CN112759913B - Flame-retardant polycarbonate composition and preparation method and application thereof - Google Patents
Flame-retardant polycarbonate composition and preparation method and application thereof Download PDFInfo
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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 invention relates to a flame-retardant polycarbonate composition, and a preparation method and application thereof. The flame-retardant polycarbonate composition comprises polycarbonate, SAN, ASA rubber powder, phosphazene flame retardant, triazine UV absorber, benzotriazole weather-resistant agent, hindered amine weather-resistant agent, anti-dripping agent, toner, antioxidant, metal passivator and other processing aids. The polycarbonate composition provided by the invention not only has better UVA and UVB radiation resistance, but also has better UVC radiation resistance, and can effectively prevent aging and yellowing of materials; and has better flame retardant property, and can be widely applied to ultraviolet sterilization products.
Description
Technical Field
The invention belongs to the technical field of engineering plastics, and particularly relates to a flame-retardant polycarbonate composition, and a preparation method and application thereof.
Background
Ultraviolet rays are classified into short wave UVC (200-280 nm), medium wave UVB (280-320 nm) and long wave UVA (320-400 nm) according to the wavelength length thereof. Some ultraviolet sterilization devices at present mainly use ultraviolet rays with wave bands of 250-280 nm to realize sterilization. However, the ultraviolet wavelength in the band is short, the energy is strong, and the device is very damaged, so that higher requirements are put on the ultraviolet radiation resistance of the device material, in particular to the UVC radiation. The polycarbonate and the alloy thereof are widely applied to ultraviolet disinfection equipment such as outdoor, kitchen and bath due to the excellent performance. At present, polycarbonate and an alloy thereof mainly improve the ultraviolet resistance of a material by adding a weather resistant agent, but the existing common weather resistant agent can mainly improve the UVA and UVB resistance and has no means for effectively improving the UVC radiation resistance. For example, patent CN107298838A discloses a polycarbonate composition in which shielding against ultraviolet rays is achieved by adding melanin. It is primarily capable of achieving both UVA and UVB shielding, and it is not mentioned whether UVA is effectively shielded.
Therefore, the development of the flame-retardant polycarbonate composition with better UVC resistance has important research significance and application value.
Disclosure of Invention
The invention aims to overcome the defect or defect of poor UVC radiation resistance of the existing flame-retardant polycarbonate and alloy thereof, and provides a flame-retardant polycarbonate composition. The flame-retardant polycarbonate composition provided by the invention has better UVA and UVB radiation resistance, also has better UVC radiation resistance, can effectively prevent ageing and yellowing of materials, has better flame retardant property, and can be widely applied to ultraviolet sterilization products.
It is another object of the present invention to provide a method for preparing the above flame retardant polycarbonate composition.
It is another object of the present invention to provide the use of the above flame retardant polycarbonate composition in the preparation of uv sterilized articles.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the flame-retardant polycarbonate composition comprises the following components in parts by weight:
ASA has better weather resistance, PCASA alloy is formed by compounding ASA and polycarbonate, so that the weather resistance of the polycarbonate composition can be improved to a certain extent, but the toughness of ASA is poor. The toughness of the PCASA is regulated by utilizing the ASA rubber powder, and the blend of the polycarbonate, the SAN and the ASA rubber powder is used as the main resin, so that the PCASA has better toughness, and the weather resistance is improved to a certain extent.
However, the existing weather-resistant agent mainly has good absorption effect on UVA and UVB, and has poor absorption effect on UVC, for example, when the existing weather-resistant agent is added into the PCASA blend, the UVC resistance is still poor.
The inventor of the invention discovers through multiple researches that the triazine UV absorber, the benzotriazole weather-resistant agent and the hindered amine weather-resistant agent are selected for compounding, and besides the good absorption effect on UCA and UVB, the polycarbonate composition can greatly improve the absorption effect on UVC, endow the polycarbonate composition with good UVC radiation resistance, effectively prevent aging and yellowing of materials, and can be widely applied to ultraviolet sterilization products.
