CN102337017A - Polycarbonate composition with LED (Light-emitting Diode) photoconversion function and application thereof - Google Patents
Polycarbonate composition with LED (Light-emitting Diode) photoconversion function and application thereof Download PDFInfo
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Abstract
The invention discloses a polycarbonate composition with LED (Light-emitting Diode) photoconversion function and application thereof. The polycarbonate composition comprises the following components in percentage by weight: (a) 40-98.9 percent of polycarbonate resin; (b) 1-50 percent of fluorescent powder; and (c) 0.1-10 percent of other additives, wherein the other additives are one or more varieties of flame retardants, antioxidants, mold parting agents and weathering agents, and the starting temperature for thermal decomposition of each additive is equal to or larger than 260 DEG C. The polycarbonate composition with LED photoconversion function has the advantages that the added additives have the characteristic of high thermal stability, so that the additives have stable performance and are not easy to decompose, and the polycarbonate composition has high light transmittance rate and superior comprehensive properties.
Description
Technical field
The present invention relates to the LED field of light emitting materials, relate in particular to a kind of polycarbonate compositions that can in the luminous field of LED, use with light transition function.
Background technology
Led light source is the abbreviation of photodiode, has the brightness height, the advantage of saving energy, and at present, white light LEDs has begun to get into the commercial application stage.Utilize the LED technology to realize that the method for white light mainly contains three kinds: 1. red, green, blue three-primary color LED chipset is fitted together the realization white light, the shortcoming of this method is to cause the drift of the chromaticity coordinates of mixed white light easily; 2. combine with the jaundice emitting phosphor YAG:Ce that can effectively be excited by blue light with the blue led chip, form white light LEDs, a part of blue light is absorbed by fluorescent material; Excitated fluorescent powder emission gold-tinted; The gold-tinted and the remaining blue light of emission are regulated and control their strength ratio, can obtain the white light of various colour temperatures; Because what adopt is light-converting material; In fact lack the red spectrum composition in this white light, so the color developing of light source is relatively poor, also can add can blue-light excited be glowed, green light fluorescent powder obtains white light; 3. the near ultraviolet excitation red, green, blue three primary colors fluorescent powder that utilizes the near ultraviolet LED chip to send obtains white light.2. present stage mainly adopts, 3. the kind method prepare white light LEDs.
At present, mainly adopting fluorescent material and silica gel or epoxy resin uniform mixing and be coated on the led chip is that " some glue " technology prepares led light source.Because the defective of this technology and material itself causes this explained hereafter efficient low, accepted product percentage is not high; The White-light LED chip of producing has not good, the easy problems such as chip light emitting consistence difference that wear out, make of thermal diffusivity.Therefore, need to adopt more reliable material and more easy-operating technology to eliminate above-mentioned defective.
Chinese invention patent CN102020819A discloses plastics light conversion fluorescence pellet and application thereof; It is characterized in that fluorescent material is carried out surface treatment with silane coupling agent; And in prescription, adding erucicamide, N, N-ethylene bis stearamide, whiteruss and polyethylene wax improve the dispersing property of fluorescent material, but these auxiliary agents can cause the transmittance of material to descend to some extent; And can generation separate out behind the life-time service, all can cause disadvantageous effect to the optical property of material.
Chinese invention patent CN101737723A discloses a kind of method of manufacture of LED light converting plate, and this patent has been set forth fluorescent material is obtained light converting plate with the method that various macromolecule resin material blend are extruded simply.Though this method also can obtain to have the material of light transition function, because this method is not considered fast light, the heat aging performance and the processing characteristics of light conversion agent itself, so it does not reach the requirement of practical application to material long-term aging performance and processing characteristics.
Summary of the invention
The object of the present invention is to provide the polycarbonate compositions of the high LED light transition function of a kind of efficiency of conversion, satisfy the actual user demand of LED illumination.
Polycarbonate compositions with LED light transition function according to the invention comprises following component by weight percentage: (a) polycarbonate resin 40 ~ 98.9%; (b) fluorescent material 1-50%; (c) other additives 0.1 ~ 10%; Described other additives are one or more in each based flame retardant, oxidation inhibitor, releasing agent, the weather resisting agent, and thermolysis starting temperature >=260 of every kind of additive ℃.
