CN109370190A - A kind of thin wall type high CTI value flame resistant polycarbonate blends and preparation method thereof - Google Patents
A kind of thin wall type high CTI value flame resistant polycarbonate blends and preparation method thereof Download PDFInfo
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- CN109370190A CN109370190A CN201811153383.0A CN201811153383A CN109370190A CN 109370190 A CN109370190 A CN 109370190A CN 201811153383 A CN201811153383 A CN 201811153383A CN 109370190 A CN109370190 A CN 109370190A
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- polycarbonate
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
Abstract
The present invention relates to technical field of alloy material, disclose a kind of thin wall type high CTI value flame resistant polycarbonate blends and preparation method thereof, compared to the prior art, the present invention joined phosphonitrile fire retardant in composition of raw materials, on the one hand, the phosphonitrile fire retardant can effectively overcome the drawbacks of polycarbonate heat distortion temperature and toughness is greatly reduced because adding organophosphate ester flame retardant in the prior art, effectively promote the heat resistance and toughness of polycarbonate compositions；On the other hand, effective phosphorus nitrogen quantity in the phosphonitrile fire retardant has good fire retardation, can effectively promote the flame retardant rating of polycarbonate compositions, and the phosphonitrile fire retardant is also greatly improved the anti creepage trace performance of polycarbonate compositions simultaneously.
Description
Technical field
The present invention relates to technical field of alloy material, especially a kind of thin wall type high CTI value flame resistant polycarbonate blends
And preparation method thereof.
Background technique
Polycarbonate has many advantages, such as compared with high-impact, heat resistance, good dimensional stability, electrical insulation capability,
Thus it is widely used in the fields such as auto parts and components, household electrical appliances, electronic apparatus.Joint of the material surface in electric field and electrolyte
The process that conductive path is gradually formed under effect is known as creepage trace, and CTI value is that a kind of measurement material creepage trace sensibility refers to
Mark shows that material surface is able to take highest of the 50 drop electrolyte without forming tracking under certain voltage conditions
Voltage value.The CTI value of material depends on the generation and accumulation of material surface free carbon, and spark discharge has the aggregation of removal free carbon
With the effect of accumulation, therefore creepage trace process is actually the dynamic equilibrium that free carbon is assembled and removed on the surface of the material
Journey.Point out that nobody sees in the long-term unattended security appliance standard (IEC60335-1) that European Union International Power association IEC is proposed
Pipe electric appliance actual use material must satisfy: UL-94V-0 and CTI value is greater than or equal to 250V.However PC primary resin much reaches not
To this safety standard, thus it need to be modified.In the prior art, in order to which the height for meeting Flame Retardancy and CTI value is wanted
It asks, it will usually aromatic phosphate acid ester flame retardant or Sulfonates fire retardant be added, but the addition of aromatic phosphate acid ester flame retardant is logical
Can often plasticization be generated to PC resin, influence the impact strength and heat resistance of PC resin；And Sulfonates fire retardant adds, though
So the heat resistance of PC resin is made to be maintained, but the thin-wall flame retardance of PC resin will receive limitation, and CTI value is not also high.?
Electronic apparatus shell application field, many occasions, which require plastics, to be had compared with high CTI value, and due to heat release use environment, is also needed
The specific higher heat distortion temperature of material is wanted, but few products that can meet the two requirements simultaneously in the market.
Summary of the invention
The purpose of the present invention is to provide a kind of thin wall type high CTI value flame resistant polycarbonate blends and preparation method thereof,
To meet CTIPLC2 standard and under the thickness of 0.8mm with V0 performance, hence it is evident that improve the heat-resisting of polycarbonate compositions
Property, especially suitable for the occasion for using thin wall type environmental requirement relatively high.
To realize above-mentioned technical purpose and the technique effect, the invention discloses a kind of thin wall type high CTI value is fire-retardant
Polycarbonate Alloys, by weight percentage, polycarbonate compositions include:
Polycarbonate 80-95%,
Organosilicon halogen-free flame retardants 0.05%-0.2%,
Phosphonitrile fire retardant 1-10%,
Anti-dripping agent 0.1-1%,
Other auxiliary agent 3%-10%,
The sum of percentage of each component is 100%,
Wherein polycarbonate Alloys meet 2 standard of CTIPLC and have V0 performance under the thickness of 0.8mm.
