CN102532857B - Polycarbonate composite material suitable for LED (light-emitting diode) lamp cover and preparation method thereof - Google Patents

Polycarbonate composite material suitable for LED (light-emitting diode) lamp cover and preparation method thereof Download PDF

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Publication number
CN102532857B
CN102532857B CN2012100401031A CN201210040103A CN102532857B CN 102532857 B CN102532857 B CN 102532857B CN 2012100401031 A CN2012100401031 A CN 2012100401031A CN 201210040103 A CN201210040103 A CN 201210040103A CN 102532857 B CN102532857 B CN 102532857B
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polycarbonate
light
master batch
nano
district temperature
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CN102532857A (en
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丁鹏
施利毅
徐晓磊
汪庆
李宗周
宋娜
唐圣福
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04Particle-shaped
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means 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
    • B29C48/40Means 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

Abstract

The invention discloses a polycarbonate composite material suitable for an LED (light-emitting diode) lamp cover and a preparation method thereof. Based on the 100 weight parts PHR (parts per hundreds of rubber or resin) of a substrate polycarbonate material, the composition of the composite comprises the following components in PHR: 100PHR of polycarbonate, 5-15PHR of light scattering master batch, 0.2-1.0PHR of flame retardant, 1-3PHR of nano master batch and 0.2-1.0PHR of other additives. In the method, engineering plastic polycarbonate is used as a main body; and the light scattering master batch and the nano additive master batch are firstly prepared through an internal mixer and then smashed at high speed, and finally, the light scattering master batch and other raw materials are subjected to blending, extruding and granulating by adopting a side feeding method. By using the method, the problem that the dispersion of a light dispersing agent and other additives is not uniform is solved, and the obtained light dispersing material has high transmissivity and haze. The polycarbonate composite material disclosed by the invention can be used for preparation of related products in the optical field, is environment-friendly, high in safety and excellent in various physical and mechanical properties, and is suitable for preparing the LED lamp covers and other light guiding materials.