Said thermolysis starting temperature is defined as material weightless temperature that was reached under nitrogen atmosphere at 1% o'clock.
The transmittance of polycarbonate resin >=85%, as be lower than the light transmission that this transmittance will influence the light conversion PC material of making, thus reduce the light efficiency of whole LED optics.
Described polycarbonate resin is the aromatic polycarbonate resin that those skilled in that art know, and comprises linear polycarbonate resin, branched polycarbonate, copoly type polycarbonate, preferred linear polycarbonate resin; Weight-average molecular weight M
WBe 12000～40000, preferred 20000～30000, described weight-average molecular weight M
WBe to adopt GPC (gel chromatography) to measure.As weight-average molecular weight M
WBe lower than at 12000 o'clock, because molecular weight is too low, cause the mechanical property of materials not good, deterioration easily is not suitable for being used for doing the matrix of light-converting material; And weight-average molecular weight M
WAfter being higher than 40000, the material melt viscosity is high, and it is mobile poor to cause, and is difficult for processing, is unfavorable for the dispersion of fluorescent material, and the high-molecular weight polycarbonate since in building-up process easily because of part " implode " produces " brilliant point ", transmittance can reduce.Solve but also can use through the polycarbonate resin combination collocation of different molecular structures and molecular weight.
Described fluorescent material can be that in blue-light excited type fluorescent material, the near ultraviolet excitation type fluorescent material one or more mix with arbitrary proportion according to the exciting light type; Blue-light excited type fluorescent material can comprise yellow fluorescent powder, red fluorescence powder and green emitting phosphor; Wherein preferred yellow fluorescent powder, and YAG (yttrium aluminum garnet Y most preferably in the yellow fluorescent powder
3Al
5O
12): Ce
3+
Yellow fluorescent powder YAG:Ce
3+Also can pass through Gd
3+, Lu
3+, La
3+, Yb
3+, Tb
3+And Ga
3+, In
3+Plasma part respectively replaces Y
3+And Al
3+Ion has reached change YAG crystalline structure, realizes emmission spectrum red shift and blue shift, thereby makes light-converting material obtain higher colour rendering index (CRI) and correlated(color)temperature (CCT).
The preparation method and the technology of fluorescent material are not limit, and can comprise existing high temperature solid-state method, chemical synthesis and physics synthesis method.
Other additives that added are one or more in each based flame retardant, oxidation inhibitor, releasing agent, the weather resisting agent; And thermolysis starting temperature >=260 of every kind of additive ℃; This patent research learns that the decline of LED light transition function compsn optical property mainly is the decomposition owing to additive, and due to being mingled in the polycarbonate body material; Its impurity of sneaking into is in state of aggregation mostly; Thereby cause whole compsn color spot, brilliant point to occur, and change its optical property in the part and cause its transmittance to descend, thereby the additive of selecting to have certain decomposition starting temperature is necessary.
Fire retardant can be the combination of existing any one fire retardant or several kinds of fire retardants, and said fire retardant can be any one or a few in halogenated flame retardant, the halogen-free flame retardants.As a kind of preferred version, said halogenated flame retardant is tetrabromobisphenol A carbonic ester oligopolymer or oligopolymer and dichloro diphenyl sulfone potassium sulfonate; Said halogen-free flame retardants is Sulfonates fire retardant, phosphoric acid ester fire retardant and silicone based flame retardant; Preferred Sulfonates fire retardant; Like commercially available potassium diphenylsulfone sulfonate or perfluoro butyl potassium sulfonate, above-mentioned selection of fire retardant is a prerequisite with the not obvious light transmission that influences polycarbonate.
