CN103724979B - A kind of high flowing heatproof LED PPO/PA composition and method of making the same - Google Patents
A kind of high flowing heatproof LED PPO/PA composition and method of making the same Download PDFInfo
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Abstract
The present invention relates to a kind of high flowing heatproof LED PPO/PA composition and method of making the same, be made up of the component of following mass percentage: polyphenylene oxide 20-50%; Polymeric amide 20-50%; Compatilizer 2-8%; Fire retardant 5-15%; Polyolefine 2-15%; Titanium dioxide 10-25%; Toughner 2-10%; Dispersion agent 1-4%; Oxidation inhibitor 0.2-0.6%, by titanium dioxide dry add dispersion agent, polyphenylene oxide, polymeric amide, compatilizer, toughner and oxidation inhibitor, added by twin-screw extrusion owner spout; Added by feeding pump by twin screw extruder the 4th section of cylindrical shell after fire retardant and polyolefine are mixed in proportion; Extruding pelletization.Height flowing heatproof LED PPO/PA composition of the present invention, there is superior thermotolerance, the opacifying property of superelevation and the mobility of excellence, and good flame retardant resistance and dimensional stability, meet the requirement of ROHS and Reach regulation, realize the production of the product such as LED charactron and lattice module of 0.2mm thickness.
Description
Technical field
The invention belongs to polymeric material field, especially relate to a kind of high flowing heatproof LED PPO/PA composition and method of making the same.
Background technology
Polyphenylene oxide (Polyphenyleneether, be called for short PPE or PPO) be a kind of high performance thermoplastic engineering plastic with good mechanical property, chemical stability, dielectric properties, thermotolerance and flame retardant resistance, but PPO molecular chain rigidity is larger, notch shock is very responsive, its higher melt viscosity, causes it shortcoming such as oil-proofness difference of injection moulding and PPO can not significantly limit its application.Usual PPO and other macromolecular materials use as composition, common are PPO/HIPS composition, PPO/PA composition etc.
In existing invention technology, about the LED composition of the PPO composition of high shading mainly PPO and HIPS, the temperature tolerance of this composition is poor, and LED industry requires more and more higher to the temperature tolerance of material.As patent CN101195704A discloses a kind of PPO/HIPS composition, but the temperature tolerance of this material is not high, and dispersed not ideal enough, and performance is on the low side.For LED industry, under the prerequisite meeting opacifying property, product gets over Bao Yuehao, while this just requires that material therefor has high opacifying property, requirement material is had to have high workability, to meet the injection moulding requirement of thin-wall product, a kind of PPO/HIPS composition disclosed in patent CN101307179A, although adopt LLDPE or TPE etc. to improve and toughner as mobility, but the impact property of material and mobility are still undesirable, and the production of 0.3MM thin-gage goods can only be met, and adopt PPO/HIPS composition, the temperature tolerance of material is still undesirable; And for example patent CN103021281A discloses a kind of light-emitting diode display PPO height light screening material, have employed PPO and titanium dioxide as overcover, although the temperature tolerance of material is improved, but well-known pure PPO mobility is very poor, can not injection moulding, therefore the injection moulding demand of thin-wall product can not be met, simultaneously due to its poor mobility, the bad dispersibility of overcover in resin, opacifying power is undesirable and production cost is higher.
Application number be 200810067341.5 Chinese patent disclose a kind of flame-retardant PPO/PA Alloy And Preparation Method, adopt following component and formula: PPO30-50, PA10-60, toughner 3-15, composite flame-retardant agent 5-15, compatilizer 3-10, other auxiliary agent 0.5-2, although be a kind of fire-retardant PPO/PA alloy material, but this material does not possess opacifying property, can not meet the requirement of LED industry to the high opacifying property of material therefor.Secondly, adopt nitrogen-phosphorus compound flame retardant, the flowing property of material and mechanical property have obvious decline.