Wherein, polycarbonate is aromatic copolycarbonate, fatty poly-ester carbonate, aromatic-aliphatic polycarbonate, branch
Change at least one of polycarbonate.
Preferably, polycarbonate is the aromatic copolycarbonate that viscosity average molecular weigh is 13000-40000.
Wherein, organosilicon halogen-free flame retardants be random silsesquioxane, trapezoidal half siloxane, bridge type silsesquioxane and
One or more of cage-type silsesquioxane mixing compounding.
Preferably, the end group of organosilicon halogen-free flame retardants is that amino, alkoxy, methyl, phenyl are one such or two
Kind or two or more compositions, main structure are straight chain type or branch.
Preferably, cage model sesquialter organosiloxane is poly- (trimethylsiloxy group) silsesquioxane of cage modle eight, unfilled corner phenyl
Cage-type silsesquioxane, cage modle aminopropyl silsesquioxane, epoxy cage type sesquialter siloxane and vinyl ladder type silsesquioxane
One or more of alkane mixing compounding.
Wherein, phosphonitrile fire retardant has a structure that
,
Repetitive unit n is the integer of 3-25, and R1 group and R2 group are identical or different, represents unsubstituted phenyl or at least
The phenyl that the alkyl or allyl of a kind of 1-6 carbon atom replace.
Wherein, anti-dripping agent is the polymer comprising vinyl fluoride structure.
Wherein, other auxiliary agents are self toughening agent, in heat stabilizer, antioxidant, light stabilizer, plasticizer, filler, colorant
At least one.
The invention also discloses a kind of preparation method of thin wall type high CTI value flame resistant polycarbonate blends, use is above-mentioned
Any polycarbonate Alloys preparation, comprising the following steps:
Polycarbonate, the halogen-free flame retardants of formula ratio, phosphonitrile fire retardant, other auxiliary agents are first weighed, and is all put into mixing machine
It is blended, is put into again in double screw extruder after mixing and carry out melting mixing extruding pelletization to get the high CTI value is arrived
High-fire resistance polycarbonate compositions；Wherein, the screw diameter of the double screw extruder is 36-40:1, each section of barrel temperature
It is set as 230-260 DEG C, screw speed 400-500rpm.
The invention has the following advantages:
Compared to the prior art, the present invention joined phosphonitrile fire retardant in composition of raw materials, on the one hand, the phosphonitrile fire retardant can
Effectively overcome and polycarbonate heat distortion temperature and toughness is greatly reduced because adding organophosphate ester flame retardant in the prior art
Drawback effectively promotes the heat resistance and toughness of polycarbonate compositions；On the other hand, effective phosphorus nitrogen in the phosphonitrile fire retardant
Amount has good fire retardation, can effectively promote the flame retardant rating of polycarbonate compositions, and the phosphonitrile fire retardant simultaneously
Also it is greatly improved the anti creepage trace performance of polycarbonate compositions.
In addition to this, which also has fabulous compatibility with polycarbonate, will not have plasticising to make to alloy
With can be in the case where not influencing polycarbonate compositions flame retardant rating, toughness, hence it is evident that improve the resistance to of polycarbonate compositions
It is hot, relatively high occasion is required especially suitable for use environment.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.
Embodiment 1
The invention discloses a kind of thin wall type high CTI value flame resistant polycarbonate blends and preparation method thereof, by weight percentage
Meter, polycarbonate compositions include:
Polycarbonate 80-95%, organosilicon halogen-free flame retardants 0.05%-0.2%, phosphonitrile fire retardant 1-10%, anti-dripping agent 0.1-1%,
The sum of other auxiliary agent 3%-10%, percentage of each component are 100%,
Wherein polycarbonate Alloys meet 2 standard of CTIPLC and have V0 performance under the thickness of 0.8mm.
Polycarbonate is that aromatic copolycarbonate, fatty poly-ester carbonate, aromatic-aliphatic polycarbonate, branching are poly-
At least one of carbonic ester.
Organosilicon halogen-free flame retardants is random silsesquioxane, trapezoidal half siloxane, bridge type silsesquioxane and cage modle
One or more of silsesquioxane mixing compounding.The end group of organosilicon halogen-free flame retardants is amino, alkoxy, methyl, benzene
Base it is one such two kinds or it is two or more constitute, main structure be straight chain type or branch.
