CN112759913A - 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
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- 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
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- 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
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Abstract
The invention relates to a flame-retardant polycarbonate composition, a preparation method and application thereof. The flame-retardant polycarbonate composition comprises polycarbonate, SAN, ASA rubber powder, phosphazene flame retardants, triazine UV absorbers, benzotriazole weather-resistant agents, hindered amine weather-resistant agents, anti-dripping agents, toner, antioxidants, metal passivators 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 materials from aging and yellowing; 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
The ultraviolet rays are divided into short-wave UVC (200-280 nm), medium-wave UVB (280-320 nm) and long-wave UVA (320-400nm) according to the wavelength. At present, some ultraviolet sterilization equipment mainly utilizes ultraviolet rays with the wave band of 250-280 nm to realize sterilization and disinfection. However, the ultraviolet wavelength of the wave band is short, the energy is strong, and the device has very strong destructive power, so that higher requirements are provided for the ultraviolet radiation resistance of the device material, especially the UVC radiation. Polycarbonate and its alloy are widely used in ultraviolet disinfection equipment such as outdoor and kitchen and toilet because of their excellent properties. At present, polycarbonate and alloy thereof are mainly used for improving the ultraviolet resistance of materials by adding weather resistant agents, but the existing common weather resistant agents can mainly improve the UVA resistance and the UVB resistance, and a means for effectively improving the UVC radiation resistance is not provided. For example, patent CN107298838A discloses a polycarbonate composition, which is shielded from uv light by adding a black pigment. However, it can mainly achieve shielding of UVA and UVB, and it is not mentioned whether UVA can be 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 deficiency of poor UVC radiation resistance of the conventional flame-retardant polycarbonate and the alloy thereof, and provides a flame-retardant polycarbonate composition. The flame-retardant polycarbonate composition provided by the invention not only has better UVA and UVB radiation resistance, but also has better UVC radiation resistance, can effectively prevent materials from aging and yellowing, has better flame-retardant property, and can be widely applied to ultraviolet sterilization products.
Another object of the present invention is to provide a method for preparing the above flame retardant polycarbonate composition.
The invention also aims to provide application of the flame-retardant polycarbonate composition in preparing ultraviolet sterilization products.
In order to achieve the purpose, the invention adopts the following technical scheme:
a flame-retardant polycarbonate composition comprises the following components in parts by weight:
60-90 parts of polycarbonate;
0.1-25 parts of SAN;
0.1-10 parts of ASA rubber powder;
0.1-20 parts of phosphazene flame retardant;
0.1-3 parts of triazine UV absorbent;
0.1-3 parts of benzotriazole weather resistant agent;
0.1-3 parts of hindered amine weather resistant agent;
0.01-2 parts of anti-dripping agent;
0.1-10 parts of toner.
0.1-1 part of antioxidant
0.01-0.5 parts of metal passivator;
0-2 parts of other processing aids.
ASA has good weather resistance, and the PCASA alloy formed by compounding ASA and polycarbonate can improve the weather resistance of the polycarbonate composition to a certain extent, but the toughness of the ASA is poor. The invention utilizes ASA rubber powder to adjust the toughness, and blends the polycarbonate, SAN and ASA rubber powder to obtain PCASA blend which is used as main resin and has better toughness, and simultaneously improves the weather resistance to a certain extent.
However, the existing weather resisting agent mainly has a good absorption effect on UVA and UVB, and has a poor absorption effect on UVC, and if the existing weather resisting agent is added into a PCASA blend, the UVC resistance is still not good.
Through multiple researches, the inventor of the invention discovers that the triazine UV absorbent, the benzotriazole weather resistant agent and the hindered amine weather resistant agent are compounded, so that the absorption effect on UVC can be greatly improved besides a good absorption effect on UCA and UVB, the polycarbonate composition is endowed with better UVC radiation resistance, the material is effectively prevented from aging and yellowing, and the polycarbonate composition can be widely applied to ultraviolet sterilization products.
In the PCASA resin system, a bromine flame retardant and a phosphorus flame retardant can be generally selected, the bromine flame retardant has insufficient weather resistance, and the phosphorus flame retardant can be oligomeric phosphate, solid phosphate or phosphazene flame retardant.
