WO2015196532A1 - 一种高透光高雾度的pmma光扩散剂及一种光扩散pmma材料 - Google Patents

一种高透光高雾度的pmma光扩散剂及一种光扩散pmma材料 Download PDF

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WO2015196532A1
WO2015196532A1 PCT/CN2014/084049 CN2014084049W WO2015196532A1 WO 2015196532 A1 WO2015196532 A1 WO 2015196532A1 CN 2014084049 W CN2014084049 W CN 2014084049W WO 2015196532 A1 WO2015196532 A1 WO 2015196532A1
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light
agent
parts
pmma
diffusing
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PCT/CN2014/084049
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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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    • 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
    • C08K5/01—Hydrocarbons
    • 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 PMMA light diffusing agent with high light transmittance and high haze and a light diffusing PMMA 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.
  • a high-haze PMMA material (polymethyl methacrylate) has been used as a matrix, and a silicone-based light-scattering agent is prepared by blending into a light-transmitting material for LED lighting products.
  • the material has good performance in light transmittance and refractive index, but the materials such as anti-aging performance, impact strength and thermal processing stability are affected.
  • the light transmittance performance of the above PMMA material is not stable, especially in LED lighting products, which tends to age after working for a long time, high temperature and strong light, and finally leads to a decrease in light transmittance.
  • the present invention provides a light diffusing agent capable of providing a PMMA material with stable high light transmittance and high atomization.
  • a PMMA with high light transmittance and high haze A light diffusing agent whose raw materials include the following components in parts by weight:
  • Light scattering agent 1 1 ⁇ 2 parts
  • Light scattering agent 2 5 to 8 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 0.01 to 0.07 parts by weight of cetyltrimethylammonium bromide and 0.5 to 0.7 parts of ethyl acetoacetate; the curing agent is a mixture of persulfate and tetrahydrofuran;
  • the R 1 is an acyloxy group, and the R 2 is a linear alkyl group having 1 to 3 carbon atoms; and the freeze-milled polysiloxane particles refer to a polymerization having an average particle diameter of 2.5 ⁇ m After the silicone particles were cooled to -10 ° C to -20 ° C, the obtained silicone particles were ultrasonically pulverized at 60 to 100 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.
  • 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 1 and the light scattering agent 2 mixture can fill small cracks as a medium for conducting light, thereby greatly increasing the light transmittance of the above-mentioned frozen finely divided polysiloxane particles and reducing the light loss thereof.
  • the light diffusing agent of the present invention 1 , light diffusing agent 2 has a higher affinity for PMMA, that is, the use of both for PMMA The impact of its own impact strength, thermal processing stability and other properties is small.
  • the cetyltrimethylammonium bromide, ethyl acetate, and tetrahydrofuran are all commercially available products.
  • the curing agent functions to make the light scattering agent 1 and the light scattering agent 2
  • the resulting mixed system is capable of being present in the silicone particles for a long period of time.
  • the peroxide and the persulfate produced by the tetrahydrofuran after being exposed to light can cause the light scattering agent 1 and the light scattering agent 2 It is fixed to the silicone particles and is not easily degraded or escaped during processing.
  • the curing agent comprises 1 to 3 parts by weight of ammonium persulfate and 2 to 5 parts of tetrahydrofuran.
  • the curing agent comprises from 2 to 7 parts by weight of potassium persulfate and from 8 to 11 parts of tetrahydrofuran.
  • the light scattering agent 1 may be a substance having any of the following structural formulas:
  • the light scattering agent 1 may be a substance having the following structure:
  • the light scattering agent 2 may preferably be a substance having the following structure:
  • Diacetone acrylamide can be achieved using commercially available products.
  • the above two substances are used as the light scattering agent 1 and the light scattering agent 2 of the present invention.
  • the two have better compatibility and the system formed is more stable.
  • this hybrid system can withstand higher temperatures, stronger light without denaturation, and maintain PMMA.
  • the optical properties of the material have a promoting effect.
