WO2015196533A1 - 一种聚碳酸酯用光扩散剂及一种光扩散聚碳酸酯材料 - Google Patents

一种聚碳酸酯用光扩散剂及一种光扩散聚碳酸酯材料 Download PDF

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WO2015196533A1
WO2015196533A1 PCT/CN2014/084050 CN2014084050W WO2015196533A1 WO 2015196533 A1 WO2015196533 A1 WO 2015196533A1 CN 2014084050 W CN2014084050 W CN 2014084050W WO 2015196533 A1 WO2015196533 A1 WO 2015196533A1
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light
agent
parts
diffusing
polycarbonate
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PCT/CN2014/084050
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English (en)
French (fr)
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杜崇铭
林湖彬
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惠州市昌亿新材料有限公司
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Publication of WO2015196533A1 publication Critical patent/WO2015196533A1/zh

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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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/07—Aldehydes; Ketones
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/20—Carboxylic acid amides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes

Definitions

  • the invention relates to the technical field of polymer materials, in particular to a light diffusing agent for polycarbonate and a light diffusing polycarbonate material.
  • Light diffusing material refers to a material that can convert point and line light sources into line and surface light sources. Generally, it is prepared by dispersing light-diffusing particles having different refractive indices different from the substrate in a transparent substrate, and is mostly used as a backlight material for a liquid crystal display. Also known as light scattering materials or astigmatism materials.
  • LED light emitting diode
  • the use of light diffusing materials for light emitting diode (LED) illumination has opened up a new field of application in recent years. LED lighting is stronger than liquid crystal backlight, softer light performance; used for LED Illuminated light diffusing materials must minimize light loss and have good toughness while diffusing light.
  • an organic light diffusing agent and polycarbonate are often used to prepare an LED having high light transmittance and high light diffusing property by a blending method.
  • Light diffusing material for lighting can be generally classified into silicones and acrylics, wherein the acrylic light diffusing agents have larger particle diameters, high light transmittance but poor atomization effect, and can maintain poly
  • the present invention provides a light diffusing agent capable of imparting high light transmittance and high atomization degree to a polycarbonate material.
  • a light diffusing agent for polycarbonate the raw material of which comprises the following components by weight:
  • Light scattering agent 2 11 to 15 parts
  • the light scattering agent 1 is a substance having the following formula
  • the light scattering agent 2 is a substance having the following formula
  • the compatibilizing agent is a mixture of 1 to 3 parts by weight of dodecyldimethylbenzylammonium chloride and 0.5 to 0.7 parts of ethyl acetoacetate; the R 1 is an acyl group, and the R 2 is a linear alkyl group having 1 to 3 carbon atoms; the frozen finely divided polysiloxane particles are obtained by cooling a silicone particle having an average particle diameter of 2 ⁇ m to -10 ° C to -20 ° C, The obtained silicone particles were ultrasonically pulverized at 60 kHz.
  • the silicone particles are commercially available silicone particle products. The designer found that the silicone particles are ultrasonically pulverized in a low temperature environment, and at a low temperature, the volume of the silicone particles shrinks sharply, causing internal cracks, and ultrasonic pulverization can promote the process, and finally Many fine cracks are created inside the particle. When the light passes through these small cracks, it will undergo multiple refractions, and finally achieve the effect of increasing the degree of atomization. Although other methods can be used to process fine cracks in the silicone particles, the method of freezing and pulverizing can make the cracks more evenly distributed and the atomization effect can be further improved.
  • the light transmittance of the frozen finely divided polysiloxane particles is more serious, and the designer unexpectedly finds that when the crack is filled with the light scattering agent When the mixture of the light scattering agent 2 and the light scattering agent 2 is used, the light transmittance of the frozen finely divided polysiloxane particles can be greatly increased, and the light loss can be reduced.
  • the function of the compatibilizer is to make the light scattering agent 1 and the light scattering agent 2 Formed in a uniform, stable system, and stably present in the freeze-milled polysiloxane particles to avoid denaturation during processing added to the polycarbonate material.
  • the dodecyldimethylbenzylammonium chloride and acetoacetate acetate are commercially available products.
  • the polycarbonate material to which the light diffusing agent of the present invention is added is tested to refract incident light at most 58 °.
  • the freeze-micropulverized silicone particles when combined with the polycarbonate material, have a good retention effect on the impact resistance and processing heat stability of the polycarbonate material.
  • the R 1 is one of a formyl group, an acetyl group or a sulfinyl group.
  • the light scattering agent 1 may be any one of the following:
  • the light scattering agent 1 is diacetyl, which can be achieved by using a commercially available product.
  • R 2 is a methyl group, the light scattering agent 2 is diacetone acrylamide, which can be achieved by using a commercially available product.
  • the inventors have found that the above-mentioned light scattering agent 1 is mixed with the light scattering agent 2, and the unique structure of the mixture allows the incident light to be refracted in a random direction, and even if the atomization effect is further characterized, it is advantageous to make the light emitted by the LED softer. Since both the light scattering agent 1 and the light scattering agent 2 can be realized by using a commercially available product, the production cost and the processing difficulty of the present invention are both reduced, which is particularly advantageous for the large-scale popularization of the present technology.
  • the invention also provides a method for preparing the light diffusing agent, comprising the following steps:
  • the silicone particles are cooled to -10 °C to -20 °C for 2 min to 5 min, and the frequency is 60 KHz. Ultrasonic pulverizing it for 15 minutes to 20 minutes to prepare the frozen finely pulverized silicone particles;
  • the freeze-milled polysiloxane particles are added, and the rotary shaker is used.
  • the light diffusing agent is obtained by shaking at a speed of 200 to 400 rpm for 30 to 40 minutes.
  • the light scattering agent 1, the light scattering agent 2 and the compatibilizing agent can be sufficiently infiltrated into the gap of the frozen finely divided polysiloxane particles.
