CN104098836A - Halogen-free flame-retardant reinforced polypropylene material containing polyamide charring agent and preparation method thereof - Google Patents
Halogen-free flame-retardant reinforced polypropylene material containing polyamide charring agent and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a halogen-free flame-retardant reinforced polypropylene material containing a polyamide charring agent and a preparation method thereof. The material comprises the following components in parts by mass: 30-60 percent of polypropylene, 22-28 percent of a halogen-free flame-retardant agent, 5-8 percent of a polyamide charring agent, 3-6 percent of a compatilizer, 10-30 percent of alkali-free glass fiber yarn, 0.2-0.5 percent of an antioxidant and 0.4-0.8 percent of a processing aid. The preparation method of the compounded material comprises the steps as follows: the components are weighed according to the weight percentages; the components are mixed in a low-speed mixer for 3-5 minutes and then discharged; extrusion and granulation are performed on the mixture on a twin-screw extruder, wherein the processing temperature is 190-210 DEG C, and the rotation rate of screws is 420-460 rpm. Compared with the prior art, the material, disclosed by the invention, adopts the novel polyamide charring agent to retard the combustion of the polypropylene and has excellent compatibility and a charring effect; the obtained halogen-free flame-retardant reinforced polypropylene material has the characteristics of avoidance of precipitation, good easiness in processing and good mechanical property, satisfies the requirement on environmental protection and is favorable in flame-retardant performance; test sample strips with different thicknesses (1.6/2.5/3.2mm) all meet the grade UL94V0; the glow wire flame-retardant performance is good; the material can be widely applied to household appliances and electronic and electric industries.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent and preparation method thereof, this material can be widely used in an electrical article, the field such as electric.
Background technology
Polypropylene (PP), as a kind of commodity polymeric material of high comprehensive performance, has been widely used in the fields such as electronic apparatus, automobile and electric wire.But, because the limiting oxygen index(LOI) of PP only has 17.4, belong to inflammable material, after burning, form a large amount of molten drops and flame and be easy to propagate, therefore greatly limit the Application Areas of PP material.Halogen-free expansion type flame-proof (IFR) polypropylene, because of its environmental protection low toxicity, few cigarette, without advantages such as obnoxious flavour generations, becomes an eco-friendly family macromolecule material.When IFR polypropylene flame redardant, often adopt using ammonium polyphosphate (APP), tetramethylolmethane (PER), trimeric cyanamide (MA) respectively as acid source, carbon source and the source of the gas of expansion type flame retardant.But this system small molecular char-forming agent PER polarity is large, easily migration, water absorbability are strong, and poor with non-polar polyolefinic matrix phase capacitive, fire retardant disperses uneven in resin matrix, easily reunion, has affected the aesthetics of flame retardant effect and the goods of material.
Being chosen to charcoal polymkeric substance, to replace polyol can be used for overcoming fire retardant greatly water-soluble and the problem such as easily separate out.Polymeric amide-6(PA6) as widely used material in polymeric amide family, be that one has charcoal polymkeric substance of one's own, in the time that it is used as the fire retarding synergist of PP, the difficult point of maximum is exactly the improvement of consistency and the coupling of processing temperature.Chinese patent 200710202263 discloses a kind of method of preparing low melting point nylon, and patent CN 102286199 B also disclose a kind of formula and preparation method of composite low melting point nylon-6.Because polymeric amide and polyolefine are extremely inconsistent systems, thereby nylon-6 for polyolefinic fire-retardant be not the apparent thinking in field of the same trade and technology, and the fire-retardant dual function of the increase-volume that nano imvite particle has and synergistic can not be ignored, it also has into the effect of charcoal and anti-molten drop when can increasing polymeric amide with matrix phase capacitive.Therefore, in conjunction with these 2 for we provide preparation and PP consistency good and with the method for the approaching low melting point nylon of PP processing temperature, for the polymeric amide char-forming agent of polypropylene flame redardant.
Summary of the invention
The object of the present invention is to provide a kind of mechanical property better, thermotolerance is good, and vertical combustion performance and glowing filament flame retardant properties are good, can be widely used in high performance halogen-free flame-proof reinforced polypropylene material of electrical equipment inner piece, connector etc. and preparation method thereof.
The technical problem that the present invention further will solve is, reduce the fusing point of polymeric amide polymeric amide char-forming agent can be applicable in the processing environment of polypropylene flame redardant, and with the compound good high-performance halogen-free flame retardant Reinforced Polypropylene material of a kind of mechanical property excellence, flame retardant properties and preparation method thereof that provides of glass fibre.