Phosphonitrile fire retardant has a structure that
,
Repetitive unit n is the integer of 3-25, and R1 group and R2 group are identical or different, represents unsubstituted phenyl or at least
The phenyl that the alkyl or allyl of a kind of 1-6 carbon atom replace.
Anti-dripping agent is the polymer comprising vinyl fluoride structure.
Other auxiliary agents be self toughening agent, heat stabilizer, antioxidant, light stabilizer, plasticizer, filler, in colorant extremely
Few one kind.
The invention also discloses a kind of preparation method of thin wall type high CTI value flame resistant polycarbonate blends, use is above-mentioned
Any polycarbonate Alloys preparation, comprising the following steps:
Polycarbonate, the halogen-free flame retardants of formula ratio, phosphonitrile fire retardant, other auxiliary agents are first weighed, and is all put into mixing machine
It is blended, is put into again in double screw extruder after mixing and carry out melting mixing extruding pelletization to get the high CTI value is arrived
High-fire resistance polycarbonate compositions；Wherein, the screw diameter of the double screw extruder is 36-40:1, each section of barrel temperature
It is set as 230-260 DEG C, screw speed 400-500rpm.
Embodiment 2
The present embodiment discloses a kind of thin wall type high CTI value flame resistant polycarbonate blends and its preparation based on embodiment 1
Method, by weight percentage, polycarbonate compositions include:
Polycarbonate 80%, organosilicon halogen-free flame retardants 0.05%, phosphonitrile fire retardant 10%, anti-dripping agent 1%, other auxiliary agents 8.95%,
The sum of percentage of each component is 100%.
Wherein, polycarbonate is fatty poly-ester carbonate, and organosilicon halogen-free flame retardants is random silsesquioxane, phosphonitrile resistance
Fire agent:
,
Repetitive unit n is the integer of 3-25, and R1 group is identical with R2 group, represents unsubstituted phenyl, anti-dripping agent for containing
The polymer of vinyl fluoride structure, other auxiliary agents include: self toughening agent 2%, heat stabilizer 3.55% and antioxidant 3.4%.
Embodiment 3
The present embodiment discloses a kind of thin wall type high CTI value flame resistant polycarbonate blends and its preparation based on embodiment 1
Method, by weight percentage, polycarbonate compositions include:
Polycarbonate 85%, organosilicon halogen-free flame retardants 0.1%, phosphonitrile fire retardant 8%, anti-dripping agent 0.5%, other auxiliary agents 6.4%,
The sum of percentage of each component is 100%.
Wherein, polycarbonate is aromatic copolycarbonate, and organosilicon halogen-free flame retardants is trapezoidal half siloxane, phosphonitrile resistance
Fire agent are as follows:
,
Repetitive unit n is the integer of 3-25, and R1 group is identical as R2 group, represents the alkane for containing at least one 1-6 carbon atom
The phenyl that base replaces, anti-dripping agent are the polymer of fluorine-containing ethylene unit, other auxiliary agents include: light stabilizer 3.2%, plasticizer
3.2%。
Embodiment 4
The present embodiment discloses a kind of thin wall type high CTI value flame resistant polycarbonate blends and its preparation based on embodiment 1
Method, by weight percentage, polycarbonate compositions include:
Polycarbonate 90%, organosilicon halogen-free flame retardants 0.15%, phosphonitrile fire retardant 5%, anti-dripping agent 0.3%, other auxiliary agents
4.55%, the sum of percentage of each component is 100%.
Wherein, polycarbonate is aromatic-aliphatic polycarbonate, and organosilicon halogen-free flame retardants is bridge type silsesquioxane
Alkane, phosphonitrile fire retardant are as follows:
,
Repetitive unit n be 3-25 integer, R1 group and R2 group be not identical, represent containing at least one of allyl substitution
Phenyl, anti-dripping agent be fluorine-containing ethylene unit polymer, other auxiliary agents include: filler 2%, colorant 2.55%.
Embodiment 5
The present embodiment discloses a kind of thin wall type high CTI value flame resistant polycarbonate blends and its preparation based on embodiment 1
Method, by weight percentage, polycarbonate compositions include:
It is polycarbonate 95%, organosilicon halogen-free flame retardants 0.2%, phosphonitrile fire retardant 1%, anti-dripping agent 0.1%, other auxiliary agents 4%, each
The sum of percentage of component is 100%.
