CN106147187B - A kind of high glaze halogen-free flame retardant PC material and preparation method thereof - Google Patents
A kind of high glaze halogen-free flame retardant PC material and preparation method thereof Download PDFInfo
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- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C08L2310/00—Masterbatches
Abstract
The invention discloses a kind of high glaze halogen-free flame retardant PC material and preparation method thereof, which is prepared by the raw material of following mass percentage：PC resin：91~97.1%；Toughener：1~5%；Halogen-free flame retardants：0.1~0.4%；Anti-dripping agent：0.5~1%；Primary antioxidant：0.1~0.3%；Auxiliary antioxidant：0.1~0.3%；Black masterbatch：1~1.5%；Lubricant：0.1~0.5%.Its preparation method comprises the following steps：1）PC resin is dried；2）Each raw material is sufficiently mixed uniformly by proportioning；3）By step 2）Material add in double screw extruder in, extruding pelletization obtains high glaze halogen-free flame retardant PC material.The high glaze halogen-free flame retardant PC Flame Retardancy of the present invention can excellent, good combination property, can be widely used for the thin-wall parts such as electronic apparatus shell, the surface of thin-walled parts high glaze of preparation, without point；The preparation method of the present invention is simple, and technological operation is easily achieved, and production cost is low, is easy to industrialized production.
Description
Technical field
The present invention relates to a kind of high glaze halogen-free flame retardant PC materials and preparation method thereof, belong to high polymer material technology neck
Domain.
Background technology
PC (makrolon) is a kind of thermoplastic engineering plastic of excellent combination property, weather resistance, shock resistance
Excellent with electrical insulation capability, light transmittance is high, is widely used in the products such as electronic apparatus shell.
PC itself has certain anti-flammability, but fire-retardant rank is relatively low, is only UL94V2 grades.At present, often by adding phosphorus
The halogen-free flame retardants such as flame retardant, sulfonate flame retardant improve the flame retardant property of PC materials, but all there are it is apparent the defects of.
Phosphorus flame retardant can seriously reduce the heat resistance of PC materials；Although sulfonate flame retardant has the additive amount few, efficient etc. excellent
Point, but it can not meet the flame-retardancy requirements of some particular products such as thin wall parts when being used alone.
The fire-retardant rank of PC thin wall parts is generally all difficult to reach UL94V0 grades, main cause be material in combustion
Molten drop drippage is easily generated, usually to achieve the purpose that inhibit drippage, currently used anti-dripping melt by adding in anti-dripping agent
Agent is the pure powder of high molecular weight polytetrafluoroethyldispersions or the polytetrafluoroethylene (PTFE) by acrylonitritrile-styrene resin cladding, due to poly- four
Vinyl fluoride molecular weight is high, and PC material melt viscosities are high, although can improve polytetrafluoro by optimized production process in process
The dispersiveness of ethylene, but still can exist and disperse undesirable situation, in the black product of shaping bloom minute surface with regard to fiber crops can be clearly visible
Point, influences appearance.
Therefore, it is a kind of available for the high glaze halogen-free flame retardant PC material of thin-wall part, article surface without point there is an urgent need for developing.
The content of the invention
It is an object of the invention to provide a kind of high glaze halogen-free flame retardant PC materials and preparation method thereof.
The technical solution used in the present invention is：
A kind of high glaze halogen-free flame retardant PC material, is prepared by the raw material of following mass percentage：
PC resin：91~97.1%；
Toughener：1~5%；
Halogen-free flame retardants：0.1~0.4%；
Anti-dripping agent：0.5~1%；
Primary antioxidant：0.1~0.3%；
Auxiliary antioxidant：0.1~0.3%；
Black masterbatch：1~1.5%；
Lubricant：0.1~0.5%.
The melt index of the PC resin is 18~30g/10min.
The toughener is acrylonitrile-butadiene-styrene copolymer, methyl methacrylate-propylene of nucleocapsid structure
Acid ester copolymer, methacrylate butadi ene styrene copolymer, nucleocapsid structure acrylic acid esters co-polymer in extremely
Few one kind.