  • Another object of the present invention is to provide a polycarbonate having high light transmittance and high haze.
  • a light diffusing polycarbonate material comprising a light diffusing agent as described above.
  • the raw materials thereof include the following components in parts by weight.
  • the invention is directed to LED
  • the composition of the light diffusing polycarbonate material was designed using the characteristics of the lampshade.
  • the above polycarbonate, a diffusing agent, a lubricant, an ultraviolet absorber, and a whitening agent can be used in a commercially available product.
  • the diffusing agent is an EBS diffusing agent
  • the lubricant is a modified wax lubricant
  • the ultraviolet absorber is a UV absorber UV-234
  • the brightener is an oxazole whitening agent.
  • EBS Diffusion agent Chinese full name is vinyl bis-stearamide, which can improve the diffusibility and coupling of each raw material component, so that each raw material component can be a uniform and stable system, and the polycarbonate material obtained can be guaranteed. Stable performance. special, The EBS diffusing agent enables the light diffusing agent of the present invention to be uniformly distributed in the polycarbonate material and to reduce its polarity.
  • the lubricant is a modified wax lubricant, such as the Mengdan wax produced by Clariant WE-40
  • the internal fluidity and demolding effect of the polycarbonate material of the present invention can be improved.
  • the whitening agent is an oxazole whitening agent, such as model OB-1 A whitening agent which can effectively improve the appearance of the polycarbonate material produced and increase the whiteness of the polycarbonate material.
  • OB-1 model OB-1 A whitening agent which can effectively improve the appearance of the polycarbonate material produced and increase the whiteness of the polycarbonate material.
  • the light diffusing polycarbonate material of the present invention can be optionally prepared by a blending method which can be used for polycarbonate.
  • the above components are all designed for the characteristics of the light diffusing agent of the present invention, and the light-diffusing polycarbonate material prepared by using the raw material formula provided by the invention not only has the advantages of high light transmittance and good atomization effect, etc.
  • the impact resistance, processing thermal stability, extrusion properties, and anti-aging properties are also maintained within a relatively excellent range.
  • the present invention has the following beneficial effects:
  • the invention adopts a method of low temperature freezing and ultrasonic pulverization, and converts the commercially available polysiloxane particles into low temperature micropulverized polysiloxane particles, which is added to the polycarbonate material, so that the polycarbonate material can obtain excellent fog.
  • the low-temperature finely pulverized polysiloxane particles of the present invention also overcome the influence of the existing silicone light diffusing agent on the properties of the polycarbonate material, so that the light-diffusing polycarbonate material prepared by the invention can maintain excellent performance. Its impact resistance, processing thermal stability and other properties.
  • the invention selects light scattering agent 1 and light scattering agent 2 Filled in the gap of the low-temperature finely pulverized silicone particles, the problem of large light loss of the low-temperature finely pulverized silicone particles is solved, and the polycarbonate material to which the light diffusing agent of the present invention is added can be kept high. Luminosity.
  • the unique molecular structure of diacetyl and diacetone acrylamide further refracts the light passing through the mixture of the two, thereby further improving the atomization effect of the light diffusing agent.
  • the light-diffusing polycarbonate material provided by the present invention the type and amount of the raw material components are optimized for the performance of the light diffusing agent of the present invention, ensuring that the light diffusing agent can be uniformly and stably present in the polycarbonate material, and
  • the final light diffused polycarbonate material has good impact resistance, high thermal stability and excellent processing properties.
  • the present embodiment provides a high light transmittance and high haze light diffusing agent for polycarbonate, the raw materials of which include the following components by weight:
  • the light scattering agent 1 is a substance having the following formula
  • the light scattering agent 2 is a substance having the following formula
  • the compatibilizer is 2 parts by weight of dodecyldimethylbenzylammonium chloride, 0.6 parts of ethyl acetoacetate; the R 1 is an acyl group, the R 2 is a methyl group;
  • the finely pulverized silicone particles are silicone particles obtained by subjecting polysiloxane particles having an average particle diameter of 2 ⁇ m to -17 ° C and ultrasonically pulverizing at 60 kHz.
  • the above polysiloxane particles can be made to Tospearl of GE Corporation of the United States.
  • the embodiment further provides a method for preparing the above light diffusing agent, which comprises the following steps:
  • the silicone particles were cooled to -17 °C, and after 3 minutes, they were pulverized by ultrasonic waves with a frequency of 60 kHz.
  • the frozen finely divided polysiloxane particles were prepared at 18 min;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer was uniformly mixed, the freeze-pulverized polysiloxane particles were added and shaken at 330 rpm for 37 minutes using a rotary shaker to prepare the light diffusing agent.
  • the present embodiment provides a high light transmittance and high haze light diffusing agent for polycarbonate, the raw materials of which include the following components by weight:
  • the light scattering agent 1 is a substance having the following formula
  • the light scattering agent 2 is a substance having the following formula
  • the compatibilizer is 1 part by weight of dodecyldimethylbenzylammonium chloride, 0.7 part of ethyl acetoacetate; the R 1 is an acyl group, and the R 2 is a carbon atom
  • the linear alkyl group; the freeze-milled polysiloxane particles are silicone particles obtained by ultrasonically pulverizing 60 KHz after cooling the silicone particles having an average particle diameter of 2 ⁇ m to -20 ° C. .
  • the embodiment further provides a method for preparing the above light diffusing agent, which comprises the following steps:
  • the silicone particles were cooled to -20 °C, and after 2 minn, they were pulverized with ultrasonic waves at a frequency of 60 kHz. 20 min, the frozen finely divided polysiloxane particles were prepared;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer was uniformly mixed, the freeze-pulverized polysiloxane particles were added and shaken at 200 rpm for 30 min using a rotary shaker to prepare the light diffusing agent.
