CN114736500A - Halogen-free flame-retardant polycarbonate/styrene resin alloy and preparation method and application thereof - Google Patents
Halogen-free flame-retardant polycarbonate/styrene resin alloy and preparation method and application thereof Download PDFInfo
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- CN114736500A CN114736500A CN202210290772.8A CN202210290772A CN114736500A CN 114736500 A CN114736500 A CN 114736500A CN 202210290772 A CN202210290772 A CN 202210290772A CN 114736500 A CN114736500 A CN 114736500A
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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
- C08L2201/22—Halogen free composition
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
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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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a halogen-free flame-retardant polycarbonate/styrene resin alloy and a preparation method and application thereof. The halogen-free flame-retardant polycarbonate/styrene resin alloy resistant to damp-heat aging comprises the following components in parts by weight: 35-45 parts of polycarbonate resin, 15-35 parts of silicon copolymerized polycarbonate resin, 25-45 parts of styrene resin, 5-15 parts of phosphazene halogen-free flame retardant, 2-5 parts of compatilizer, 0.5-2 parts of talcum powder and 0.5-1.5 parts of other auxiliary agents. The moisture and heat resistance of the halogen-free flame retardant polycarbonate/styrene resin alloy is improved through the synergistic effect of the phosphazene halogen-free flame retardant, the silicon copolymerized polycarbonate resin, the talcum powder and other components, the mechanical property retention rate is high in a moist and hot environment, the alloy oxygen index is high, and the flame retardant performance is good.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a halogen-free flame-retardant polycarbonate/styrene resin alloy and a preparation method and application thereof.
Background
Polycarbonate (PC) resin is colorless and transparent, has excellent heat resistance, high strength and impact resistance, is stable in size and good in flame retardance, and belongs to engineering plastics with wide application. The styrene resin mainly comprises acrylonitrile-butadiene-styrene copolymer (ABS), acrylonitrile-acrylate-styrene copolymer (ASA) and acrylonitrile-ethylene propylene diene monomer-styrene copolymer (AES), and the styrene resin coordinates the superior performances of the three copolymerization components, so that the styrene resin has excellent impact strength, good processing performance and chemical stability, is easy to mold and form, has rich luster of products, and has toughness and flexibility as well as excellent comprehensive performance.
The polycarbonate/styrene resin alloy integrates the advantages of the resins of all components, and is widely applied to the industries such as automobile industry, electronic and electric appliance industry, light industry and household appliances, textile, building and the like due to the excellent comprehensive performance of the polycarbonate/styrene resin alloy. However, the polycarbonate styrene alloy resin has poor wet heat resistance and serious deterioration of mechanical properties in a wet heat environment. Ordinary polycarbonate styrene alloy resin can not be directly applied to parts in a damp and hot environment, and the halogen-free flame-retardant polycarbonate/styrene alloy resin is particularly suitable for the damp and hot environment.
Aiming at the defect of poor humidity resistance of polycarbonate/styrene resin alloy, the prior art reports a high temperature and high humidity resistant polycarbonate composition and a preparation method thereof, and the mechanical property retention rate of the polycarbonate composition under the high temperature and high humidity condition is improved by adding an organic silicon toughening agent and an oxazoline-based chain extender; however, oxazoline groups are toxic organic compounds, and the application range of polycarbonate compositions containing oxazoline chain extenders is very limited. The prior art discloses a moisture-heat resistant PC/ABS flame-retardant composite material and a preparation method thereof, wherein the hydrolysis resistance of PC/ABS is improved by introducing a phosphorus flame retardant, an auxiliary flame retardant and melamine benzene sulfonate; however, the phosphorus flame retardant and the melamine benzene sulfonate are acidic in the PC system, and are easy to cause degradation of PC.
Therefore, there is a need for a halogen-free flame retardant polycarbonate/styrene resin alloy with good humidity resistance and heat resistance, which has high mechanical property retention rate under humid and hot environment on the basis of good flame retardant property.
Disclosure of Invention
The invention aims to overcome the defect of poor humidity resistance in the prior art, and provides the halogen-free flame-retardant polycarbonate/styrene resin alloy.
The invention also aims to provide a preparation method of the halogen-free flame-retardant polycarbonate/styrene resin alloy.