According to the research of the invention, the oligomeric phosphate and the solid phosphate can be aged under the irradiation of strong UVC light, the flame retardant performance can not reach UL 94V-0 grade after aging, and the phosphazene flame retardant is selected, and the flame retardant grade can be maintained at V-0 grade after aging, probably because the molecular structure of the phosphazene flame retardant is good in compatibility with a resin matrix, the phosphazene flame retardant has stable structure, and is not easy to be damaged by an external aging source in an aging environment, so that the self-hydrolysis degradation of the phosphazene flame retardant can cause chain scission decomposition of resin, and the deterioration of appearance quality, mechanical performance and flame retardant grade can be caused.
The flame-retardant polycarbonate composition provided by the invention has a good absorption effect on UV radiation of a 250-400 nm waveband, and has good flame-retardant property.
Preferably, the flame retardant polycarbonate composition comprises the following components in parts by weight:
65-85 parts of polycarbonate;
4-15 parts of SAN;
2-7 parts of ASA rubber powder;
2-12 parts of a phosphazene flame retardant;
0.4-1 part of triazine UV absorbent;
0.4-1 part of benzotriazole weather resistant agent;
0.5-1 part of hindered amine weather resistant agent;
0.1-1 part of anti-dripping agent;
0.5-8 parts of toner.
0.1-0.5 part of antioxidant
0.05-0.2 parts of metal passivator;
0.1-0.5 part of other processing aids.
Polycarbonates conventional in the art may be used in the present invention.
Preferably, the polycarbonate is bisphenol A polycarbonate synthesized by a phosgene method, and the melt index is 3-20 g/10min under the conditions of 300 ℃ and 1.2 kg.
SAN is acrylonitrile-styrene-acrylate copolymer (ASA).
Preferably, the content of acrylonitrile in the SAN is 20-35 wt%.
Preferably, the rubber particle size 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.
In the field, the conventional triazine UV absorbent, benzotriazole weather-resistant agent and hindered amine weather-resistant agent can be used in the invention, so that a good synergistic effect is realized.
Preferably, the triazine UV absorber is a substance having the following structure:
wherein R is1、R2、R3And R4Independently selected from alkyl or H, R5Is alkylOr hydroxy ethers (e.g., UV-1164, UV-1577, UV-400, UV-405, etc.).
More preferably, the triazine-based 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; 2- (4, 6-diphenyl-1, 3, 5-triazin-2-yl) -5-n-hexylalkoxyphenol (e.g., UV-1577).
Preferably, the benzotriazole weather resisting agent is one or two of a reaction product (UV-1130) of methyl 3- (3- (2H-benzotriazole-2-yl) -5-tert-butyl-4-hydroxyphenyl) propionate and PEG300 or 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-amylphenyl) benzotriazole (UV-328).
Preferably, the hindered amine weathering agent is a hindered amine radical scavenger (e.g., ADK STAB L46).
Preferably, the phosphazene flame retardant is a phenoxyphosphazene compound, for example, a cyclic phenoxyphosphazene, a chain phenoxyphosphazene, a crosslinked phenoxyphosphazene, or 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 n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate or pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (antioxidant 1010), the auxiliary antioxidant is one or more of tris (2, 4-di-tert-butylphenyl) phosphite (antioxidant 168), pentaerythritol tetrakis (3-laurylthiopropionate), 3- (dodecylthio) propionic acid-2, 2-bis [ [3- (dodecylthio) -propionyloxy ] methyl ] -1, 3-propanediol ester (Rinox412s) cyclic pentanetetrakis (2, 6-di-tert-butyl-4-methylphenyl phosphite) (PEP-36).
Further preferred are n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and phosphite esters. N-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate. The formulation system of the + phosphite ester can endow the polycarbonate composition of the invention with further UV radiation resistance.
Preferably, the toner is one or two of titanium dioxide or carbon black.
More preferably, the titanium dioxide is rutile type titanium dioxide obtained by a chlorination method, and further preferably siloxane coated titanium dioxide.
The titanium dioxide can reflect light, and the UV radiation resistance is further improved.
Preferably, the metal deactivator is a substance which reacts with metal ions to form chelate complexes and thus loses its oxidation, and includes carbonyl condensates containing amine groups, such as propylenediamine salicylate, and esters containing phosphorus elements, such as MD-1024 (formula C)34H52N2O4) N, N' -bis [ beta (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl]A hydrazine.
Other processing aids known 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 aids comprise one or more of a lubricant or a flow modifier.
The types and the weight parts of the processing aids can be selected and regulated according to conventional control conditions.