Wherein, polycarbonate is branching polycarbonate, and organosilicon halogen-free flame retardants is cage-type silsesquioxane, and phosphonitrile is fire-retardant
Agent are as follows:
,
Repetitive unit n be 3-25 integer, R1 group is identical with R2 group, represent containing at least one of allyl substitution
Phenyl, anti-dripping agent are the polymer of fluorine-containing ethylene unit, other auxiliary agents include: heat stabilizer 2%, light stabilizer 2%.
Embodiment 6
The present embodiment carries out following properties of product characterization using embodiment 2-5 as experimental subjects, for product is obtained prepared by the present invention:
Melt mass flow rate, measurement standard: the melt mass flow of ISO 1133-1-2011 plastics measurement thermoplastic
Rate (MFR) and melt volume flow rate (MVR) part 1；
Heat distortion temperature, measurement standard: the measurement part 1 of ISO 75-1-2013 plastics load deformation temperature；
Rubber-plastics material flammability test, measurement standard: UL-94；
Comparative tracking index, measurement standard: IEC 60112-2009 solid insulating material is let out trace relatively in humid conditions and is referred to
The several and resistance to recommendation measuring method for letting out trace index.
In order to preferably compare the performance of product obtained by the present invention, comparative example 1-4 is constructed as comparison object, and control pair
Material used by polycarbonate used by ratio 1-4, phosphonitrile fire retardant, anti-dripping agent and other auxiliary agents and embodiment 2-5,
Proportion is consistent, and only changing organosilicon halogen-free flame retardants is sulfonate salt flame, equally carries out above-mentioned experiment and control experiment results.
The 1 experimental result table of comparisons of table
| Project | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Melt mass flow rate | 12 | 11 | 11 | 10 | 11 | 11 | 12 | 12 |
| Heat distortion temperature | 125 | 124 | 123 | 122 | 121 | 125 | 124 | 123 |
| UL-94/3.2mm | V-O | V-O | V-O | V-O | V-O | V-O | V-O | V-O |
| UL-94/1.6mm | V-O | V-O | V-O | V-O | V-O | V-O | V-O | V-O |
| UL-94/0.8mm | NV | V-2 | V-2 | V-0 | V-0 | Failure | V-O | V-O |
| Comparative tracking index | Failure | Failure | Failure | Pass through | Pass through | Failure | Failure | Failure |
Note: UL-94/3.2mm is test sample thickness 3.2mm, other parameters.
In embodiment, phosphorus content is relatively high in the phosphonitrile homopolymer, has good fire retardation, can effectively be promoted
The flame retardant rating of polycarbonate compositions, while the phosphonitrile fire retardant is also greatly improved the resistance to electric leakage of polycarbonate compositions
Trace performance.In addition to this, which also has fabulous compatibility with polycarbonate, will not have plasticising to make to alloy
With can be in the case where not influencing polycarbonate compositions flame retardant rating, toughness, hence it is evident that improve the resistance to of polycarbonate compositions
It is hot, relatively high occasion is required especially suitable for use environment.
The poly- carbonic acid vinegar composition product of thin-walled high CTI value high heat resistance obtained by the present invention can be widely applied to such as frequency conversion
Device, a part of kitchen appliance or electrical shell, automobile component, the shell of building field or lid and electrical appliance
Shell and frame etc.；It has a vast market foreground and market efficiency.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of thin wall type high CTI value flame resistant polycarbonate blends, it is characterised in that: by weight percentage, described is poly-
Carbonate composition includes:
Polycarbonate 80-95%,
Organosilicon halogen-free flame retardants 0.05%-0.2%,
Phosphonitrile fire retardant 1-10%,
Anti-dripping agent 0.1-1%,
Other auxiliary agent 3%-10%,
The sum of percentage of each component is 100%,
Wherein the polycarbonate Alloys meet 2 standard of CTIPLC and have V0 performance under the thickness of 0.8mm.
2. a kind of thin wall type high CTI value flame resistant polycarbonate blends as described in claim 1, it is characterised in that: described
Polycarbonate is aromatic copolycarbonate, in fatty poly-ester carbonate, aromatic-aliphatic polycarbonate, branching polycarbonate
At least one.
3. a kind of thin wall type high CTI value flame resistant polycarbonate blends as claimed in claim 2, it is characterised in that: described
Polycarbonate is the aromatic copolycarbonate that viscosity average molecular weigh is 13000-40000.
