CN101104730A - Low-fluorine anti-flaming polycarbonate/cinnamenyl resin composition - Google Patents
Low-fluorine anti-flaming polycarbonate/cinnamenyl resin composition Download PDFInfo
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- CN101104730A CN101104730A CNA2006100289394A CN200610028939A CN101104730A CN 101104730 A CN101104730 A CN 101104730A CN A2006100289394 A CNA2006100289394 A CN A2006100289394A CN 200610028939 A CN200610028939 A CN 200610028939A CN 101104730 A CN101104730 A CN 101104730A
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Abstract
The invention relates to a flame-retardant polycarbonate/styryl resin composition with low fluorine content, whose components and proportions are as follow: polycarbonate 50 percent to 85 percent, styrol resin 5 percent to 30 percent, phosphorus-containing flame retardant 5 percent to 15 percent, epoxy resin 0.5 percent to 5 percent, white carbon black 1 percent to 10 percent, fluoropolymer 0 to 0.1 percent and antioxidant 0 to 0.5 percent, the above contents are all in weight percentage. The content of polytetrafluoroethylene in the resin composition of the invention is not over 0.1 percent, and the resin composition can satisfy the operation requirement in higher temperature and stricter environmental protection conditions.
Description
Technical field
The present invention relates to a kind of fire-retardant polycarbonate/styren-based resin composition of low fluorine content.
Background technology
Polycarbonate (PC) and ABS composition have good thermotolerance, impact and good processibility.This alloy is widely used in automobile component, household electrical appliance and electronic devices and components.The material that is used for household electrical appliance and business automation equipment shell has fire-retardant requirement, adds halogen compounds usually so that flame retardant resistance to be provided.The fire-retardant PC/ABS composition of Halogen has excellent performance, but because the fire-retardant resin of halogen contained compound can discharge a large amount of cigarettes and obnoxious flavour when burning, the use order benefit of halogen flame is restricted, and using halogen-free flame retardants is the direction that develops at present.
The halogen-free, flame-retardant composition that contains the poly-carbonic acid vinegar resin of aromatics, styryl graft copolymer, fluoropolymer and phosphor-containing flame-proof compound is known, for example U.S. Pat 5,204,394 patents have been announced the halogen-free flame retardant PC/ABS of phosphor-containing flame-proof compound, these compositions have excellent flame-retardant performance and thermotolerance, but contain the tetrafluoroethylene of 0.2-0.5% weight part at the composition of per 100 parts of resins.In some applications, fluorine content in the flame-retardant material composite is subjected to the restriction of government regulations, for example (check of cable and insulated conductor: regulation the checking of halogen compound) is limited in admissible fluorine content and is less than or equal to 0.1wt% at DIN/VDE 0472 Part 815.
CN 1300308 has announced that a kind of fluorine content equals the preparation method of the fire-retardant combination of 0.1wt%, but in these compositions,, used more high-load phosphonium flame retardant although fluorine content is no more than 0.1wt%, the resistance toheat that causes composition reduces as vicat softening temperature.
Summary of the invention
The object of the invention provides a kind of halogen-free and flame-retardant polycarbonate/styren-based resin composition of low fluorine content, with satisfy DIN/VDE 0472 Part 815 require low fluorine content, have a composition of good flame retardancy simultaneously.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of fire-retardant polycarbonate/styren-based resin composition of low fluorine content, its composition and proportioning are: polycarbonate is 50%-85%, styrene resin is 5%-30%, phosphonium flame retardant is 5%-15%, Resins, epoxy is 0.5%-5%, white carbon black is 1%-10%, and fluoropolymer is 0-0.1%., oxidation inhibitor is 0-0.5%, above content is weight percentage.
Described polycarbonate is the bisphenol A-type aromatic copolycarbonate.
Described styrene base resin is selected from a kind of in the graft resin of the multipolymer of multipolymer, vinylbenzene or the vinylbenzene of vinylbenzene or vinylbenzene and vinyl monomer and vinyl monomer and diene rubber.
Described superfine white carbon black be particle diameter between 5nm ~ 5 μ m, surface-area is at 150 ~ 400m
2The vapor phase process of/g or precipitated silica compound.
Described fire retardant is selected from phosplate, one or more in the biphosphonate.
Described composition also can comprise filler, thermo-stabilizer, static inhibitor, fortifying fibre, lubricant, coupling agent, anti-dripping agent etc.
In preferred embodiments, polycarbonate resin component of the present invention is the linear polycarbonate derived from the dihydroxyphenyl propane photoreactive gas.
In preferred embodiments, the weight-average molecular weight of polycarbonate resin of the present invention is 20000-40000g/mol, and polycarbonate resin of the present invention is known and can obtains by a plurality of commercial source.
