner obviously can promote material while expection improves toughness of material, make the apparent modified effect of toughner acquisition except toughness reinforcing.
Claims (1)
1. a preparation method for red phosphorus flame-retardant nylon composite, is characterized in that, comprises the following steps:
Dry nylon resin, red phosphorus combustion inhibitor, toughner, lubricant and oxidation inhibitor are taken as following weight percent and puts into after mixing machine mixes, be placed in the hopper of twin screw extruder, glass fibre is fed from side and is added, twin screw extruder each district temperature controls respectively at 180-280 DEG C, through melt extruding granulation, prepare red phosphorus flame-retardant nylon composite;
Wherein, nylon resin, glass fibre, red phosphorus combustion inhibitor, toughner, lubricant and oxidation inhibitor proportioning is by weight percentage:
Raw material sources:
Nylon resin adopts PA66, and it is the PA66EPR27 of trade mark god horse; Glass fibre adopts the long fine 988A of trade mark megalith; Red phosphorus combustion inhibitor adopts Sichuan morning twilight 440B; Toughner is POE-g-MAH, adopts the light N409 of energy; Lubricant adopts trade mark silicone powder GM100; Oxidation inhibitor adopts the mixture of antioxidant 1010 and irgasfos 168, and both weight ratios are 1:1.
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