  • the present embodiment provides a high light transmittance and high haze light diffusing agent for polycarbonate, the raw materials of which include the following components by weight:
  • the light scattering agent 1 is a substance having the following formula
  • the light scattering agent 2 is a substance having the following formula
  • the compatibilizer is 3 parts by weight of dodecyldimethylbenzylammonium chloride, 0.5 parts of ethyl acetoacetate; the R 1 is an acyl group, and the R 2 is a carbon atom containing 3 carbon atoms.
  • the linear alkyl group; the freeze-milled polysiloxane particles are silicone particles obtained by ultrasonically pulverizing 60 KHz after cooling the silicone particles having an average particle diameter of 2 ⁇ m to -10 °C. .
  • the embodiment further provides a method for preparing the above light diffusing agent, which comprises the following steps:
  • the silicone particles were cooled to -10 °C, and after 5 minutes, they were pulverized by ultrasonic waves with a frequency of 60 kHz. Preparing the frozen finely divided polysiloxane particles at 15 minmin;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer was uniformly mixed, the freeze-pulverized polysiloxane particles were added and shaken at 400 rpm for 30 minutes using a rotary shaker to prepare the light diffusing agent.
  • the present embodiment provides a high light transmittance and high haze light diffusing agent for polycarbonate, the raw materials of which include the following components by weight:
  • the light scattering agent 1 is a substance having the following formula
  • the light scattering agent 2 is a substance having the following formula
  • the compatibilizer is 2.5 parts by weight of dodecyldimethylbenzylammonium chloride, 0.6 parts of ethyl acetoacetate; the R 1 is an acyl group, and the R 2 is an ethyl group;
  • the micropulverized silicone particles refer to silicone particles obtained by ultrasonically pulverizing 60 KHz after cooling the silicone particles having an average particle diameter of 2 ⁇ m to -10 °C.
  • the present embodiment provides a high light transmittance and high haze light diffusing agent for polycarbonate, the raw materials of which include the following components by weight:
  • Light scattering agent 1 3.5 parts
  • the light scattering agent 1 is a substance having the following formula
  • the light scattering agent 2 is a substance having the following formula
  • the compatibilizing agent is 1 to 3 parts by weight of dodecyldimethylbenzylammonium chloride, 0.5 to 0.7 parts of ethyl acetoacetate; the R 1 is an acyl group, and the R 2 is a methyl group.
  • the frozen finely divided polysiloxane particles are silicone particles obtained by ultrasonically pulverizing 60 KHz after cooling the silicone particles having an average particle diameter of 2 ⁇ m to -20 °C.
  • the embodiment further provides a method for preparing the above light diffusing agent, which comprises the following steps:
  • the silicone particles were cooled to -20 °C, and after 3 minutes, they were pulverized by ultrasonic waves with a frequency of 60 kHz. 19 min, the frozen finely divided polysiloxane particles were prepared;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer was uniformly mixed, the freeze-pulverized polysiloxane particles were added and shaken at 350 rpm for 39 minutes using a rotary shaker to prepare the light diffusing agent.
  • the present embodiment provides a light-diffusing polycarbonate, the raw materials of which include the following components in parts by weight
  • UV absorber 0.4 parts
  • the diffusing agent is an EBS diffusing agent
  • the lubricant is a modified wax lubricant
  • the ultraviolet absorber is a UV absorber. UV-234
  • the brightener is an oxazole whitening agent.
  • the lubricant is Mengdan wax WE-40 produced by Clariant, and the brightener is OB-1. Brightener.
  • the above light diffusing agent is the light diffusing agent provided in Example 1.
  • the above diffusing agent and ultraviolet absorber can be realized by using a commercially available product.
  • the light-diffusing polycarbonate material obtained in this example was tested using ASTM International Standard, and the results are shown in Table 1:
  • the present embodiment provides a light-diffusing polycarbonate, the raw materials of which include the following components in parts by weight
  • the diffusing agent is an EBS diffusing agent
  • the lubricant is a modified wax lubricant
  • the ultraviolet absorber is a UV absorber. UV-234
  • the brightener is an oxazole whitening agent.
  • the lubricant is Mengdan wax WE-40 produced by Clariant, and the brightener is OB-1. Brightener.
  • the above light diffusing agent is the light diffusing agent provided in Example 1.
  • the above diffusing agent and ultraviolet absorber can be realized by using a commercially available product.
  • the light-diffusing polycarbonate material obtained in this example was tested using ASTM International Standard, and the results are shown in Table 2:
  • the present embodiment provides a light-diffusing polycarbonate, the raw materials of which include the following components in parts by weight
  • UV absorber 0.5 parts
  • the diffusing agent is an EBS diffusing agent
  • the lubricant is a modified wax lubricant
  • the ultraviolet absorber is a UV absorber. UV-234
  • the brightener is an oxazole whitening agent.
  • the lubricant is Mengdan wax WE-40 produced by Clariant, and the brightener is OB-1. Brightener.
  • the above light diffusing agent is the light diffusing agent provided in Example 1.
  • the above diffusing agent and ultraviolet absorber can be realized by using a commercially available product.
  • the light-diffusing polycarbonate material obtained in this example was tested using ASTM International Standard, and the results are shown in Table 3:
  • This comparative example provides a light diffusing polycarbonate whose light diffusing agent is a commercially available silicone light diffusing agent, and the remaining components are in accordance with Example 6.
  • the light-diffusing polycarbonate material obtained in this comparative example was tested using ASTM International Standard. The results are shown in Table 4:
  • This comparative example provides a light diffusing polycarbonate whose light diffusing agent is a commercially available silicone light diffusing agent, and the remaining components are the same as in Example 6 Consistent.