The invention also aims to provide application of the halogen-free flame-retardant polycarbonate/styrene resin alloy.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a halogen-free flame-retardant polycarbonate/styrene resin alloy comprises the following components in parts by weight:
35-45 parts of polycarbonate resin (PC),
15-35 parts of silicon copolymerized polycarbonate resin (silicon copolymerized PC),
25-45 parts of styrene resin,
5-15 parts of phosphazene halogen-free flame retardant,
2-5 parts of a compatilizer,
0.5 to 2 parts of talcum powder,
0.5-1.5 parts of other additives.
According to the invention, the moisture and heat resistance of the halogen-free flame retardant polycarbonate/styrene resin alloy is improved through the synergistic effect of the phosphazene halogen-free flame retardant, the silicon copolymerized polycarbonate resin, the talcum powder and other components, the mechanical property retention rate is high in a moist and hot environment, the alloy oxygen index is high, and the flame retardant property is good.
After the phosphazene halogen-free flame retardant is heated and decomposed, gases such as carbon dioxide, ammonia gas, nitrogen gas, water vapor and the like are released, so that the supply of oxygen can be blocked, and the heat concentration on the surface of the material can be effectively reduced. The silicon copolymerization PC has Si-O-Si groups, has the performances of inorganic materials and organic materials, and has synergistic effect with the phosphazene halogen-free flame retardant to realize synergistic flame retardance. Meanwhile, the Si-O-Si group in the silicon copolymerized PC and the O ═ Si ═ O group contained in the talcum powder generate synergistic effect, so that the silicon copolymerized PC is uniformly dispersed on the surface of the halogen-free flame-retardant polycarbonate/styrene resin alloy, and the effect of improving the wet-heat aging resistance is achieved.
The content of silicon copolymerized PC is not preferably too high or too low. The inventor researches and discovers that the content of silicon copolymerized PC is too low, the oxygen index of the prepared alloy material is lower, and the flame retardant property is poorer. When the content of the silicon copolymerized PC is too high, due to the interaction of the copolymerization structure of the silicon copolymerized PC and the styrene resin, the system crosslinking degree of the polycarbonate/styrene resin alloy is greatly improved, the system viscosity is increased, the melt index is rapidly reduced, and under the action of the talcum powder, the shearing force is strengthened, so that the styrene resin is excessively sheared, the mechanical property of the prepared alloy material is reduced, particularly the impact resistance is poor, and the retention rate of the impact resistance under a damp-heat environment is lower.
Preferably, the mass ratio of the silicon copolymerized PC to the styrene-based resin is 1: (1-2).
Preferably, the polysiloxane content of the silicon co-PC is 5.5 to 6.2 wt.%.
Optionally, the styrene resin is one or more of ABS, ASA or AES.
Preferably, the phosphazene halogen-free flame retardant is hexaphenoxycyclotriphosphazene and/or polydiphenoxyphosphazene.
Preferably, the average particle size of the talcum powder is 10-30 μm.
Preferably, the compatilizer is glycidyl methacrylate grafted styrene resin and/or maleic anhydride grafted styrene resin.
More preferably, the compatibilizer is glycidyl methacrylate grafted styrenic resin.
Preferably, the other auxiliary agent is one or more of an antioxidant, a light stabilizer or a lubricant.
Optionally, the antioxidant is a hindered phenolic antioxidant and/or a phosphite antioxidant.
Optionally, the light stabilizer is a benzotriazole ultraviolet light absorber and/or a hindered amine light stabilizer.
Optionally, the lubricant is one or more of pentaerythritol stearate, silicone lubricant or amide lubricant.
The invention also provides a preparation method of the halogen-free flame-retardant polycarbonate/styrene resin alloy, which comprises the following steps:
mixing polycarbonate resin, silicon copolymerized polycarbonate resin, styrene resin, phosphazene halogen-free flame retardant, compatilizer, talcum powder and other auxiliary agents, adding the mixture into an extruder, and performing melt mixing, extrusion and granulation to obtain the halogen-free flame retardant polycarbonate/styrene resin alloy.
Preferably, the extruder is a double-screw extruder, and the melting temperature is 220-250 ℃.
The invention also protects the application of the halogen-free flame-retardant polycarbonate/styrene resin alloy in preparing battery separators of electric vehicles, battery pack shells or charging gun shells.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a halogen-free flame-retardant polycarbonate/styrene resin alloy resistant to damp-heat aging. Through the synergistic effect of the phosphazene halogen-free flame retardant, the silicon copolymerized polycarbonate resin, the talcum powder and other components, the humidity resistance and heat resistance of the halogen-free flame retardant polycarbonate/styrene resin alloy are improved, the mechanical property retention rate is high in a damp and hot environment, the alloy oxygen index is high, and the flame retardant property is good.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The raw materials in the examples and comparative examples are commercially available;
reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Examples 1 to 17
Examples 1 to 17 provide a polycarbonate/styrene resin alloy having the component contents shown in table 1, and the preparation method is as follows:
mixing the components according to the table 1, adding the mixture into a double-screw extruder, carrying out melt mixing at 220-250 ℃, extruding and granulating to obtain the polycarbonate/styrene resin alloy.