Oxidation inhibitor is divided into primary antioxidant and auxiliary antioxidant by effect, and both part by weight scopes are 1:5 ~ 5:1, preferable range 1:3 ~ 3:1.Primary antioxidant comprises phenols and amine; Preferred phenols is as the oxidation inhibitor of polycarbonate; Comprise season amylalcohol four (3-(3, the 5-di-tert-butyl)-4-hydroxybenzene (antioxidant 1010), octadecyl-3-(3,5-two uncles Ding-4-hydroxybenzene)-propionic ester (antioxidant 1076), N; N-normal hexane-1; The 6-dihydroxyl (3-(3,5-di-t-butyl-4-phenylor phenol acetic ester (oxidation inhibitor 1098), vinyl-two (ethenoxy group) two-(3-(5-tertiary butyl-4-hydroxy-tolyl)-propionic ester) (oxidation inhibitor 245), 2,2 '-methylene bis (4-methyl-6-tert butyl phenol (antioxidant 2246).
Auxiliary antioxidant comprises phosphorous acid esters, thioesters class.Phosphorous acid esters comprise: three (2; The 4-di-tert-butyl-phenyl) phosphorous acid ester (oxidation inhibitor 168), triphenyl phosphite (TPP), two (2; 6-two-tertiary butyl-4-tolyl) pentaerythritol phosphite (PEP-36), four (2; 4-two-trimethylphenylmethane base)-4,4 ' biphenyl-two phosphorus phosphorous acid ester (P-EPQ), two (2,4-two withered phenyl) pentaerythritol phosphite (S9228).The thioesters class comprises: sulphur diethylammonium two [3-(3,5-di-t-butyl-4-hydroxybenzene) propionic ester] (oxidation inhibitor 1035), the two lauryl alcohol esters (DLTDP) of thio-2 acid, thio-2 acid stearyl alcohol ester (DSTDP), tetramethylolmethane four (3-lauryl thiopropionate) are (412S).
Described releasing agent comprises organic silicone compound, pentaerythritol tetrastearate (PETS), Zerol, montanic acid wax and other fatty acid ester compounds; Wherein preferred pentaerythritol tetrastearate (PETS) also can be with itself and other one or more composite uses.
Described weather resisting agent comprises hindered amine light stabilizer (HALS) and UV light absorber, and UV light absorber comprises benzotriazole category UV light absorber, benzophenone UV light absorber and Whitfield's ointment ester group UV light absorber.
Hindered amine light stabilizer (HALS) comprising: two (2,2,6,6 ,-tetramethyl pyridine base) sebates (TINUVIN 770), gather-{ 6-[(1; 1,3, the 3-tetramethyl butyl)-amido]-1,3,5-triazines-2; 4-two bases] [(2,2,6, the 6-tetramethyl-piperidyl)-imino--hexa-methylene-[4-(2,2 for 2-; 6,6-tetramethyl-piperidyl)-imino-]] (944), gather [1-(2 '-hydroxyethyl)-2,2,6,6-tetramethyl--4 hydroxy piperidine succinate] (622).
The benzotriazole category UV light absorber comprises: 2-(2-hydroxyl-3; 5-two (1; 1-dimethyl--phenyl)-2H-benzotriazole (TINUVIN 234), 2-(2 '-hydroxyl-5 '-aminomethyl phenyl)-5-benzotriazole (UV-P), 2; 2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-5-chlorinated benzotriazole (UV-327).
UVNUL MS-40 base UV light absorber comprises: 2-hydroxyl-4-eight alkoxy benzophenones (UV-531).
Whitfield's ointment ester group UV light absorber comprises that salol, Whitfield's ointment are to butyl phenyl ester and p-octylphenyl salicylate.
As the photostabilizer of polycarbonate, preferred benzotriazole category UV light absorber also can be with itself and other composite use of one or more UV light absorbers.
The present invention also provides described compsn directly is made into the different shape of LED luminescence chip and the light conversion layer of thickness, makes the light that sends be transformed into white light.Replace existing " some glue " technology through this light conversion layer, thereby enhance productivity and accepted product percentage, improve the thermal diffusivity of led chip, luminous consistence and life-span simultaneously.
The preparation method of the present composition has no particular limits; For example can adopt single screw rod or twin screw extruder to melt extrude above-mentioned each component through mixed uniformly mixture; In order to guarantee the dispersing uniformity of each component of compsn, preferentially adopt the better double screw extrusion method of dispersion effect.