  • the light-diffusing polycarbonate material obtained in this comparative example was tested using ASTM International Standard. The results are shown in Table 5:
  • Example 6 Numbering Haze /% Transmittance /% Example 6 (thickness 1mm) 91.9 89.3 Example 6 (thickness 2mm) 92.7 89.0 Example 7 (thickness 1mm) 92.1 88.7 Example 7 (thickness 2mm) 92.5 88.1 Example 8 (thickness 1 mm) 91.8 88.5 Example 8 (thickness 2mm) 91.8 88.3 Comparative Example 1 (thickness 1 mm) 83.7 75.6 Comparative Example 1 (thickness 2 mm) 84.1 73.2 Comparative Example 2 (thickness 1 mm) 85.4 72.9 Comparative Example 2 (thickness 2mm) 85.6 72.0
  • Example 6 (thickness 1mm) 58
  • Example 6 (thickness 2mm) 58
  • Example 7 (thickness 1mm) 51
  • Example 7 (thickness 2mm) 51
  • Example 8 (thickness 1 mm) 49
  • Comparative Example 1 (thickness 1 mm) 30
  • Comparative Example 1 (thickness 2 mm) 30
  • Comparative Example 2 (thickness 1 mm) 18 Comparative Example 2 (thickness 2mm) 18
  • Example 1 Numbering Containment factor Example 1 0.8
  • Example 2 1.0
  • Example 3 Commercially available 2 ⁇ m polysilane particles 0.01

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Abstract

本发明公开一种聚碳酸酯用光扩散剂，其原料包括冷冻粉碎的聚硅氧烷颗粒、光散射剂 1 、光散射剂 2 、相容剂。本发明采用低温冷冻与超声波粉碎的方法，将市售的聚硅氧烷颗粒转化为低温微粉碎聚硅氧烷颗粒，其添加至聚碳酸酯材料中，可使聚碳酸酯材料获得优秀的雾化效果;同时本发明的低温微粉碎聚硅氧烷颗粒也克服了现有聚氨酯丙烯酸类光扩散剂对聚碳酸酯材料性能的影响，使本发明所制得的光扩散聚碳酸酯材料能够保持优秀的抗冲击性能、加工热稳定性等性能。

Description

一种聚碳酸酯用光扩散剂及一种光扩散聚碳酸酯材料 技术领域
本发明涉及高分子材料技术领域，具体涉及一种聚碳酸酯用光扩散剂及一种光扩散聚碳酸酯材料。
背景技术
光扩散材料指能将点、线光源转化成线、面光源的材料， 一般通过将与基材不同折射系数的光扩散粒子分散在透明基材中制备得到， 早期多用于液晶显示器的背光源材料， 又称为光散射材料或散光材料。将光扩散材料用于发光二极管（LED）照明是近年来开辟的一个新应用领域。LED照明较液晶背光源更强，柔和光线性能更高；用于LED 照明的光扩散材料在扩散光的同时，须尽量减少光损失，且有良好的韧性。因此，多采用有机光扩散剂和聚碳酸酯（PC）通过共混法制备兼有高透光率和高光扩散性能的LED 照明用光扩散材料。现有的用于聚碳酸酯的有机光扩散剂一般可分为有机硅类及丙烯酸类，其中丙烯酸类光扩散剂其粒子粒径更大，透光率高但雾化效果差，可保持聚碳酸酯材料的高抗冲性能及良好的加工热稳定性；有机硅类的雾化效果较好，其使用又将一定程度地降低最终制得的聚碳酸酯材料的抗冲击性及加工热稳定性，且其透光率较低，光损严重。
发明内容
有鉴于此，本发明提供一种能够使聚碳酸酯材料兼具高透光率及高雾化程度的光扩散剂。
本发明的目的通过以下技术方案实现：
一种聚碳酸酯用光扩散剂，其原料按重量份计包括以下组分：
冷冻微粉碎聚硅氧烷颗粒 30 ～ 60 份；
光散射剂 1 2 ～ 8 份；
光散射剂 2 11 ～ 15 份；
相容剂 5 ～ 10 份；
所述光散射剂 1 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000001
 ；
所述光散射剂 2 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000002
 ；
所述相容剂为按重量计 1 ～ 3 份十二烷基二甲基苄基氯化铵、 0.5 ～ 0.7 份乙酰乙酸乙酯的混合物；所述的 R1 为酰基，所述 R2 为含有 1 ～ 3 个碳原子的直链烷基；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2 μ m 的聚硅氧烷颗粒降温至 -10 ℃～ -20 ℃后，以 60KHz 的超声波粉碎获得的聚硅氧烷颗粒。