Summary of the invention
Object of the present invention is exactly provide a kind of high flowing heatproof LED PPO/PA composition and method of making the same to overcome defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
A kind of high flowing heatproof LED PPO/PA composition, is prepared by the component of following mass percentage:
Preferably, in described polyphenylene oxide 25 DEG C of chloroforms, particular viscosity is 0.2 ~ 0.6dl/g.PPOLXR038, PPOLXR045 and PPOLXR050 that polyphenylene oxide can select Ruicheng branch office of Lanxing Chemical New Material Co., Ltd. to produce.
Preferably, described polymeric amide comprises PA6 and PA66.The PA66EPR2.7 that tafelberg Shen Ma company produces can be selected, the PA61013B that Jiangsu Rui Meifu Industrial Co., Ltd. produces.
Preferably, described compatilizer is SEBS grafts.The FG1901 that Ke Teng company of the U.S. produces can be selected.
Preferably, described halogen-free flame retardants is organic phosphorus flame retardant.
Preferably, described phosphorus flame retardant is one or more in tricresyl phosphate second fat, metaphenylene tetraphenyl diphosphate (RDP), dihydroxyphenyl propane two (diphenyl phosphoester).
Preferably, described polyolefine is polyisobutene, molecular weight 400-2400.Korea S great Lin can be selected to produce PB680.
Preferably, described titanium dioxide is rutile-type.The R-105 that du pont company produces can be selected.
Preferably, described toughner is the A-B-A type triblock copolymer (SEBS) of vinylbenzene and divinyl or A-B type Synthetic rubber, isoprene-styrene, hydrogenated, block, diblock or the blend of the two.G1650, G1651, G1652, G1657, G1660, G1730, G1701, G1643, G1645, G1536, G1702 that Ke Teng company of the U.S. produces can be selected.
Preferably, described oxidation inhibitor is high temperature resistant oxidation inhibitor 1098.
Preferably, described dispersion agent is poly-zincic acid amine.
The preparation method of high flowing heatproof LED PPO/PA composition adopts following steps:
(I) titanium dioxide weighing 10-25% by weight ratio puts into stirring and drying machine, and stirring and drying machine design temperature is 80-100 DEG C, adds 1-4% dispersion agent, remix 2-5 minute after stirring and drying 2-5 minute; Then 20-50% polyphenylene oxide is added, 20-50% polymeric amide, 2-8% compatilizer; 2-10% toughner, the oxidation inhibitor mixing of 0.2-0.6% is after 2-5 minute, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 5-15% fire retardant and 2-15% polyolefine be mixed in proportion by weight ratio, added by the feeding pump of twin screw extruder the 4th section of cylindrical shell;
(3) extrude and granulation through twin screw extruder, the rotating speed controlling screw machine is 180-600 rev/min, and temperature is 235-275 DEG C, prepares high flowing heatproof LED PPO/PA composition.
Compared with prior art, the height flowing heatproof LED PPO/PA composition that the present invention prepares has superior thermotolerance, the opacifying property of superelevation and the mobility of excellence, and good flame retardant resistance and dimensional stability, and halogen-free flameproof, meet ROHS and Reach laws and regulations requirement, the product such as LED charactron and lattice module of 0.2mm thickness can be produced, there is following beneficial effect:
(1) because the temperature tolerance of polymeric amide is obviously better than HIPS, therefore polyphenylether/polyamide composition of the present invention is compared with existing polyphenylene oxide/HIPS composition, has more excellent temperature tolerance and better mobility; Compared with existing pure polyphenyl ether material, there is the mobility of superelevation especially.
(2) adopt organic phosphorus flame retardant, one, while making composition have excellent flame retardant resistance, can meet ROHS and Reach laws and regulations requirement; Its two, organic phosphorus flame retardant also uses as softening agent, contributes to improving composition mobility.
(3) adopt polyisobutene as flow ability modifying agent, effectively improve the mobility of composition.Polyisobutene with have and phosphorus flame retardant compound use, produce the addition of forward, thus make composition of the present invention there is excellent mobility.