The not special restriction of the forming method of said polycarbonate compositions, available existing forming technique commonly used, for example injection molding method, extrusion moulding, rolling process, blow moulding, vacuum forming, press molding method, foam-formed method and other technologies.
Polycarbonate compositions with LED light transition function according to the invention, its advantage is:
Add additive have the high characteristics of thermostability can make the additive stable performance, be difficult for to decompose, thereby make said composition obtain high transmittance and excellent comprehensive performances.
Embodiment
Below in conjunction with Comparative Examples and embodiment the present invention is explained further details.This embodiment is just in order to specify, and the scope that can not be construed as limiting the invention.
Among Comparative Examples and the embodiment, the fluorescent material that is added be yellow fluorescent powder (Y, Gd)
3(Al, Ga)
5O
12: Ce, red fluorescence powder (Sr, Ba)
2Si
5N
8: Eu, green emitting phosphor (Ba, Sr, Ca)
2SiO
4: Eu.Other additives are fire retardant, oxidation inhibitor, weather resisting agent or releasing agent.
Embodiment 1:
The required raw material of preparation preparation product of the present invention: aromatic series homo-polycarbonate, yellow fluorescent powder, oxidation inhibitor season amylalcohol four (3-(3, the 5-di-tert-butyl)-4-hydroxybenzene and triphenyl phosphites; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 230 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains white light LED part.The concrete ratio of each component is said with table 1.
Embodiment 2:
The required raw material of preparation preparation product of the present invention: silane Copolycarbonate, yellow fluorescent powder, octadecyl-3-(3,5-two uncles Ding-4-hydroxybenzene)-propionic ester and thio-2 acid stearyl alcohol ester; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 240 ℃; The gained plastic pellet can be processed the product of all thickness and shape through technologies such as injection moulding, blowings, is used for the light conversion layer of LED blue chip, thereby obtains white light LED part.The concrete ratio of each component is said with table 1.
Embodiment 3:
The required raw material of preparation preparation product of the present invention: polyester-carbonic ether, yellow fluorescent powder, oxidation inhibitor vinyl-two (ethenoxy group) two-(3-(5-tertiary butyl-4-hydroxy-tolyl)-propionic ester) and tetramethylolmethane four (3-lauryl thiopropionate); Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 280 ℃, and the gained plastic pellet can mix with polycarbonate according to arbitrary proportion as required, again through injection moulding or be blow molded into different shape and the product of thickness; The light conversion layer that is used for the LED blue chip, thus white light LED part obtained.The concrete ratio of each component is said with table 1.
Embodiment 4:
The required raw material of preparation preparation product of the present invention: polycarbonate, blue-light excited type fluorescent material, oxidation inhibitor N; N-normal hexane-1,6-dihydroxyl 3-(3,5-di-t-butyl-4-phenylor phenol acetic ester) and four (2; 4-two-trimethylphenylmethane base)-4,4 ' biphenyl-two phosphorus phosphorous acid ester; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 260 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains the warm white LED device.The concrete ratio of each component is said with table 1.
Embodiment 5
The required raw material of preparation preparation product of the present invention: polyester-carbonic ether, near ultraviolet excitation type fluorescent material, fire retardant tetrabromobisphenol A carbonic ester oligopolymer; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 270 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains white light LED part.This light conversion layer has certain flame retardant properties, and does not influence the original optical characteristics of material basically.The concrete ratio of each component is said with table 1.
Embodiment 6
The required raw material of preparation preparation product of the present invention: silane Copolycarbonate, yellow fluorescent powder, oxidation inhibitor octadecyl-3-(3; 5-two uncles Ding-4-hydroxybenzene)-propionic ester and three (2; The 4-di-tert-butyl-phenyl) phosphorous acid ester, fire retardant dichloro diphenyl sulfone potassium sulfonate, weather resisting agent two (2,2,6; 6 ,-tetramethyl pyridine base) sebate; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 280 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains white light LED part.That this light conversion layer has is fast light preferably, heat aging performance and flame retardant properties, and does not influence the original optical characteristics of material basically.The concrete ratio of each component is said with table 1.