The technical solution adopted for the present invention to solve the technical problems is: containing the halogen-free flame-proof reinforced polypropylene material of polymeric amide char-forming agent, by forming in the raw material of weight part below:
PP resin 30 ~ 60%
Halogen-free flame retardants 22 ~ 28%
Polymeric amide char-forming agent 5 ~ 8%
Compatilizer 3 ~ 6%
Alkali-free glass fiber yarn 10 ~ 30%
Oxidation inhibitor 0.2 ~ 0.5%
Processing aid 0.4 ~ 0.8%.
Described PP resin is a kind of homopolymerization PP, or the mixture of a kind of homopolymerization PP and another kind of copolymerization PP, and the molten finger of homopolymerization PP is 10 ~ 20 g/10min, and the molten finger of copolymerization PP is 3 ~ 5 g/10min (2.16 kg, 230 DEG C at record).
Described halogen-free flame retardants is phosphorus-nitrogen expansion type fire retardant, is wherein two or three mixture of ammonium polyphosphate, ortho-phosphoric acid trimeric cyanamide, polyphosphoric acid melamine, melamine cyanurate.
Described polymeric amide char-forming agent is the mixture of common nylon-6 sticky in a kind of and inorganic calcium salt, organo montmorillonite.
Described compatilizer is a kind of polar monomer graft polymkeric substance, as maleic anhydride inoculated polypropylene.
Described alkali-free glass fiber yarn is the glass fibre that a kind of alkali metal oxide content is low.
Described oxidation inhibitor is the compound of Hinered phenols antioxidant (1010) and organic phosphites oxidation inhibitor (168) 1:2.
Described processing aid is N, N'-ethylene bis stearic acid amide (EBS) or modification EBS.
Polymeric amide char-forming agent of the present invention can be prepared by the following method: after first respectively PA6 resin and organo montmorillonite, inorganic calcium salt particle being mixed by certain weight ratio, join and in twin screw extruder, extrude cooling granulation, by compound the particle obtaining melting on twin screw extruder, obtain described polymeric amide char-forming agent by two-step process again.The technique that adopts two-step approach is mainly that the silicate in order to suppress in calcium ion and organo montmorillonite reacts, thereby ensures that the good distribution of nano imvite particle in polymeric amide keeps becoming preferably charcoal effect.
The preparation method of a kind of halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent of the present invention, is characterized in that comprising the following steps:
(1) preparation of polymeric amide char-forming agent
After the PA6 resin of having dried, inorganic calcium salt particle and organo montmorillonite are mixed by a certain percentage of the weight, on twin screw extruder, extrude, granulation, obtain polymeric amide char-forming agent; Extrusion temperature is 225 ~ 245 DEG C, and engine speed is 420 ~ 440 rpm.
(2) raw-material mixing
The above-mentioned polymeric amide char-forming agent preparing is dried 4 ~ 6 hours at 120 DEG C, and moisture controlled is below 0.1%; Again polymeric amide char-forming agent, composite halogen-free flame retardants, compatilizer, oxidation inhibitor, processing aid etc. are mixed 3 ~ 5 minutes in mixer, fully stir and make each component dispersed and avoid material layering.
(3) melt extrude
By the material mixing extruding pelletization on twin screw extruder, alkali-free glass fiber yarn adds by glass fiber opening, regulates engine speed and feeding frequency, keeps certain vacuum tightness, melt extrudes temperature between 190 ~ 210 DEG C, and engine speed is 420 ~ 460 rpm.
(4) granulation and aftertreatment
The material of extruding is carried out cooling, air-dry, pelletizing, is packaged to be finished product.
The present invention adopts polymeric amide char-forming agent as the new char-forming agent of halogen-free flame-retardant system, and with the polypropylene that the composite rear combustion-proof glass fiber of halogen-free flame retardants strengthens, processing characteristics is good, and comprehensive cost is low, without separating out phenomenon; This product mechanical property is better, and thermotolerance is good, and vertical combustion performance and glowing filament flame retardant properties are good, can be widely used in electrical equipment inner piece, connector etc.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, but embodiment does not limit in any form the present invention.
PP resin is a kind of homopolymerization PP 1 and a kind of copolymerization PP2, and the trade mark is respectively V30G and K8003, and molten finger is respectively 15 and 3 g/10min(2.16 kg, records at 230 DEG C); Halogen-free flame retardants is composite phosphorus-nitrogen expansion type fire retardant, is preferably the compound of ammonium polyphosphate and polyphosphoric acid melamine; Polymeric amide char-forming agent is self-control fire retardant, and wherein PA6 resin is middle viscosity resin, and the trade mark is M2800, and relative viscosity is 2.7; Compatilizer is preferably the polypropylene of maleic anhydride graft, and the trade mark is SWJ-1B; Alkali-free glass fiber yarn is the 998A that megalith group produces; Oxidation inhibitor is the compound of hindered amine oxidation inhibitor (1010) and organic phosphorous acid kind antioxidant (168) 1:2; Processing aid is EBS, and order number is 325 orders.