(4) adopt ammonium polyphosphate as the substep hybrid technique of dispersion agent and uniqueness, effectively raise titanium dioxide dispersion effect in the composition, make composition of the present invention compared with existing LED light screening material, there is higher opacifying property, under thin-wall product, also can meet the shading requirement of LED industry.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
It should be noted that, in following examples:
In polyphenylene oxide 25 DEG C of chloroforms, particular viscosity is 0.2 ~ 0.6dl/g.Select the PPOLXR045 that Ruicheng branch office of Lanxing Chemical New Material Co., Ltd. produces.
Polymeric amide comprises PA6 and PA66.The PA61013B that the PA66EPR2.7 selecting tafelberg Shen Ma company to produce and Jiangsu Rui Meifu Industrial Co., Ltd. produce.
Compatilizer is SEBS grafts, selects the FG1901 that Ke Teng company of the U.S. produces.
Halogen-free flame retardants is organic phosphorus flame retardant, and that select is metaphenylene tetraphenyl diphosphate (RDP).
Polyolefine is polyisobutene, molecular weight 680, selects Korea S great Lin to produce PB680.
Titanium dioxide is rutile-type, selects the R-105 that du pont company produces.
Toughner is the A-B-A type triblock copolymer (SEBS) of vinylbenzene and divinyl or A-B type Synthetic rubber, isoprene-styrene, hydrogenated, block, diblock or the blend of the two.Select G1651 and G1702 that Ke Teng company of the U.S. produces.
Oxidation inhibitor is high temperature resistant oxidation inhibitor 1098.
Dispersion agent is poly-zincic acid amine.
Example I
Raw material is taken by following weight percent content:
(1) R-105 weighing 25% by weight ratio puts into stirring and drying machine, and stirring and drying machine design temperature is 80 DEG C, and stirring and drying adds 4% poly-zincic acid amine after 2 minutes, remix 5 minutes; Then add 20%PPOLXR045,25%PA66EPR2.7,4%FG1901,5%G1651,0.6%1098 mixing is after 3 minutes, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 8%RDP and 8.4%PB680 is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 180 revs/min, and temperature is 235 DEG C.
Embodiment 2
Raw material is taken by following weight percent content:
(1) weigh 12.5%R-105 by weight ratio and put into stirring and drying machine, stirring and drying machine design temperature is 80 DEG C, and stirring and drying adds 1% poly-zincic acid amine after 5 minutes, remix 2 minutes; Then add 50%PPOLXR045,20%PA61013B, 4%FG1901,2%G1701,0.5%1098 mixing is after 5 minutes, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 5%RDP and 5%PB680 is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 600 revs/min, and temperature is 275 DEG C.
Embodiment 3
Raw material is taken by following weight percent content:
(1) weigh 10%R-105 by weight ratio and put into stirring and drying machine, stirring and drying machine design temperature is 100 DEG C, and stirring and drying adds 2% poly-zincic acid amine after 5 minutes, remix 3 minutes; Then add 20%PPOLXR045,50%PA61013B, 2%FG1901,3.8%G1651,0.2%1098 mixing is after 4 minutes, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 10%RDP and 2%PB680 is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 400 revs/min, and temperature is 245 DEG C.
Embodiment 4
Raw material is taken by following weight percent content:
(1) weigh 15%R-105 by weight ratio and put into stirring and drying machine, stirring and drying machine design temperature is 90 DEG C, and stirring and drying adds 2% poly-zincic acid amine after 5 minutes, remix 5 minutes; Then add 25%PPOLXR045,16.7%PA61013B, 10%PA66EPR2.7,5%FG1901,10%G1651,0.3%1098 mixing is after 5 minutes, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 8%RDP and 8%PB680 is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 500 revs/min, and temperature is 250 DEG C.