所述聚硅氧烷颗粒为市售的聚硅氧烷颗粒产品。设计人发现，在低温环境下对聚硅氧烷颗粒进行超声波粉碎，在低温下，聚硅氧烷颗粒体积急剧收缩，导致内部产生裂缝，而超声波粉碎又可促进这一过程的进行，最终可使颗粒内部产生许多细小裂痕。光线在通过这些细小裂缝的时候，将发生多次折射，最终实现提高其雾化程度的效果。虽然可采用其他方法在聚硅氧烷颗粒内加工出细小裂缝，但冷冻粉碎的方法可以使裂缝分布得更加均匀，雾化效果得以进一步提高。但这种冷冻微粉碎聚硅氧烷颗粒的透光率下降较为严重，设计人意外地发现当所述裂缝中充盈所述有的光散射剂 1 及光散射剂 2 混合物时，能够大幅提升上述冷冻微粉碎聚硅氧烷颗粒的透光率，降低其光损。相容剂的作用则是使所述光散射剂 1 与光散射剂 2 形成以均匀、稳定的体系，而稳定存在于所述冷冻微粉碎聚硅氧烷颗粒之中，避免其添加至聚碳酸酯材料的加工过程中发生变性。所述十二烷基二甲基苄基氯化铵、乙酸乙酰乙酯为市售产品。经测试，添加有本发明光扩散剂的聚碳酸酯材料，最多可使入射光折射 58 °。除此以外，经冷冻微粉碎后的聚硅氧烷颗粒，其与聚碳酸酯材料结合后，对聚碳酸酯材料的抗冲击性能、加工热稳定性能均有良好的保持作用。
进一步的，所述 R1 为甲酰基、乙酰基或亚硫酰基中的一种。
及所述光散射剂 1 可以是如下物质中的任一种：
Figure YGHZ14017GMJ-appb-M000003
 ；
Figure YGHZ14017GMJ-appb-M000004
 ；
Figure YGHZ14017GMJ-appb-M000005
。
特别的，设计人发现当 R1 为乙酰基， R2 为甲基时，即光散射剂 2 为如下物质时
Figure YGHZ14017GMJ-appb-M000006
二者可在所述的冷冻微粉碎聚硅氧烷颗粒中长期共存而不会分离。当 R1 为乙酰基时，所述光散射剂 1 为双乙酰，可采用市售产品实现。当 R2 为甲基时，所述光散射剂 2 为双丙酮丙烯酰胺，可采用市售产品实现。发明人发现，上述光散射剂 1 与光散射剂 2 混合后，其混合物独特的结构可使入射光线发生随机方向的折射，即使雾化效果进一步特色，有利于使 LED 发出的光线更加柔和。由于光散射剂 1 与光散射剂 2 均可采用市售产品实现，使本发明的生产成本及加工难度均有所下降，特别有利于本技术的大规模推广。
本发明还提供一种制备所述光扩散剂的方法，包括以下工序：
将聚硅氧烷颗粒降温至 -10 ℃～ -20 ℃，保持 2min ～ 5min 后，采用频率为 60KHz 的超声波将其粉碎 15min ～ 20min ，制得所述冷冻微粉碎聚硅氧烷颗粒；
将所述光散射剂 1 、光散射剂 2 以及相容剂混合均匀后，加入所述冷冻微粉碎聚硅氧烷颗粒，采用旋转式摇床以 200 ～ 400 转 /min 的转速震荡 30 ～ 40min ，制得所述光扩散剂。
通过震荡，可使光散射剂 1 、光散射剂 2 及相容剂充分渗入述冷冻微粉碎聚硅氧烷颗粒的缝隙中。
本发明的另一目的是提供一种高透光、高雾度的聚碳酸酯。
上述目的通过以下技术方案实现：
一种光扩散聚碳酸酯材料，其原料包含有所述的光扩散剂。
具体的，其原料按重量份计包括以下组分
聚碳酸酯 92 ～ 97 份；
扩散剂 0.1 ～ 0.3 份；
润滑剂 0.1 ～ 0.3 份；
光扩散剂 0.2 ～ 1.1 份；
紫外线吸收剂 0.2 ～ 0.5 份；
增白剂 0.001 ～ 0.002 份。
本发明针对 LED 用灯罩的特点，对光扩散聚碳酸酯材料的成分进行了设计。上述聚碳酸酯、扩散剂、润滑剂、紫外线吸收剂及增白剂均可采用市售产品实现。
进一步的，所述扩散剂为 EBS 扩散剂；所述润滑剂为改性蜡润滑剂；所述紫外线吸收剂为紫外线吸收剂 UV-234 ；所述增白剂为恶唑类增白剂。
EBS 扩散剂，中文全称为乙烯基双硬脂酰胺，可改善各原料组分的扩散性及偶联性，使各原料组分能够成为一均匀、稳定的体系，保证所制得的聚碳酸酯材料性能的稳定。特别的， EBS 扩散剂能够使本发明的光扩散剂均匀地分布在聚碳酸酯材料中，并降低其极性的作用。
所述润滑剂为改性蜡润滑剂，比如科莱恩公司所产的蒙旦蜡 WE-40 ，能够提高本发明聚碳酸酯材料的内部流动性与脱模效果。
所述增白剂为恶唑类增白剂，比如型号为 OB-1 的增白剂，它可以有效改善所制得的聚碳酸酯材料的外观，提高聚碳酸酯材料的白度。与光扩散剂协效，使聚碳酸酯材料能够进一步缓和 LED 发出的光线，使之更加柔和。本发明的光扩散聚碳酸酯材料，可选用任一种可用于聚碳酸酯的共混法制备。
以上组分都是针对本发明光扩散剂的特点，设计而得，采用本发明提供的原料配方制得的光扩散聚碳酸酯材料，不但具有透光率高、雾化效果好等优点，其抗冲击性能、加工热稳定性、挤出性能、抗老化性能也保持在较为优秀的范围内。
本发明相对于现有技术，具有如下的有益效果：
1. 本发明采用低温冷冻与超声波粉碎的方法，将市售的聚硅氧烷颗粒转化为低温微粉碎聚硅氧烷颗粒，其添加至聚碳酸酯材料中，可使聚碳酸酯材料获得优秀的雾化效果；同时本发明的低温微粉碎聚硅氧烷颗粒也克服了现有有机硅光扩散剂对聚碳酸酯材料性能的影响，使本发明所制得的光扩散聚碳酸酯材料能够保持优秀的抗冲击性能、加工热稳定性等性能。
2. 本发明选用了光散射剂 1 、光散射剂 2 填充于低温微粉碎聚硅氧烷颗粒的缝隙中，解决低温微粉碎聚硅氧烷颗粒光损较大的问题，使添加有本发明的光扩散剂的聚碳酸酯材料能够保持较高的透光度。而双乙酰、双丙酮丙烯酰胺独特的分子结构，使通过二者混合物的光线发生随机方向的折射，进一步提高了光扩散剂的雾化效果。
3. 本发明提供的光扩散聚碳酸酯材料，其个原料组分的类型及用量均针对本发明光扩散剂的性能进行优化，确保光扩散剂能够均匀、稳定地存在于聚碳酸酯材料中，并是最终制得的光扩散聚碳酸酯材料具有良好的抗冲击性能、较高的热稳定性及优秀的加工性能。
