CN103013087A - Special flame-retardant light diffuser grade polycarbonate composition for LED (light-emitting diode) and preparation method thereof - Google Patents
Special flame-retardant light diffuser grade polycarbonate composition for LED (light-emitting diode) and preparation method thereof Download PDFInfo
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- CN103013087A CN103013087A CN201210584205XA CN201210584205A CN103013087A CN 103013087 A CN103013087 A CN 103013087A CN 201210584205X A CN201210584205X A CN 201210584205XA CN 201210584205 A CN201210584205 A CN 201210584205A CN 103013087 A CN103013087 A CN 103013087A
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- diffusing agent
- light diffusing
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- flaming
- expansion stage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92885—Screw or gear
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
Abstract
The invention relates to a special flame-retardant light diffuser grade polycarbonate composition for an LED (light-emitting diode), which comprises the following components in parts by weight: 100 parts of polycarbonate, 0.05-10 parts of light diffuser, 0.1-3 parts of heat stabilizer, 0.1-3 parts of light stabilizer and 5-30 parts of flame retardant. According to the technical scheme, the prepared polycarbonate composition achieves the effect of high-efficiency flame retardant; and the haze and light transmittance of the material are well balanced, thereby greatly widening the application range of the polycarbonate composition in the LED field. The product prepared from the special flame-retardant light diffuser grade polycarbonate composition for an LED has the excellent properties of high environment-friendly flame retardancy and balanced haze and light transmittance, and meets the requirements for use safety of the material under the condition of a severe environment.
Description
Technical field
The invention belongs to the polymer composite field, be specifically related to a kind of LED special-purpose anti-flaming light expansion stage polycarbonate compositions.
Background technology
The more common day incandescent light of LED lamp is energy-conservation 90%, but and the environment-protective circulating utilization will replace in the near future existing general lighting equipment and come into huge numbers of families.Right LED light is strong, dazzling, luminous energy is very high, has limited to a certain extent its application.
Polycarbonate is called for short PC, has water white transparency, transmittance is high, physical strength is high, is applied in the LED industry and has great advantage.Patent CN102219989A discloses a kind of LED light fixture flame-retarding light-diffusing polycarbonate resin composite and preparation method thereof, it reaches highly effective flame-retardant and good light diffusing, but contain bromo element in its compound system that adopts, be difficult to satisfy the European Union environmental protection standard; Patent CN101906244A discloses a kind of fire-retardant light diffusion PC matrix material take PC as matrix, but it makes its goods weathering resistance not good for adding photostabilizer.The disclosed light diffusion group compound take PC as base material of US Patent No. 20090258170A1, it reaches light diffusing and flame retardant resistance, but its flame retardant resistance is lower, only reaches the V-1 level.
Summary of the invention
Technical problem to be solved by this invention provides the LED special-purpose anti-flaming light expansion stage polycarbonate compositions of a kind of Environmental Safety, high flame retardant, mist degree and transparence balance.
Another technical problem to be solved by this invention provides a kind of preparation method of LED special-purpose anti-flaming light expansion stage polycarbonate compositions
The present invention is that the technical scheme that its technical problem of solution adopts is: a kind of LED special-purpose anti-flaming light expansion stage polycarbonate compositions, comprise polycarbonate, light diffusing agent and fire retardant, described composition also includes thermo-stabilizer and photostabilizer, weight by described polycarbonate is 100 parts, the content of described light diffusing agent is the 0.05-10 weight part, the content of described thermo-stabilizer is the 0.1-3 weight part, described photostabilizer is the 0.1-3 weight part, and described fire retardant is the 5-30 weight part.
Further, described polycarbonate is the bisphenol A-type aromatic copolycarbonate, and its weight-average molecular weight is 20000-80000.
Further, described light diffusing agent is the combination of organic light diffusing agent, inorganic light diffusing agent or described organic light diffusing agent and inorganic light diffusing agent, described organic light diffusing agent is the combination of silicone based light diffusing agent, esters of acrylic acid light diffusing agent or described silicone based light diffusing agent and acrylic acid or the like light diffusing agent, and described inorganic light diffusing agent is one or more in nano barium sulfate, silicon-dioxide, calcium carbonate, quartz, the glass fibre etc.