The typical example of used styrene base resin of the present invention comprises: ABS (third rare nitrile-butadiene-styrene copolymer), ASA (the rare lonitrile copolymer of acrylate-vinylbenzene-third), SAN (the rare lonitrile copolymer of vinylbenzene-third), HIPS (high-impact polystyrene) and their miscellany.
The used Resins, epoxy of the present invention can be that oxirane value is the bisphenol A type epoxy resin of 0.1-1.0 equivalent/100 grams, and preferred oxirane value is the bisphenol A type epoxy resin of 0.4-0.6 equivalent/100 grams.
The used phosphonium flame retardant of the present invention can be: tricresyl phosphate methyl ester, tricresyl phosphate ethyl ester, Triphenyl phosphate, Resorcinol biphosphonate, preferred Resorcinol biphosphonate.
Described fluoropolymer is a tetrafluoroethylene, and oxidation inhibitor is tetramethylolmethane stearic bicine diester bis-phosphite.
The present invention is by adding the method for white carbon black and Resins, epoxy simultaneously in the composition of phosphor-containing flame-proof PC/ABS, can make that the consumption of fluoropolymer is no more than 0.1% in the composition, and composition still has good resistance burning drippage property, satisfy the requirement of UL-94 flame-retardant V 0-stage and other simultaneously, DIN/VDE 0472 Part 815 etc. for example is about being limited in admissible fluorine content the provisions of laws and regulations that is less than or equal to 0.1wt%; Simultaneously, compare with present prior art, because composition of the present invention does not improve the consumption of phosphonium flame retardant, therefore composition of the present invention has higher resistance toheat, as vicat softening temperature and more excellent mechanical mechanics property.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but described embodiment only is used to illustrate the present invention rather than restriction the present invention.
Embodiments of the invention adopt following material:
Polycarbonate-1, U.S. Dow chemical company, weight-average molecular weight is about 27,000, trade mark Calibre 201-10;
Polycarbonate-2, U.S. Dow chemical company, weight-average molecular weight is about 30,000, trade mark Calibre 301-5;
Acrylonitrile-butadiene-phenylethene grafted copolymer ABS, GE company, Blendex 338, and divinyl rubber content is 70%;
Acrylonitritrile-styrene resin SAN, Taiwan Qi Mei company, PN-127H
Resins, epoxy, the E-51 of Shanghai Resin Factory
White carbon black 1, particle diameter are 12nm, surface-area 200m
2/ g, vapor phase process
White carbon black 2, particle diameter are 2 μ m, surface-area 150m
2/ g, the precipitator method
White carbon black 3, particle diameter is about 5nm, surface-area 380m
2/ g, vapor phase process
Fire retardant RDP, Resorcinol biphosphonate, U.S. big lake company, Reofos RDP;
Fluoropolymer PTFE master batch is used the SAN resin-coated, and the quality percentage composition of fluoropolymer PTFE is 50%, Daikin AD-001;
Oxidation inhibitor, tetramethylolmethane stearic bicine diester bis-phosphite, GE plastics fine chemicals, Weston 619F.
The product performance testing method:
Tensile property: press ASTM D638 method, draw speed 50 mm/min.
Bending property: press ASTM D790 method, trial speed 2 mm/min.
IZOD notched Izod impact strength: press ASTM D256 method, the sample of 3.2 mm thick.
Vicat softening temperature: press ASTM D1525 method, 50 ℃/minute of temperature rise rates are tested under 5 kilograms of load.
Flame retardant properties: according to U.S. UL-94 standard testing vertical combustion performance, strip thickness is 1.6 millimeters.