The halogen-free flame retardants is organic sesqui siloxane resin.
The anti-dripping agent is organosiloxane type anti-dripping agent.
The primary antioxidant is at least one of Hinered phenols antioxidant, aromatic amine antioxidant.
The auxiliary antioxidant is at least one of phosphite ester kind antioxidant, sulphur ester antioxidant.
The black masterbatch is PC carrier black masterbatch.
The lubricant is stearate, stearic acid, ethylene bis stearamide, polyethylene wax, calcium stearate, stearic acid
At least one of zinc, silicone powder.
The preparation method of above-mentioned high glaze halogen-free flame retardant PC material, comprises the following steps：
1) PC resin is dried；
2) by PC resin, toughener, halogen-free flame retardants, anti-dripping agent, primary antioxidant, auxiliary antioxidant, black masterbatch and profit
Lubrication prescription is sufficiently mixed uniformly by proportioning；
3) material of step 2) is added in double screw extruder, extruding pelletization obtains high glaze halogen-free flame retardant PC material.
The beneficial effects of the invention are as follows：
1) halogen-free flame retardants of the present invention is organic sesqui siloxane, and the fast rapid-result charcoal slagging of energy can effectively inhibit
The molten drop drippage of PC materials in combustion；
2) anti-dripping agent of the present invention is organosiloxane type, and good fluidity is easily scattered, in Plastics Combustion process
It is middle can accelerate PC into charcoal rate, play the role of surface " skinning protection ", so as to achieve the effect that anti-dripping melt；
3) high glaze halogen-free flame retardant PC Flame Retardancy of the invention can be excellent, and good combination property can be widely used for electronics
The thin-wall parts such as electric appliance casing, the surface of thin-walled parts high glaze of preparation, without point；
4) preparation method of the invention is simple, and technological operation is easily achieved, and production cost is low, is easy to industrialized production.
Specific embodiment
A kind of high glaze halogen-free flame retardant PC material, is prepared by the raw material of following mass percentage：
PC resin：91~97.1%；
Toughener：1~5%；
Halogen-free flame retardants：0.1~0.4%；
Anti-dripping agent：0.5~1%；
Primary antioxidant：0.1~0.3%；
Auxiliary antioxidant：0.1~0.3%；
Black masterbatch：1~1.5%；
Lubricant：0.1~0.5%.
Preferably, the melt index of the PC resin is 18~30g/10min.
It is further preferred that the PC resin is the SC-1220R of South Korea's Samsung, the L-1225L of Japanese Supreme Being people, Japan three
At least one of H-3000R of water chestnut.
Preferably, the toughener is acrylonitrile-butadiene-styrene copolymer, the methyl methacrylate of nucleocapsid structure
Ester-acrylate copolymer, methacrylate butadi ene styrene copolymer, the acrylic ester copolymerization of nucleocapsid structure
At least one of object.
It is further preferred that the toughener is the M511 of Japan Zhong Yuan, the M711 of Japan Zhong Yuan, Dupont
At least one of EMA1125AC.
Preferably, the halogen-free flame retardants is organic sesqui siloxane resin.
It is further preferred that the halogen-free flame retardants is the FR-600 of Shan De new materials Co., Ltd of Foshan City.
Preferably, the anti-dripping agent is organosiloxane type anti-dripping agent.
It is further preferred that the anti-dripping agent is the FR-ST200 of Guangdong Quan Sheng Chemical Co., Ltd.s.
Preferably, the primary antioxidant is at least one of Hinered phenols antioxidant, aromatic amine antioxidant.
It is further preferred that the primary antioxidant is antioxidant 1010, antioxidant 1076, antioxidant MD-697, antioxidant
1098th, at least one of antioxidant 264.
Preferably, the auxiliary antioxidant is at least one of phosphite ester kind antioxidant, sulphur ester antioxidant.