Further, described fire retardant is the combination of Sulfonates fire retardant and organic silicon flame-retardant synergist.
Further, described Sulfonates fire retardant is potassium phenylsulphonyl benzene sulfonate, perfluoro butyl potassium sulfonate, 2,4, one or more in the 5-trichlorobenzene sodium sulfonate.
Further, described organic silicon flame-retardant synergist is polysiloxane, described polysiloxane comprises polydimethylsiloxane, cyclohexyl methyl siloxanes, aminosiloxane, PSI, one or more of polyethers polysiloxane, poly-aminopropyl phenyl silsesquioxane.
Further, described thermo-stabilizer is one or more in Hinered phenols, aromatic amine, Benzopyranone kind, sulfide, thioether, the inferior ester of triphosphoric acid and the phosphoric acid ester.
Further, described photostabilizer is one or more in benzophenone, benzotriazole category, salicylate class, cyanoacrylate and the triazines.
Further, described composition also includes one or more in lubricant, releasing agent, white dyes, static inhibitor, the tinting material.
A kind of preparation method of LED special-purpose anti-flaming light expansion stage polycarbonate compositions, concrete steps are as follows:
(1) takes by weighing in proportion polycarbonate, light diffusing agent, fire retardant, photostabilizer, thermo-stabilizer, selectivity adds one or more in lubricant, releasing agent, white dyes, static inhibitor, the tinting material, carries out mechanical pre-mixing even in homogenizer;
(2) melt blending in the mixed material adding twin screw extruder is extruded, forcing machine is established ten sections altogether, 180-250 ° of C of first paragraph temperature, 280 ° of C-310 ° of C of second to ten section temperature, die head temperature 300-320 ° C, extruder double-screw rotating speed 200-350r/min;
(3) water-bath cooling, air blast dry up, pelletizing.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
1, the present invention adopts environment friendly non-halogen sulfonate and organic silicon compound flame-retardant system, do not affect the transparency of polycarbonate itself, adopt simultaneously inorganic and organic light diffusing agent compound system, so that the polycarbonate compositions of preparation is when reaching efficient flame-retarding agent, the mist degree of material and transmittance reach a good balance, have greatly increased the range of application of polycarbonate compositions in the LED field.
2, the product of LED special-purpose anti-flaming light expansion stage polycarbonate compositions of the present invention preparation possesses the excellent properties of high-environmental flame retardant resistance and mist degree and transmittance balance, satisfies the materials'use safety under the severe rugged environment condition.
Embodiment
The below will come the present invention is further specified by specific embodiment, but described embodiment only is used for explaining the present invention, be not restriction the present invention.
Polycarbonate among the polycarbonate compositions embodiment of the present invention is preferentially selected the aromatic copolycarbonate of the trade mark PGPC1218 of Iranian petrochemical iy produced; Light diffusing agent is preferably used Korea S Cologne organosilicon light diffusing agent KS-500, the HES-FR Sulfonates fire retardant that fire retardant preferentially selects U.S. Arichem company to produce, the FCA-107 organic silicon flame-retardant synergist that fire retarding synergist preferentially selects Dow Corning Corporation to produce, photostabilizer is preferentially selected benzotriazole category, such as 2-(2H-benzotriazole-2-yl)-4, two (1-methyl isophthalic acid-styroyl) phenol of 6-, UV-P etc. are for commercially available; Thermo-stabilizer is preferably Hinered phenols antioxidant, such as N, and N '-hexamethylene-two-［ 3,5-di-t-butyl-4-hydroxybenzene propionic acid amide ］, N, N '-two [3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl hydrazine] etc. are for commercially available; Processing aid is lubricant, releasing agent, white dyes, static inhibitor, tinting material etc., is commercially available.
Embodiments of the invention adopt the method that is prepared as follows:
By weight, first the PC base material was dried 10 hours under 100 ° of C, PC base material, light diffusing agent, fire retardant, thermo-stabilizer, photostabilizer and the processing aid etc. that drying is good mix in high-speed mixer afterwards, join afterwards melt blending in the twin screw extruder, extruding pelletization, obtain blended compound material.