Embodiment 7:
The required raw material of preparation preparation product of the present invention: polycarbonate, yellow fluorescent powder, oxidation inhibitor 2; 2 '-methylene bis (4-methyl-6-tert butyl phenol) and tetramethylolmethane four (3-lauryl thiopropionate), the agent of Sulfonates fire retardant, weather resisting agent gather [1-(2 '-hydroxyethyl)-2; 2; 6,6-tetramethyl--4 hydroxy piperidine succinate], the releasing agent pentaerythritol tetrastearate; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 255 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains white light LED part.The machine-shaping of said composition particle is easy, and that prepared light conversion layer has is fast light preferably, heat aging performance and flame retardant properties, and does not influence the original optical characteristics of material basically.The concrete ratio of each component is said with table 1.
Embodiment 8:
The required raw material of preparation preparation product of the present invention: aromatic series homo-polycarbonate, blue-light excited type fluorescent material, oxidation inhibitor vinyl-two (ethenoxy group) two-(3-(5-tertiary butyl-4-hydroxy-tolyl)-propionic ester) and two (2,6-two-tertiary butyl-4-tolyl) pentaerythritol phosphite, silicone based flame retardant fire retardant, weather resisting agent p-octylphenyl salicylate, releasing agent pentaerythritol tetrastearate; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 245 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains the warm white LED device.The machine-shaping of said composition particle is easy, and that prepared light conversion layer has is fast light preferably, heat aging performance and flame retardant properties, and does not influence the original optical characteristics of material basically.The concrete ratio of each component is said with table 1.
Embodiment 9
The required raw material of preparation preparation product of the present invention: polycarbonate, near ultraviolet excitation type fluorescent material, phenolic antioxidant and thioesters kind antioxidant, fire retardant perfluoro butyl potassium sulfonate, weather resisting agent are gathered [1-(2 '-hydroxyethyl)-2; 2; 6,6-tetramethyl--4 hydroxy piperidine succinate], the releasing agent montanic acid wax; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 260 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains the warm white LED device.The machine-shaping of said composition particle is easy, and prepared light conversion layer has fast light preferably and heat aging performance, and excellent flame-retardant, and does not influence the original optical characteristics of material basically.The concrete ratio of each component is said with table 1.
Embodiment 10
The required raw material of preparation preparation product of the present invention: polycarbonate, blue-light excited type fluorescent material, phosphite ester kind antioxidant, fire retardant perfluoro butyl potassium sulfonate, weather resisting agent UV light absorber, releasing agent Zerol; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 240 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains the warm white LED device.The machine-shaping of said composition particle is easy, and prepared light conversion layer has fast light preferably and heat aging performance, and excellent flame-retardant, and does not influence the original optical characteristics of material basically.The concrete ratio of each component is said with table 1.
Embodiment 11
The required raw material of preparation preparation product of the present invention: polycarbonate, yellow fluorescent powder, phenolic antioxidant, fire retardant dichloro diphenyl sulfone potassium sulfonate, weather resisting agent benzotriazole category UV light absorber, releasing agent Zerol; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 250 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains the warm white LED device.The machine-shaping of said composition particle is easy, and prepared light conversion layer has fast light preferably and heat aging performance, and excellent flame-retardant, and does not influence the original optical characteristics of material basically.The concrete ratio of each component is said with table 1.
Embodiment 12
The required raw material of preparation preparation product of the present invention: aromatic series homo-polycarbonate, blue-light excited type fluorescent material, releasing agent pentaerythritol tetrastearate; Each component is even according to formula rate thorough mixing in high mixer; Join in the twin screw extruder then extrude, tie rod, granulation; Processing temperature is set in 270 ℃; The gained plastic pellet can or be blow molded into different shape and the product of thickness through injection moulding, is used for the light conversion layer of LED blue chip, thereby obtains white light LED part.The concrete ratio of each component is said with table 1.
Comparative Examples 1:
Said raw materials by weight proportioning is following: polycarbonate 96.5%, yellow fluorescent powder 3.0%; Each component is even according to formula rate thorough mixing in high mixer, join in the twin screw extruder then extrude, tie rod, granulation, processing temperature is set in 250 ℃.