  • the invention also provides a preparation method of the above light diffusing agent, comprising the steps of: cooling the polysiloxane particles to -10 ° C to -20 ° C, maintaining After 2 min to 5 min, the ultrasonically pulverized polysiloxane particles are obtained by pulverizing the ultrasonic waves with a frequency of 60 to 100 kHz for 15 minutes to 20 minutes;
  • the freeze-milled polysiloxane particles are added, and the rotary shaker is used.
  • the speed of 200 ⁇ 400 rpm is oscillated for 30 ⁇ 40min; the curing agent is added, and under the shading condition, the rotary shaker is used at 5 ⁇ 8 °C for 150 ⁇ 300
  • the rotation speed of the /min is oscillated for 25 to 50 minutes; the light diffusing agent is obtained by air drying under the illumination of 1500 to 3000 lux.
  • Light scattering agent 1 light scattering agent 2 can be oscillated And the compatibilizing agent sufficiently penetrates into the gap of the frozen finely divided polysiloxane particles. At the same time, since tetrahydrofuran is sensitive to light, light may cause it to react in advance. Therefore, it needs to enter the system of polysiloxane particles under light-shielding and low-temperature conditions, and then initiate curing reaction by light to complete the light scattering agent. 1. Curing of light scattering agent 2.
  • the present invention also provides a light diffusing PMMA material comprising the above light diffusing agent.
  • the raw materials thereof include the following components in parts by weight:
  • UV absorber 0.2-0.5 parts
  • the diffusing agent is an EBS diffusing agent
  • the ultraviolet absorber is a UV absorber UV-531
  • the brightener is an oxazole whitening agent.
  • the PMMA material of the present invention can be prepared by any of the existing blending methods. All of the above components can be achieved using commercially available products.
  • 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 to ensure the performance of the prepared PMMA material. stable.
  • the EBS diffusing agent enables the light diffusing agent of the present invention to be uniformly distributed in the PMMA material and to reduce its polarity.
  • the whitening agent is an oxazole whitening agent, such as model OB-1 A brightener which effectively improves the appearance of the PMMA material produced and improves the whiteness of the PMMA material.
  • UV absorber UV-531 can be achieved with commercially available products to enhance the PMMA produced.
  • the anti-aging properties of the material make it less prone to yellowing and embrittlement.
  • the present invention has the following beneficial effects:
  • the present invention uses a method of low temperature freezing and ultrasonic pulverization to convert commercially available polysiloxane particles into low temperature micropulverized silicone particles, which are added to PMMA material can obtain excellent atomization effect in PMMA material; at the same time, the low temperature micro-crushed polysiloxane particles of the invention also overcome the existing silicone-based light diffusing agent to PMMA The effect of material properties enables the light-diffusing PMMA material produced by the present invention to maintain excellent impact resistance, processing thermal stability and the like.
  • the invention selects light scattering agent 1 and light scattering agent 2 Filled in the gap of the low-temperature finely pulverized silicone particles to solve the problem of large light loss of the low-temperature finely pulverized silicone particles, and the PMMA to which the light diffusing agent of the present invention is added
  • the material is able to maintain a high degree of light transmission.
  • the present invention is directed to a light scattering agent 1
  • the type of light scattering agent is limited to butyl acrylate and diacetone acrylamide.
  • the two can form a uniform and stable system under the action of the compatibilizer, so that the light passing through the mixture of the two can be repeatedly refracted in a random direction, thereby further improving.
  • the atomization effect of the light diffusing agent can make the above system stably exist in the light diffusing agent, and is not easy to be decomposed, oxidized or escaped during processing or long-term use.
  • Light diffusion PMMA provided by the present invention
  • the material, 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 PMMA material, and is the finally produced light diffusing PMMA.
  • the material has good impact resistance, high thermal stability, excellent processing performance and anti-aging properties.