Embodiment 1
It is 55 parts by PP resin (mass ratio PP1:PP2=1:1) weight percent, 24.2 parts of halogen-free flame retardantss, 6.3 parts of polymeric amide char-forming agents, 3.0 parts of compatilizers, 10 parts, alkali-free glass fiber yarn, 0.5 part, oxidation inhibitor, 1 part of processing aid, in stirrer low speed mixing 240s again high-speed mixing become 180s, glass fibre adds at forcing machine glass fiber opening (screw rod Si district), is that 190 ~ 210 DEG C of twin screw extruders are extruded, through cooling, pelletizing, sieve, be packaged to be product through melt temperature.Wherein engine speed is 425, and feed frequency is 24.
Embodiment 2
It is 42 parts by PP resin (mass ratio PP1:PP2=1:1) weight percent, 26.7 parts of halogen-free flame retardantss, 6.3 parts of polymeric amide char-forming agents, 3.5 parts of compatilizers, 20 parts, alkali-free glass fiber yarn, 0.5 part, oxidation inhibitor, 1 part of processing aid, in stirrer low speed mixing 240s again high-speed mixing become 180s, glass fibre adds at forcing machine glass fiber opening, is that 190 ~ 210 DEG C of twin screw extruders are extruded, through cooling, pelletizing, sieve, be packaged to be product through melt temperature.Wherein engine speed is 440, and feed frequency is 20.
Embodiment 3
It is 35 parts by PP resin (mass ratio PP1:PP2=1:1) weight percent, 23.7 parts of halogen-free flame retardantss, 6.3 parts of polymeric amide char-forming agents, 4.0 parts of compatilizers, 29.5 parts, alkali-free glass fiber yarn, 0.5 part, oxidation inhibitor, 1 part of processing aid, in stirrer low speed mixing 240s again high-speed mixing become 180s, glass fibre adds at forcing machine glass fiber opening, is that 190 ~ 210 DEG C of twin screw extruders are extruded, through cooling, pelletizing, sieve, be packaged to be product through melt temperature.Wherein engine speed is 460, and feed frequency is 16.
Performance evaluation mode and implementation standard
Performance to embodiment 1, embodiment 2 and a kind of halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent of embodiment 3 gained is as follows:
Note: 1, shock strength is that socle girder impact test instrument obtains IZOD notched Izod impact strength;
2, GWIT is shown glowing filament ignition temperature, and GWFI is shown glowing filament flammability index.
The content of polymeric amide char-forming agent remains the weight percent of 6.3 parts in an embodiment of the present invention, glass fiber content in the corresponding formula of embodiment 1-3 is respectively 10,20,29.5 parts, along with the increase of glass fiber content, the content of PP resin reduces, and the addition of halogen-free flame retardants slightly changes.In the time that glass fiber content is 29.5 parts, the tensile strength of product is up to 60 MPa, and flexural strength can reach 73 MPa, and modulus in flexure and shock strength also increase successively, and best result is not 3800 MPa and 7.4 kJ/m
2.Meanwhile, the thermotolerance of material significantly improves, and flame retardant properties all can meet UL94 V0 level, glowing filament flame retardant properties is good, illustrate that in the present invention, the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent has been realized high performance, economically feasible, is applicable to comparatively harsh applied environment.
In sum, be preferred embodiment of the present invention, all changes of making according to technical solution of the present invention, when the function producing fails to exceed the scope of technical solution of the present invention, all belong to protection scope of the present invention.
Claims (10)
1. containing a halogen-free flame-proof reinforced polypropylene material for polymeric amide char-forming agent, it is characterized in that being formed by following component by weight percentage:
PP resin 30 ~ 60%
Halogen-free flame retardants 22 ~ 28%
Polymeric amide char-forming agent 5 ~ 8%
Compatilizer 3 ~ 6%
Alkali-free glass fiber yarn 10 ~ 30%
Oxidation inhibitor 0.2 ~ 0.5%
Processing aid 0.4 ~ 0.8%.
2. the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, is characterized in that: described PP resin is acrylic resin, can be single homopolymerization PP resin, or the mixture of a certain proportion of homopolymerization PP and copolymerization PP.
3. the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, it is characterized in that: described halogen-free flame retardants is P-N type halogen-free environmental expansion type flame retardant, is two or three mixture in ammonium polyphosphate, ortho-phosphoric acid trimeric cyanamide, polyphosphoric acid melamine and melamine cyanurate.
4. the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, it is characterized in that: described polymeric amide char-forming agent is homemade PA6 mixture, is the mixture that PA6 resin, inorganic calcium salt particle and organo montmorillonite are composited according to a certain percentage.