In the PCASA resin system, a brominated flame retardant and a phosphorus flame retardant can be generally selected, the brominated flame retardant has insufficient weather resistance, and the phosphorus flame retardant can be selected from oligomeric phosphate, solid phosphate or phosphazene flame retardant.
According to the invention, the research shows that the phosphate in an oligomeric form and the solid phosphate can be subjected to accelerated aging under the irradiation of strong UVC light, the flame retardant performance can not reach UL 94V-0 level after aging, and the phosphazene flame retardant is selected, and the flame retardant level can still be maintained at V-0 level after aging, which is probably because the phosphazene flame retardant has good compatibility of a molecular structure and a resin matrix, has a stable structure, is not easily damaged by an external aging source in an aging environment, and causes self hydrolytic degradation to cause chain scission type decomposition of the resin, thereby causing the degradation of appearance quality, mechanical property and flame retardant level.
The flame-retardant polycarbonate composition provided by the invention has a good absorption effect on UV radiation with the wave band of 250-400 nm and has good flame-retardant property.
Preferably, the flame retardant polycarbonate composition comprises the following components in parts by weight:
polycarbonates conventional in the art can be used in the present invention.
Preferably, the polycarbonate is bisphenol A polycarbonate synthesized by a phosgene method, and the melt index under the condition of 1.2kg at 300 ℃ is 3-20 g/10min.
SAN is an acrylonitrile-styrene-acrylate copolymer (ASA).
Preferably, the acrylonitrile content in the SAN is 20 to 35 wt.%.
Preferably, the particle size of the rubber of the ASA rubber powder is 150-600 nm, and the rubber content is 35-80 wt%.
The ASA rubber powder under the condition has more excellent toughening effect.
The triazine UV absorber, the benzotriazole weather-resistant agent and the hindered amine weather-resistant agent which are conventional in the art can be used in the invention, so that a better synergistic effect is realized.
Preferably, the triazine UV absorber is a substance of the following structure:
wherein R is 1 、R 2 、R 3 And R is 4 Independently selected from alkyl or H, R 5 Is an alkyl or hydroxy ether (e.g., UV-1164, UV-1577, UV-400, UV-405, etc.).
More preferably, the triazine UV absorber is 2- (4, 6-bis (2, 4-dimethylphenyl) -1,3, 5-triazin-2-yl) -5-octyloxyphenol (e.g., cyasorb UV 1164) or 2- (4, 6-diphenyl-1, 3, 5-triazin-2-yl) -5-hexyloxy-phenol; one or both of 2- (4, 6-diphenyl-1, 3, 5-triazin-2-yl) -5-n-hexoxyphenol (e.g., UV-1577).
Preferably, the benzotriazole weathering agent is one or both of methyl 3- (3- (2H-benzotriazol-2-yl) -5-tert-butyl-4-hydroxyphenyl) propionate and the reaction product of PEG300 (UV-1130) or 2- (2 ' -hydroxy-3 ',5' -di-tert-pentylphenyl) benzotriazole (UV-328).
Preferably, the hindered amine weatherproofing agent is a hindered amine radical scavenger (e.g., ADK STAB L46).
Preferably, the phosphazene flame retardant is a phenoxy phosphazene compound, for example, such as cyclic phenoxy phosphazene, chain phenoxy phosphazene, crosslinked phenoxy phosphazene, and the like.
Anti-drip agents, antioxidants, toners and metal deactivators conventional in the art may be used in the present invention.
Preferably, the content of PTFE in the anti-dripping agent is 50-70 wt% and SAN coating or PS coating is adopted.