Embodiment 5
Raw material is taken by following weight percent content:
(I) weigh 15%R-105 by weight ratio and put into stirring and drying machine, stirring and drying machine design temperature is 80 DEG C, and stirring and drying adds 4% poly-zincic acid amine after 5 minutes, remix 2 minutes; Then add 20%PPOLXR045,24.4%PA66EPR2.7,8%FG1901,2.5%G1651,2.5%G1701,0.6%1098 mixing is after 5 minutes, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 15%RDP and 8%PB680 is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 500 revs/min, and temperature is 245 DEG C.
Embodiment 6
Raw material is taken by following weight percent content:
(1) weigh 25%R-105 by weight ratio and put into stirring and drying machine, stirring and drying machine design temperature is 80 DEG C, and stirring and drying adds 4% poly-zincic acid amine after 5 minutes, remix 2 minutes; Then add 20%PPOLXR045,20%PA66EPR2.7,3.8%FG1901,4%G1651,0.2%1098 mixing is after 5 minutes, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 8%RDP and 15%PB680 is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 500 revs/min, and temperature is 245 DEG C.
Comparative example 1
Raw material is taken by following weight percent content:
Wherein HIPS adopts the HIPS622P of Shanghai match section petrochemical iy produced.
Weigh 30%PPOLXR045 by weight ratio, 40%HIPS622P, 20%R-105,5%FG1901,5%G1651 add high mixer mix 5 minutes after by twin screw extruder extruding pelletization, the rotating speed of screw machine is 400 revs/min, and temperature is 245 DEG C.
Comparative example 2
Raw material is taken by following weight percent content:
(1) weigh 25%R-105 by weight ratio and put into stirring and drying machine, stirring and drying machine design temperature is 80 DEG C, and stirring and drying adds 4% poly-zincic acid amine after 5 minutes, remix 2 minutes; Then add 30%PPOLXR045,25%PA66EPR2.7,3.8%FG1901,4%G1651,0.2%1098 mixing is after 5 minutes, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 8%RDP is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 500 revs/min, and temperature is 245 DEG C.
Comparative example 3
Raw material is taken by following weight percent content:
(1) 22%PPOLXR045 is weighed by weight ratio, 22%PA66EPR2.7,3.8%FG1901,4%G1651,0.2%1098; After 25%R-105 mixes 5 minutes, discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 8%RDP and 15%PB680 is mixed in proportion by weight ratio, added by feeding pump by twin screw extruder the 4th section of cylindrical shell.
(3) extrude and granulation by twin screw extruder, the rotating speed of screw machine is 500 revs/min, and temperature is 245 DEG C.
The composition obtained for embodiment 1-6 and comparative example 1-2 carries out physical property detection, and its result is as following table:
Compared with comparative example 1, the height flowing heatproof LED PPO/PA composition prepared by the present invention, under the prerequisite of obscurity reaching peer-level, has more excellent temperature tolerance than the PPO/HIPS material of routine, higher mobility.Compared with comparative example 2, the present invention by adding the polyisobutene improved liquidity, material mobility be greatly improved because the raising of material flowability, cause the fillers dispersed of filling to have clear improvement, the opacifying property of composition is significantly improved.Can find compared with comparative example 3, the present invention adopts ammonium polyphosphate as dispersion agent, adopts unique substep hybrid technique simultaneously, improves titanium dioxide dispersion effect in the composition, thus effectively improves said composition opacifying property.
Height flowing heatproof LED PPO/PA composition of the present invention, there is superior thermotolerance, the opacifying property of superelevation and the mobility of excellence, and good flame retardant resistance and dimensional stability, and halogen-free flameproof, meet ROHS and Reach laws and regulations requirement, the product such as LED charactron and lattice module of 0.2mm thickness can be produced.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (8)
1. a high flowing heatproof LED PPO/PA composition, it is characterized in that, said composition is prepared by the component of following mass percentage:
Described fire retardant is organic phosphorus flame retardant, is selected from one or more in tricresyl phosphate second fat, metaphenylene tetraphenyl diphosphate (RDP) or dihydroxyphenyl propane two (diphenyl phosphoester); Described polyolefine is polyisobutene; Described dispersion agent is poly-zincic acid amine.
