CN104497560A - Polyamide flame-retardant composition and preparation method thereof - Google Patents

Polyamide flame-retardant composition and preparation method thereof Download PDF

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Publication number
CN104497560A
CN104497560A CN201410765081.4A CN201410765081A CN104497560A CN 104497560 A CN104497560 A CN 104497560A CN 201410765081 A CN201410765081 A CN 201410765081A CN 104497560 A CN104497560 A CN 104497560A
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district
temperature
flame
retardant
polyamide composition
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Inventor
张现军
田晋丽
张永
梁惠强
金学峰
周华龙
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Jiangsu Kingfa New Material Co Ltd
Tianjin Kingfa Advanced Materials Co Ltd
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Jiangsu Kingfa New Material Co Ltd
Tianjin Kingfa Advanced Materials Co Ltd
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Priority to CN201410765081.4A priority Critical patent/CN104497560A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06Polyamides derived from polyamines and polycarboxylic acids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention discloses a polyamide flame-retardant composition and a preparation method of the polyamide flame-retardant composition. The polyamide flame-retardant composition is prepared from the following raw materials in parts by mass: 40-74 parts of polyamide resins, 10-25 parts of hollow glass fibers, 10-18 parts of flame retardant, 5-7 parts of flame-retardant synergists, and 1-10 parts of other auxiliaries. Compared with the prior art, the polyamide flame-retardant composition is high in flame-retardant performance which reaches UL94 V-0 grade; moreover, the hollow glass fibers are added into a preparation formula, so that the density of materials is reduced while the mechanical performance of the materials can be improved, the dielectric property of the materials is improved, and the polyamide flame-retardant composition is high in heat insulation performance and has soundproof and noise-reduction functions.

