CN109608758B - Photodiffusion PP material and preparation method thereof - Google Patents
Photodiffusion PP material and preparation method thereof Download PDFInfo
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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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- 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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/18—Spheres
Abstract
The invention relates to the technical field of functional polymer materials, and provides a light diffusion PP material and a preparation method thereof, aiming at solving the problem that the traditional PP material has low utilization rate in the lamp industry due to poor thermal stability and weak impact resistance, wherein the light diffusion PP material comprises the following components in parts by weight: 90-98 parts of polypropylene, 0.2-1 part of light diffusant, 0.05-3 parts of flame retardant, 0.05-1 part of antioxidant, 0.05-1 part of lubricant and 0.5-5 parts of anti-UV agent. The light-responsive gel factor compound light diffusant and the green environment-friendly flame retardant are utilized, so that the light-diffusing PP material system is more uniform in distribution, better in fluidity, and stronger in impact resistance and light-induced regulation capacity; the modified light diffusion PP material has better thermal stability, and the softening temperature can reach 105 ℃. The modified light-diffusion PP material disclosed by the invention has better ageing resistance, and can still ensure the yellowing performance under the irradiation of high-intensity ultraviolet rays.
Description
Technical Field
The invention relates to the technical field of functional polymer materials, in particular to a light diffusion PP material and a preparation method thereof.
Background
An LED is an abbreviation of "Light Emitting Diode", which is translated into "Light Emitting Diode" in chinese, and is a novel semiconductor solid-state Light Emitting device, and when a forward voltage is applied across the two terminals, carriers in a semiconductor are recombined to cause photon emission, thereby generating Light. LEDs made of different materials emit light of different wavelengths, thereby forming different colors. The LED has the characteristics of low energy consumption, small volume, long service life, no pollution, quick response, low driving voltage, strong shock resistance, high color purity and the like, and is praised as a new generation of lighting source and a green light source.
Light rays pass through the diffusion layer of the plastic base material, and when the light rays meet media (diffusion particles) with different refractive indexes, the phenomena of multi-angle and multi-direction refraction, reflection and scattering can occur, so that the point light source achieves a light diffusion effect, and a more uniform and more comfortable light emitting effect is provided for the lighting lamp. Currently, the mainstream diffusion plates in the market are made of Polycarbonate (PC) material and Polystyrene (PS) material. The PC material has insufficient hardness, is easy to scratch, is not corrosion-resistant, is not ultraviolet-resistant and is easy to age; the PS material has excellent electrical insulation, the light transmittance is second to that of organic glass, the fragmentation is high, the solvent resistance is poor, the thermal expansion coefficient is large, and the internal stress is easy to generate.
Compared with PC materials and PS materials in the market, the polypropylene (PP) material can be widely used as the safest resin material of products such as food containers and the like, is 100 percent recyclable, nontoxic and lighter in density, but the traditional PP material can be vitrified at low temperature due to factors such as low temperature resistance, high shrinkage, low rigidity, high warping and the like, and the impact resistance is greatly reduced, so that the utilization rate of the PP material in the lamp industry is very low.
Chinese patent literature discloses a flame-retardant scratch-resistant photodiffusion PP material and a preparation method thereof, wherein the publication number is CN104292637A, and the photodiffusion PP material disclosed by the invention is characterized in that on the basis of taking a PP material as a base material, a plurality of synergistic functional additives such as nano antimony trioxide, an organic silicon polymer, an acid absorbent and the like are added, so that the flame-retardant scratch-resistant photodiffusion PP material can stably improve the flame-retardant scratch-resistant photodiffusion PP material and has excellent light efficiency. However, the invention does not effectively solve the problems of poor thermal stability and weak impact resistance of the PP material.
Disclosure of Invention
In order to overcome the problem that the traditional PP material is low in utilization rate in the lamp industry due to poor thermal stability and weak impact resistance, the invention provides the light diffusion PP material with good thermal stability and strong impact resistance, so that the thermal stability of the PP material is improved, the shrinkage rate is reduced, the rigidity is improved, and the warping rate is reduced.
