CN109422961B - Flame-retardant light-diffusion polypropylene composite material for LED and product thereof - Google Patents
Flame-retardant light-diffusion polypropylene composite material for LED and product thereof Download PDFInfo
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- CN109422961B CN109422961B CN201811058182.2A CN201811058182A CN109422961B CN 109422961 B CN109422961 B CN 109422961B CN 201811058182 A CN201811058182 A CN 201811058182A CN 109422961 B CN109422961 B CN 109422961B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V1/00—Shades for light sources, i.e. lampshades for table, floor, wall or ceiling lamps
- F21V1/14—Covers for frames; Frameless shades
- F21V1/16—Covers for frames; Frameless shades characterised by the material
- F21V1/22—Covers for frames; Frameless shades characterised by the material the material being plastics
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V7/00—Reflectors for light sources
- F21V7/22—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors
- F21V7/24—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors characterised by the material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
- F21Y2115/00—Light-generating elements of semiconductor light sources
- F21Y2115/10—Light-emitting diodes [LED]
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Abstract
The invention relates to a flame-retardant photodiffusion polypropylene composite material for an LED and a product thereof; the composite material comprises the following components in parts by weight: 100 parts of homopolymerized polypropylene, 2-5 parts of compound flame retardant, 1-5 parts of organic silicon light diffusant, 1-5 parts of barium sulfate light diffusant, 1-2 parts of light stabilizer and 2-3 parts of chemical modifier. Compared with the prior art, the flame-retardant photodiffusion polypropylene composite material prepared by the invention has the advantages of excellent mechanical property, high light transmittance, excellent flame retardance and no precipitation of flame retardant.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a flame-retardant light-diffusion polypropylene composite material for an LED and a product thereof.
Background
With the development of LED light sources, light diffusion plates for LEDs and reflector materials are rapidly developed, the traditional reflecting materials are metal die-casting or modified PC materials, the metal die-casting is high in cost and complex in process, and the modified PC materials are expensive.
The polypropylene has the characteristics of low density, corrosion resistance, easiness in processing, low cost, recoverability, excellent mechanical property and the like, and is widely applied to industries such as automobiles, household appliances and the like. But no report is made about the application of polypropylene materials in the fields of LED shading and reflection. The polypropylene has certain permeability under the condition of thin wall, so that the polypropylene has a wide prospect for the research on the modification of the light-shielding property of the polypropylene.
The Chinese patent with the application number of 201210519772.7 discloses a light diffusion modified polypropylene material and a preparation method thereof, wherein the light diffusion modified polypropylene material comprises the following components in percentage by weight: 98.5 to 99 percent of polypropylene, 0.3 to 0.8 percent of light diffusant, 0.05 to 0.5 percent of transparent modifier, 0.1 to 0.5 percent of antioxidant and 0.1 to 0.3 percent of light stabilizer.
Chinese patent with application number 201210233346.7 discloses a high-fluidity precipitation-resistant halogen-free flame-retardant polypropylene composite material, which is prepared from the following raw materials in percentage by weight: 50-70% of high-melting block copolymerized polypropylene, 5-20% of ultrahigh-melting homopolymerized polypropylene, 5-21% of ammonium polyphosphate, 10-21% of pentaerythritol, 5-11% of melamine urate, 3-10% of maleic anhydride grafted polypropylene, 78-1.2% of antioxidant PS 8020.1 and 1680.1-1.2% of antioxidant; 10100.1-1.0% of antioxidant; 0.5-3.0% of lubricant TAF, solves the flame retardant problem and precipitation resistance of the polypropylene material, but does not have the light diffusion effect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a flame-retardant light-diffusion polypropylene composite material for an LED and a lamp product thereof.
The purpose of the invention can be realized by the following technical scheme:
the invention relates to a flame-retardant photodiffusion polypropylene composite material, which comprises the following components in parts by weight:
preferably, the melt index of the homopolymerized polypropylene is 10g/10min at 230 ℃ under the test condition of 2.16 kg. If the melt index is lower than 10g/10min, the viscosity of the material is too high, the coating of the light diffusant and the flame retardant is adversely affected, and the light diffusion effect and the flame retardant effect of the material are affected; if the molecular weight is higher than 10g/10min, the number average molecular weight of the material is lower, and the flame retardance of the product is influenced; if the ultrahigh melt index of 1800 is adopted, namely homopolymerized polypropylene, agglomeration of the light diffusant and the flame retardant is easily caused to influence the dispersion effect, so that the light diffusion and the flame retardant effect are influenced.