It is further preferred that the auxiliary antioxidant is irgasfos 168, antioxidant 626, antioxidant 618, antioxidant 412S
At least one of.
Preferably, the black masterbatch is PC carrier black masterbatch.
It is further preferred that the PC carriers black masterbatch is the 5523 of Shan De new materials Co., Ltd of Foshan City.
Preferably, the lubricant for stearate, stearic acid, ethylene bis stearamide, polyethylene wax, calcium stearate,
At least one of zinc stearate, silicone powder.
It is further preferred that the lubricant is stearate.
Still further preferably, the lubricant is the husky Glycolube PETS of U.S. dragon.
The preparation method of above-mentioned high glaze halogen-free flame retardant PC material, comprises the following steps：
1) PC resin is dried；
2) by PC resin, toughener, halogen-free flame retardants, anti-dripping agent, primary antioxidant, auxiliary antioxidant, black masterbatch and profit
Lubrication prescription is sufficiently mixed uniformly by proportioning；
3) material of step 2) is added in double screw extruder, extruding pelletization obtains high glaze halogen-free flame retardant PC material.
Preferably, each area's processing temperature of the step 3) double screw extruder is 250~260 DEG C, screw speed 250
~300rpm.
The present invention is made further explanation and description with reference to specific embodiment.
Embodiment 1：
A kind of preparation method of high glaze halogen-free flame retardant PC material includes the following steps：
1) PC resin SC-1220R at 120 DEG C is dried into 4h, the moisture content of PC resin is made to be less than 0.02%；
2) Halogen of the PC resin SC-1220R of 96.5 mass parts, the toughener M711 of 1 mass parts, 0.2 mass parts is hindered
Fire agent FR-600, the anti-dripping agent FR-ST200 of 0.5 mass parts, the primary antioxidant 1076 of 0.2 mass parts, 0.3 mass parts it is auxiliary
Aid anti-oxidants 168,1 mass parts 5523 and 0.3 mass parts of black masterbatch lubricant PETS add in high mixer in, mixing 3~
4min；
3) material of step 2) being added in double screw extruder, extruding pelletization obtains high glaze halogen-free flame retardant PC material,
Wherein, each area's processing temperature of double screw extruder is 260 DEG C, and screw rod revolution is 300rpm.
Embodiment 2：
A kind of preparation method of high glaze halogen-free flame retardant PC material includes the following steps：
1) PC resin H-3000R at 120 DEG C is dried into 4h, the moisture content of PC resin is made to be less than 0.02%；
2) by the PC resin H-3000R of 94.4 mass parts, the toughener 1125AC of 2.5 mass parts, 0.4 mass parts Halogen
Fire retardant FR -600, the anti-dripping agent FR-ST200 of 0.7 mass parts, the primary antioxidants 1098 of 0.2 mass parts, 0.2 mass parts
Auxiliary antioxidant 626,1.2 mass parts 5523 and 0.4 mass parts of black masterbatch lubricant PETS add in high mixer in, mixing 3
~4min；
3) material of step 2) being added in double screw extruder, extruding pelletization obtains high glaze halogen-free flame retardant PC material,
Wherein, each area's processing temperature of double screw extruder is 250 DEG C, and screw rod revolution is 300rpm.
Embodiment 3：
A kind of preparation method of high glaze halogen-free flame retardant PC material includes the following steps：
1) PC resin L-1225L at 120 DEG C is dried into 4h, the moisture content of PC resin is made to be less than 0.02%；
2) Halogen of the PC resin L-1225L of 94.1 mass parts, the toughener M711 of 2.5 mass parts, 0.1 mass parts is hindered
Fire agent FR-600, the anti-dripping agent FR-ST200 of 1 mass parts, the primary antioxidant 1010 of 0.3 mass parts, the auxiliary of 0.3 mass parts
Irgasfos 168,1.5 mass parts 5523 and 0.2 mass parts of black masterbatch lubricant PETS add in high mixer in, mixing 3~
4min；
3) material of step 2) being added in double screw extruder, extruding pelletization obtains high glaze halogen-free flame retardant PC material,
Wherein, each area's processing temperature of double screw extruder is 260 DEG C, and screw rod revolution is 250rpm.