TABLE 1 examples 1 to 17 composition amounts (parts by weight) of polycarbonate/styrene resin alloy
Comparative examples 1 to 6
Comparative examples 1 to 6 provide a polycarbonate/styrene resin alloy, the component contents of which are shown in table 2, and the preparation method is as follows:
mixing the components according to the table 2, adding the mixture into a double-screw extruder, carrying out melt mixing at 220-250 ℃, extruding and granulating to obtain the polycarbonate/styrene resin alloy.
TABLE 2 ingredient contents (parts by weight) of comparative examples 1 to 6 polycarbonate/styrene resin alloys
Performance testing
The polycarbonate/styrene resin alloys prepared in the above examples and comparative examples were tested for their properties by the following specific methods:
flame retardant property: the oxygen index was measured according to the standard method of GBT 2406-1993;
moisture and heat resistance: injecting the polycarbonate/styrene resin alloy into a standard sample strip, and detecting the initial Charpy impact strength and tensile strength; placing the standard sample strip in a constant temperature and humidity aging box at 85 ℃ and 85% RH, aging for 1000 hours, and detecting the Charpy impact strength and the tensile strength again after aging; calculating the Charpy impact strength and tensile strength retention rate according to detection values before and after aging;
retention rate is measured after aging/measured before aging × 100%;
the Charpy impact strength is tested according to ISO 179-2010 standard;
tensile strength was tested in accordance with ISO 527-.
The test results of examples 1 to 17 are shown in Table 3, and the test results of comparative examples 1 to 6 are shown in Table 4.
TABLE 3 test results for examples 1 to 17
According to the test results in Table 3, the polycarbonate/styrene resin alloy prepared in each example of the invention has good flame retardant property, the oxygen index is more than or equal to 25%, and the Charpy impact strength retention rate and the tensile strength retention rate are more than or equal to 80% after thermal aging treatment.
According to examples 1 to 3, when the polysiloxane content in the silicon-copolymerized PC is 5.5 to 6.2 wt.%, the mechanical property retention rate of the polycarbonate/styrene resin alloy after humid heat aging is higher, which indicates that the humid heat aging resistance is better.
In example 1 and examples 9 to 12, it can be seen that as the content of silicon copolymerized PC decreases and the content of styrene resin increases, the oxygen index of the alloy material decreases and the flame retardant performance tends to slightly decrease; the Charpy impact strength retention rate is increased, and the toughness retention rate in a damp and hot environment is more increased. Wherein the Charpy impact strength retention rate of the alloy in the embodiment 1 is less than 90 percent, and the tensile strength retention rate is lower and is 91 percent; the oxygen index of the alloy of example 12 is low, only 25%. In general terms, the flame retardant property and the moisture and heat resistance of the alloys of examples 9 to 11 are better, and therefore the mass ratio of the silicon-copolymerized PC to the styrene resin is preferably 1: (1-2).
TABLE 4 test results for comparative examples 1 to 6
In comparative example 1, no silicon copolymerized PC was contained, and the resultant polycarbonate/styrene resin had an excessively low alloy index and poor flame retardancy. In the case of the silicon-free copolymerized PC, the wet heat resistance of the polycarbonate/styrene-based resin alloy was also significantly reduced as compared with example 1.
In comparative example 2, the content of silicon copolymerized PC was too high, and the viscosity of the material increased and the shear force became strong under the interaction with the styrene resin and talc, resulting in excessive shear, so that the mechanical properties of the material decreased and the wet and heat resistance deteriorated, and the mechanical property retention rate after the treatment in the wet and heat environment was low. In comparative example 3, the amount of silicon copolymerized PC is too small, so that the silicon copolymerized PC is difficult to have effective synergistic action with the phosphazene halogen-free flame retardant and the talcum powder, and the prepared alloy has poor flame retardant performance and wet and heat resistance.
The flame retardant in comparative example 4 is a non-phosphazene halogen-free flame retardant, but diphenyl phosphate. The phosphorus-containing flame retardant is easy to degrade PC in a PC system, and the PC degradation rate is higher in a damp-heat environment, so that the damp-heat resistance of the alloy material is very poor.