Preferably, the antioxidant comprises a main antioxidant and an auxiliary antioxidant, wherein the main antioxidant is one or more of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl alcohol ester or tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (antioxidant 1010), and the auxiliary antioxidant is one or more of tri- (2, 4-di-tert-butylphenyl) phosphite (antioxidant 168), pentaerythritol tetra- (3-laurylthiopropionate), 3- (dodecylthio) propionic acid-2, 2-bis [ [3- (dodecylthio) -propionyloxy ] methyl ] -1, 3-propanediol ester (Rinox 412 s) cyclic quaternary pentane tetra-di (2, 6-di-tert-butyl-4-methylphenyl phosphite) (PEP-36).
Further preferred are n-stearyl-beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and phosphite esters. Beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-stearyl alcohol ester. The +phosphite compounding system may impart further UV radiation resistance to the polycarbonate compositions of the present invention.
Preferably, the toner is one or two of titanium dioxide and carbon black.
More preferably, the titanium dioxide is rutile titanium dioxide of a chlorination method, and even more preferably is siloxane coated titanium dioxide.
The titanium dioxide can reflect light, and further improves the UV radiation resistance.
Preferably, the metal deactivator is a substance which reacts with metal ions to form chelates and lose oxidation, and comprises carbonyl condensates containing amine groups, such as propylenediamine salicylate, or esters containing phosphorus elements, such as MD-1024 (formula C 34 H 52 N 2 O 4 ) N, N' -bis [ beta (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl]And (3) hydrazine.
Other processing aids in the art may also be used in the present invention to impart better or new properties to the polycarbonate compositions of the present invention.
Preferably, the other processing aid is one or more of a lubricant or a flow modifier.
The types and the parts by weight of the processing aids can be selected and regulated according to the conventional control conditions.
Preferably, the other processing aid is a lubricant (e.g., oxidized polyethylene wax lubricant, ethylene acrylic acid copolymer type lubricant, polyethylene wax lubricant, high acid value polyethylene wax lubricant, pentaerythritol stearate, etc., in an amount of 0.1 to 1 part by weight), a flow modifier (e.g., an aliphatic unsaturated hydrocarbon (especially C) 2 －C 4 Olefins) and acrylic acid derivative monomer, the weight part of which is one or more of 0.01-2 parts).
The preparation method of the flame-retardant polycarbonate composition comprises the following steps: polycarbonate, SAN, ASA rubber powder, phosphazene flame retardant, triazine UV absorber, benzotriazole weather resistant agent, hindered amine weather resistant agent, anti-dripping agent, toner, antioxidant, metal passivator and other processing aids are mixed, melted, extruded and granulated to obtain the flame retardant polycarbonate composition.
Specifically, polycarbonate, SAN, ASA rubber powder, phosphazene flame retardant, triazine UV absorber, benzotriazole weather resistant agent, hindered amine weather resistant agent, anti-dripping agent, toner, antioxidant, metal passivating agent and other processing aids are premixed in a high-speed mixer to obtain premix, and then the premix is put into a double-screw extruder to be melted, mixed, extruded and granulated to obtain the flame-retardant polycarbonate composition.
The use of the polycarbonate composition in the preparation of ultraviolet sterilized articles is also within the scope of the present invention.
Compared with the prior art, the invention has the following beneficial effects:
the flame-retardant polycarbonate composition provided by the invention has better UVA and UVB radiation resistance, also has better UVC radiation resistance, can effectively prevent ageing and yellowing of materials, has better flame retardant property, and can be widely applied to ultraviolet sterilization products.
Detailed Description
The invention is further illustrated below with reference to examples. These examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. The experimental procedures in the examples below, without specific details, are generally performed under conditions conventional in the art or recommended by the manufacturer; the raw materials, reagents and the like used, unless otherwise specified, are those commercially available from conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art in light of the above teachings are intended to be within the scope of the invention as claimed.
