CN103205118A - Method for preparing black halogen-free polyamide composite material with high performance - Google Patents

Method for preparing black halogen-free polyamide composite material with high performance Download PDF

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Publication number
CN103205118A
CN103205118A CN2013101308176A CN201310130817A CN103205118A CN 103205118 A CN103205118 A CN 103205118A CN 2013101308176 A CN2013101308176 A CN 2013101308176A CN 201310130817 A CN201310130817 A CN 201310130817A CN 103205118 A CN103205118 A CN 103205118A
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China
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parts
districts
region
polyamide
free
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CN2013101308176A
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Chinese (zh)
Inventor
方云祥
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Changshu Kailida Honeycomb Package Material Co Ltd
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Changshu Kailida Honeycomb Package Material Co Ltd
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Priority to CN2013101308176A priority Critical patent/CN103205118A/en
Publication of CN103205118A publication Critical patent/CN103205118A/en
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    • 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
    • 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
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • 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
    • 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
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895Barrel or housing

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a method for preparing a black halogen-free polyamide composite material with high performance and belongs to the technical field of preparation of high polymer material. The method comprises the following steps of: firstly, feeding 60 to 72 parts by weight of polyamide 66 resin, 12 to 18 parts by weight of polyamide 6 resin, 15 to 21 parts by weight of toughening agent, 5 to 10 parts by weight of compatilizer, 8 to 17 parts by weight of phosphate, 0.6 to 1.1 parts by weight of antioxidant, 24 to 32 parts by weight of reinforced fiber and 2.2 to 3.3 parts by weight of carbon black into a high-speed mixer; secondly, introducing the mixture obtained in the first step into a parallel double-screw extruder so as to be fused and extruded, and then obtaining a finished product after being cut and being dried, wherein the temperatures of the first region to the tenth region of the parallel double-screw extrude are respectively that: 210 DEG C in the first region, 220 DEG C in the second region, 230 DEG C in the third region, 235 DEG C in the fourth region, 240 DEG C in the fifth region, 230 DEG C in the sixth region, 235 DEG C from the seventh region to the tenth region. After being tested, the prepared black halogen-free polyamide composite material with the high performance has the following performance indexes: tensile strength being more than 125 to 135MPa, bending strength being more than 216 to 234MPa, impact strength on gap of a cantilever beam being more than 10 to 13kj/m<2>, and flame retardancy being V-0(UL-94-1.5mm).