Comparative Examples 2:
Said raw materials by weight proportioning is following: polycarbonate 96.5%, yellow fluorescent powder 3.0%, polyethylene wax 0.3%; Each component is even according to formula rate thorough mixing in high mixer, join in the twin screw extruder then extrude, tie rod, granulation, processing temperature is set in 270 ℃.
Each embodiment weight percentages of components of table 1
| ? | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Example 12 |
| Polycarbonate | 96.5 | 89.5 | 49.5 | 89.5 | 96.3 | 96 | 95.7 | 88.7 | 85.7 | 85.7 | 85.7 | 96.5 |
| Yellow fluorescent powder | 3 | 10 | 50 | 10 | 3 | 3 | 3 | 10 | 10 | 10 | 10 | 3 |
| Red fluorescence powder | - | - | - | 0.01 | - | - | - | 0.01 | - | 0.01 | 0.01 | - |
| Fire retardant | - | - | - | - | 0.2 | 0.2 | 0.2 | 0.2 | 3.2 | 5.2 | 8.2 | - |
| Oxidation inhibitor | 0.5 | 0.5 | 0.5 | 0.49 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | - |
| Releasing agent | - | - | - | - | - | - | 0.3 | 0.29 | 0.3 | 0.29 | 0.3 | 0.3 |
| Weather resisting agent | - | - | - | - | - | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.29 | - |
The test result (1) of the said product of each embodiment of table 2
| Project | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Tensile strength | Mpa | 60.7 | 61.4 | 62.4 | 60.8 | 61.2 | 60.3 | 60.3 |
| Flexural strength | Mpa | 96 | 98 | 102 | 97 | 96 | 96 | 96 |
| Modulus in flexure | Mpa | 2270 | 2230 | 2700 | 2280 | 2250 | 2220 | 2250 |
| The IZOD notched Izod impact strength | J/m | 640 | 608 | 420 | 570 | 610 | 602 | 585 |
| 125 ℃ of balls are pressed | ? | Through | Through | Through | Through | Through | Through | Through |
| Flame retardant resistance (1) | Class | 0.5mmHB | 0.5mmHB | 0.5mmHB | 0.5mmHB | 0.5mmV-2 | 0.5mmV-2 | 0.5mmV-2 |
| Flame retardant resistance (2) | Class | 2.0mmV-2 | 2.0mmV-2 | 2.0mmV-2 | 2.0mmV-2 | 2.0mmV-0 | 2.0mmV-0 | 2.0mmV-1 |
| 100 ℃/1000h of thermal ageing | ΔE | 3.2 | 3.4 | 3.3 | 3.4 | 3.3 | 3.3 | 3.5 |
| The xenon lamp aging test | ΔE | 4.2 | 4.3 | 5.1 | 4.5 | 4.6 | 2.6 | 2.9 |
| The glow wire test | ℃ | 750 | 750 | 700 | 700 | 850 | 850 | 850 |
| Transmittance | % | 46 | 27 | 18 | 25 | 45 | 45 | 43 |
The test result (2) of the said product of each embodiment of table 3
| Project | Unit | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 | Embodiment 12 | Comparative Examples 1 | Comparative Examples 2 |
| Tensile strength | Mpa | 60.2 | 61.5 | 61.2 | 61.8 | 61.2 | 60.5 | 60.8 |
| Flexural strength | Mpa | 96 | 97 | 98 | 98 | 105 | 96 | 80 |
| Modulus in flexure | Mpa | 2260 | 2270 | 2290 | 2330 | 2240 | 2260 | 2230 |
| The IZOD notched Izod impact strength | J/m | 550 | 520 | 510 | 495 | 540 | 560 | 480 |
| 125 ℃ of balls are pressed | ? | Through | Through | Through | Through | Through | Through | Through |
| Flame retardant resistance (1) | Class | 0.5mmV-2 | 0.5mmV-2 | 0.5mmV-1 | 0.5mmV-0 | 0.5mmHB | 0.5mmHB | 0.5mmHB |
| Flame retardant resistance (2) | Class | 2.0mmV-1 | 2.0mmV-0 | 2.0mmV-2 | 1.5mmV-0 | 2.0mmHB | 2.0mmHB | 2.0mmHB |
| 100 ℃/1000h of thermal ageing | ΔE | 3.8 | 3.9 | 3.9 | 4.1 | 4.3 | 4.6 | 4.7 |
| The xenon lamp aging test | ΔE | 3.2 | 3.4 | 3.6 | 3.7 | 4.7 | 4.8 | 5.0 |
| The glow wire test | ℃ | 800 | 850 | 900 | 950 | 575 | 550 | 550 |
| Transmittance | % | 24 | 23 | 23 | 23 | 44 | 46 | 23 |
Comparative Examples 1 ~ 2 and embodiment 1 ~ 12 resulting composition pellet is dull and stereotyped through 120 ℃ of dryings are injection molded into standard bar and long 100mm * wide 80mm * thick 2.0mm under 280 ℃ of temperature after 4 hours light face, and the mould temperature control is at 100 ℃.