具体实施方式
为了便于本领域技术人员理解，下面将结合实施例对本发明作进一步详细描述：
实施例 1
本实施例提供一种高透光高雾度的聚碳酸酯用光扩散剂，其原料按重量份计包括以下组分：
冷冻微粉碎聚硅氧烷颗粒 49 份；
光散射剂 1 7 份；
光散射剂 2 13 份；
相容剂 8 份；
所述光散射剂 1 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000004
；
所述光散射剂 2 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000006
 ；
所述相容剂为按重量计 2 份十二烷基二甲基苄基氯化铵、 0.6 份乙酰乙酸乙酯；所述的 R1 为酰基，所述 R2 为甲基；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2 μ m 的聚硅氧烷颗粒降温至 -17 ℃后，以 60KHz 的超声波粉碎获得的聚硅氧烷颗粒。
本实施例中，上述聚硅氧烷颗粒可以使美国 GE 公司的 Tospearl 。
本实施例还提供一种上述光扩散剂的制备方法，包括以下工序：
将聚硅氧烷颗粒降温至 -17 ℃，保持 3min 后，采用频率为 60KHz 的超声波将其粉碎 18min ，制得所述冷冻微粉碎聚硅氧烷颗粒；
将所述光散射剂 1 、光散射剂 2 以及相容剂混合均匀后，加入所述冷冻微粉碎聚硅氧烷颗粒，采用旋转式摇床以 330 转 /min 的转速震荡 37min ，制得所述光扩散剂。
实施例 2
本实施例提供一种高透光高雾度的聚碳酸酯用光扩散剂，其原料按重量份计包括以下组分：
冷冻微粉碎聚硅氧烷颗粒 30 份；
光散射剂 1 8 份；
光散射剂 2 11 份；
相容剂 10 份；
所述光散射剂 1 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000004
；
所述光散射剂 2 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000007
 ；
所述相容剂为按重量计 1 份十二烷基二甲基苄基氯化铵、 0.7 份乙酰乙酸乙酯；所述的 R1 为酰基，所述 R2 为含有 1 个碳原子的直链烷基；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2 μ m 的聚硅氧烷颗粒降温至 -20 ℃后，以 60KHz 的超声波粉碎获得的聚硅氧烷颗粒。
本实施例还提供一种上述光扩散剂的制备方法，包括以下工序：
将聚硅氧烷颗粒降温至 -20 ℃，保持 2minn 后，采用频率为 60KHz 的超声波将其粉碎 20min ，制得所述冷冻微粉碎聚硅氧烷颗粒；
将所述光散射剂 1 、光散射剂 2 以及相容剂混合均匀后，加入所述冷冻微粉碎聚硅氧烷颗粒，采用旋转式摇床以 200 转 /min 的转速震荡 30min ，制得所述光扩散剂。
实施例 3
本实施例提供一种高透光高雾度的聚碳酸酯用光扩散剂，其原料按重量份计包括以下组分：
冷冻微粉碎聚硅氧烷颗粒 60 份；
光散射剂 1 2 份；
光散射剂 2 15 份；
相容剂 5 份；
所述光散射剂 1 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000008
；
所述光散射剂 2 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000009
；
所述相容剂为按重量计 3 份十二烷基二甲基苄基氯化铵、 0.5 份乙酰乙酸乙酯；所述的 R1 为酰基，所述 R2 为含有 3 个碳原子的直链烷基；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2 μ m 的聚硅氧烷颗粒降温至 -10 ℃后，以 60KHz 的超声波粉碎获得的聚硅氧烷颗粒。
本实施例还提供一种上述光扩散剂的制备方法，包括以下工序：
将聚硅氧烷颗粒降温至 -10 ℃，保持 5min 后，采用频率为 60KHz 的超声波将其粉碎 15minmin ，制得所述冷冻微粉碎聚硅氧烷颗粒；
将所述光散射剂 1 、光散射剂 2 以及相容剂混合均匀后，加入所述冷冻微粉碎聚硅氧烷颗粒，采用旋转式摇床以 400 转 /min 的转速震荡 30min ，制得所述光扩散剂。
实施例 4
本实施例提供一种高透光高雾度的聚碳酸酯用光扩散剂，其原料按重量份计包括以下组分：
冷冻微粉碎聚硅氧烷颗粒 41 份；
光散射剂 1 5 份；
光散射剂 2 12.7 份；
相容剂 8.5 份；
所述光散射剂 1 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000008
 ；
所述光散射剂 2 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000009
 ；
所述相容剂为按重量计 2.5 份十二烷基二甲基苄基氯化铵、 0.6 份乙酰乙酸乙酯；所述的 R1 为酰基，所述 R2 为乙基；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2 μ m 的聚硅氧烷颗粒降温至 -10 ℃后，以 60KHz 的超声波粉碎获得的聚硅氧烷颗粒。
实施例 5
本实施例提供一种高透光高雾度的聚碳酸酯用光扩散剂，其原料按重量份计包括以下组分：
冷冻微粉碎聚硅氧烷颗粒 33 份；
光散射剂 1 3.5 份；
光散射剂 2 12 份；