Embodiment 4：
A kind of preparation method of high glaze halogen-free flame retardant PC material includes the following steps：
1) PC resin SC-1220R at 120 DEG C is dried into 4h, the moisture content of PC resin is made to be less than 0.02%；
2) Halogen of the PC resin SC-1220R of 91.8 mass parts, the toughener M511 of 5 mass parts, 0.4 mass parts is hindered
Fire agent FR-600, the anti-dripping agent FR-ST200 of 0.5 mass parts, the primary antioxidant 1076 of 0.2 mass parts, 0.3 mass parts it is auxiliary
Aid anti-oxidants 618,1.5 mass parts 5523 and 0.3 mass parts of black masterbatch lubricant PETS add in high mixer in, mixing 3~
4min；
3) material of step 2) being added in double screw extruder, extruding pelletization obtains high glaze halogen-free flame retardant PC material,
Wherein, each area's processing temperature of double screw extruder is 260 DEG C, and screw rod revolution is 300rpm.
Comparative example 1：
A kind of preparation method of common halogen-free flame retardant PC material includes the following steps：
1) PC resin SC-1220R at 120 DEG C is dried into 4h, the moisture content of PC resin is made to be less than 0.02%；
2) by the PC resin SC-1220R of 91.8 mass parts, the toughener M711 of 5 mass parts, 0.4 mass parts the U.S.
Sulfonate halogen-free flame retardants KSS F-535 of Arichem companies, the anti-dripping agent FR-ST200 of 0.5 mass parts, 0.2 mass parts
Primary antioxidant 1076, the auxiliary antioxidants 168 of 0.3 mass parts, 1.5 mass parts 5523 and 0.3 mass parts of black masterbatch profit
Lubrication prescription PETS is added in high mixer, mixes 3~4min；
3) material of step 2) being added in double screw extruder, extruding pelletization obtains halogen-free flame retardant PC material, wherein,
Each area's processing temperature of double screw extruder is 260 DEG C, and screw rod revolution is 300rpm.
Comparative example 2：
A kind of preparation method of common halogen-free flame retardant PC material includes the following steps：
1) PC resin SC-1220R at 120 DEG C is dried into 4h, the moisture content of PC resin is made to be less than 0.02%；
2) Halogen of the PC resin SC-1220R of 96.5 mass parts, the toughener M711 of 1 mass parts, 0.2 mass parts is hindered
Fire agent FR-600,1 mass parts Daikin company anti-dripping agent M532 (the pure powder of PTFE), the primary antioxidant of 0.2 mass parts
1076th, the auxiliary antioxidant 168 of 0.3 mass parts, the lubricant PETS of 5523 and 0.3 mass parts of black masterbatch of 0.5 mass parts add
Enter in high mixer, mix 3~4min；
3) material of step 2) being added in double screw extruder, extruding pelletization obtains halogen-free flame retardant PC material, wherein,
Each area's processing temperature of double screw extruder is 260 DEG C, and screw rod revolution is 300rpm.
Comparative example 3：
A kind of preparation method of common halogen-free flame retardant PC material includes the following steps：
1) PC resin SC-1220R at 120 DEG C is dried into 4h, the moisture content of PC resin is made to be less than 0.02%；
2) Halogen of the PC resin SC-1220R of 96.5 mass parts, the toughener M711 of 1 mass parts, 0.2 mass parts is hindered
Fire agent FR-600, the anti-dripping agent SA50 (AS coats PTFE) of Shan De new materials Co., Ltd of Foshan City of 1 mass parts, 0.2 matter
Measure the primary antioxidant 1076 of part, the auxiliary antioxidant 168 of 0.3 mass parts, 5523 and 0.3 mass parts of black masterbatch of 0.5 mass parts
Lubricant PETS add in high mixer in, mix 3~4min；
3) material of step 2) being added in double screw extruder, extruding pelletization obtains halogen-free flame retardant PC material, wherein,
Each area's processing temperature of double screw extruder is 260 DEG C, and screw rod revolution is 300rpm.