Description

Flame-retardant polyamide composition and preparation method thereof
Technical field
The present invention relates to polymeric material field, relate to a kind of flame-retardant polyamide composition and preparation method thereof specifically.
Background technology
Polymeric amide (PA) is also called nylon, is that DuPont develops the resin used as fiber at first, realizes industrialization in nineteen thirty-nine.Start development and production injection-molded item the 1950's, the requirement meet the lightweight of downstream industry goods with substituted metal, reducing costs.PA plastics have good over-all properties, comprise mechanical property, thermotolerance, wearability, chemical proofing and self lubricity, and frictional coefficient are low, there is certain flame retardant resistance, be easy to processing, be suitable for, by glass fibre and other filler filling enhancing modified, improving performance and broadened application scope.
In modifying plastics industry, generally can use as the inorganic minerals such as glass fibre, talcum powder, mica, calcium carbonate, glass microballon, wollastonite strengthen component as filling, the performance such as rigidity, thermotolerance, molding shrinkage, chemical resistant properties, surface gloss, incendivity of nylon material is improved, to meet the service requirements of final plastics by blending and modifying.But because the density of these inorganic mineral filler is often large than the density of plastics, therefore add the weight that mineral filler can increase the finished product relatively in the plastic.Also have research to adopt hollow glass micropearl as filler modified polyamide material, to reach the object of weight reduction, but the performance such as the intensity of modified polyamide material and rigidity is all far away from glass-fibre reinforced polyamide material.And hollow glass fibre strengthens thermoplastic composite and has the features such as light weight, good rigidly, specific inductivity are low.
Flameproof polyamide conventional at present adopts halogen flame retardant to reach good flame retardant effect, adopts glass fiber reinforcement to reach good mechanical properties.Polymkeric substance, when making electrical insulating material or capacitor material uses, requires that its dielectric loss is the smaller the better.When Flameproof polyamide is applied to electric parts and electronic component etc., except good mechanical property and the evening of flame retardant properties will be had, also to have good dielectric properties, and common fire-retarding reinforced polyamide material show in this respect slightly poor.
Summary of the invention
In order to overcome above-mentioned defect, the invention provides a kind of flame-retardant polyamide composition and preparation method thereof, there is the flame retardant properties of low density and excellence, mechanical property, dielectric properties, heat insulation and sound-proofing properties.
The present invention in order to the technical scheme solving its technical problem and adopt is: a kind of flame-retardant polyamide composition, is made up of the raw material of following mass fraction proportioning:
As a further improvement on the present invention, described polyamide resin is one in PA6, PA66 or its mixture.
As a further improvement on the present invention, described hollow glass fibre has ring section, and its hollowness is 10% ~ 65%, and diameter is 10 ~ 70 μm.
As a further improvement on the present invention, described fire retardant is brominated Polystyrene, and described retardant synergist is antimonous oxide.
As a further improvement on the present invention, other described auxiliary agents are selected from one in impact modifying agent, oxidation inhibitor, coupling agent or its mixture.
As a further improvement on the present invention, described impact modifying agent is maleic anhydride graft POE, and percentage of grafting is 0.8 ~ 1.2.
As a further improvement on the present invention; described oxidation inhibitor is N; N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine and two (2.4-di-tert-butyl-phenyl) pentaerythritol diphosphites mixture.
As a further improvement on the present invention, described coupling agent is containing amino silane coupling agent.
The present invention also improves a kind of preparation method of above-mentioned flame-retardant polyamide composition, comprise the following steps: the polyamide resin in formula ratio, fire retardant, other auxiliary agents are mixed in super mixer, then it is added this twin screw extruder from the main opening for feed of twin screw extruder, the side opening for feed of hollow glass fibre in formula ratio by this twin screw extruder is added in this twin screw extruder simultaneously, extrude and cool, dry, pelletizing.