The invention also provides a preparation method of the photodiffusion PP material, which is simple to operate, has no special requirements on equipment and is easy to realize large-scale industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a light diffusion PP material comprises the following components in parts by weight: 90-98 parts of polypropylene, 0.2-1 part of light diffusant, 0.05-3 parts of flame retardant, 0.05-1 part of antioxidant, 0.05-1 part of lubricant and 0.5-5 parts of anti-UV agent. The lubricant is at least one of Ethylene Bis Stearamide (EBS), erucamide, oleamide and silicone.
Preferably, the light diffusing agent is prepared by coating acrylic resin microspheres with a light-responsive gelator.
Preferably, the coating process comprises the following steps: and uniformly dispersing the material to be coated in the photoresponse type gel factor suspension liquid under the dark condition, standing and drying.
Preferably, the volume ratio of the material to be coated to the photoresponsive gelator is (20-5): 1.
preferably, the structure formula of the photoresponsive gelator is:
the selected photoresponse type gelator is preferably a binary organic salt gelator, which is subjected to gel damage when anthracene groups undergo dimerization under ultraviolet light irradiation and becomes a precipitate after standing; the precipitate can be returned to the gel state after being reheated. The invention adopts the light-responsive gel factor coated acrylic resin microspheres as a novel light diffusant, and the novel light diffusant is added into a pp material, so that different gel cycle changes can be generated aiming at light with different wavelengths emitted by an LED lamp, and the acrylic resin microspheres are organic light diffusant. According to the invention, after the surface of the organic light diffusant is coated with the light response gel factor, the gel factor can be automatically adjusted according to the emitted light of different light sources, and meanwhile, the gel conversion is realized by means of the heat generated by the light sources, so that the thermal stability of the light diffusion PP material is improved, the light is softer, the light loss is smaller, and the light diffusion PP material is more intelligent.
Preferably, based on the total mass of the acrylic resin microspheres, the acrylic resin microspheres have the following size fractions by mass percent: the microspheres with the particle size of 1-2 microns account for 25-35%, the microspheres with the particle size of 3-5 microns account for 45-55%, and the microspheres with the particle size of 6-15 microns account for 10-25%.
The light diffusant has different particle sizes and different refractive indexes by adjusting the acrylic resin microspheres with different particle sizes and mass percentage contents, so that light rays passing through the acrylic resin microspheres with different particle sizes are refracted for countless times and penetrate through the acrylic resin microspheres, strong light is refracted and uniformly dispersed, a point light source is changed into a surface light source, a light emitting surface is enlarged, and light rays are softer and have little light loss; meanwhile, the fluidity of the system is greatly increased and the shock resistance of the photodiffusion PP material is enhanced by the synergistic blending of different particle sizes and mass percentage contents.
Preferably, the flame retardant is polycaprolactone modified ammonium polyphosphate or nucleoside modified ammonium polyphosphate.
Preferably, the molecular weight of the polycaprolactone is 500-10000 g/mol.
Polycaprolactone is degradable polyhydric alcohol, ammonium polyphosphate is a halogen-free flame retardant, and the environment is protected; according to the invention, the polycaprolactone modified ammonium polyphosphate is adopted, and the abundant active hydroxyl groups on the surface of the polycaprolactone are utilized to be more compatible with the PP material, so that the interface binding force is increased, the addition amount of the flame retardant is reduced, and simultaneously, the impact strength of the photodiffusion PP material is improved by cooperating with a formula system.
Preferably, the nucleoside is a protonated nucleoside having the formula:
the method for modifying the ammonium polyphosphate by the nucleoside comprises the following steps: ammonium polyphosphate and protonated nucleoside are mixed according to the mass ratio (5-10): 1, and uniformly mixing to obtain the nucleoside modified ammonium polyphosphate. The flame retardant of nucleoside modified ammonium polyphosphate is a bio-based flame retardant, nucleoside is formed by connecting basic groups and pentose, is a natural compound integrating an air source and a carbon source, reduces the consumption of petroleum resources, protects the environment, has a simple preparation method, and is beneficial to realizing industrial production.
A preparation method of a photodiffusion PP material comprises the following steps: mixing the raw materials according to the proportion to obtain a mixed material, and then carrying out melt extrusion and granulation to obtain the photodiffusion PP material.