Test case：
By Examples 1 to 4 and halogen-free flame retardant PC material injection prepared by comparative example 1~3 into standard testing batten and diameter
The bloom minute surface disk of 10cm is simultaneously tested for the property, and test result is as shown in table 1.
Molding technological condition：Nozzle temperature is 260 DEG C, and each area's temperature is 255 DEG C, 265 DEG C, 260 DEG C, the dwell time 6~
10s, injection pressure 40MPa~60MPa.
The test method of properties is as follows：
Melt index：It is tested according to ASTM D1238 standards；
Lzod notch impact strengths：It is tested according to ASTM D256 standards；
Anti-flammability：It is tested according to UL94 standards.
The performance test data of the halogen-free flame retardant PC material of 1 Examples 1 to 4 of table and comparative example 1~3
As shown in Table 1：High glaze halogen-free flame retardant PC Flame Retardancy prepared by the present invention can be good, and impact resistance is excellent,
Its article surface glossiness is high, and surface is without point.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. a kind of high glaze halogen-free flame retardant PC material, it is characterised in that：It is prepared by the raw material of following mass percentage：
PC resin：91~97.1%；
Toughener：1~5%；
Halogen-free flame retardants：0.1~0.4%；
Anti-dripping agent：0.5~1%；
Primary antioxidant：0.1~0.3%；
Auxiliary antioxidant：0.1~0.3%；
Black masterbatch：1~1.5%；
Lubricant：0.1~0.5%；
The halogen-free flame retardants is organic sesqui siloxane resin；
The anti-dripping agent is organosiloxane type anti-dripping agent.
2. high glaze halogen-free flame retardant PC material according to claim 1, it is characterised in that：The melt index of the PC resin
For 18~30g/10min.
3. high glaze halogen-free flame retardant PC material according to claim 1, it is characterised in that：The toughener for acrylonitrile-
Butadiene-styrene copolymer, methacrylate butadi ene styrene copolymer, the esters of acrylic acid of nucleocapsid structure are total to
At least one of polymers.
4. high glaze halogen-free flame retardant PC material according to claim 1, it is characterised in that：The primary antioxidant is hindered phenol
At least one of kind antioxidant, aromatic amine antioxidant.
5. high glaze halogen-free flame retardant PC material according to claim 1, it is characterised in that：The auxiliary antioxidant is phosphorous
At least one of acid esters kind antioxidant, sulphur ester antioxidant.
6. high glaze halogen-free flame retardant PC material according to claim 1, it is characterised in that：The black masterbatch is black for PC carriers
Color masterbatch.
7. high glaze halogen-free flame retardant PC material according to claim 1, it is characterised in that：The lubricant is stearic acid
At least one of ester, stearic acid, ethylene bis stearamide, polyethylene wax, calcium stearate, zinc stearate, silicone powder.
8. the preparation method of the high glaze halogen-free flame retardant PC material in claim 1~7 described in any one, it is characterised in that：
Comprise the following steps：
1）PC resin is dried；
2）By PC resin, toughener, halogen-free flame retardants, anti-dripping agent, primary antioxidant, auxiliary antioxidant, black masterbatch and lubricant
It is sufficiently mixed uniformly by proportioning；
3）By step 2）Material add in double screw extruder in, extruding pelletization obtains high glaze halogen-free flame retardant PC material.
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7405251B2 (en) * | 2002-05-16 | 2008-07-29 | Dow Corning Corporation | Flame retardant compositions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971149A (en) * | 2019-03-22 | 2019-07-05 | 广东聚石化学股份有限公司 | A kind of halogen-free flame retardant PC material of resistance to long term heat ageing and preparation method thereof |
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