Preferably, the other processing aids are lubricants (such as oxidized polyethylene wax lubricant, ethylene acrylic acid copolymer lubricant, polyethylene wax lubricant, high acid value polyethylene wax lubricant, pentaerythritol stearate, etc., in an amount of 0.1 to 1 part by weight), flow modifiers (such as aliphatic unsaturated hydrocarbons (especially C)2－C4Olefins) and acrylic acid derivative monomer, the weight portion of the copolymer is 0.01-2 portions) and one or more of the materials.
The preparation method of the flame-retardant polycarbonate composition comprises the following steps: 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 are mixed, melted, extruded and granulated to obtain the flame-retardant polycarbonate composition.
Specifically, polycarbonate, SAN, ASA gelatine 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 are premixed in a high-speed mixer to obtain premix, and then the premix is put into a double-screw extruder to be subjected to melt mixing, extrusion and granulation to obtain the flame-retardant polycarbonate composition.
The application of the polycarbonate composition in preparing ultraviolet sterilization products is also within the protection scope of the invention.
Compared with the prior art, the invention has the following beneficial effects:
the flame-retardant polycarbonate composition provided by the invention not only has better UVA and UVB radiation resistance, but also has better UVC radiation resistance, can effectively prevent materials from aging and yellowing, has better flame-retardant property, and can be widely applied to ultraviolet sterilization products.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Some of the reagents selected in the examples and comparative examples of the present invention are described below:
polycarbonate PC1#, Nippon Kogyo, IR1900, bisphenol A polycarbonate, having a melt index of 20g/10min as measured at 300 ℃ under 1.2 kg;
polycarbonate PC2#, Mitsubishi FN1500, bisphenol A polycarbonate, having a melt index of 50g/10min as measured at 300 ℃ under 1.2 kg;
SAN1#, brocade lake, korea, SAN-350, acrylonitrile content 32 wt%;
SAN2#, brocade lake, korea, AS 310TR, acrylonitrile content 18 wt%;
ASA rubber powder No. 1, of the east China sea plastics industry, Q500, with a rubber content of 60 wt%, and a rubber particle size of 200 nm;
ASA rubber powder No. 2, Mitsubishi, SX006, rubber content of 50 wt%, rubber particle size of 100 nm;
phosphazene flame retardant 1#, haishan science and technology, GC-PNP, cyclic phenoxyphosphazene;
phosphazene flame retardant 2#, Fushimi Pharmaceutical Co., Ltd FP-110, cyclic phenoxyphosphazene;
oligomeric phosphate flame retardants, Ediko FP-600;
solid phosphate flame retardants, myriad, PX-202;
brominated flame retardant, Gekko, BC-58 (brominated polycarbonate).
Triazine UV absorber 1#, Solvay, Cyasorb UV-1164;
triazine UV absorber 2#, Jinkangtai chemical industry, UV-1577;
benzotriazole weather resistance agent # 1, taiwan qitai, CHIGUARD 5411;
benzotriazole weather resistant agent 2#, linalon, RIASORB UV-1130;
hindered amine weatherometer # 1, adico, ADK STAB L46;
hindered amine weathering agent # 2, basf, TINUVIN 622;
toner, titanium dioxide cornoki titanium dioxide 2233;
antioxidant: the main antioxidant beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, Ciba IRANOX and the antioxidant 1076; secondary antioxidant phosphite ester, ADK PEP-36 and PEP-36.
Metal passivator: german Laien chemical, MD-1024.
Other processing aids: lubricants, American Dragon Sand, Glycolube-P.
The polycarbonate compositions of the examples and comparative examples were prepared as follows:
mixing polycarbonate, SAN, ASA rubber powder, flame retardant (phosphazene flame retardant, brominated flame retardant, oligomeric phosphate flame retardant and solid phosphate 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 polycarbonate composition. Wherein the length-diameter ratio of a screw of the double-screw extruder is 40:1, the temperature of a screw barrel is 230-260 ℃, and the rotating speed of the screw is 500 rpm.
Evaluation method of UVC radiation resistance: at 254nm, 0.3w/m2Under the irradiation intensity of (3), continuously irradiating for 100H, observing the color change of the sample, wherein the smaller the color difference change is, the better the UVC radiation resistance is.
Evaluation method of flame retardancy: testing according to UL94, wherein the initial flame retardant performance is selected from samples without light treatment; the sample with the flame retardant property after irradiation is subjected to 254nm and 0.3w/m2The test is carried out after the treatment of continuous illumination for 100 hours under the irradiation intensity of (2).