相容剂 9 份；
所述光散射剂 1 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000005
 ；
所述光散射剂 2 为具有如下通式的物质
Figure YGHZ14017GMJ-appb-M000007
；
所述相容剂为按重量计 1 ～ 3 份十二烷基二甲基苄基氯化铵、 0.5 ～ 0.7 份乙酰乙酸乙酯；所述的 R1 为酰基，所述 R2 为甲基；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2 μ m 的聚硅氧烷颗粒降温至 -20 ℃后，以 60KHz 的超声波粉碎获得的聚硅氧烷颗粒。
本实施例还提供一种上述光扩散剂的制备方法，包括以下工序：
将聚硅氧烷颗粒降温至 -20 ℃，保持 3min 后，采用频率为 60KHz 的超声波将其粉碎 19min ，制得所述冷冻微粉碎聚硅氧烷颗粒；
将所述光散射剂 1 、光散射剂 2 以及相容剂混合均匀后，加入所述冷冻微粉碎聚硅氧烷颗粒，采用旋转式摇床以 350 转 /min 的转速震荡 39min ，制得所述光扩散剂。
实施例 6
本实施例提供一种光扩散聚碳酸酯，其原料按重量份计包括以下组分
聚碳酸酯 95 份；
扩散剂 0.2 份；
润滑剂 0.1 份；
光扩散剂 0.8 份；
紫外线吸收剂 0.4 份；
增白剂 0.0017 份。
本实施例中，所述扩散剂为 EBS 扩散剂；所述润滑剂为改性蜡润滑剂；所述紫外线吸收剂为紫外线吸收剂 UV-234 ；所述增白剂为恶唑类增白剂。
更进一步的，本实施例中，上述润滑剂为科莱恩公司所产的蒙旦蜡 WE-40 ，上述增白剂为型号为 OB-1 的增白剂。
上述光扩散剂为实施例 1 所提供的光扩散剂。上述扩散剂、紫外线吸收剂均可采用市售产品实现。
使用 ASTM 国际标准对本实施例所得的光扩散聚碳酸酯材料进行测试，其结果如表 1 所示：
性质 方法 单位 数据
比重 ASTM D792 - 1.2
模收缩 ASTM D955 % 0.5-0.7
拉伸强度 ASTM D638 Mpa 56
弯曲强度 ASTM D790 Mpa 92
延伸率 ASTM D638 % 59
弯曲模数 ASTM D790 Mpa 2380
缺口冲击强度 (1/8') ASTM D256 J/M 780
热变形温度 ASTM D648 ℃ 132
耐燃性 UL94 (1/8') V2
外观 - - 淡白
抗 UV 强度 - 级 4
实施例 7
本实施例提供一种光扩散聚碳酸酯，其原料按重量份计包括以下组分
聚碳酸酯 92 份；
扩散剂 0.3 份；
润滑剂 0.1 份；
光扩散剂 1.1 份；
紫外线吸收剂 0.2 份；
增白剂 0.002 份。
本实施例中，所述扩散剂为 EBS 扩散剂；所述润滑剂为改性蜡润滑剂；所述紫外线吸收剂为紫外线吸收剂 UV-234 ；所述增白剂为恶唑类增白剂。
更进一步的，本实施例中，上述润滑剂为科莱恩公司所产的蒙旦蜡 WE-40 ，上述增白剂为型号为 OB-1 的增白剂。
上述光扩散剂为实施例 1 所提供的光扩散剂。上述扩散剂、紫外线吸收剂均可采用市售产品实现。
使用 ASTM 国际标准对本实施例所得的光扩散聚碳酸酯材料进行测试，其结果如表 2 所示：
性质 方法 单位 数据
比重 ASTM D792 - 1.2
模收缩 ASTM D955 % 0.5-0.7
拉伸强度 ASTM D638 Mpa 55
弯曲强度 ASTM D790 Mpa 91
延伸率 ASTM D638 % 55
弯曲模数 ASTM D790 Mpa 2250
缺口冲击强度 (1/8') ASTM D256 J/M 730
热变形温度 ASTM D648 ℃ 131
耐燃性 UL94 (1/8') V2
外观 - - 淡白
抗 UV 强度 - 级 4
实施例 8
本实施例提供一种光扩散聚碳酸酯，其原料按重量份计包括以下组分
聚碳酸酯 97 份；
扩散剂 0.1 份；
润滑剂 0.3 份；
光扩散剂 0.2 份；
紫外线吸收剂 0.5 份；
增白剂 0.001 份。
本实施例中，所述扩散剂为 EBS 扩散剂；所述润滑剂为改性蜡润滑剂；所述紫外线吸收剂为紫外线吸收剂 UV-234 ；所述增白剂为恶唑类增白剂。
更进一步的，本实施例中，上述润滑剂为科莱恩公司所产的蒙旦蜡 WE-40 ，上述增白剂为型号为 OB-1 的增白剂。
上述光扩散剂为实施例 1 所提供的光扩散剂。上述扩散剂、紫外线吸收剂均可采用市售产品实现。
使用 ASTM 国际标准对本实施例所得的光扩散聚碳酸酯材料进行测试，其结果如表 3 所示：
性质 方法 单位 数据
比重 ASTM D792 - 1.2
模收缩 ASTM D955 % 0.5-0.7
拉伸强度 ASTM D638 Mpa 57
弯曲强度 ASTM D790 Mpa 93
延伸率 ASTM D638 % 57
弯曲模数 ASTM D790 Mpa 2350
缺口冲击强度 (1/8') ASTM D256 J/M 770
热变形温度 ASTM D648 ℃ 130
耐燃性 UL94 (1/8') V2
外观 - - 淡白
抗 UV 强度 - 级 4
对照例 1
本对照例提供一种光扩散聚碳酸酯，其光扩散剂为市售的有机硅光扩散剂，其余组分与实施例 6 一致。
使用 ASTM 国际标准对本对照例所得的光扩散聚碳酸酯材料进行测试，其结果如表 4 所示：
性质 方法 单位 数据
拉伸强度 ASTM D638 Mpa 20
弯曲强度 ASTM D790 Mpa 62
延伸率 ASTM D638 % 41
弯曲模数 ASTM D790 Mpa 1250
缺口冲击强度 (1/8') ASTM D256 J/M 460