Preferably, the compound flame retardant is a compound of ammonium polyphosphate and melamine polyphosphate, and the compound mass ratio is 1:1. The ammonium polyphosphate is a phosphorus flame retardant and has excellent flame retardant effect and precipitation resistance; the melamine polyphosphate is a flame retardant containing phosphorus and nitrogen; in the system, the melamine polyphosphate and the ammonium polyphosphate have excellent synergistic flame retardant effect, and have optimal flame retardant effect in 1:1 compounding.
Preferably, the polymerization degree n of the ammonium polyphosphate is more than 1000, the phosphorus content is more than 29 percent, and the average particle size is 10-20 mu m; the phosphorus content of the melamine polyphosphate is more than 14 percent, and the average grain diameter is 5-15 mu m. The ammonium polyphosphate with high polymerization degree (the polymerization degree n is more than 1000) has more excellent anti-precipitation performance of the flame retardant; the higher the phosphorus content, the better the flame retardancy. In the system, the flame retardants with different average particle sizes are selected for compounding, so that the dispersion of the flame retardants is improved, and the flame retardant effect is improved.
Preferably, the silicone light diffusing agent has an average particle diameter of 1 to 5 μm and a refractive index of 1.43.
Preferably, the barium sulfate light diffusant is synthetic barium sulfate and has a spherical structure, the particle size is 2-6 mu m, and the refractive index is 1.63.
Preferably, the light stabilizer is a hindered amine light stabilizer.
Preferably, the chemical modifier is maleic anhydride modified polypropylene.
Preferably, the maleic anhydride-modified polypropylene has a number average molecular weight of 15000-20000 and a viscosity of 400-600 mPa.s. In the system of the invention, the low molecular weight modified polypropylene with the number average molecular weight of 15000-20000 and the viscosity of 400-600mPa.s is selected, which is more favorable for the combination with the flame retardant and the light diffusant to improve the dispersion effect.
In a second aspect, the present invention relates to a method for preparing the flame-retardant light diffusion polypropylene composite material, comprising the following steps:
s1, preparing materials according to the components and the parts by weight; putting the mixture into a high-speed mixer for mixing for 2-5 min, and discharging;
s2, putting the mixed raw materials into a double-screw machine for extrusion granulation, wherein the rotating speed of the double-screw machine is 200-400 r/min, and the temperature is 180-220 ℃, so as to prepare the flame-retardant light diffusion polypropylene composite material for the LED.
In a third aspect, the invention also relates to an LED lamp product prepared from the flame-retardant light diffusion polypropylene composite material.
Preferably, the LED lamp part is an LED butterfly lamp part.
Compared with the prior art, the invention has the following beneficial effects:
(1) the prepared flame-retardant light diffusion polypropylene composite material for the LED achieves excellent light transmittance and precipitation resistance of the flame retardant by using the homopolymerized polypropylene with the melt index of 10g/10min (230 ℃ C. by 2.16kg), the homopolymerized polypropylene material can have excellent light transmittance due to high crystallinity and fine crystal nuclei, and meanwhile, the flame retardant can be better fixed in an amorphous region to prevent migration due to the characteristics of high crystallinity and fine crystal nuclei. Meanwhile, the 10-fused-finger material can obtain better processability, excellent impact property and more excellent coating property on the flame retardant powder.
(2) According to the prepared flame-retardant light-diffusion polypropylene composite material for the LED, by adding the compound of ammonium polyphosphate and melamine polyphosphate, the two substances have excellent phosphorus contents, so that the flame retardance of the system can be effectively improved in a synergistic manner; meanwhile, melamine polyphosphate with the particle size of 5-15 mu m and ammonium polyphosphate with the particle size of 10-20 mu m are used, so that the flame retardance is improved, and the melamine polyphosphate and the ammonium polyphosphate can be better dispersed synergistically to achieve the purpose of preventing precipitation.
(3) The light diffusion effect and the light transmittance are improved by adding the silicone light diffusing agent and the spherical barium sulfate, the refractive index of the polypropylene is 1.54, different refractive index differences among materials are achieved by compounding the silicone light diffusing agent 1.43 and the barium sulfate 1.63, the problem that light rays penetrate through resin better in a good cooperation mode can be solved, and the transmittance and the diffusion effect are achieved.
(3) By adding the maleic anhydride modified polypropylene chemical modifier with the molecular weight of 15000-20000 and the viscosity of 400-600mPa.s, the dispersion of the flame retardant and the light diffusant can be effectively improved, and the flame retardant can be prevented from being separated out.