  • a high light transmittance and high haze PMMA light diffusing agent the raw materials of which include the following components by weight:
  • Light scattering agent 1 1.3 parts;
  • the light scattering agent 1 is a substance having the following structure
  • the light scattering agent 2 is a substance having the following structure
  • the compatibilizer is 0.04 parts by weight of cetyltrimethylammonium bromide and 0.3 A portion of ethyl acetoacetate; the curing agent is a mixture of persulfate and tetrahydrofuran; and the freeze-milled polysiloxane particles mean that the silicone particles having an average particle diameter of 2.5 ⁇ m are cooled to -17 After °C, to Polysiloxane particles obtained by ultrasonic pulverization at 80 kHz.
  • the curing agent included 2.8 parts by weight of ammonium persulfate and 4.1 parts of tetrahydrofuran.
  • This embodiment also provides a method of the above light diffusing agent, comprising the steps of: cooling the silicone particles to -17 ° C for 3 min. After that, it is pulverized by ultrasonic waves having a frequency of 70 kHz for 18 minutes to obtain the frozen finely pulverized silicone particles;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer is uniformly mixed, the frozen micro-pulverized polysiloxane particles are added and shaken at a speed of 330 rpm for 35 minutes using a rotary shaker; and the curing agent is added under shading conditions at 6
  • the light diffusing agent was prepared by shaking with a rotary shaker at 200 rpm for 45 min in °C and air drying under 2000 lux of light.
  • a high light transmittance and high haze PMMA light diffusing agent the raw materials of which include the following components by weight:
  • Light scattering agent 1 1 part
  • the light scattering agent 1 is a substance having the following structure
  • the light scattering agent 2 is a substance having the following structure
  • the compatibilizer is 0.01 parts by weight of cetyltrimethylammonium bromide and 0.5 to 0.7 A portion of ethyl acetoacetate; the curing agent is a mixture of persulfate and tetrahydrofuran; and the freeze-milled polysiloxane particles mean that the silicone particles having an average particle diameter of 2.5 ⁇ m are cooled to -20 After °C, to Polysiloxane particles obtained by ultrasonic pulverization at 60 kHz.
  • the curing agent comprises 3 parts by weight of ammonium persulfate and 2 parts of tetrahydrofuran.
  • the embodiment further provides a method for the above light diffusing agent, comprising the steps of: cooling the silicone particles to -20 ° C for 2 min. Thereafter, it is pulverized by ultrasonic waves having a frequency of 100 kHz for 15 minutes to prepare the frozen finely pulverized silicone particles;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer is uniformly mixed, the frozen micro-pulverized polysiloxane particles are added, and the rotating shaker is used to oscillate at a speed of 400 rpm; and the curing agent is added under a light-shielding condition at 8
  • the light diffusing agent was prepared by shaking with a rotary shaker at 150 rpm for 50 min in °C and air drying under 1500 lux of light.
  • a high light transmittance and high haze PMMA light diffusing agent the raw materials of which include the following components by weight:
  • the light scattering agent 1 is a substance having the following structure
  • the light scattering agent 2 is a substance having the following structure
  • the compatibilizer is 0.07 parts by weight of cetyltrimethylammonium bromide and 0.5 A portion of ethyl acetoacetate; the curing agent is a mixture of persulfate and tetrahydrofuran; and the freeze-milled polysiloxane particles mean that the silicone particles having an average particle diameter of 2.5 ⁇ m are cooled to -20 After °C, to Polysiloxane particles obtained by ultrasonic pulverization at 60 kHz.
  • the curing agent comprises 3 parts by weight of ammonium persulfate and 2 parts of tetrahydrofuran.
  • the embodiment further provides a method for the above light diffusing agent, comprising the steps of: cooling the silicone particles to -20 ° C for 2 min. Thereafter, it is pulverized by ultrasonic waves having a frequency of 100 kHz for 15 minutes to prepare the frozen finely pulverized silicone particles;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer is uniformly mixed, the freeze-milled polysiloxane particles are added, and the mixture is shaken at a speed of 400 rpm for 30 minutes using a rotary shaker; and the curing agent is added under shading conditions at 8
  • the light diffusing agent was prepared by shaking with a rotary shaker at 150 rpm for 50 min in °C and air drying under 3000 lux of light.