热变形温度 ASTM D648 ℃ 110
对照例 2
本对照例提供一种光扩散聚碳酸酯，其光扩散剂为市售的有机硅类光扩散剂，其余组分与实施例 6 一致。
使用 ASTM 国际标准对本对照例所得的光扩散聚碳酸酯材料进行测试，其结果如表 5 所示：
性质 方法 单位 数据
拉伸强度 ASTM D638 Mpa 33
弯曲强度 ASTM D790 Mpa 71
延伸率 ASTM D638 % 33
弯曲模数 ASTM D790 Mpa 1360
缺口冲击强度 (1/8') ASTM D256 J/M 530
热变形温度 ASTM D648 ℃ 103
采用 GB/T 2410 - 2008 对实施例 6-8 、对照例 1-2 的雾度、透光率进行测试，其结果如表 6 所示。
编号 雾度 /% 透光率 /%
实施例 6 （厚度 1mm ） 91.9 89.3
实施例 6 （厚度 2mm ） 92.7 89.0
实施例 7 （厚度 1mm ） 92.1 88.7
实施例 7 （厚度 2mm ） 92.5 88.1
实施例 8 （厚度 1mm ） 91.8 88.5
实施例 8 （厚度 2mm ） 91.8 88.3
对照例 1 （厚度 1mm ） 83.7 75.6
对照例 1 （厚度 2mm ） 84.1 73.2
对照例 2 （厚度 1mm ） 85.4 72.9
对照例 2 （厚度 2mm ） 85.6 72.0
入射光线折射角度测试
取一半径 1cm 的 LED 光源，在其下方距离 2cm 处平行放置厚度均一的聚碳酸酯材料板，使 LED 光源的光线垂直照射在厚度为 h 的聚碳酸酯材料板上，测量聚碳酸酯材料板底部形成的光斑半径 r 。求得折射角： arctan[(r-1)/h], 。
对实施例 6-8 、对照例 1-2 的折射角进行测试，其结果如表 7 所示。
编号 折射角 /°
实施例 6 （厚度 1mm ） 58
实施例 6 （厚度 2mm ） 58
实施例 7 （厚度 1mm ） 51
实施例 7 （厚度 2mm ） 51
实施例 8 （厚度 1mm ） 49
实施例 8 （厚度 2mm ） 49
对照例 1 （厚度 1mm ） 30
对照例 1 （厚度 2mm ） 30
对照例 2 （厚度 1mm ） 18
对照例 2 （厚度 2mm ） 18
冷冻微粉碎聚硅氧烷颗粒缝隙容纳性测试。
将聚硅氧烷颗粒在 40 ℃下烘干 5 小时后，进行称重，获得其质量 M1, ；将聚硅氧烷颗粒浸泡于去离子水中 5 小时，沥干水分后进行称重，获得其质量 M2 ；求得其容纳系数 m= （ M2-M1 ） /M1 。
采用上述方法对实施例 1 ～ 3 的冷冻微粉碎聚硅氧烷颗粒以及市售的 2 μ m 聚硅烷颗粒进行测试，其结果如表 8 所示。
编号 容纳系数
实施例 1 0.8
实施例 2 1.0
实施例 3 0.9
市售的 2μm 聚硅烷颗粒 0.01
以上为本发明的其中具体实现方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些显而易见的替换形式均属于本发明的保护范围。

Claims (6)

  1. 一种聚碳酸酯用光扩散剂，其原料按重量份计包括以下组分：
    冷冻微粉碎聚硅氧烷颗粒 30 ～ 60 份；
    光散射剂 1 2 ～ 8 份；
    光散射剂 2 11 ～ 15 份；
    相容剂 5 ～ 10 份；
    其中，所述光散射剂 1 为具有如下通式的物质
    Figure YGHZ14017GMJ-appb-M000001
     ；
    所述光散射剂 2 为具有如下通式的物质
    Figure YGHZ14017GMJ-appb-M000002
     ；
    所述相容剂为按重量计 1 ～ 3 份十二烷基二甲基苄基氯化铵、 0.5 ～ 0.7 份乙酰乙酸乙酯的混合物；所述的 R1 为酰基，所述 R2 为含有 1 ～ 3 个碳原子的直链烷基；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2 μ m 的聚硅氧烷颗粒降温至 -10 ℃～ -20 ℃后，以 60KHz 的超声波粉碎获得的聚硅氧烷颗粒。
  2. 根据权利要求1所述的光扩散剂，其特征在于：所述R1为甲酰基、乙酰基或亚硫酰基中的一种。
  3. 一种制备权利要求1所述光扩散剂的方法，包括以下工序：
    将聚硅氧烷颗粒降温至-10℃～-20℃，保持2min～5min后，采用频率为60KHz的超声波将其粉碎15min～20min，制得所述冷冻微粉碎聚硅氧烷颗粒；
    将所述光散射剂1、光散射剂2以及相容剂混合均匀后，加入所述冷冻微粉碎聚硅氧烷颗粒，采用旋转式摇床以200～400转/min的转速震荡30～40min，制得所述光扩散剂。
  4. 一种光扩散聚碳酸酯材料，其特征在于：其原料包含有如权利要求1所述的光扩散剂。
  5. 根据权利要求4所述的光扩散聚碳酸酯材料，其特征在于：其原料按重量份计包括以下组分
    聚碳酸酯 92～97份；
    扩散剂 0.1～0.3份；
    润滑剂 0.1～0.3份；
    光扩散剂 0.2～1.1份；
    紫外线吸收剂 0.2～0.5份；
    增白剂 0.001～0.002份。
  6. 根据权利要求5所述的光扩散聚碳酸酯材料，其特征在于：所述扩散剂为EBS扩散剂；所述润滑剂为改性蜡润滑剂；所述紫外线吸收剂为紫外线吸收剂UV-234；所述增白剂为恶唑类增白剂 。
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