Description

The preparation method of high-performance black halogen-free polyamide compoiste material
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of preparation method of high-performance black halogen-free polyamide compoiste material.
Background technology
Though polyamide material can be widely used in fields such as automobile, electronics, building, along with the extreme environment of material contact is more and more, thereby also more and more higher to the pursuit of material property.High performance polyamide material is the direction of endeavouring to study always.Along with the research to material combustion, to find to change into poisonous smog after the halogen burning, it is unfavorable that material is used.So, require material non-halogen, namely not halogen-containing in material.Therefore exploring rational preparation method makes polyamide material embody Halogen and significantly improves toughness and intensity has positive effect.
Summary of the invention
Task of the present invention is to provide a kind of preparation method of high-performance black halogen-free polyamide compoiste material, and the polyamide compoiste material that is prepared by this method has the high and not halogen-containing characteristics of intensity.
Task of the present invention is finished like this, a kind of preparation method of high-performance black halogen-free polyamide compoiste material, it is in 24 ~ 32 parts of 0.6 ~ 1.1 part in 8 ~ 17 parts of 5 ~ 10 parts of 15~21 parts of 12~18 parts of 60~72 parts of polyamide 66 resins, polyamide 6 resins, toughner, compatilizers, phosphoric acid salt, oxidation inhibitor, the fortifying fibres that will take by weighing by weight earlier and 2.2 ~ 3.3 parts of input high-speed mixers of carbon black and mixes 9min under the speed of 480n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after pelletizing and drying, obtain high-performance black halogen-free polyamide compoiste material, wherein: the temperature in a district to ten district of parallel twin screw extruder is controlled to be respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, 240 ℃ in five districts, 230 ℃ in six districts, seven districts to ten district is 235 ℃.
In one embodiment of the invention, described polyamide 66 resin be fusing point more than 230 ℃, the limiting viscosity index is 2.4 polyamide resin.
In another embodiment of the present invention, described polyamide 6 resin is that fusing point is at the polycaprolactam polyimide resin more than 210 ℃.
In yet another embodiment of the present invention, described toughner is acrylonitrile-butadiene-styrene copolymer.
In another embodiment of the present invention, described compatilizer is the acrylonitrile-butadiene-styrene copolymer of maleic anhydride graft.
Also have among the embodiment of the present invention, described phosphoric acid salt is hypo-aluminum orthophosphate.
More of the present invention and among embodiment, described oxidation inhibitor is 2, the 5-ditert-butylhydro quinone.
In of the present invention and then embodiment, described fortifying fibre is the alkali-free short glass fiber of length 6mm.
Of the present invention again more and among embodiment, described carbon black is thermally oxidized black.
The high-performance black halogen-free polyamide compoiste material of the inventive method preparation has following performance index after tested: tensile strength is greater than 125~135MPa, and flexural strength is greater than 216~234MPa, and the socle girder notched Izod impact strength is greater than 10~13kj/m 2, flame retardant resistance reaches V-0 (UL-94-1.5mm).
Embodiment
Embodiment 1:
The fusing point that will take by weighing by weight is more than 230 ℃ and the limiting viscosity index is 2.4 60 parts of polyamide resins, fusing point at 18 parts of the polycaprolactam polyimide resins more than 210 ℃, 18 parts of acrylonitrile-butadiene-styrene copolymers, by 12 parts of 10 parts of acrylonitrile-butadiene-styrene copolymers, the hypo-aluminum orthophosphates of maleic anhydride graft, 2 earlier, 1.1 parts of 5-ditert-butylhydro quinones, length are in 27 parts of the alkali-free short glass fibers of 6mm and 2.2 parts of input high-speed mixers of carbon black of being produced by channel process and mix 9min under the speed of 480n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after pelletizing and drying, obtain high-performance black halogen-free polyamide compoiste material, wherein: the temperature in a district to ten district of parallel twin screw extruder is controlled to be respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, 240 ℃ in five districts, 230 ℃ in six districts, seven districts to ten district respectively is 235 ℃.
Embodiment 2:
The fusing point that will take by weighing by weight is more than 230 ℃ and the limiting viscosity index is 2.4 72 parts of polyamide resins, fusing point at 12 parts of the polycaprolactam polyimide resins more than 210 ℃, 15 parts of acrylonitrile-butadiene-styrene copolymers, by 8 parts of 5 parts of acrylonitrile-butadiene-styrene copolymers, the hypo-aluminum orthophosphates of maleic anhydride graft, 2 earlier, 0.6 part of 5-ditert-butylhydro quinone, length are in 24 parts of the alkali-free short glass fibers of 6mm and 3.3 parts of input high-speed mixers of carbon black of being produced by channel process and mix 9min under the speed of 480n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after pelletizing and drying, obtain high-performance black halogen-free polyamide compoiste material, wherein: the temperature in a district to ten district of parallel twin screw extruder is controlled to be respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, 240 ℃ in five districts, 230 ℃ in six districts, seven districts to ten district respectively is 235 ℃.
Embodiment 3:
The fusing point that will take by weighing by weight is more than 230 ℃ and the limiting viscosity index is 2.4 64 parts of polyamide resins, fusing point at 16 parts of the polycaprolactam polyimide resins more than 210 ℃, 21 parts of acrylonitrile-butadiene-styrene copolymers, by 14 parts of 9 parts of acrylonitrile-butadiene-styrene copolymers, the hypo-aluminum orthophosphates of maleic anhydride graft, 2 earlier, 0.8 part of 5-ditert-butylhydro quinone, length are in 32 parts of the alkali-free short glass fibers of 6mm and 2.6 parts of input high-speed mixers of carbon black of being produced by channel process and mix 9min under the speed of 480n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after pelletizing and drying, obtain high-performance black halogen-free polyamide compoiste material, wherein: the temperature in a district to ten district of parallel twin screw extruder is controlled to be respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, 240 ℃ in five districts, 230 ℃ in six districts, seven districts to ten district respectively is 235 ℃.
Embodiment 4:
The fusing point that will take by weighing by weight is more than 230 ℃ and the limiting viscosity index is 2.4 68 parts of polyamide resins, fusing point at 14 parts of the polycaprolactam polyimide resins more than 210 ℃, 19 parts of acrylonitrile-butadiene-styrene copolymers, by 17 parts of 7 parts of acrylonitrile-butadiene-styrene copolymers, the hypo-aluminum orthophosphates of maleic anhydride graft, 2 earlier, 1 part of 5-ditert-butylhydro quinone, length are in 30 parts of the alkali-free short glass fibers of 6mm and 2.8 parts of input high-speed mixers of carbon black of being produced by channel process and mix 9min under the speed of 480n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after pelletizing and drying, obtain high-performance black halogen-free polyamide compoiste material, wherein: the temperature in a district to ten district of parallel twin screw extruder is controlled to be respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, 240 ℃ in five districts, 230 ℃ in six districts, seven districts to ten district respectively is 235 ℃.
The high-performance black halogen-free polyamide compoiste material that is obtained by above-described embodiment 1 to 4 has following technique effect after tested:
Test event Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Tensile strength MPa 125 128 132 135
Flexural strength MPa 217 224 228 233
Socle girder notched Izod impact strength kj/m 2 10.1 10.8 11.7 12.9
Flame retardant resistance (UL-94-1.5mm) V-0 V-0 V-0 V-0