Description

Be applicable to polycarbonate composite material of LED lampshade and preparation method thereof
Technical field
The present invention relates to macromolecular material and lighting technical field, relate to a kind of photodiffusion material and preparation method thereof and application, particularly a kind of to the photodiffusion material that incident light absorbs less, diffuser efficiency is high, namely be applicable to polycarbonate composite material of LED lampshade and preparation method thereof.
Background technology
Lighting engineering is indispensable among the human lives.For the illumination of most cases, all need illumination light to have uniform spatial light intensity (or luminance brightness) and distribute.The size of LED tube core is very little, and light-emitting zone is also very little, is real pointolite for illumination, but the unidirectional dazzling dazzling problem of simultaneous.For realizing even illumination, it is luminous that just the light that pointolite or line source need be sent is transformed into face.Method commonly used is exactly to add the light diffusing sheet with scattering of light before light source, realizes above-mentioned conversion.
Light diffusing sheet can be divided into printed form, injection moulding and scattering of light polymer-type by the difference of its principle of work.Printed form typically uses the ink that the high material of reflectivity is mixed and made into, and is printed as stipple pattern in the diffuser plate bottom.The light of directive lower surface can be absorbed and emit again.Utilize this character can change the propagation direction of light, and make light no longer satisfy total reflection condition and penetrate diffuser plate.The injection molding diffuser plate is to form the scattering decorative pattern simultaneously to reduce the thickness of light guiding plate in process of injection molding, is more convenient for being applied to portable product.The light diffusing agent different with the base material specific refractory power evenly mixed in the scattering of light polymkeric substance.Light changes the propagation direction by scattering on these particles, side scattered light penetrates and goes, and the forward scatter light that can not penetrate also can continue to propagate to far-end, carries out scattering next time.Scattering of light occurs in the whole plate, so light travel path in light guiding plate is shorter, the light utilising efficiency is higher.Light diffusing agent is actually the particle with a certain size distribution, its material can be inorganic also can be organic.Inorganic particulate commonly used has silicon-dioxide, zinc oxide, titanium dioxide, zirconium white, aluminum oxide, zinc sulphide, barium sulfate, with and composition thereof with the finishing thing.Organic granular commonly used comprises styrenic polymer, acrylic polymers, type siloxane polymkeric substance.
The main technical details that characterizes the photodiffusion material performance comprises transmittance and mist degree.Transmittance is represented photodiffusion material to the overall utilization ratio of incident light, and mist degree represents that then incident light departs from the degree of former incident direction, so can characterize service efficiency and the diffusion that photodiffusion material is introduced incident light with the two.For the photodiffusion material based on particle scattering, the increase of mist degree generally will cause reducing of transmittance.Its transmittance of the lampshade that uses in people's daily life is all not high, that is to say that many a part of luminous energies are lost.Therefore, it is very important for effectively utilizing electric energy that exploitation has the photodiffusion material of high transmission rate and high mist degree.In sum, because LED is typical pointolite, convert thereof into the soft effect of the uniform area source competence exertion illumination of illumination, and the photodiffusion material with high mist degree and high transmission rate is the critical material of realizing above-mentioned conversion.
Summary of the invention
First technical problem that the present invention will solve is: polycarbonate composite material of a kind of LED of being applicable to lampshade and preparation method thereof is provided, make and not only satisfy outside the various processing requests of light diffusing polycarbonate and the physicals requirement, also make it have high transmission rate and high flame retardant.
First technical problem that the present invention will solve is: a kind of method that more equably light granule proliferation and fire retardant etc. is dispersed in the photodiffusion material production process in the matrix (polycarbonate) is provided, and this method can be to produce light to spread the handiness that the process of expecting has high-level efficiency and operation.
For solving the problems of the technologies described above, the objective of the invention is to be achieved through the following technical solutions.
A kind of polycarbonate composite material that is applicable to the LED lampshade and preparation method thereof is 100 weight parts (PHR) by matrix polycarbonate material, forms proportioning to be: polycarbonate 100 PHR; Scattering of light master batch 5~15 PHR; Fire retardant 0.2~1.0 PHR; Nanometer master batch 1~3 PHR; Other auxiliary agent (antioxidant/anti ultraviolet agent) 0.2~1.0 PHR.
Wherein, described polycarbonate is the bisphenol A-type polycarbonate, and middle height is sticking, and melting index is at 8~12 g/10min.
Wherein, described scattering of light master batch mixes polycarbonate by light diffusing agent and forms.Its light diffusing agent is selected organic silicon resin ball-shaped micro powder for use, and (more believe the KMP-590 that produces such as Japan, one or more mixtures KMP-470), particle diameter are more than 1 μ m, and preferable particle size is at 1-5 μ m.