(4) The prepared product has smooth surface, good light diffusivity, excellent light transmittance, no precipitation of the flame retardant, attractive appearance and low cost.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic structural diagram of a flame-retardant light-diffusing polypropylene part for an LED.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
Example 1
The embodiment relates to a flame-retardant light diffusion polypropylene composite material for an LED, which is prepared from the following components in parts by weight:
all the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the flame-retardant light diffusion polypropylene composite material for the LED. Wherein the process temperature is 200 ℃, and the screw rotating speed is 400 r/min.
An LED lamp manufactured by using the flame retardant light diffusing polypropylene composite material for LED of this embodiment is shown in fig. 1.
Example 2
The embodiment relates to a flame-retardant light diffusion polypropylene composite material for an LED, which is prepared from the following components in percentage by weight:
all the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the flame-retardant light diffusion polypropylene composite material for the LED. Wherein the process temperature is 190 ℃, and the screw rotating speed is 300 r/min.
Example 3
The embodiment relates to a flame-retardant light diffusion polypropylene composite material for an LED, which is prepared from the following components in percentage by weight:
all the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the flame-retardant light diffusion polypropylene composite material for the LED. Wherein the process temperature is 180 ℃, and the screw rotating speed is 350 r/min.
Comparative example 1
The comparative example relates to a flame-retardant photodiffusion polypropylene composite material for an LED, which is basically the same as the composite material in example 1 in terms of components and parts by weight, and is characterized in that: does not contain synthetic barium sulfate.
All the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the polypropylene composite material. Wherein the process temperature is 200 ℃, and the screw rotating speed is 400 r/min.
Comparative example 2
The comparative example relates to a flame-retardant photodiffusion polypropylene composite material for an LED, which is basically the same as the composite material in example 1 in terms of components and parts by weight, and is characterized in that: the synthetic barium sulfate with the refractive index of 1.63 is replaced by silica with the refractive index of 1.6.
All the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the polypropylene composite material. Wherein the process temperature is 200 ℃, and the screw rotating speed is 400 r/min.
Comparative example 3
The comparative example relates to a flame-retardant photodiffusion polypropylene composite material for an LED, which is basically the same as the composite material in example 1 in terms of components and parts by weight, and is characterized in that:
the selected compound flame retardant is a compound of ammonium polyphosphate and melamine urate, and the compound mass ratio is 1:1.
All the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the polypropylene composite material. Wherein the process temperature is 200 ℃, and the screw rotating speed is 400 r/min.
Comparative example 4
The comparative example relates to a flame-retardant photodiffusion polypropylene composite material for an LED, which is basically the same as the composite material in example 1 in terms of components and parts by weight, and is characterized in that: the viscosity of the adopted chemical modifier, namely maleic anhydride modified polypropylene, is 800 mPa.s.
All the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the polypropylene composite material. Wherein the process temperature is 200 ℃, and the screw rotating speed is 400 r/min.
Comparative example 5
The comparative example relates to a flame-retardant photodiffusion polypropylene composite material for an LED, which is basically the same as the composite material in example 1 in terms of components and parts by weight, and is characterized in that:
high-transparency random copolymer polypropylene with the melt index of 10.0g/10min (230 ℃ C. 2.16kg) is adopted; rather than the homopolypropylene of the present invention.
All the raw materials are put into a high-speed mixer together to be mixed for 2-5 min, and then the materials are discharged; and then putting the mixture into a double-screw extruder for extrusion granulation to prepare the polypropylene composite material. Wherein the process temperature is 200 ℃, and the screw rotating speed is 400 r/min.
Comparative example 6
The comparative example relates to a flame-retardant photodiffusion polypropylene composite material for an LED, which is prepared by the following steps in parts by weight in the same preparation method as example 1, except that: the compound flame retardant is a compound of ammonium polyphosphate and melamine polyphosphate with the compound ratio of 1: 1.2.
Comparative example 7
The comparative example relates to a flame-retardant photodiffusion polypropylene composite material for an LED, which is prepared by the following steps in parts by weight in the same preparation method as example 1, except that: the compound flame retardant is a compound of ammonium polyphosphate and melamine polyphosphate with the compound ratio of 1.2: 1.
Incidentally, the melt index of the homo-polypropylene described in examples 1 to 3 was 10g/10min (230 ℃ C. and 2.16 kg). The compound flame retardant is a compound of ammonium polyphosphate and melamine polyphosphate, the compound proportion is 1:1, the polymerization degree n of the ammonium polyphosphate is more than 1000, the phosphorus content is 29-31%, the average grain diameter is 10-20 mu m, the phosphorus content of the melamine polyphosphate is 14-16%, and the average grain diameter is 5-15 mu m. The average grain diameter of the organic silicon light diffusant is 1-5 mu m, and the refractive index is 1.43. The synthetic barium sulfate has a spherical structure, a particle size of 2-6 mu m and a refractive index of 1.63. The light stabilizer is a hindered amine light stabilizer. The chemical modifier is maleic anhydride modified polypropylene, the molecular weight is 15000-20000, and the viscosity is 400-600 mPa.s.