A preparation method of a photodiffusion PP material comprises the following steps:
(1) weighing the raw materials according to the proportion for later use, and coating the surface of the acrylic resin microsphere with the particle size of 6-15 mu m with a photoresponse gel factor to obtain a first light diffusant;
(2) uniformly mixing the first light diffusant and polypropylene, and then sequentially adding an antioxidant, a lubricant, a flame retardant and an anti-UV agent to obtain a mixed material;
(3) adding acrylic resin microspheres with the particle size of 3-5 microns into the mixture, uniformly mixing, and performing melt extrusion and granulation to obtain a granular material;
(4) coating a photoresponse gel factor on the surface of the particle material to obtain a second light diffusant;
(5) and adding acrylic resin microspheres with the particle size of 1-2 mu m into the second dispersing agent, uniformly mixing, and carrying out melt extrusion and granulation to obtain the photodiffusion PP material.
By adding the acrylic resin microspheres with different particle sizes in different steps, the acrylic resin microspheres are more uniformly distributed in a photodiffusion PP material system, the flowability is better, and the impact resistance and the photoinduction regulation capability are stronger.
Therefore, the invention has the following beneficial effects:
(1) by utilizing the photoresponse type gel factor compound light diffusant and the green environment-friendly flame retardant, the light diffusion PP material system is more uniform in distribution, better in fluidity and stronger in impact resistance and photoinduction regulation capacity;
(2) through modification, the PP material achieves better light diffusivity, so that the PP material can meet the impact test of IEC60598 and GB7000.1 when being manufactured into a diffusion cover with the wall thickness of 0.5mm-1.5mm, the common PP material can be vitrified at low temperature, the impact resistance is greatly reduced, and the PP material can still meet the impact test of IEC60598 and GB7000.1 when the temperature is low to 35 ℃. The modified light diffusion PP has better thermal stability, and the softening temperature can reach 105 ℃. The modified light-diffusion PP has better anti-aging performance, and can still ensure yellowing performance under high-intensity ultraviolet irradiation;
(3) the preparation process is simple to operate, low in cost, free of special requirements for equipment and easy to realize industrial production.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
(1) Respectively weighing 90g of polypropylene, 0.2g of light diffusant, 0.05g of flame retardant, 0.05g of antioxidant, 0.05g of erucamide and 5g of anti-UV agent according to the following mixture ratio; the light diffusant is prepared by coating acrylic resin microspheres with a light-responsive gelator, and the volume ratio of the acrylic resin microspheres to the light-responsive gelator is 20: 1; the flame retardant is polycaprolactone modified ammonium polyphosphate, and the molecular weight of polycaprolactone is 500 g/mol;
(2) mixing the raw materials to obtain a mixed material, and then performing melt extrusion and granulation to obtain the photodiffusion PP material.
Example 2
(1) Weighing the raw materials for later use, uniformly dispersing acrylic resin microspheres with the particle size of 6-15 microns in a photoresponse gel factor suspension under a dark condition, standing, and drying, wherein the volume ratio of the acrylic resin microspheres to the photoresponse gel factors is 5: 1, coating a light-responsive gel factor on the surface of an acrylic resin microsphere to obtain a first light diffusant;
(2) uniformly mixing the first light diffusant and 98g of polypropylene, and then sequentially adding 1g of antioxidant, 1g of Ethylene Bis Stearamide (EBS), 3g of nucleoside modified ammonium polyphosphate and 0.5g of anti-UV agent to obtain a mixed material;
(3) adding acrylic resin microspheres with the particle size of 3-5 microns into the mixture, uniformly mixing, and performing melt extrusion and granulation to obtain a granular material;
(4) uniformly dispersing the granules in a photoresponse type gel factor suspension liquid under the dark condition, standing and drying, wherein the volume ratio of the granules to the photoresponse type gel factor is 15: 1, coating a light-responsive gel factor on the surface of the particle material to obtain a second light diffusant;
(5) adding acrylic resin microspheres with the particle size of 1-2 microns into the second dispersing agent, uniformly mixing, and carrying out melt extrusion and granulation to obtain the photodiffusion PP material;
wherein, taking 1g of the total mass of the acrylic resin microspheres as a reference (the mass of the photoresponse type gel factor can be ignored), the size fraction and the mass percentage of the acrylic resin microspheres are as follows: the microspheres with the particle size of 1-2 microns account for 25%, the microspheres with the particle size of 3-5 microns account for 55%, and the microspheres with the particle size of 6-15 microns account for 20%.