Embodiment 1-3 and reference examples 1-2:
After mixing by proportion of composing in the table 1, exsiccant PC resin, ABS resin and fire retardant and other auxiliary agent join twin screw extruder (screw diameter 35mm passing through, length-to-diameter ratio L/D=36) in the main barrel, wherein Resorcinol biphosphonate RDP fire retardant is to use the liquid feeding device of band well heater to pump into from the extruder barrel middle part.Each section of main barrel controlled temperature (exporting from charging opening to head) is respectively 180 ℃, 210 ℃, 240 ℃, 250 ℃, 250 ℃, 250 ℃, 240 ℃, and the twin screw rotating speed is 300 rev/mins, and the extruded stock bar obtains product through tank cooling back pelletizing.The said products is injection molded into standard batten with plastic-injection moulding machine in 85 ℃ of dryings after 5 hours in convection oven, 250 ℃ of injection temperatures.The batten of injection formed is in 50% relative humidity, and performance test is carried out in 23 ℃ of placements at least after 24 hours.Actual test result sees Table 1
The composition of the halogen-free flame retardant PC/ABS of table 1 low fluorine content and performance
| Form | Reference examples 1, existing patent | Reference examples 2 | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| PC-1 | 84 | 84 | 84 | ||
| PC-2 | 84.05 | 84 | |||
| The ABS high glue powder | 6 | 6 | 6 | 6 | 6 |
| RDP | 9 | 7 | 7 | 7 | 7 |
| White carbon black-1 | 2 | 2 | |||
| White carbon black-2 | 2 | ||||
| Resins, epoxy E51 | 1 | 1 | 1 | ||
| The master batch that contains 50% fluoropolymer PTFE | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| TiO 2And other additive | 0.75 | ||||
| 619F | 0.2 | 0.2 | 0.4 | 0.2 | |
| Test result | Reference examples 1 | Reference examples 2 | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Tensile strength (MPa) | 64 | 63 | 63 | 54 | 55 |
| Flexural strength (MPa) | 92 | 91 | 90 | 90 | 89 |
| Modulus in flexure (MPa) | 2600 | 2650 | 2600 | 2550 | 2530 |
| Notched Izod impact strength (kJ/m 2) | 52.6 | 53 | 48 | 40 | 62 |
| Vicat softening temperature (℃) | 111.4 | 122 | 123 | 125 | 126 |
| Flame retardant resistance UL94 (1.6mm) | V0 | V2 (drippage) | V0 | V0 | V0 |
As mentioned above, fire-proof resin composition of the present invention, be by in the fire-retardant PC/ABS resin of aromatic phosphoric ester, having added the preparation of specific superfine white carbon black and Resins, epoxy, because the effect (seeing reference examples 2 and embodiment 1-3) that prevents to burn and drip has been played in the adding of superfine white carbon black and Resins, epoxy.Compare with existing patented technology simultaneously, composition provided by the invention adopts the phosphate flame retardant RDP of less amount can arrive the UL-94 flame-retardant V 0-stage, but has the vicat softening temperature (seeing reference examples 1 and embodiment 3) of more superior mechanical property and Geng Gao.
Embodiment 4-8:
Employing is with complete processing and the testing method of embodiment 1-3, just use PC, the ABS resin of different content respectively, the white carbon black of different-grain diameter and content and the Resins, epoxy of different content have prepared halogen-free flame retardant PC/ABS resin composition by the proportion of composing of table 2, and performance test is as shown in table 2.
The composition of the halogen-free flame retardant PC/ABS of table 2 low fluorine content and performance
| Form | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| PC-2 | 50 | 60 | 75 | 85 |
| The ABS high glue powder | 13 | 10 | 6 | 6 |
| SAN | 10 | 10 | ||
| RDP | 15 | 12 | 9 | 6 |
| White carbon black-1 | 6 | 5 | ||
| White carbon black-3 | 10 | 2 | ||
| Resins, epoxy E51 | 2 | 2 | 5 | 1 |
| The master batch that contains 50% fluoropolymer PTFE | 0 | 0.2 | 0.1 | 0.2 |
| 619F | 0.2 | 0.2 | 0 | 0.2 |
| Test result | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Tensile strength (MPa) | 57 | 58 | 56 | 62 |
| Flexural strength (MPa) | 90 | 93 | 90 | 89 |
| Modulus in flexure (MPa) | 2600 | 2670 | 2550 | 2530 |
| Notched Izod impact strength (kJ/m 2) | 23 | 35 | 41 | 62 |
| Vicat softening temperature (℃) | 85 | 96 | 115 | 128 |
| Flame retardant resistance UL94 (1.6mm) | V0 | V0 | V0 | V0 |
As mentioned above, when the Resins, epoxy of white carbon black that uses different-grain diameter and content respectively and different content joins in the fire-retardant PC/ABS resin combination of the aromatic phosphoric ester of different PC, ABS content, because the effect of the drippage that prevents to burn has been played in the adding of superfine white carbon black and Resins, epoxy, the content that therefore can control tetrafluoro ethylene polymer is no more than 0.1% and can satisfies the requirement of UL-94 flame-retardant V 0-stage; Compare with existing patented technology simultaneously, composition provided by the invention adopts the phosphate flame retardant RDP of less amount thereby has the vicat softening temperature of more superior mechanical property and Geng Gao.
The present invention is by adding the method for white carbon black and Resins, epoxy simultaneously in the composition of phosphor-containing flame-proof PC/ABS, can make that the consumption of fluoropolymer is no more than 0.1% in the composition, and composition still has good resistance burning drippage property, satisfy the requirement of UL-94 flame-retardant V 0-stage and other simultaneously, DIN/VDE 0472 Part 815 etc. for example, laws and regulations are about being limited in admissible fluorine content the requirement that is less than or equal to 0.1wt%; Simultaneously, compare with present prior art, because composition of the present invention does not improve the consumption of phosphonium flame retardant, therefore composition of the present invention has higher resistance toheat, as vicat softening temperature and more excellent mechanical mechanics property, therefore has fabulous widespread popularity.Therefore, fire-proof resin composition of the present invention can satisfy the service requirements under higher temperature and the stricter environmental protection condition.