As a further improvement on the present invention, one district's temperature of described twin screw extruder is 210-230 DEG C, two district's temperature are 220-240 DEG C, three district's temperature are 220-240 DEG C, and four district's temperature are 220-240 DEG C, and five district's temperature are 230-250 DEG C, six district's temperature are 240-260 DEG C, seven district's temperature are 230-250 DEG C, and eight district's temperature are 220-240 DEG C, and nine district's temperature are 200-220 DEG C; Engine speed is 250-350 rev/min.
The invention has the beneficial effects as follows: compared with prior art, flame-retardant polyamide composition of the present invention has excellent flame retardant properties, reach UL94V-0 level, and hollow glass fibre is added in preparation formula, the density of material can reduce while improving the mechanical property of materials, improve the dielectric properties of material, and there is good heat-proof quality and sound insulation and decrease of noise functions.
Embodiment
Below in conjunction with embodiment and comparative example, the invention will be further described.But protection scope of the present invention is not limited to following embodiment, the simple equivalence namely in every case done with the present patent application the scope of the claims and description changes and modifies, and all still belongs within patent covering scope of the present invention.
In following examples and comparative example, polyamide resin is selected from one or more the mixture of PA6, PA66, as PA6 can select VOLGAMID25, VOLGAMID27 of Kuibyshev's nitrogen engineering plastics company limited production and selling, the 50BWFS etc. of the EPR27 that PA66 can select Henan Shenma Nylon Chemical Co., Ltd to produce and Shou Nuo company of U.S. production and selling; Hollow glass fibre selects the Hollex S-2 high strength hollow glass fibre of OCF glass company of the U.S.; Brominated Polystyrene selects the FR-1718 of BASF; Antimonous oxide is produced by Hunan flash star antimony industry; The ECS11-4.5-560A that glass fibre selects megalith group to produce; Hollow glass micropearl, trade mark S32, Minnesota Mining and Manufacturing Company produces; Maleic anhydride graft POE is selected from the KHEP-680C3 that Haier's sectionization is produced; The IRGANOX1098 of vapour Bagong department production and selling and the AT-626 of Albemarle Corporation of U.S. production and selling selected by oxidation inhibitor; Coupling agent selects the commercially available trade mark to be the amino silicane coupling agent of KH550.
Embodiment 1:
Take 32KG PA6VOLGAMID25,30KG PA6650BWFS, 10KG hollow glass fibre, 18KG brominated Polystyrene, 5KG antimonous oxide, 3KG maleic anhydride graft POE, 1KG coupling agent, 0.7KG oxidation inhibitor 1098,0.3KG oxidation inhibitor AT-626.Above-mentioned PA6, PA66, brominated Polystyrene, antimonous oxide, maleic anhydride graft POE, oxidation inhibitor, coupling agent are mixed in super mixer; Then mixture is added twin screw extruder from main opening for feed, hollow glass fibre is being added in twin screw extruder by side opening for feed, is extruding rear cooling, drying, pelletizing.The processing conditions of twin screw extruder is: district's temperature 220 DEG C, two district's temperature 230 DEG C, three district's temperature 240 DEG C, four district's temperature 240 DEG C, five district's temperature 250 DEG C, six district's temperature 250 DEG C, seven district's temperature 245 DEG C, eight district's temperature 235 DEG C, nine district's temperature 220 DEG C; Engine speed 290 revs/min.
Embodiment 2:
Take 37KG PA6VOLGAMID25,10KG PA6650BWFS, 25KG hollow glass fibre, 15KG brominated Polystyrene, 6KG antimonous oxide, 3KG maleic anhydride graft POE, 0.5KG oxidation inhibitor 1098,0.5KG oxidation inhibitor AT-626,3KG coupling agent.Above-mentioned PA6, PA66, brominated Polystyrene, antimonous oxide, maleic anhydride graft POE, oxidation inhibitor, coupling agent are mixed in super mixer; Then mixture is added twin screw extruder from main opening for feed, hollow glass fibre is being added in twin screw extruder by side opening for feed, is extruding rear cooling, drying, pelletizing.The processing conditions of twin screw extruder is: district's temperature 220 DEG C, two district's temperature 230 DEG C, three district's temperature 240 DEG C, four district's temperature 240 DEG C, five district's temperature 250 DEG C, six district's temperature 250 DEG C, seven district's temperature 245 DEG C, eight district's temperature 235 DEG C, nine district's temperature 220 DEG C; Engine speed 350 revs/min.
Embodiment 3:
Take 43KG PA6VOLGAMID27,25KG hollow glass fibre, 15KG brominated Polystyrene, 7KG antimonous oxide, 5KG maleic anhydride graft POE, 0.5KG oxidation inhibitor 1098,0.5KG oxidation inhibitor AT-626,4KG coupling agent.Above-mentioned PA6, brominated Polystyrene, antimonous oxide, maleic anhydride graft POE, oxidation inhibitor, coupling agent etc. are mixed in super mixer; Then mixture is added twin screw extruder from main opening for feed, hollow glass fibre is being added in twin screw extruder by side opening for feed, is extruding rear cooling, drying, pelletizing.The processing conditions of twin screw extruder is: district's temperature 220 DEG C, two district's temperature 230 DEG C, three district's temperature 240 DEG C, four district's temperature 240 DEG C, five district's temperature 250 DEG C, six district's temperature 250 DEG C, seven district's temperature 245 DEG C, eight district's temperature 235 DEG C, nine district's temperature 220 DEG C; Engine speed 330 revs/min.