5. the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, it is characterized in that: described compatilizer is polar monomer graft polymkeric substance, wherein polymer monomer is one or the mixture in multipolymer and the ethylene-acrylate-glycidyl methacrylate copolymer of polyethylene, polypropylene, vinylbenzene and divinyl, and polar monomer is a kind of or its mixture in maleic anhydride, vinylformic acid, methacrylic acid and glytidyl methacrylate.
6. the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, is characterized in that: described alkali-free glass fiber yarn is E type glass fibre, is the low glass fibre of alkali metal oxide content.
7. the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, is characterized in that: described oxidation inhibitor is the compound of Hinered phenols antioxidant and organic phosphites oxidation inhibitor.
8. the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, is characterized in that: described processing aid is the ethylene bis-fatty acid amides of ethylene bis-fatty acid amides or modification.
9. the preparation method of the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent as claimed in claim 1, is characterized in that comprising the following steps:
(1) take PA6 resin, inorganic calcium salt, nano organic montmorillonite, prepare polymeric amide char-forming agent;
(2) the polymeric amide char-forming agent, compatilizer, oxidation inhibitor, the processing aid that in PP resin, halogen-free flame retardants, (1), make are mixed in mixing tank;
(3) raw material mixed in step (2) is added to glass at glass fiber opening, extruding pelletization through twin screw extruder melting simultaneously.
10. the preparation method of the halogen-free flame-proof reinforced polypropylene material containing polymeric amide char-forming agent according to claim 9, is characterized in that comprising the following steps:
(1) take PA6 resin, inorganic calcium salt, nano organic montmorillonite according to parts by weight, extrude and prepare polymeric amide char-forming agent by two-step process;
(2) take according to parts by weight the polymeric amide char-forming agent, compatilizer, oxidation inhibitor, the processing aid low speed mixing 240s in mixing tank that in PP resin, halogen-free flame retardants, (1), make, then high-speed mixing 180s, guarantee that mixing of materials is even;
(3) raw material mixed step (2) is melt extruded and adds glass at glass fiber opening through twin screw extruder simultaneously; Twin screw extruder processing condition are: twin screw extruder one district temperature 150-170 DEG C, two district temperature 160-180 DEG C, three district temperature 180-200 DEG C, four district temperature 170-190 DEG C, five district temperature 170-190 DEG C, six district temperature 180-200 DEG C, seven district temperature 180-200 DEG C, eight district temperature 190-210 DEG C, die head temperature is 180-200 DEG C, compound time of delivery in screw rod is 1 ~ 2 minute; Screw speed is 420 ~ 460 rpm, and feed frequency is 14 ~ 25 rpm, the number of share of stock that the control of glass fiber content can add by adjusting screw(rod) rotating speed, feed frequency and glass.
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| CN104448392A (en) * | 2014-12-24 | 2015-03-25 | 东莞市迪彩塑胶五金有限公司 | M-ALP (Membrane-type Alkaline Phosphatase) flame retardant, composite flame retardant material thereof and preparation method |
| CN104448389A (en) * | 2014-12-24 | 2015-03-25 | 东莞市迪彩塑胶五金有限公司 | CTAB-phosphate flame retardant, composite flame retardant material of CTAB-phosphate flame retardant and preparation method of CTAB-phosphate flame retardant |
| CN104672612A (en) * | 2015-02-04 | 2015-06-03 | 苏州康华净化系统工程有限公司 | Flame retardant polypropylene material and preparation method thereof |
| CN105086129A (en) * | 2015-08-07 | 2015-11-25 | 余姚市中发工程塑料有限公司 | Anti-static halogen-free flame-retardant polypropylene composition and preparation method |
| CN106189566A (en) * | 2016-07-25 | 2016-12-07 | 太原理工大学 | A kind of expandable flame retardant coating for engineering plastic surface and preparation method thereof |
| WO2018090802A1 (en) * | 2016-11-16 | 2018-05-24 | 金发科技股份有限公司 | Glass fiber-reinforced, halogen-free, and flame-retardant polypropylene material and preparation method and application of same |
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Cited By (17)
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| CN104448392A (en) * | 2014-12-24 | 2015-03-25 | 东莞市迪彩塑胶五金有限公司 | M-ALP (Membrane-type Alkaline Phosphatase) flame retardant, composite flame retardant material thereof and preparation method |
| CN104448389A (en) * | 2014-12-24 | 2015-03-25 | 东莞市迪彩塑胶五金有限公司 | CTAB-phosphate flame retardant, composite flame retardant material of CTAB-phosphate flame retardant and preparation method of CTAB-phosphate flame retardant |
| CN104448392B (en) * | 2014-12-24 | 2018-11-02 | 东莞市迪彩塑胶五金有限公司 | M-ALP fire retardants and its composite flame-proof material and preparation method |
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