Examples 1 to 10
This example provides a series of flame retardant polycarbonate compositions having the formulation shown in Table 1 and prepared according to the methods described above.
TABLE 1 formulation (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 having the formulation shown in Table 2 and prepared as described above.
TABLE 2 formulation (parts) of polycarbonate compositions of comparative examples 1 to 5
Table 3 shows the results of the UVC radiation resistance and flame retardant performance.
TABLE 3 UVC radiation resistance and flame retardancy Performance results for the flame retardant polycarbonate compositions of the examples and comparative examples
As shown in Table 3, the flame retardant polycarbonate composition of each example of the invention has excellent UVC radiation resistance and better flame retardant property (up to UL 94V-0 grade). The polycarbonate composition without the weather-resistant agent (comparative example 4) and with only 2 weather-resistant agents (comparative examples 1-3) has poor UVC radiation resistance and large color difference change; polycarbonate compositions (e.g., comparative examples 5-7) with brominated flame retardants or other unsuitable phosphorus-containing flame retardants added thereto have poor flame retardancy or large color difference variations.
It will be appreciated by those of ordinary skill in the art that the examples provided herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited examples and embodiments. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (10)
1. The flame-retardant polycarbonate composition is characterized by comprising the following components in parts by weight:
2. the flame retardant polycarbonate composition of claim 1, comprising the following components in parts by weight:
65-85 parts of polycarbonate;
4-15 parts of SAN;
2-7 parts of ASA rubber powder;
2-12 parts of a phosphazene flame retardant;
0.4-1 part of triazine UV absorbent;
0.4-1 part of benzotriazole weather resistant agent;
0.5-1 part of hindered amine weather resistant agent;
0.1-1 part of anti-dripping agent;
0.5-8 parts of toner.
0.1-0.5 part of antioxidant
0.05-0.2 parts of metal passivator;
0.1-0.5 part of other processing aids.
3. The flame-retardant polycarbonate composition according to claim 1, wherein the polycarbonate is a bisphenol A polycarbonate synthesized by a phosgene method, and has a melt index of 3-20 g/10min at 300 ℃ and 1.2 kg;
the content of acrylonitrile in the SAN is 20-35 wt%;
the rubber particle size 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 triazine-based UV absorber is a material having the structure:
wherein R is1、R2、R3And R4Independently selected from alkyl or H, R5Is alkyl or hydroxy ether.
5. The flame retardant polycarbonate composition of claim 1, wherein the benzotriazole weather resistant agent is one or two of methyl 3- (3- (2H-benzotriazole-2-yl) -5-tert-butyl-4-hydroxyphenyl) propionate and PEG300 or 2- (2 ' -hydroxy-3 ', 5 ' -di-tert-amylphenyl) benzotriazole.
6. The flame retardant polycarbonate composition of claim 1, wherein the hindered amine based weathering agent is a hindered amine based radical scavenger.
7. The flame retardant polycarbonate composition of claim 1, wherein the phosphazene flame retardant is a phenoxyphosphazene 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-octadecyl ester or tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, and the auxiliary antioxidant is one or more of tris (2, 4-di-tert-butylphenyl) phosphite, pentaerythritol tetrakis (3-laurylthiopropionate), 3- (dodecylthio) propionic acid-2, 2-bis [ [3- (dodecylthio) -propionyloxy ] methyl ] -1, 3-propanediol ester cyclic pentaerythritol tetrakisbis (2, 6-di-tert-butyl-4-methylphenyl phosphite);
the toner is one or two of titanium dioxide or carbon black;
the metal passivator is carbonyl condensate containing amino or ester containing phosphorus.
8. The flame retardant polycarbonate composition of claim 1, wherein the other processing aid is one or more of a lubricant or a flow modifier.
9. The method for preparing the flame retardant polycarbonate composition of any one of claims 1 to 8, comprising the steps of: 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.
10. Use of the flame retardant polycarbonate composition of any of claims 1 to 8 in the preparation of a UV curable article.
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| CN115433447A (en) * | 2022-08-04 | 2022-12-06 | 青岛国恩科技股份有限公司 | Weather-resistant charging pile shell material and preparation method thereof |
| CN115975367A (en) * | 2023-02-24 | 2023-04-18 | 金发科技股份有限公司 | Polycarbonate composition with good processing stability and preparation method and application thereof |
| CN115975367B (en) * | 2023-02-24 | 2024-05-14 | 金发科技股份有限公司 | Polycarbonate composition with good processing stability, and preparation method and application thereof |
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