Claims (9)

1. A kind of preparation method of high-performance black halogen-free polyamide compoiste material, it is characterized in that it is in 24 ~ 32 parts of 0.6 ~ 1.1 part in 8 ~ 17 parts of 5 ~ 10 parts of 15~21 parts of 12~18 parts of 60~72 parts of polyamide 66 resins, polyamide 6 resins, toughner, compatilizers, phosphoric acid salt, oxidation inhibitor, the fortifying fibres that will take by weighing by weight earlier and 2.2 ~ 3.3 parts of input high-speed mixers of carbon black and mixes 9min under the speed of 480n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after pelletizing and drying, obtain high-performance black halogen-free polyamide compoiste material, wherein: the temperature in a district to ten district of parallel twin screw extruder is controlled to be respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, 240 ℃ in five districts, 230 ℃ in six districts, seven districts to ten district is 235 ℃.
2. High-performance black halogen-free polyamide compoiste material according to claim 1, it is characterized in that described polyamide 66 resin be fusing point more than 230 ℃, the limiting viscosity index is 2.4 polyamide resin.
3. High-performance black halogen-free polyamide compoiste material according to claim 1 is characterized in that described polyamide 6 resin is that fusing point is at the polycaprolactam polyimide resin more than 210 ℃.
4. High-performance black halogen-free polyamide compoiste material according to claim 1 is characterized in that described toughner is acrylonitrile-butadiene-styrene copolymer.
5. High-performance black halogen-free polyamide compoiste material according to claim 1 is characterized in that described compatilizer is the acrylonitrile-butadiene-styrene copolymer of maleic anhydride graft.
6. High-performance black halogen-free polyamide compoiste material according to claim 1 is characterized in that described phosphoric acid salt is hypo-aluminum orthophosphate.
7. High-performance black halogen-free polyamide compoiste material according to claim 1 is characterized in that described oxidation inhibitor is 2,5-ditert-butylhydro quinone.
8. High-performance black halogen-free polyamide compoiste material according to claim 1 is characterized in that described fortifying fibre is the alkali-free short glass fiber of length 6mm.
9. High-performance black halogen-free polyamide compoiste material according to claim 1 is characterized in that described carbon black is thermally oxidized black2.
CN2013101308176A 2013-04-16 2013-04-16 Method for preparing black halogen-free polyamide composite material with high performance Pending CN103205118A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104774457A (en) * 2015-04-21 2015-07-15 广东顺德顺炎新材料有限公司 High-impact environment-friendly halogen-free flame-retardant reinforced nylon material, and preparation method and application thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1569931A (en) * 2004-04-26 2005-01-26 东莞市正昱塑胶五金有限公司 Fiber reinforced thermolplastic plastic preparation method
CN101070426A (en) * 2007-06-12 2007-11-14 巨石集团有限公司 Glass-fiber reinforced fire-retardant polyamide resin composition
CN102643541A (en) * 2012-04-27 2012-08-22 常熟市发东塑业有限公司 Antibacterial halogen-free flame retardant nylon alloy material
CN102675866A (en) * 2012-05-22 2012-09-19 苏州新区华士达工程塑胶有限公司 Formula of enhanced flame retardant nylon 6
CN103013030A (en) * 2012-12-06 2013-04-03 上海日之升新技术发展有限公司 Flame-retardant glass fiber-reinforced ABS/PA6/PA66 alloy material with high CTI value and high GWIT value

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1569931A (en) * 2004-04-26 2005-01-26 东莞市正昱塑胶五金有限公司 Fiber reinforced thermolplastic plastic preparation method
CN101070426A (en) * 2007-06-12 2007-11-14 巨石集团有限公司 Glass-fiber reinforced fire-retardant polyamide resin composition
CN102643541A (en) * 2012-04-27 2012-08-22 常熟市发东塑业有限公司 Antibacterial halogen-free flame retardant nylon alloy material
CN102675866A (en) * 2012-05-22 2012-09-19 苏州新区华士达工程塑胶有限公司 Formula of enhanced flame retardant nylon 6
CN103013030A (en) * 2012-12-06 2013-04-03 上海日之升新技术发展有限公司 Flame-retardant glass fiber-reinforced ABS/PA6/PA66 alloy material with high CTI value and high GWIT value

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104774457A (en) * 2015-04-21 2015-07-15 广东顺德顺炎新材料有限公司 High-impact environment-friendly halogen-free flame-retardant reinforced nylon material, and preparation method and application thereof

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Application publication date: 20130717