Gained composite material by adopting following methods of the present invention or standard are carried out performance test, all need at 23 ° of C ± 2 ° C of temperature, under the condition of humidity 50% ± 5%, deposit and be not less than 16 hours before all batten tests:
Tensile strength: test clamp distance according to standard A STM D638: 110mm; Rate of extension: 50mm/min; Thickness of sample: 3.2mm; Sample width: 12.7mm;
Notched Izod impact strength: press ASTM D256 method, the sample that 3.2mm is thick;
Heat-drawn wire: test by ASTM D648,120 ° of C/h of temperature rise rate test under the 1.82MPa load.
Transmittance: test by ASTM D1003.
Mist degree: test by ASTM D1003.
Vertical combustion: test the test of 1.6mm batten by UL-94.
Xenon lamp aging: test irradiance 0.51W/ (m by ASTM G155/G26 standard
2.Nm) 340nm, illumination 102min, (65+2) ° CBST, (40 ~ 60) %RH, illumination and spray 18min, filter: Daylight, total open-assembly time 263KJ/m2 (168h).
The ash mark is estimated: press the ISO105-A02 standard as judgement criteria.
For the ease of better explanation, the below lists in table 1 for each Example formulations that the present invention provides, and its test result is listed in table 2.
Each Example formulations of table 1
| Component | Comparative Examples 1 | Comparative Examples 2 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| PC/% | 97 | 89 | 87.2 | 85.2 | 83.2 | 81.2 |
| Light diffusing agent/% | 3 | 0 | 1 | 3 | 3 | 5 |
| Fire retardant/% | 0 | 8 | 8 | 8 | 10 | 8 |
| Fire retarding synergist/% | 0 | 3 | 3 | 3 | 3 | 5 |
| Thermo-stabilizer/% | 0 | 0 | 0.3 | 0.3 | 0.3 | 0.3 |
| Photostabilizer/% | 0 | 0 | 0.3 | 0.3 | 0.3 | 0.3 |
| Processing aid/% | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
Each embodiment resulting materials the performance test results of table 2
| Project | Comparative Examples 1 | Comparative Examples 2 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Tensile strength/MPa | 64 | 66 | 68 | 68 | 70 | 66 |
| Notched Izod impact strength J/m | 80 | 80 | 82 | 89 | 86 | 84 |
| Heat-drawn wire/° C | 143 | 142 | 141 | 142 | 141 | 142 |
| Transmittance/% | 85 | 80 | 78 | 78 | 80 | 76 |
| Mist degree/% | 80 | 50 | 56 | 80 | 80 | 88 |
| Vertical combustion/level | V-2 | V-1 | V-1 | V-1 | V-0 | V-0 |
| Gray level/level | 3 | 3 | 4 | 4 | 4 | 4 |
Can be found out by embodiment, the not only halogen-free environmental of polycarbonate composite material of the present invention, and have premium propertiess such as high flame retardant, mist degree and transmittance balance, high-weatherability, and kept the good mechanical property of polycarbonate, can satisfy the materials'use safety under the severe rugged environment condition, enlarge the range of application of LED.
Above the present invention has been done detailed description, but the present invention is not limited to above embodiment, the equivalence that all essence according to the present invention is done changes or modifies, all within protection scope of the present invention.
Claims (10)
1. LED special-purpose anti-flaming light expansion stage polycarbonate compositions, comprise polycarbonate, light diffusing agent and fire retardant, it is characterized in that: described composition also includes thermo-stabilizer and photostabilizer, weight by described polycarbonate is 100 parts, the content of described light diffusing agent is the 0.05-10 weight part, the content of described thermo-stabilizer is the 0.1-3 weight part, and described photostabilizer is the 0.1-3 weight part, and described fire retardant is the 5-30 weight part.
2. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 1, it is characterized in that: described polycarbonate is the bisphenol A-type aromatic copolycarbonate, its weight-average molecular weight is 20000-80000.
3. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 1, it is characterized in that: described light diffusing agent is the combination of organic light diffusing agent, inorganic light diffusing agent or described organic light diffusing agent and inorganic light diffusing agent, described organic light diffusing agent is the combination of silicone based light diffusing agent, esters of acrylic acid light diffusing agent or described silicone based light diffusing agent and acrylic acid or the like light diffusing agent, and described inorganic light diffusing agent is one or more in nano barium sulfate, silicon-dioxide, calcium carbonate, quartz, the glass fibre etc.
4. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 1, it is characterized in that: described fire retardant is the combination of Sulfonates fire retardant and organic silicon flame-retardant synergist.
5. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 4, it is characterized in that: described Sulfonates fire retardant is potassium phenylsulphonyl benzene sulfonate, perfluoro butyl potassium sulfonate, 2,4, one or more in the 5-trichlorobenzene sodium sulfonate.
6. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 4, it is characterized in that: described organic silicon flame-retardant synergist is polydimethylsiloxane, cyclohexyl methyl siloxanes, aminosiloxane, PSI, one or more of polyethers polysiloxane, poly-aminopropyl phenyl silsesquioxane.
7. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 1 is characterized in that: described thermo-stabilizer is one or more in Hinered phenols, aromatic amine, Benzopyranone kind, sulfide, thioether, the inferior ester of triphosphoric acid and the phosphoric acid ester.
8. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 1, it is characterized in that: described photostabilizer is one or more in benzophenone, benzotriazole category, salicylate class, cyanoacrylate and the triazines.
9. LED special-purpose anti-flaming light expansion stage polycarbonate compositions according to claim 1, it is characterized in that: described composition also includes one or more in lubricant, releasing agent, white dyes, static inhibitor, the tinting material.
10. the preparation method of each described LED special-purpose anti-flaming light expansion stage polycarbonate compositions of claim 1 ~ 9 is characterized in that, concrete steps are as follows:
Take by weighing in proportion polycarbonate, light diffusing agent, fire retardant, photostabilizer, thermo-stabilizer, selectivity adds one or more in lubricant, releasing agent, white dyes, static inhibitor, the tinting material, carries out mechanical pre-mixing even in homogenizer;
Mixed material is added in the twin screw extruder melt blending extrude, forcing machine is established ten sections altogether, 180 ~ 250 ℃ of first paragraph temperature, 280 ~ 310 ℃ of second to ten section temperature, 300 ~ 320 ℃ of die head temperatures, extruder double-screw rotating speed 200 ~ 350r/min;
Water-bath cooling, air blast dry up, pelletizing.
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| CN103242593A (en) * | 2013-05-15 | 2013-08-14 | 北京化工大学 | Antistatic material, self-cleaning light diffusion plate prepared therefrom, and preparation method of self-cleaning light diffusion plate |
| CN103319871A (en) * | 2013-05-30 | 2013-09-25 | 傅轶 | Remotely-excited fluorescent polycarbonate composite material and preparation method thereof |
| CN103387741A (en) * | 2013-08-20 | 2013-11-13 | 南通市东方塑胶有限公司 | Polycarbonate material with excellent transparent light diffusion function and preparation method thereof |
| CN103709708A (en) * | 2013-12-19 | 2014-04-09 | 上海日之升新技术发展有限公司 | High-flowability fiberglass-reinforced halogen-free flame-retardant PC (polycarbonate) material and preparation method for same |
| CN103724971A (en) * | 2013-12-31 | 2014-04-16 | 上海长伟锦磁工程塑料有限公司 | Transparent halogen-free low smoke antiflaming polycarbonate composite material and preparation method thereof |
| CN103788614A (en) * | 2014-01-14 | 2014-05-14 | 深圳市奥晶科技有限公司 | Halogen-free flame retardant super-tough type polycarbonate material |
| CN104341761A (en) * | 2013-07-31 | 2015-02-11 | 深圳市奥晶科技有限公司 | Glass fiber alloy flame-retardant material and preparation method thereof |
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| CN105968771A (en) * | 2016-06-28 | 2016-09-28 | 中广核俊尔新材料有限公司 | High-flame-resistance high-strength high-reflection polycarbonate material as well as preparation method thereof and application thereof |
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