CN103205109A - Preparation method of black flame resistant polyamide composite material reinforced by glass fibers - Google Patents
Preparation method of black flame resistant polyamide composite material reinforced by glass fibers Download PDFInfo
- Publication number
- CN103205109A CN103205109A CN2013101326615A CN201310132661A CN103205109A CN 103205109 A CN103205109 A CN 103205109A CN 2013101326615 A CN2013101326615 A CN 2013101326615A CN 201310132661 A CN201310132661 A CN 201310132661A CN 103205109 A CN103205109 A CN 103205109A
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- parts
- flame retardant
- fibre reinforced
- glass fibre
- black
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means 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
- B29C48/40—Means 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
Abstract
The invention discloses a preparation method of a black flame resistant polyamide composite material reinforced by glass fibers, and belongs to the technical field of high molecular material preparation. The preparation method comprises: throwing 50-57 parts of polyamide 6 resin, 6-11 parts of polypropylene resin, 5-8 parts of bulking agent, 13-21 parts of fire retardant, 6-11 parts of stuffing, 0.4-0.9 parts of antioxidant, 3-5 parts of milled glass fibers, 22-28 parts of reinforced fibers and 2-3.2 parts of carbon black into a high speed mixer, mixing the materials for 6 minutes, wherein the rotating speed of the high speed mixer is 650 n/min; throwing, smelting and extruding the mixed materials in a parallel double-screw extruder, and pelleting to obtain finished products, wherein the temperatures of the first region to the twelfth region of the double-screw extruder are as follows: the temperature of the first region is 210 DEG C, the temperature of the second region is 220 DEG C, the temperature of the third region is 230 DEG C, the temperature of the fourth region is 235 DEG C, and the temperatures of the fifth region to the twelfth region are 240 DEG C. The composite material has the following performance indexes: the tensile strength is larger than 110-120 MPa, the bending strength is larger than 190-220 MPa, the impact strength of a cantilever beam notch is larger than 8-11 kj/m<2>, and the fire resistance reaches to V-0(UL-94-1.5 mm).
Description
Technical field
The invention belongs to field of polymer material preparing technology, be specifically related to a kind of preparation method of glass fibre reinforced flame retardant polyamide compoiste material of black.
Background technology
Polymeric amide is the world wide production maximum, the engineering plastics that range of application is the widest.At present, fire has an accident often, and the reason that much causes fire all is because decoration, material of construction, plastic material fire-retardant causing not causes to result in greater loss.Therefore, the flame retardant resistance to material requires harsh gradually.The present invention takes into account the problem of improving flame retardant resistance when exploring the preparation high performance material.
Summary of the invention
Task of the present invention is the preparation method that a kind of glass fibre reinforced flame retardant polyamide compoiste material of black will be provided, and the polyamide compoiste material that is obtained by this method has excellent fire retardant effect and intensity.
Task of the present invention is finished like this, a kind of preparation method of glass fibre reinforced flame retardant polyamide compoiste material of black, it is to mix 6min in 3 ~ 5 parts of 0.4 ~ 0.9 part in 6 ~ 11 parts of 13 ~ 21 parts of 5 ~ 8 parts of 6~11 parts of 50~57 parts of polyamide 6 resins, acrylic resins, expanding materials, fire retardants, fillers, oxidation inhibitor, the milled glass fibers that will take by weighing by weight earlier and 22 ~ 28 parts of fortifying fibres and 2 ~ 3.2 parts of input high-speed mixers of carbon black, the rotating speed of high-speed mixer is 650n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after granulation, obtain the glass fibre reinforced flame retardant polyamide compoiste material of black, wherein: a district of twin screw extruder to the temperature of No.12 District is respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, five districts to No.12 District is 240 ℃.
In one embodiment of the invention, described polyamide 6 resin be fusing point more than 210 ℃, the limiting viscosity index is 2.3 polycaprolactam polyimide resin.
In another embodiment of the present invention, described acrylic resin is Co-polypropylene, and molten finger is 2~3g/10min, 170 ℃ of fusing points.
In yet another embodiment of the present invention, described expanding material is the polypropylene of maleic anhydride graft, and percentage of grafting is 0.6%.
In another embodiment of the present invention, described fire retardant is TDE.
Also have among the embodiment of the present invention, described filler is magnesium hydroxide, and particle diameter is more than 7000 orders.
More of the present invention and among embodiment, described oxidation inhibitor is the two diphosphites of two (2,4-di-tert-butyl-phenyl) tetramethylolmethanes.
In of the present invention and then embodiment, the particle diameter of described milled glass fiber is 150 microns.