Example 3
(1) Weighing the raw materials for later use, uniformly dispersing acrylic resin microspheres with the particle size of 6-15 microns in a photoresponse gel factor suspension under a dark condition, standing, and drying, wherein the volume ratio of the acrylic resin microspheres to the photoresponse gel factor is 15: 1, coating a light-responsive gel factor on the surface of an acrylic resin microsphere to obtain a first light diffusant;
(2) uniformly mixing the first light diffusant and 95g of polypropylene, and then sequentially adding 0.5g of antioxidant, 0.5g of silicone, 2g of polycaprolactone-modified ammonium polyphosphate (the molecular weight of polycaprolactone is 10000g/mol) and 3g of anti-UV agent to obtain a mixed material;
(3) adding acrylic resin microspheres with the particle size of 3-5 microns into the mixture, uniformly mixing, and performing melt extrusion and granulation to obtain a granular material;
(4) uniformly dispersing the granules in a photoresponsive gel factor suspension liquid under the dark condition, standing and drying, wherein the volume ratio of the granules to the photoresponsive gel factor is 12: 1, coating a light-responsive gel factor on the surface of the particle material to obtain a second light diffusant;
(5) adding acrylic resin microspheres with the particle size of 1-2 microns into the second dispersing agent, uniformly mixing, and carrying out melt extrusion and granulation to obtain the photodiffusion PP material;
wherein, the total mass of the acrylic resin microspheres is 0.8g as a reference (the mass of the photoresponse gel factor can be ignored), and the particle size and the mass percentage of the acrylic resin microspheres are as follows: 30% of microspheres with the diameter of 1-2 microns, 45% of microspheres with the diameter of 3-5 microns and 25% of microspheres with the diameter of 6-15 microns.
Example 4
(1) Weighing the raw materials for later use, uniformly dispersing acrylic resin microspheres with the particle size of 6-15 microns in a photoresponse gel factor suspension under a dark condition, standing, and drying, wherein the volume ratio of the acrylic resin microspheres to the photoresponse gel factor is 18: 1, coating a light-responsive gel factor on the surface of an acrylic resin microsphere to obtain a first light diffusant;
(2) uniformly mixing the first light diffusant and 92g of polypropylene, and sequentially adding 0.2g of antioxidant, 0.8g of oleamide, 2g of nucleoside modified ammonium polyphosphate and 4g of anti-UV agent to obtain a mixed material;
(3) adding acrylic resin microspheres with the particle size of 3-5 microns into the mixture, uniformly mixing, and performing melt extrusion and granulation to obtain a granular material;
(4) uniformly dispersing the granules in a photoresponse type gel factor suspension liquid under the dark condition, standing and drying, wherein the volume ratio of the granules to the photoresponse type gel factor is 15: 1, coating a light-responsive gel factor on the surface of the particle material to obtain a second light diffusant;
(5) adding acrylic resin microspheres with the particle size of 1-2 microns into the second dispersing agent, uniformly mixing, and carrying out melt extrusion and granulation to obtain the photodiffusion PP material;
wherein, the total mass of the acrylic resin microspheres is 0.8g as a reference (the mass of the photoresponse gel factor can be ignored), and the particle size and the mass percentage of the acrylic resin microspheres are as follows: 35% of microspheres with the diameter of 1-2 microns, 55% of microspheres with the diameter of 3-5 microns and 10% of microspheres with the diameter of 6-15 microns.
Comparative example 1
The difference between the comparative example 1 and the example 1 is that the light diffusion agent is acrylic resin microspheres, and the rest process conditions are completely the same.
Comparative example 2
The comparative example 2 is different from the example 1 in that the flame retardant is ammonium polyphosphate and the rest of the process conditions are completely the same.
Comparative example 3
Comparative example 3 is different from example 2 in that there is no step of coating the photo-responsive gelator and the rest of the process conditions are identical.