Mechanical property is according to the ASTM standard testing, and flame retardant properties is according to the UL94 standard testing, and ball impression temperature (Ball Pressure Test) and glow wire test (GWFI) are respectively according to IEC60695-10-2 and IEC60695-2-12 test.
Thermal ageing test: light face flat board that will long 100mm * wide 80mm * thick 2.0mm is put into 100 ℃ of convection oven and is placed 1000h.
The transmittance test: adopt distant place PMS-80 transmission measurement appearance to carry out the transmittance test by ASTM D1003 standard the flat board behind Comparative Examples 2 and embodiment 12 thermal ageing tests, the test light wavelength region is at 380 ~ 780nm.
Photoaging test: light face flat board is put into xenon lamp aging case (U.S. ATLAS Ci3000+ type) carry out according to ASTM D4459 standard; Test condition is: 100% illumination, humidity 55%, 55 ℃ of blackboard temperatures; Adopt glass filter, 340nm wavelength light irradiance is 0.3w/m
2, the test duration is 500h.
Adopt color difference meter (U.S. XRITE COLOR EYE 7000A type) to detect the dull and stereotyped color value of chromatism of thermal ageing and the aging front and back of photoaging.
Test result is shown in table 2 and table 3.
See that by Comparative Examples 1-2 and embodiment 1-12 result additive has certain influence to each item performance of material, particularly bigger to the transmittance influence, so the selection of additive is most important to the preparation light-converting material.Find according to test result, the thermotolerance of additive and with the consistency of polycarbonate be key factor, therefore additive is screened.And measuring the result shows; Polycarbonate compositions with light transition function of the present invention has favorable mechanical performance and resistance toheat; Show more excellent heat-resisting, photooxidation aging property, and can satisfy the safety requirement that the LED illuminating industry is used macromolecular material.
Claims (13)
1. the polycarbonate compositions with LED light transition function is characterized in that, comprises following component by weight percentage:
Polycarbonate resin 40 ~ 98.9%;
Fluorescent material 1-50%;
Other additives 0.1 ~ 10%;
Described other additives are one or more in each based flame retardant, oxidation inhibitor, releasing agent, the weather resisting agent, and thermolysis starting temperature >=260 of every kind of additive ℃.
2. according to the said polycarbonate compositions of claim 1, it is characterized in that the transmittance of described polycarbonate resin >=85% with LED light transition function.
3. according to the said polycarbonate compositions of claim 1, it is characterized in that said polycarbonate resin is one or more in aromatic series homo-polycarbonate, silane Copolycarbonate, the polyester-carbonate copolymer with LED light transition function.
4. according to the said polycarbonate compositions of claim 1, it is characterized in that said polycarbonate resin molecular structure is straight chain type, branched chain type or both mixtures with LED light transition function.
5. according to the said polycarbonate compositions of claim 1, it is characterized in that the weight-average molecular weight M of said polycarbonate resin with LED light transition function
WScope is 12000 ~ 40000.
6. according to the said polycarbonate compositions of claim 1, it is characterized in that described fluorescent material is that in blue-light excited type fluorescent material, the near ultraviolet excitation type fluorescent material one or more mix with arbitrary proportion with LED light transition function.