2. a kind of high flowing heatproof LED PPO/PA composition according to claim 1, it is characterized in that, the particular viscosity of described polyphenylene oxide in 25 DEG C of chloroforms is 0.2 ~ 0.6dl/g.
3. a kind of high flowing heatproof LED PPO/PA composition according to claim 1, it is characterized in that, described polymeric amide is selected from one or more in PA6 or PA66.
4. a kind of high flowing heatproof LED PPO/PA composition according to claim 1, it is characterized in that, described compatilizer is SEBS grafts.
5. a kind of high flowing heatproof LED PPO/PA composition according to claim 1, it is characterized in that, described titanium dioxide is rutile titanium dioxide.
6. a kind of high flowing heatproof LED PPO/PA composition according to claim 1, it is characterized in that, described toughner is the A-B-A type triblock copolymer (SEBS) of vinylbenzene and divinyl or A-B type Synthetic rubber, isoprene-styrene, hydrogenated, block, diblock or the blend of the two.
7. a kind of high flowing heatproof LED PPO/PA composition according to claim 1, it is characterized in that, described oxidation inhibitor is high temperature resistant oxidation inhibitor 1098.
8. the height flowing heatproof LED preparation method of PPO/PA composition according to any one of claim 1-7, it is characterized in that, the method adopts following steps:
(1) titanium dioxide weighing 10-25% by weight ratio puts into stirring and drying machine, and stirring and drying machine design temperature is 80-100 DEG C, adds 1-4% dispersion agent, remix 2-5 minute after stirring and drying 2-5 minute; Then 20-50% polyphenylene oxide is added, 20-50% polymeric amide, 2-8% compatilizer; 2-10% toughner, the oxidation inhibitor mixing of 0.2-0.6% is after 2-5 minute, and discharging, is added by twin-screw extrusion owner spout after cooling;
(2) take after 5-15% fire retardant and 2-15% polyolefine be mixed in proportion by weight ratio, added by the feeding pump of twin screw extruder the 4th section of cylindrical shell;
(3) extrude and granulation through twin screw extruder, the rotating speed controlling screw machine is 180-600 rev/min, and temperature is 235-275 DEG C, prepares high flowing heatproof LED PPO/PA composition.
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| KR101757578B1 (en) * | 2015-03-10 | 2017-07-13 | 주식회사 엘지화학 | Modified poly(arylene ether) resin composition and molded article produced thereof |
| CN104962072A (en) * | 2015-06-18 | 2015-10-07 | 宁波高新区卓尔化工科技有限公司 | Flame-retardant PPO/PA (poly-p-phenylene oxide /poly-A) alloy |
| CN107141782A (en) * | 2017-06-20 | 2017-09-08 | 苏州旭光聚合物有限公司 | High glaze fiberglass reinforced modification of nylon |
| CN108299823A (en) * | 2017-12-27 | 2018-07-20 | 上海普利特复合材料股份有限公司 | A kind of PPO/PA alloy materials and preparation method thereof suitable for being thinning |
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| CN103044895A (en) * | 2012-12-06 | 2013-04-17 | 上海日之升新技术发展有限公司 | High glow wire halogen-free flame retardant reinforced PPO/PA alloy and preparation method thereof |
| CN103160108A (en) * | 2011-12-09 | 2013-06-19 | 上海杰事杰新材料(集团)股份有限公司 | Halogen-free flame-retardant polyphenylene oxide/polyamide 6 blend alloy as well as preparation and application for same |
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| CN103044895A (en) * | 2012-12-06 | 2013-04-17 | 上海日之升新技术发展有限公司 | High glow wire halogen-free flame retardant reinforced PPO/PA alloy and preparation method thereof |
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