The reagents selected for the examples and comparative examples of the present invention are described below:
polycarbonate PC1#, japanese glowing, IR1900, bisphenol A type polycarbonate, melt index at 20g/10min measured at 300℃under 1.2 kg;
polycarbonate PC2#, mitsubishi FN1500, bisphenol A type polycarbonate, melt index at 50g/10min at 300℃under 1.2kg conditions;
SAN1#, korean Jinhu, SAN-350, acrylonitrile content of 32wt%;
SAN2#, korean Jinhu, AS 310TR, acrylonitrile content of 18wt%;
ASA rubber powder No. 1, Q500, rubber content 60wt% and rubber particle size 200nm;
ASA rubber powder No. 2, mitsubishi, SX006, the rubber content is 50wt%, the rubber particle size is 100nm;
phosphazene flame retardant No. 1, haishan technology, GC-PNP, cyclic phenoxy phosphazene;
phosphazene flame retardant 2#, fushimi Pharmaceutical co., ltd FP-110, cyclic phenoxy phosphazene;
an oligomeric phosphate flame retardant, ai Dike FP-600;
solid phosphate flame retardants, mo Cheng, PX-202;
brominated flame retardants, american polyethylene, BC-58 (brominated polycarbon);
triazine UV absorber # 1, sorvy, cyasorb UV-1164;
triazine UV absorber # 2, jin Kangtai chemical industry, UV-1577;
benzotriazole weather resistant agent 1#, taiwan Qigo, chiuard 5411;
benzotriazole weathering agent No. 2, li Anlong, RIASORB UV-1130;
hindered amine weather resistant agent 1#, ai Dike, ADK STAB L46;
hindered amine weatherproofing agent # 2, basf, TINUVIN 622;
toner, titanium dioxide Kang Nuoji, titanium dioxide 2233;
an antioxidant: n-stearyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, ciba IRANOX, antioxidant 1076; auxiliary antioxidant phosphite ester, ADK PEP-36, PEP-36;
metal passivating agent: leen chemical, germany, MD-1024;
other processing aids: lubricants, dragon's blood, GLYCOLUBE-P.
The polycarbonate compositions of the examples and comparative examples were prepared as follows:
the polycarbonate composition is prepared by mixing polycarbonate, SAN, ASA rubber powder, flame retardants (phosphazene flame retardants, brominated flame retardants, oligomeric phosphate flame retardants and solid phosphate flame retardants), triazine UV absorbers, benzotriazole weather-resistant agents, hindered amine weather-resistant agents, anti-dripping agents, toner, antioxidants, metal deactivators and other processing aids, melting, extruding and granulating. Wherein the length-diameter ratio of the screw of the double-screw extruder is 40:1, the temperature of the screw cylinder is 230-260 ℃, and the rotating speed of the screw is 500rpm.
Evaluation method of UVC radiation resistance: at 254nm,0.3w/m 2 Under the irradiation intensity of (2), the illumination is continued for 100H, the color change of the sample is observed, and the smaller the color difference change is, the better the UVC radiation resistance is.
Evaluation method of flame retardant property: testing according to UL94, wherein the sample selected for initial flame retardant properties is not light treated; sample with selected flame retardant property after irradiation is processed by 254nm and 0.3w/m 2 And (3) carrying out the test after the treatment of continuous illumination for 100 hours under the irradiation intensity.
Examples 1 to 10
This example provides a series of flame retardant polycarbonate compositions, formulated as in table 1, prepared as described above.
Table 1 formulations (parts) of flame retardant polycarbonate compositions of examples 1 to 10
Comparative examples 1 to 5
This comparative example provides a series of polycarbonate compositions, the formulations of which are shown in Table 2, and the preparation methods of which are as described above.
Table 2 formulations (parts) of polycarbonate compositions of comparative examples 1 to 5
Table 3 shows the results of UVC radiation resistance and flame retardant properties.