Concrete making method is: the polycarbonate and the light diffusing agent that take by weighing certain mass, account for weight percent 90% according to polycarbonate, 10% the ratio of accounting for light diffusing agent drops in the Banbury mixer, setting technology is: a district temperature 255-265 ℃, two district temperature 260-270 ℃, rotating speed 30~60 rpm, the residence time 2~5min; At last the mixture that mixes in the Banbury mixer is taken out then to smash via high-speed mixer and obtain light diffusion masterbatch;
Wherein, described nanometer master batch selects for use particle size to mix in Banbury mixer at particle and the polycarbonate of 10-100 nanometer, be preferably the inorganic nano-particle of 10-30 nanometer, comprise nano titanium oxide, nano silicon, nanomete talc powder, nano layered double hydroxides.
Concrete making method is: the polycarbonate and the nano-powder that take by weighing certain mass, account for weight percent 90% according to polycarbonate, 10% the ratio of accounting for nano-powder drops in the Banbury mixer, setting technology is: a district temperature 255-265 ℃, two district temperature 260-270 ℃, rotating speed 30~60 rpm, the residence time 2~10min; At last the mixture that mixes in the Banbury mixer is taken out then to smash via high-speed mixer and obtain the nanometer masterbatch;
Wherein, described fire retardant is a kind of fluorine type polymer fire retardant, as the tetrafluoroethylene of high molecular.
Wherein, described other auxiliary agent comprises phosphorous acid class antioxidant and coumarins white dyes.
A kind of preparation method who is applicable to the polycarbonate composite material of LED lampshade is characterized in that, comprises step:
A: take by weighing polycarbonate, light diffusing agent, nano assistant, fire retardant and other auxiliary agents by weight ratio;
B: press the described preparation light diffusion of preamble master batch;
C: press the described preparation nanometer of preamble master batch;
E: matrix polycarbonate and nanometer master batch and other auxiliary agent fire retardants are put into the loading hopper of twin screw extruder, and light diffusion masterbatch is fed a mouthful charging through side, through melt extruding granulation; Complete processing is as follows: twin screw extruder one district temperature 240-250 ℃, and two district temperature 250-260 ℃, three district temperature 260-270 ℃, four district temperature 270-275 ℃, five district temperature 265-270 ℃, six district temperature 270-280 ℃, die head temperature is 275-280 ℃, and pressure is 2-2.5MPa.
The light diffusion masterbatch side feeding feed process that the present invention takes can solve light diffusing agent and other auxiliary agents disperse uneven problem, makes the photodiffusion material that obtains have higher transmittance and mist degree, has added a small amount of nano assistant simultaneously and has improved the optics mist degree.
The present invention has following beneficial effect:
1: the nano assistant of use is composite, material is had the effect of certain enhancing light diffusion.
2: the technology of use can guarantee that light diffusing agent, each auxiliary agent and fire retardant disperse evenly with polycarbonate, and keeps excellent compatibility.
Embodiment
Polycarbonate composite material that is applicable to the LED lampshade provided by the invention and preparation method thereof is 100 weight parts (PHR) by matrix polycarbonate material, forms proportioning to be: polycarbonate 100 PHR; Scattering of light master batch 5~15 PHR; Fire retardant 0.2~1.0 PHR; Nanometer master batch 1~3 PHR; Other auxiliary agent 0.2~1.0 PHR.
Wherein, described polycarbonate is the bisphenol A-type polycarbonate, and middle height is sticking, and MFI is at 8~12g/10MIN for its melting index; The scattering of light master batch mixes polycarbonate by light diffusing agent to be formed, and light scattering agent is a kind of silicone resin, and particle diameter is at 1-5 μ m; Fire retardant is a kind of fluorine type polymer fire retardant; The nanometer master batch mixes polycarbonate by nanoparticle and forms, nano material is that particle size is in the 10-100 nanometer, be preferably the inorganic nano-particle of 10-30 nanometer, comprise nano titanium oxide, nano silicon, nanomete talc powder, nano layered double hydroxides; Other auxiliary agent comprises antioxidant and anti ultraviolet agent.
In the present invention, first (PHR) by weight ratio takes by weighing every raw material.Earlier prepare light diffusion master batch and nanometer master batch with Banbury mixer, then matrix polycarbonate and nanometer master batch and other auxiliary agent fire retardants are put into the loading hopper of twin screw extruder, and light diffusion masterbatch is fed a mouthful charging through side, through melt extruding granulation; Complete processing is as follows: twin screw extruder one district temperature 240-250 ℃, and two district temperature 250-260 ℃, three district temperature 260-270 ℃, four district temperature 270-275 ℃, five district temperature 265-270 ℃, six district temperature 270-280 ℃, die head temperature is 275-280 ℃, and pressure is 2-2.5MPa.
For ease of the present invention is further understood, now describe the present invention in conjunction with specific embodiments:
In the material prescription of the following example, light diffusing agent is organosilicon compound, selects for use Japanese SHIN-ETSU HANTOTAI to produce, and trade names are KMP-590; Nanoparticle is the silicon-dioxide of 30 nanometers; Fire retardant is the fluorine type polymer fire retardant, selects Daikin company for use, and trade names are FA-500.Other auxiliary agents comprise white dyes 124 Triazole-phenyl tonka bean camphor, and oxidation inhibitor adopts triphenyl phosphite.
Embodiment 1