Of the present invention again more and among embodiment, described fortifying fibre refers to the alkali-free short glass fiber of length 3mm.
In again of the present invention and then embodiment, described carbon black is thermally oxidized black.
The glass fibre reinforced flame retardant polyamide compoiste material of the black that the inventive method obtains has following performance index after tested: tensile strength is greater than 110~120MPa; , flexural strength is greater than 190~220MPa; The socle girder notched Izod impact strength is greater than 8~11kj/m
2Flame retardant resistance reaches V-0 (UL-94-1.5mm).
Embodiment
Embodiment 1:
At first, with the fusing point that takes by weighing by weight more than 210 ℃ and the limiting viscosity index be 53 parts of 2.3 polycaprolactam polyimide resins, molten finger is that 2~3g/10min and fusing point are 170 ℃ 11 parts of Co-polypropylene, maleic anhydride graft and percentage of grafting be 6 parts of 0.6% polypropylene, 21 parts of TDE, particle diameter is 11 parts of the above magnesium hydroxides of 7000 orders, two (2, the 4-di-tert-butyl-phenyl) the two diphosphites of tetramethylolmethane are 0.7 part, particle diameter is 150 microns 3 parts of milled glass fibers, length is in 28 parts of the alkali-free short glass fibers of 3mm and 2 parts of input high-speed mixers of carbon black that channel process is produced and mixes 6min under the speed of 650n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after granulation, obtain the glass fibre reinforced flame retardant polyamide compoiste material of black, wherein: a district of twin screw extruder to the temperature of No.12 District is respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, five districts to No.12 District is 240 ℃.
Embodiment 2:
At first, with the fusing point that takes by weighing by weight more than 210 ℃ and the limiting viscosity index be 50 parts of 2.3 polycaprolactam polyimide resins, molten finger is that 2~3g/10min and fusing point are 170 ℃ 6 parts of Co-polypropylene, maleic anhydride graft and percentage of grafting be 8 parts of 0.6% polypropylene, 13 parts of TDE, particle diameter is 6 parts of the above magnesium hydroxides of 7000 orders, two (2, the 4-di-tert-butyl-phenyl) the two diphosphites of tetramethylolmethane are 0.9 part, particle diameter is 150 microns 4 parts of milled glass fibers, length is in 22 parts of the alkali-free short glass fibers of 3mm and 2.4 parts of input high-speed mixers of carbon black that channel process is produced and mixes 6min under the speed of 650n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after granulation, obtain the glass fibre reinforced flame retardant polyamide compoiste material of black, wherein: a district of twin screw extruder to the temperature of No.12 District is respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, five districts to No.12 District is 240 ℃.
Embodiment 3:
At first, with the fusing point that takes by weighing by weight more than 210 ℃ and the limiting viscosity index be 57 parts of 2.3 polycaprolactam polyimide resins, molten finger is that 2~3g/10min and fusing point are 170 ℃ 8 parts of Co-polypropylene, maleic anhydride graft and percentage of grafting be 5 parts of 0.6% polypropylene, 17 parts of TDE, particle diameter is 9 parts of the above magnesium hydroxides of 7000 orders, two (2, the 4-di-tert-butyl-phenyl) the two diphosphites of tetramethylolmethane are 0.4 part, particle diameter is 150 microns 5 parts of milled glass fibers, length is in 26 parts of the alkali-free short glass fibers of 3mm and 2.8 parts of input high-speed mixers of carbon black that channel process is produced and mixes 6min under the speed of 650n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after granulation, obtain the glass fibre reinforced flame retardant polyamide compoiste material of black, wherein: a district of twin screw extruder to the temperature of No.12 District is respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, five districts to No.12 District is 240 ℃.
Embodiment 4:
At first, with the fusing point that takes by weighing by weight more than 210 ℃ and the limiting viscosity index be 55 parts of 2.3 polycaprolactam polyimide resins, molten finger is that 2~3g/10min and fusing point are 170 ℃ 10 parts of Co-polypropylene, maleic anhydride graft and percentage of grafting be 7 parts of 0.6% polypropylene, 19 parts of TDE, particle diameter is 8 parts of the above magnesium hydroxides of 7000 orders, two (2, the 4-di-tert-butyl-phenyl) the two diphosphites of tetramethylolmethane are 0.6 part, particle diameter is 150 microns 4.5 parts of milled glass fibers, length is in 24 parts of the alkali-free short glass fibers of 3mm and 3.2 parts of input high-speed mixers of carbon black that channel process is produced and mixes 6min under the speed of 650n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after granulation, obtain the glass fibre reinforced flame retardant polyamide compoiste material of black, wherein: a district of twin screw extruder to the temperature of No.12 District is respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, five districts to No.12 District is 240 ℃.