Claims (11)
1. fire-retardant polycarbonate/the styren-based resin composition of a low fluorine content, its composition and proportioning are: polycarbonate is 50%-85%, styrene resin is 5%-30%, phosphonium flame retardant is 5%-15%, Resins, epoxy is 0.5%-5%, and white carbon black is 1%-10%, and fluoropolymer is 0-0.1%, oxidation inhibitor is 0-0.5%, and above percentage ratio is weight percentage.
2. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 1, it is characterized in that: described polycarbonate is the bisphenol A-type aromatic copolycarbonate.
3. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 1 is characterized in that: described styrene base resin is selected from a kind of in the graft resin of the multipolymer of graft resin, vinylbenzene and vinyl monomer of multipolymer, vinylbenzene and diene rubber of vinylbenzene, vinylbenzene and vinyl monomer and diene rubber.
4. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 1 is characterized in that: described superfine white carbon black be particle diameter between 5nm ~ 5 μ m, surface-area is at 150 ~ 400m
2The silicon dioxide compound of/g.
5. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 1, it is characterized in that: described fire retardant is selected from phosplate, one or more in the biphosphonate.
6. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 1 is characterized in that: described styrene base resin is one or more the mixture in third rare nitrile-butadiene-styrene copolymer, the rare lonitrile copolymer of acrylate-vinylbenzene-third, the rare lonitrile copolymer of vinylbenzene-third or the high-impact polystyrene.
7. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 1 is characterized in that: the used Resins, epoxy of the present invention is that oxirane value is the bisphenol A type epoxy resin of 0.1-1.0 equivalent/100 grams.
8. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 7 is characterized in that: the used Resins, epoxy of the present invention is that oxirane value is the bisphenol A type epoxy resin of 0.4-0.6 equivalent/100 grams.
9. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 1, it is characterized in that: described phosphonium flame retardant is a tricresyl phosphate methyl ester, the tricresyl phosphate ethyl ester, a kind of in Triphenyl phosphate and the Resorcinol biphosphonate.
10. fire-retardant polycarbonate/the styren-based resin composition of a kind of low fluorine content according to claim 9, it is characterized in that: the used phosphonium flame retardant of the present invention is the Resorcinol biphosphonate.
11. the fire-retardant polycarbonate/styren-based resin composition of a kind of low fluorine content according to claim 1 is characterized in that: described fluoropolymer is a tetrafluoroethylene, and oxidation inhibitor is tetramethylolmethane stearic bicine diester bis-phosphite.
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| CN102898806A (en) * | 2012-11-06 | 2013-01-30 | 上海冠旗电子新材料股份有限公司 | Antistatic polycarbonate/polyester alloy material and preparation method thereof |
| CN101759981B (en) * | 2008-12-23 | 2013-06-12 | 上海普利特复合材料股份有限公司 | Scale-free low-volatility polycarbonate compound |
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| JP3865295B2 (en) * | 2001-10-11 | 2007-01-10 | 旭化成ケミカルズ株式会社 | Flame retardant resin composition |
| CN1978528A (en) * | 2005-12-05 | 2007-06-13 | 中国石油天然气集团公司 | Low-smoke flame-retarded PC/ABS alloy plate special material |
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| CN101787188B (en) * | 2009-02-06 | 2012-05-23 | 深圳市科聚新材料有限公司 | Flame-retardant PC/HIPS composite material and preparation method thereof |
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| CN104004338B (en) * | 2014-06-16 | 2016-01-13 | 上海中镭新材料科技有限公司 | Hydrolysis antistatic PC/ASA Alloy And Preparation Method |
| WO2018095357A1 (en) * | 2016-11-23 | 2018-05-31 | 厦门大学 | Fluorine-containing silicon polyphosphate ester and method for preparation thereof |
| US11046816B2 (en) | 2016-11-23 | 2021-06-29 | Xiamen University | Method for preparing fluorine-silicon-containing polyphosphate ester and flame retardant epoxy resin |
| CN106957518A (en) * | 2017-05-05 | 2017-07-18 | 安徽彩晶光电有限公司 | Shell alloy material after a kind of high-ductility LCD TV |
| CN107141758A (en) * | 2017-06-27 | 2017-09-08 | 过春明 | A kind of transparent PC material fire-retardant master granule and its preparation method and application |
| CN107383664A (en) * | 2017-09-15 | 2017-11-24 | 安徽江淮汽车集团股份有限公司 | A kind of PS PC composites and preparation method thereof |
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