7. according to the said polycarbonate compositions of claim 1, it is characterized in that said fire retardant is any one or a few in halogenated flame retardant, the halogen-free flame retardants with LED light transition function; Said halogenated flame retardant is tetrabromobisphenol A carbonic ester oligopolymer or oligopolymer and dichloro diphenyl sulfone potassium sulfonate; Said halogen-free flame retardants is Sulfonates fire retardant, phosphoric acid ester fire retardant or silicone based flame retardant.
8. according to the said polycarbonate compositions of claim 1 with LED light transition function; It is characterized in that; Said oxidation inhibitor is divided into primary antioxidant and auxiliary antioxidant by effect, and primary antioxidant comprises phenols and amine, and auxiliary antioxidant comprises phosphorous acid esters, thioesters class.
9. said according to Claim 8 polycarbonate compositions with LED light transition function; It is characterized in that; Said primary antioxidant comprises season amylalcohol four (3-(3, the 5-di-tert-butyl)-4-hydroxybenzene, octadecyl-3-(3,5-two uncles Ding-4-hydroxybenzene)-propionic ester, N; N-normal hexane-1; 6-dihydroxyl 3-(3,5-di-t-butyl-4-phenylor phenol acetic ester), vinyl-two (ethenoxy group) two-(3-(5-tertiary butyl-4-hydroxy-tolyl)-propionic ester), 2,2 '-methylene bis (4-methyl-6-tert butyl phenol); Said auxiliary antioxidant comprises three (2; The 4-di-tert-butyl-phenyl) phosphorous acid ester, triphenyl phosphite, two (2; 6-two-tertiary butyl-4-tolyl) pentaerythritol phosphite, four (2; 4-two-trimethylphenylmethane base)-4; 4 ' biphenyl-two phosphorus phosphorous acid ester, two (2,4-two withered phenyl) pentaerythritol phosphite, sulphur diethylammonium two [3-(3,5-di-t-butyl-4-hydroxybenzene) propionic ester], the two lauryl alcohol esters of thio-2 acid, thio-2 acid stearyl alcohol ester, tetramethylolmethane four (3-lauryl thiopropionate).
10. according to the said polycarbonate compositions of claim 1 with LED light transition function; It is characterized in that described releasing agent comprises one or more the composite uses in organic silicone compound, pentaerythritol tetrastearate, Zerol or the montanic acid wax; Described weather resisting agent comprises hindered amine light stabilizer and UV light absorber, and UV light absorber comprises benzotriazole category UV light absorber, benzophenone UV light absorber and Whitfield's ointment ester group UV light absorber.
11. according to the said polycarbonate compositions of claim 1 with LED light transition function; It is characterized in that; Described weather resisting agent comprises hindered amine light stabilizer and UV light absorber, and UV light absorber comprises benzotriazole category UV light absorber, benzophenone UV light absorber and Whitfield's ointment ester group UV light absorber.
12., it is characterized in that hindered amine light stabilizer is two (2,2,6 according to the said polycarbonate compositions of claim 11 with LED light transition function; 6 ,-tetramethyl pyridine base) sebate, gather-{ 6-[(1,1,3, the 3-tetramethyl butyl)-amido]-1; 3,5-triazine-2,4-two bases] [2-(2,2; 6, the 6-tetramethyl-piperidyl)-imino--hexa-methylene-[4-(2,2,6; The 6-tetramethyl-piperidyl)-imino-]], gather [1-(2 '-hydroxyethyl)-2,2,6,6-tetramethyl--4 hydroxy piperidine succinate]; The benzotriazole category UV light absorber comprises 2-(2-hydroxyl-3; 5-two (1; 1-dimethyl--phenyl)-2H-benzotriazole, 2-(2 '-hydroxyl-5 '-aminomethyl phenyl)-5-benzotriazole, 2,2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-the 5-chlorinated benzotriazole; Said UVNUL MS-40 base UV light absorber is 2-hydroxyl-4-eight alkoxy benzophenones; Said Whitfield's ointment ester group UV light absorber comprises that salol, Whitfield's ointment are to butyl phenyl ester or p-octylphenyl salicylate.
13. the said application of claim 1 ~ 12 with polycarbonate compositions of LED light transition function at preparation LED luminescence chip light conversion layer.
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