In comparative example 5, the talc powder was not contained, the Si-O-Si group in the silicon copolymerized PC failed to produce synergistic effect with other components, and the silicon copolymerized PC was difficult to be uniformly dispersed on the surface of the alloy, thereby achieving the effect of improving the resistance to wet heat aging. In comparative example 6, the talc powder was replaced with another inorganic filler (calcium carbonate), which is slightly basic, and under the hot and humid conditions, PC was easily degraded, resulting in severe deterioration of mechanical properties of the polycarbonate/styrene resin alloy.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The halogen-free flame-retardant polycarbonate/styrene resin alloy is characterized by comprising the following components in parts by weight:
35-45 parts of polycarbonate resin,
15-35 parts of silicon copolymerized polycarbonate resin,
25-45 parts of styrene resin,
5-15 parts of a phosphazene halogen-free flame retardant,
2-5 parts of a compatilizer,
0.5 to 2 parts of talcum powder,
0.5-1.5 parts of other additives.
2. The halogen-free flame-retardant polycarbonate/styrene-based resin alloy as claimed in claim 1, wherein the polysiloxane content of the silicon-copolymerized polycarbonate resin is 5.5-6.2 wt.%.
3. The halogen-free flame-retardant polycarbonate/styrene-based resin alloy according to claim 1, wherein the mass ratio of the silicon-copolymerized polycarbonate resin to the styrene-based resin is 1: (1-2).
4. The halogen-free flame-retardant polycarbonate/styrene-based resin alloy as claimed in claim 1, wherein the styrene-based resin is one or more of ABS, ASA or AES.
5. The halogen-free flame retardant polycarbonate/styrenic resin alloy of claim 1, wherein the phosphazene halogen-free flame retardant is hexaphenoxycyclotriphosphazene and/or polydiphenoxyphosphazene.
6. The halogen-free flame-retardant polycarbonate/styrene resin alloy according to claim 1, wherein the talc powder has an average particle size of 10 to 30 μm.
7. The halogen-free flame-retardant polycarbonate/styrenic resin alloy of claim 1, wherein the compatibilizer is a glycidyl methacrylate grafted styrenic resin and/or a maleic anhydride grafted styrenic resin.
8. The halogen-free flame-retardant polycarbonate/styrene resin alloy as claimed in claim 1, wherein the other auxiliary agents are one or more of an antioxidant, a light stabilizer, a lubricant or a toner.
9. The preparation method of the halogen-free flame retardant polycarbonate/styrene resin alloy according to any one of claims 1 to 8, which is characterized by comprising the following steps:
mixing polycarbonate resin, silicon copolymerized polycarbonate resin, styrene resin, phosphazene halogen-free flame retardant, compatilizer, talcum powder and other auxiliary agents, adding the mixture into an extruder, and performing melt mixing, extrusion and granulation to obtain the halogen-free flame retardant polycarbonate/styrene resin alloy.
10. Use of the halogen-free flame-retardant polycarbonate/styrene resin alloy according to any one of claims 1 to 8 in the preparation of battery separators for electric vehicles, battery pack cases or charging gun cases.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210290772.8A CN114736500B (en) | 2022-03-23 | 2022-03-23 | Halogen-free flame-retardant polycarbonate/styrene resin alloy and preparation method and application thereof |
| PCT/CN2023/082557 WO2023179555A1 (en) | 2022-03-23 | 2023-03-20 | Halogen-free flame-retardant polycarbonate/styrene resin alloy, and preparation method therefor and use thereof |
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| CN202210290772.8A CN114736500B (en) | 2022-03-23 | 2022-03-23 | Halogen-free flame-retardant polycarbonate/styrene resin alloy and preparation method and application thereof |
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| CN114736500A true CN114736500A (en) | 2022-07-12 |
| CN114736500B CN114736500B (en) | 2023-05-05 |
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| WO (1) | WO2023179555A1 (en) |
Cited By (2)
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| CN115651383A (en) * | 2022-10-20 | 2023-01-31 | 金发科技股份有限公司 | Polycarbonate alloy material and preparation method and application thereof |
| WO2023179555A1 (en) * | 2022-03-23 | 2023-09-28 | 武汉金发科技有限公司 | Halogen-free flame-retardant polycarbonate/styrene resin alloy, and preparation method therefor and use thereof |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN114736500B (en) | 2023-05-05 |
| WO2023179555A1 (en) | 2023-09-28 |
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