The glass fibre reinforced flame retardant polyamide compoiste material of the black 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 | 110.3 | 112.5 | 116.7 | 119.6 |
Flexural strength MPa | 190.2 | 200.5 | 213.4 | 218.8 |
Socle girder notched Izod impact strength kj/m 2 | 8.2 | 9.5 | 10.2 | 10.8 |
Flame retardant resistance (UL-94-1.5mm) | V-0 | V-0 | V-0 | V-0 |
Claims (10)
1.
A kind of preparation method of glass fibre reinforced flame retardant polyamide compoiste material of black, it is characterized in that it is to mix 6min in 3 ~ 5 parts of 0.4 ~ 0.9 part in 6 ~ 11 parts of 13 ~ 21 parts of 5 ~ 8 parts of 6~11 parts of 50~57 parts of polyamide 6 resins, acrylic resins, expanding materials, fire retardants, fillers, oxidation inhibitor, the milled glass fibers that will take by weighing by weight earlier and 22 ~ 28 parts of fortifying fibres and 2 ~ 3.2 parts of input high-speed mixers of carbon black, the rotating speed of high-speed mixer is 650n/min, obtains compound; Again compound is dropped in the parallel twin screw extruder and melt extrude, after granulation, obtain the glass fibre reinforced flame retardant polyamide compoiste material of black, wherein: a district of twin screw extruder to the temperature of No.12 District is respectively: 210 ℃ in a district, 220 ℃ in two districts, 230 ℃ in three districts, 235 ℃ in four districts, five districts to No.12 District is 240 ℃.
2.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1, it is characterized in that described polyamide 6 resin be fusing point more than 210 ℃, the limiting viscosity index is 2.3 polycaprolactam polyimide resin.
3.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1 is characterized in that described acrylic resin is Co-polypropylene, and molten finger is 2~3g/10min, 170 ℃ of fusing points.
4.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1 is characterized in that described expanding material is the polypropylene of maleic anhydride graft, and percentage of grafting is 0.6%.
5.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1 is characterized in that described fire retardant is TDE.
6.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1 is characterized in that described filler is magnesium hydroxide, and particle diameter is more than 7000 orders.
7.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1 is characterized in that described oxidation inhibitor is the two diphosphites of two (2,4-di-tert-butyl-phenyl) tetramethylolmethanes.
8.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1, the particle diameter that it is characterized in that described milled glass fiber is 150 microns.
9.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1 is characterized in that described fortifying fibre refers to the alkali-free short glass fiber of length 3mm.
10.
The glass fibre reinforced flame retardant polyamide compoiste material of black according to claim 1 is characterized in that described carbon black is thermally oxidized black
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111499973A (en) * | 2020-04-30 | 2020-08-07 | 上海锦湖日丽塑料有限公司 | Conductive carbon fiber resin composition and preparation method thereof |
Citations (4)
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CN101987917A (en) * | 2009-07-30 | 2011-03-23 | 现代自动车株式会社 | Conductive polyamide composite composition and fuel transport tube using the same |
CN102234422A (en) * | 2011-05-06 | 2011-11-09 | 深圳市兴迪塑胶有限公司 | Flame-retardant nylon resin composition and preparation method thereof |
CN102464882A (en) * | 2010-11-18 | 2012-05-23 | 合肥杰事杰新材料股份有限公司 | Material for toilet lid and toilet seat and preparation method thereof |
CN102675865A (en) * | 2012-05-04 | 2012-09-19 | 金发科技股份有限公司 | Polyamide resin composition and preparation method and application thereof |
-
2013
- 2013-04-16 CN CN2013101326615A patent/CN103205109A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101987917A (en) * | 2009-07-30 | 2011-03-23 | 现代自动车株式会社 | Conductive polyamide composite composition and fuel transport tube using the same |
CN102464882A (en) * | 2010-11-18 | 2012-05-23 | 合肥杰事杰新材料股份有限公司 | Material for toilet lid and toilet seat and preparation method thereof |
CN102234422A (en) * | 2011-05-06 | 2011-11-09 | 深圳市兴迪塑胶有限公司 | Flame-retardant nylon resin composition and preparation method thereof |
CN102675865A (en) * | 2012-05-04 | 2012-09-19 | 金发科技股份有限公司 | Polyamide resin composition and preparation method and application thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111499973A (en) * | 2020-04-30 | 2020-08-07 | 上海锦湖日丽塑料有限公司 | Conductive carbon fiber resin composition and preparation method thereof |
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Application publication date: 20130717 |