Comparative example 4
The comparative example is different from example 2 in that the flame retardant is ammonium polyphosphate and the rest of the process conditions are completely the same.
The properties of the light-diffusing PP materials obtained in examples 1 to 4 and comparative examples 1 to 4 were measured, and the results are shown in Table 1:
TABLE 1 test results
The light diffusion PP material can meet IEC6098, pin flame, 650 ℃ glow wire and 120 ℃ ball pressure by adding the flame retardant. By adding the light diffusion agent, the light passing through the material product is softer. The light diffusion PP material achieves better light diffusion, so that the light diffusion PP material can meet the impact test of IEC60598 and GB7000.1 when a diffusion cover with the wall thickness of 0.5mm-1.5mm is manufactured, the common PP material can be vitrified at low temperature, the impact resistance is greatly reduced, and the light diffusion PP material can still meet the impact test of IEC60598 and GB7000.1 when the wall thickness of a product is 0.5mm-1.5mm at the low temperature of-35 ℃. The modified light diffusion PP has better thermal stability, and the softening temperature can reach 105 ℃. The modified light-diffusion PP material disclosed by the invention has better ageing resistance, and can still ensure the yellowing performance under the irradiation of high-intensity ultraviolet rays.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (5)
1. The light diffusion PP material is characterized by comprising the following components in parts by weight: 90-98 parts of polypropylene, 0.2-1 part of light diffusant, 0.05-3 parts of flame retardant, 0.05-1 part of antioxidant, 0.05-1 part of lubricant and 0.5-5 parts of anti-UV agent;
the light diffusant consists of a light response type gel factor and acrylic resin microspheres;
based on the total mass of the acrylic resin microspheres, the acrylic resin microspheres have the following size fraction and mass percentage content: 25-35% of microspheres with the diameter of 1-2 microns, 45-55% of microspheres with the diameter of 3-5 microns and 10-25% of microspheres with the diameter of 6-15 microns;
the structural formula of the photoresponse type gelator is as follows:
the preparation method of the light diffusion PP material comprises the following steps:
(1) weighing the raw materials according to a ratio for later use, and coating the surface of the acrylic resin microsphere with the particle size of 6-15 mu m with a photoresponse gel factor;
(2) uniformly mixing the coated acrylic resin microspheres and polypropylene, and sequentially adding an antioxidant, a lubricant, a flame retardant and an anti-UV agent to obtain a mixed material;
(3) adding acrylic resin microspheres with the particle size of 3-5 microns into the mixture, uniformly mixing, and performing melt extrusion and granulation to obtain a granular material;
(4) coating a photoresponse type gel factor on the surface of the granular material;
(5) and adding acrylic resin microspheres with the particle size of 1-2 mu m into the coated granular material, uniformly mixing, and carrying out melt extrusion and granulation to obtain the photodiffusion PP material.
2. The photodiffusion PP material of claim 1, wherein the coating process comprises: and uniformly dispersing the material to be coated in the photoresponse type gel factor suspension liquid under the dark condition, standing and drying.
3. The photodiffusion PP material of claim 1, wherein the flame retardant is nucleoside-modified ammonium polyphosphate.
4. A method for preparing a light-diffusing PP material according to any of claims 1 to 3, comprising the steps of: mixing the raw materials according to the proportion to obtain a mixed material, and then carrying out melt extrusion and granulation to obtain the photodiffusion PP material.
5. A method for preparing a light-diffusing PP material according to any of claims 1 to 3, comprising the steps of:
(1) weighing the raw materials according to a ratio for later use, and coating the surface of the acrylic resin microsphere with the particle size of 6-15 mu m with a photoresponse gel factor;
(2) uniformly mixing the coated acrylic resin microspheres and polypropylene, and sequentially adding an antioxidant, a lubricant, a flame retardant and an anti-UV agent to obtain a mixed material;
(3) adding acrylic resin microspheres with the particle size of 3-5 microns into the mixture, uniformly mixing, and performing melt extrusion and granulation to obtain a granular material;
(4) coating a photoresponse type gel factor on the surface of the granular material;
(5) and adding acrylic resin microspheres with the particle size of 1-2 mu m into the coated granular material, uniformly mixing, and carrying out melt extrusion and granulation to obtain the photodiffusion PP material.
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