(PHR) takes by weighing following raw material by weight ratio: polycarbonate 100PHR; Light diffusion master batch 5 PHR; Fire retardant 0.3 PHR; Nanometer master batch (silicon-dioxide) 1 PHR, other auxiliary agent 0.2 PHR.Matrix polycarbonate and nanometer master batch and other auxiliary agent fire retardants are put into the loading hopper of twin screw extruder, and light diffusion masterbatch is fed a mouthful charging through side, through melt extruding granulation; Complete processing is as follows: twin screw extruder one district temperature 240-250 ℃, and two district temperature 250-260 ℃, three district temperature 260-270 ℃, four district temperature 270-275 ℃, five district temperature 265-270 ℃, six district temperature 270-280 ℃, die head temperature is 275-280 ℃, and pressure is 2-2.5MPa.
Embodiment 2
(PHR) takes by weighing following raw material by weight ratio: polycarbonate 100 PHR; Light diffusion master batch 7 PHR; Fire retardant 0.7 PHR; Nanometer master batch (silicon-dioxide) 1 PHR, other auxiliary agent 0.6 PHR.Matrix polycarbonate and nanometer master batch and other auxiliary agent fire retardants are put into the loading hopper of twin screw extruder, and light diffusion masterbatch is fed a mouthful charging through side, through melt extruding granulation; Complete processing is as follows: twin screw extruder one district temperature 240-250 ℃, and two district temperature 250-260 ℃, three district temperature 260-270 ℃, four district temperature 270-275 ℃, five district temperature 265-270 ℃, six district temperature 270-280 ℃, die head temperature is 275-280 ℃, and pressure is 2-2.5MPa.
Embodiment 3
(PHR) takes by weighing following raw material by weight ratio: polycarbonate 100 PHR; Light diffusion master batch 10 PHR; Fire retardant 1.0 PHR; Nanometer master batch (silicon-dioxide) 1 PHR, other auxiliary agent 0.9 PHR.Matrix polycarbonate and nanometer master batch and other auxiliary agent fire retardants are put into the loading hopper of twin screw extruder, and light diffusion masterbatch is fed a mouthful charging through side, through melt extruding granulation; Complete processing is as follows: twin screw extruder one district temperature 240-250 ℃, and two district temperature 250-260 ℃, three district temperature 260-270 ℃, four district temperature 270-275 ℃, five district temperature 265-270 ℃, six district temperature 270-280 ℃, die head temperature is 275-280 ℃, and pressure is 2-2.5MPa.
Comparative Examples 1
(PHR) takes by weighing following raw material by weight ratio: polycarbonate 100 PHR; Light diffusing agent 0.7 PHR and 6.3 PHR polycarbonate; Fire retardant 0.7 PHR; Nanoparticle 0.1 PHR and 0.9 PHR polycarbonate; Other auxiliary agent 0.6 PHR.All materials are mixed in plastic containers, afterwards, the material that mixes is joined in the hopper of twin screw extruder, through melt blending, extruding pelletization becomes matrix material.Wherein, screw rod is respectively distinguished the processing temperature setting and is respectively: complete processing is as follows: twin screw extruder one district temperature 240-250 ℃, two district temperature 250-260 ℃, three district temperature 260-270 ℃, four district temperature 270-275 ℃, five district temperature 265-270 ℃, six district temperature 270-280 ℃, die head temperature is 275-280 ℃, and pressure is 2-2.5MPa.
Comparative Examples 2
(PHR) takes by weighing following raw material by weight ratio: polycarbonate 100 PHR; Light diffusion master batch 7 PHR; Fire retardant 0.7 PHR; Other auxiliary agent 0.6 PHR.Matrix polycarbonate and other auxiliary agent fire retardants are put into the loading hopper of twin screw extruder, and light diffusion masterbatch is fed a mouthful charging through side, through melt extruding granulation; Complete processing is as follows: twin screw extruder one district temperature 240-250 ℃, and two district temperature 250-260 ℃, three district temperature 260-270 ℃, four district temperature 270-275 ℃, five district temperature 265-270 ℃, six district temperature 270-280 ℃, die head temperature is 275-280 ℃, and pressure is 2-2.5MPa.
Performance test:
Tensile strength is tested by GB/T 1040 standards.Specimen types is the I type, batten size (mm): 170 * 20 * 4, and draw speed is 50mm/min;
Transmittance test and mist degree test are according to American society association criterion ASTM D1003-61 (1997), and test sample plate thickness is 2MM;
Flame retardant properties is according to the UL94 standard testing, batten size (mm): 128 * 12.7 * 3.2.
Embodiment 1~3 and Comparative Examples prescription and material property see Table 1:
Table 1: experimental formula and The performance test results
Figure 2012100401031100002DEST_PATH_IMAGE001
Annotate: light diffusion master batch and nanometer master batch are without crossing the material that Banbury mixer is handled, expression light diffusing agent/nanoparticle consumption before the plus sige, expression polycarbonate consumption behind the plus sige in the * comparative example 1.
Analyze from embodiment 1~3, with the increase of fire retardant add-on, the physical and mechanical property variable effect of material is little, and material is never fire-retardant to be changed into fire-retardantly, and simultaneously, along with the increase of light scattering agent add-on, mist degree increases gradually, and transmittance descends gradually.And can analyze from Comparative Examples, should use up diffusion master batch and side feed method, the dispersing property of material obviously improves, and transmitance and mist degree have obvious lifting; Can find to add behind the nano assistant by embodiment 2 and the data of comparative example 2 simultaneously that mist degree has obvious lifting under the prerequisite of not losing transmittance.
More than polycarbonate composite material of a kind of LED of being applicable to lampshade provided by the present invention and preparation method thereof is described in detail, used specific case herein principle of the present invention and embodiment are set forth, thought of the present invention can adopt the alternate manner beyond the above-named embodiment to realize.