Performance test of examples 1 to 3 and comparative examples 1 to 7
The polypropylene composite materials prepared in examples 1-3 and comparative examples 1-7 are subjected to optical performance, flame retardant performance and precipitation performance tests, the composite materials are subjected to injection molding to form a 2 mm-thick polished plate and a 3.2 mm-thick UL94 standard sample strip, the 2 mm-thick polished plate is subjected to light transmittance and haze tests, the light transmittance and haze are tested according to GB/T2410-2008, and the reflectance test adopts a D65 light source and is subjected to an incident angle of 10 degrees. And testing the precipitation condition of the flame retardant by using a polishing plate with the thickness of 2mm, and performing precipitation test by placing the sample plate into an oven with the temperature of 90 ℃ to be dried for 48 hours and then visually observing the surface precipitation condition. The flame retardancy was measured by 3.2mm UL94 bar test.
TABLE 1 mechanical Properties of examples 1-3 and comparative examples 1-7
As can be seen from Table 1, the polypropylene composites prepared in examples 1-3 have excellent flame retardancy and light diffusibility, and can fully meet the standard of lamps GB7000.1 when used in the product of the present invention.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and additions can be made without departing from the method of the present invention, and these modifications and additions should also be regarded as the protection scope of the present invention.
Claims (6)
1. The flame-retardant photodiffusion polypropylene composite material is characterized by comprising the following components in parts by weight:
100 parts of homopolymerized polypropylene, namely 100 parts of homopolymerized polypropylene,
2-5 parts of a compound flame retardant,
1-5 parts of organic silicon light diffusant,
1-5 parts of barium sulfate light diffusant,
1-2 parts of a light stabilizer, namely,
2-3 parts of a chemical modifier;
the average grain diameter of the organic silicon light diffusant is 1-5 mu m, and the refractive index is 1.43;
the barium sulfate light diffusant is synthetic barium sulfate and has a spherical structure, the particle size is 2-6 mu m, and the refractive index is 1.63;
the melt index of the homopolymerized polypropylene is 10g/10min under the test conditions of 230 ℃ and 2.16 kg;
the chemical modifier is maleic anhydride modified polypropylene, the molecular weight is 15000-20000, and the viscosity is 400-600 mPa.s.
2. The flame-retardant light-diffusing polypropylene composite material according to claim 1, wherein the compound flame retardant is a compound of ammonium polyphosphate and melamine polyphosphate, and the compound mass ratio is 1:1.
3. The flame-retardant light-diffusing polypropylene composite material according to claim 2, wherein the degree of polymerization n of the ammonium polyphosphate is more than 1000, the phosphorus content is more than 29%, and the average particle size is 10-20 μm; the phosphorus content of the melamine polyphosphate is more than 14 percent, and the average grain diameter is 5-15 mu m.
4. The flame retardant, light diffusing polypropylene composite of claim 1 wherein the light stabilizer is a hindered amine light stabilizer.
5. A method for preparing the flame-retardant light-diffusing polypropylene composite material according to any one of claims 1 to 4, wherein the method comprises the following steps:
s1, preparing materials according to the components and the parts by weight; putting the mixture into a high-speed mixer for mixing for 2-5 min, and discharging;
s2, putting the mixed raw materials into a double-screw machine for extrusion granulation, wherein the rotating speed of the double-screw machine is 200-400 r/min, and the temperature is 180-220 ℃, so as to prepare the flame-retardant light diffusion polypropylene composite material.
6. An LED lamp part made of the flame-retardant light-diffusing polypropylene composite material as claimed in any one of claims 1 to 4.
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| CN109608758B (en) * | 2018-10-12 | 2021-04-13 | 宁波凯耀电器制造有限公司 | Photodiffusion PP material and preparation method thereof |
| CN114479262B (en) * | 2020-10-23 | 2023-02-28 | 中国石油化工股份有限公司 | Flame-retardant photodiffusion polypropylene composition and application thereof, flame-retardant photodiffusion polypropylene and preparation method and application thereof |
| CN114479261B (en) * | 2020-10-23 | 2023-03-14 | 中国石油化工股份有限公司 | Light diffusion polypropylene composition, light diffusion polypropylene and application thereof |
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