Embodiment 4:
Take 66KG PA66EPR27,10KG hollow glass fibre, 18KG brominated Polystyrene, 5KG antimonous oxide, 0.5KG oxidation inhibitor 1098,0.5KG oxidation inhibitor AT-626.Above-mentioned PA66, brominated Polystyrene, antimonous oxide, oxidation inhibitor etc. are mixed in super mixer; Then mixture is added twin screw extruder from main opening for feed, hollow glass fibre is being added in twin screw extruder by side opening for feed, is extruding rear cooling, drying, pelletizing.The processing conditions of twin screw extruder is: district's temperature 220 DEG C, two district's temperature 230 DEG C, three district's temperature 240 DEG C, four district's temperature 240 DEG C, five district's temperature 250 DEG C, six district's temperature 250 DEG C, seven district's temperature 245 DEG C, eight district's temperature 235 DEG C, nine district's temperature 220 DEG C; Engine speed 300 revs/min.
Embodiment 5:
Take 49KG PA6VOLGAMID25,15KG hollow glass fibre, 10KG brominated Polystyrene, 7KG antimonous oxide, 5KG maleic anhydride graft POE, 0.5KG oxidation inhibitor 1098,0.5KG oxidation inhibitor AT-626,4KG coupling agent.Above-mentioned PA, brominated Polystyrene, antimonous oxide, maleic anhydride graft POE, oxidation inhibitor, coupling agent etc. are mixed in super mixer; Then mixture is added twin screw extruder from main opening for feed, hollow glass fibre is being added in twin screw extruder by side opening for feed, is extruding rear cooling, drying, pelletizing.The processing conditions of twin screw extruder is: district's temperature 220 DEG C, two district's temperature 230 DEG C, three district's temperature 240 DEG C, four district's temperature 240 DEG C, five district's temperature 250 DEG C, six district's temperature 250 DEG C, seven district's temperature 245 DEG C, eight district's temperature 235 DEG C, nine district's temperature 220 DEG C; The engine speed of twin screw extruder 300 revs/min.
Comparative example 1:
Take 49KG PA6VOLGAMID25,15KG glass fibre, 19KG brominated Polystyrene, 7KG antimonous oxide, 5KG maleic anhydride graft POE, 0.5KG oxidation inhibitor 1098,0.5KG oxidation inhibitor AT-626,4KG coupling agent.Above-mentioned PA, brominated Polystyrene, antimonous oxide, maleic anhydride graft POE, oxidation inhibitor, coupling agent etc. are mixed in super mixer; Then mixture is added twin screw extruder from main opening for feed, hollow glass fibre is being added in twin screw extruder by side opening for feed, is extruding rear cooling, drying, pelletizing.The processing conditions of twin screw extruder is: district's temperature 220 DEG C, two district's temperature 230 DEG C, three district's temperature 240 DEG C, four district's temperature 240 DEG C, five district's temperature 250 DEG C, six district's temperature 250 DEG C, seven district's temperature 245 DEG C, eight district's temperature 235 DEG C, nine district's temperature 220 DEG C; Engine speed 300 revs/min.
The pellet prepared is put into convection oven, under 120 DEG C of conditions, dries 4h, then by dried pellet injection molding batten in injection moulding machine.Injecting molding die temperature is 90 DEG C.The performance test standard of gained daiamid composition of the present invention is as shown in table 1.
The physical parameter of above embodiment 1 ~ 5 and the daiamid composition obtained by comparative example is in table 2.
As can be seen from Table 2, flame-retardant polyamide composition of the present invention has excellent flame retardant properties, reach UL94V-0 level, and obviously reduce than common alkali free glass fibre enhancing fire-retardant polyamide material density, and keep the good mechanical property such as tensile strength, flexural strength, modulus in flexure.Meanwhile, flame-retardant polyamide composition of the present invention also has good dielectric properties, heat-proof quality and sound insulation and decrease of noise functions.Flame-retardant polyamide composition of the present invention can be widely used in electric field.
The test event of table 1 Material Physics mechanical property and the testing method of correspondence
Test event Testing method and condition
Density ISO 1183
Tensile strength ISO 527 (speed 10mm/min)
Flexural strength ISO 178 (speed 10mm/min)
Modulus in flexure ISO 178 (speed 10mm/min)
Simply supported beam notched Izod impact strength ISO 180
Heat-drawn wire ISO 75
Dielectric strength IEC 60243
Thermal conductivity ISO 8302
Flame retardant properties UL 94
The physical parameter of table 2 daiamid composition