4. a kind of thin wall type high CTI value flame resistant polycarbonate blends as described in claim 1, it is characterised in that: described
Organosilicon halogen-free flame retardants is random silsesquioxane, trapezoidal half siloxane, bridge type silsesquioxane and cage model sesquialter silicon oxygen
One or more of alkane mixing compounding.
5. a kind of thin wall type high CTI value flame resistant polycarbonate blends as claimed in claim 4, it is characterised in that: described
The end group of organosilicon halogen-free flame retardants is amino, alkoxy, methyl, phenyl one such two kinds or two or more structures
It is straight chain type or branch at, main structure.
6. a kind of thin wall type high CTI value flame resistant polycarbonate blends as claimed in claim 4, it is characterised in that: described
Cage model sesquialter organosiloxane be poly- (trimethylsiloxy group) silsesquioxane of cage modle eight, unfilled corner phenyl cage-type silsesquioxane,
One or more of cage modle aminopropyl silsesquioxane, epoxy cage type sesquialter siloxane and vinyl ladder type silsesquioxane
Mixing compounding.
7. a kind of thin wall type high CTI value flame resistant polycarbonate blends as described in claim 1, it is characterised in that: described
Phosphonitrile fire retardant has a structure that
,
Wherein, repetitive unit n be 3-25 integer, R1 group and R2 group are identical or different, represent unsubstituted phenyl or
The phenyl that the alkyl or allyl of at least one 1-6 carbon atom of person replace.
8. a kind of thin wall type high CTI value flame resistant polycarbonate blends as described in claim 1, it is characterised in that: described
Anti-dripping agent is the polymer comprising vinyl fluoride structure.
9. a kind of thin wall type high CTI value flame resistant polycarbonate blends as described in claim 1, it is characterised in that: described
Other auxiliary agents are at least one of self toughening agent, heat stabilizer, antioxidant, light stabilizer, plasticizer, filler, colorant.
10. a kind of preparation method of thin wall type high CTI value flame resistant polycarbonate blends, which is characterized in that use claim
Any polycarbonate Alloys preparation described in 1-9, comprising the following steps:
Polycarbonate, the halogen-free flame retardants of formula ratio, phosphonitrile fire retardant, other auxiliary agents are first weighed, and is all put into mixing machine
It is blended, is put into again in double screw extruder after mixing and carry out melting mixing extruding pelletization to get the high CTI value is arrived
High-fire resistance polycarbonate compositions；Wherein, the screw diameter of the double screw extruder is 36-40:1, each section of barrel temperature
It is set as 230-260 DEG C, screw speed 400-500rpm.
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| CN111073248A (en) * | 2019-12-16 | 2020-04-28 | 上海长伟锦磁工程塑料有限公司 | Hydrolysis-resistant, illumination-resistant and low-temperature-resistant halogen-free flame-retardant polycarbonate composite material and preparation method thereof |
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| CN113913004A (en) * | 2020-07-10 | 2022-01-11 | 汉达精密电子(昆山)有限公司 | Halogen-free flame-retardant PC conductive material and product thereof |
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| CN114075382A (en) * | 2020-08-21 | 2022-02-22 | 汉达精密电子(昆山)有限公司 | High-performance glass fiber reinforced PC material and product thereof |
| CN114276662A (en) * | 2020-09-28 | 2022-04-05 | 汉达精密电子(昆山)有限公司 | High-performance flame-retardant PC/PBT alloy and product thereof |
| WO2023061493A1 (en) * | 2021-10-15 | 2023-04-20 | 金发科技股份有限公司 | Flame retardant pc/abs alloy composition, preparation method therefor and application thereof |
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| WO2023180227A1 (en) * | 2022-03-25 | 2023-09-28 | Covestro Deutschland Ag | Polycarbonate compositions having a high cti |
| CN115477788A (en) * | 2022-10-10 | 2022-12-16 | 漳州鑫艺隆新材料科技有限公司 | Application of compound slipping agent in anti-sticking master batch, anti-sticking master batch for polyolefin film, preparation method and film thereof |
| CN115477788B (en) * | 2022-10-10 | 2024-03-01 | 漳州鑫艺隆新材料科技有限公司 | Application of compound slipping agent in anti-adhesion master batch, anti-adhesion master batch for polyolefin film, preparation method and film thereof |
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