Table 3 results of UVC radiation resistance and flame retardant properties of the flame retardant polycarbonate compositions of the examples and comparative examples
As can be seen from Table 3, the flame retardant polycarbonate compositions of the various embodiments of the present invention are excellent in UVC radiation resistance and have good flame retardant properties (up to UL 94V-0 level). The polycarbonate compositions to which no weathering agent (comparative example 4) was added and to which only 2 weathering agents (comparative examples 1 to 3) were added were inferior in UVC radiation resistance and large in color difference change; polycarbonate compositions (e.g., comparative examples 5-7) with the addition of brominated flame retardants or other unsuitable phosphorus-containing flame retardants have poor flame retardant properties or have large color variations.
Those of ordinary skill in the art will recognize that the embodiments herein are intended to assist the reader in understanding the principles of the invention and should be understood that the scope of the invention is not limited to such specific statements and embodiments. Those of ordinary skill in the art can make various other specific modifications and combinations from the teachings of the present disclosure without departing from the spirit thereof, and such modifications and combinations remain within the scope of the present disclosure.
Claims (9)
1. The flame-retardant polycarbonate composition is characterized by comprising the following components in parts by weight:
the triazine UV absorber is a substance with the following structure:
wherein R is 1 、R 2 、R 3 And R is 4 Independently selected from alkyl or H, R 5 Is alkyl or hydroxy ether.
2. The flame retardant polycarbonate composition of claim 1, comprising the following components in parts by weight:
3. the flame retardant polycarbonate composition of claim 1, wherein the polycarbonate is bisphenol a type polycarbonate synthesized by a phosgene method, and has a melt index of 3 to 20g/10min at 300 ℃ under 1.2 kg;
the acrylonitrile content in the SAN is 20-35 wt%;
the particle size of the rubber of the ASA rubber powder is 150-600 nm, and the rubber content is 35-80 wt%.
4. The flame retardant polycarbonate composition of claim 1, wherein the benzotriazole-based weathering agent is one or both of methyl 3- (3- (2H-benzotriazol-2-yl) -5-tert-butyl-4-hydroxyphenyl) propionate and PEG300 reaction product or 2- (2 ' -hydroxy-3 ',5' -di-tert-pentylphenyl) benzotriazole.
5. The flame retardant polycarbonate composition of claim 1, wherein the hindered amine weatherproofing agent is a hindered amine radical scavenger.
6. The flame retardant polycarbonate composition of claim 1, wherein the phosphazene flame retardant is a phenoxy phosphazene compound;
the content of PTFE in the anti-dripping agent is 50-70 wt% and SAN coating or PS coating is adopted;
the antioxidant comprises a main antioxidant and an auxiliary antioxidant; the main antioxidant is one or two of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-stearyl alcohol ester or tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, and the auxiliary antioxidant is one or more of tri (2, 4-di-tert-butylphenyl) phosphite, pentaerythritol tetra (3-laurylthiopropionate), 3- (dodecylthio) propionic acid-2, 2-bis [ [3- (dodecylthio) -propionyloxy ] methyl ] -1, 3-propanediol ester cyclic quaternary pentane tetra-yl di (2, 6-di-tert-butyl-4-methylphenyl phosphite);
the toner is one or two of titanium dioxide and carbon black;
the metal passivating agent is carbonyl condensate containing amino or ester containing phosphorus element.
7. The flame retardant polycarbonate composition of claim 1, wherein the other processing aid is one or more of a lubricant or a flow modifier.
8. The method for preparing a flame retardant polycarbonate composition according to any one of claims 1 to 7, comprising the steps of: and mixing polycarbonate, SAN, ASA rubber powder, phosphazene flame retardant, triazine UV absorbent, benzotriazole weather-resistant agent, hindered amine weather-resistant agent, anti-dripping agent, toner, antioxidant, metal passivator and other processing aids, melting, extruding and granulating to obtain the flame-retardant polycarbonate composition.
9. Use of the flame retardant polycarbonate composition of any of claims 1-7 for the preparation of an ultraviolet sterilized article.
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