Claims (10)

1. a flame-retardant polyamide composition, is characterized in that: be made up of the raw material of following mass fraction proportioning:
2. flame-retardant polyamide composition according to claim 1, is characterized in that: described polyamide resin is one in PA6, PA66 or its mixture.
3. flame-retardant polyamide composition according to claim 1, is characterized in that: described hollow glass fibre has ring section, and its hollowness is 10% ~ 65%, and diameter is 10 ~ 70 μm.
4. flame-retardant polyamide composition according to claim 1, is characterized in that: described fire retardant is brominated Polystyrene, and described retardant synergist is antimonous oxide.
5. flame-retardant polyamide composition according to claim 1, is characterized in that: other described auxiliary agents are selected from one in impact modifying agent, oxidation inhibitor, coupling agent or its mixture.
6. flame-retardant polyamide composition according to claim 5, is characterized in that: described impact modifying agent is maleic anhydride graft POE, and percentage of grafting is 0.8 ~ 1.2.
7. flame-retardant polyamide composition according to claim 5; it is characterized in that: described oxidation inhibitor is N; N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine and two (2.4-di-tert-butyl-phenyl) pentaerythritol diphosphites mixture.
8. flame-retardant polyamide composition according to claim 5, is characterized in that: described coupling agent is containing amino silane coupling agent.
9. the preparation method of a flame-retardant polyamide composition according to any one of claim 1 to 8, it is characterized in that, comprise the following steps: the polyamide resin in formula ratio, fire retardant, other auxiliary agents are mixed in super mixer, then it is added this twin screw extruder from the main opening for feed of twin screw extruder, the side opening for feed of hollow glass fibre in formula ratio by this twin screw extruder is added in this twin screw extruder simultaneously, extrude and cool, dry, pelletizing.
10. the preparation method of flame-retardant polyamide composition according to claim 9, it is characterized in that: district's temperature of described twin screw extruder is 210-230 DEG C, two district's temperature are 220-240 DEG C, three district's temperature are 220-240 DEG C, and four district's temperature are 220-240 DEG C, and five district's temperature are 230-250 DEG C, six district's temperature are 240-260 DEG C, seven district's temperature are 230-250 DEG C, and eight district's temperature are 220-240 DEG C, and nine district's temperature are 200-220 DEG C; Engine speed is 250-350 rev/min.
CN201410765081.4A 2014-12-11 2014-12-11 Polyamide flame-retardant composition and preparation method thereof Pending CN104497560A (en)

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Cited By (4)

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CN104987706A (en) * 2015-07-29 2015-10-21 苏州新区华士达工程塑胶有限公司 Soundproof and noise-reduction car plastic
CN105111733A (en) * 2015-09-20 2015-12-02 成都育芽科技有限公司 Thermal insulating strip made of reinforced nylon composite material for building doors and windows
CN108440878A (en) * 2017-02-16 2018-08-24 上海安缔诺科技有限公司 A kind of composite microwave medium material and its preparation method and application
CN111961336A (en) * 2020-07-21 2020-11-20 天津金发新材料有限公司 Infrared-transmitting polyamide composition and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104987706A (en) * 2015-07-29 2015-10-21 苏州新区华士达工程塑胶有限公司 Soundproof and noise-reduction car plastic
CN105111733A (en) * 2015-09-20 2015-12-02 成都育芽科技有限公司 Thermal insulating strip made of reinforced nylon composite material for building doors and windows
CN108440878A (en) * 2017-02-16 2018-08-24 上海安缔诺科技有限公司 A kind of composite microwave medium material and its preparation method and application
CN111961336A (en) * 2020-07-21 2020-11-20 天津金发新材料有限公司 Infrared-transmitting polyamide composition and preparation method thereof
CN111961336B (en) * 2020-07-21 2023-01-31 天津金发新材料有限公司 Infrared-transmitting polyamide composition and preparation method thereof

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