Claims (2)

1. be applicable to the polycarbonate composite material of LED lampshade, it is characterized in that it is 100 weight parts by matrix polycarbonate material, the composition proportioning is:
Polycarbonate 100 weight parts;
Scattering of light master batch 5~15 weight parts;
Nanometer master batch 1~3 weight part;
Fire retardant 0.2~1.0 weight part;
Other auxiliary agent 0.2~1.0 weight part;
Described scattering of light master batch mixes polycarbonate by light diffusing agent and forms; Its light diffusing agent is selected organic silicon resin ball-shaped micro powder for use, is the KMP-590 of Japanese SHIN-ETSU HANTOTAI production, one or more mixtures among the KMP-470, and particle diameter is more than 1 μ m; Concrete making method is: the polycarbonate and the light diffusing agent that take by weighing certain mass, account for weight percent 90% according to polycarbonate, 10% the ratio of accounting for light diffusing agent drops in the Banbury mixer, setting technology is: a district temperature 255-265 ℃, two district temperature 260-270 ℃, rotating speed 30~60 rpm, the residence time 2~5min; At last the mixture that mixes in the Banbury mixer is taken out then to smash via high-speed mixer and obtain the scattering of light master batch.
2. the polycarbonate composite material that is applicable to the LED lampshade as claimed in claim 1, it is characterized in that: described nanometer master batch particle size mixes in Banbury mixer at particle and the polycarbonate of 10-100 nanometer, nano particle diameter is the 10-30 nanometer, comprises in nano titanium oxide, nano silicon, nanomete talc powder, the nano layered double hydroxides one or more; Concrete making method is: the polycarbonate and the nano-powder that take by weighing certain mass, account for weight percent 90% according to polycarbonate, 10% the ratio of accounting for nano-powder drops in the Banbury mixer, setting technology is: a district temperature 255-265 ℃, two district temperature 260-270 ℃, rotating speed 30~60 rpm, the residence time 2~10min; At last the mixture that mixes in the Banbury mixer is taken out then to smash via high-speed mixer and obtain the nanometer master batch.
CN2012100401031A 2012-02-22 2012-02-22 Polycarbonate composite material suitable for LED (light-emitting diode) lamp cover and preparation method thereof Expired - Fee Related CN102532857B (en)

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