  • a high light transmittance and high haze PMMA light diffusing agent the raw materials of which include the following components by weight:
  • Light scattering agent 1 1.3 parts;
  • the light scattering agent 1 is a substance having the following structure
  • the light scattering agent 2 is a substance having the following structure
  • the compatibilizer is 0.07 parts by weight of cetyltrimethylammonium bromide and 0.55 A portion of ethyl acetoacetate; the curing agent is a mixture of persulfate and tetrahydrofuran; and the freeze-milled polysiloxane particles mean that the silicone particles having an average particle diameter of 2.5 ⁇ m are cooled to -11 After °C, to Polysiloxane particles obtained by ultrasonic pulverization at 90 kHz.
  • the curing agent comprises 2 parts by weight of ammonium persulfate and 5 parts of tetrahydrofuran.
  • This embodiment also provides a method of the above light diffusing agent, comprising the steps of: cooling the silicone particles to -15 ° C for 45 minutes. Thereafter, it is pulverized by ultrasonic waves having a frequency of 100 kHz for 20 minutes to prepare the frozen finely pulverized silicone particles;
  • the light scattering agent 1 and the light scattering agent 2 After the compatibilizer is uniformly mixed, the frozen micro-pulverized polysiloxane particles are added and shaken at a speed of 35 rpm for 35 minutes using a rotary shaker; and the curing agent is added under shading conditions at 7
  • the light diffusing agent was prepared by shaking with a rotary shaker at 200 rpm for 40 min in °C and air drying under 3000 lux of light.
  • a high light transmittance and high haze PMMA light diffusing agent the raw materials of which include the following components by weight:
  • the light scattering agent 1 is a substance having the following structure
  • the light scattering agent 2 is a substance having the following structure
  • the compatibilizer is 0.03 parts by weight of cetyltrimethylammonium bromide and 0.6 A portion of ethyl acetoacetate; the curing agent is a mixture of persulfate and tetrahydrofuran; and the freeze-milled polysiloxane particles mean that the silicone particles having an average particle diameter of 2.5 ⁇ m are cooled to -15 After °C, to Polysiloxane particles obtained by ultrasonic pulverization at 100 kHz.
  • the curing agent comprises 2 parts by weight of ammonium persulfate and 4 parts of tetrahydrofuran.
  • a high light transmittance and high haze PMMA light diffusing agent the raw materials of which include the following components by weight:
  • the light scattering agent 1 is a substance having the following structure
  • the light scattering agent 2 is a substance having the following structure
  • the compatibilizer is 0.05 parts by weight of cetyltrimethylammonium bromide and 0.6 A portion of ethyl acetoacetate; the curing agent is a mixture of persulfate and tetrahydrofuran; and the freeze-milled polysiloxane particles mean that the silicone particles having an average particle diameter of 2.5 ⁇ m are cooled to -13 After °C, to Polysiloxane particles obtained by ultrasonic pulverization at 70 kHz.
  • the curing agent comprises 2 parts by weight of ammonium persulfate and 4 parts of tetrahydrofuran.
  • the present embodiment provides a light-diffusing PMMA material, characterized in that the raw material comprises the following components in parts by weight:
  • the light diffusing agent is the light diffusing agent provided in Example 1.
  • the light-diffusing PMMA material obtained in this example was tested using ASTM International Standard. The results are shown in Table 1:
  • the present embodiment provides a light-diffusing PMMA material, characterized in that the raw material comprises the following components in parts by weight:
  • UV absorber UV-531 0.5 parts
  • the light diffusing agent is the light diffusing agent provided in Example 2.
  • the light-diffusing PMMA material obtained in this example was tested using ASTM International Standard. The results are shown in Table 2:
  • the present embodiment provides a light-diffusing PMMA material, characterized in that the raw material comprises the following components in parts by weight:
  • the light diffusing agent is the light diffusing agent provided in Example 1.
  • the light-diffusing PMMA material obtained in this example was tested using ASTM International Standard. The results are shown in Table 3:
  • the present embodiment provides a light-diffusing PMMA material, characterized in that the raw material comprises the following components in parts by weight:
  • the light diffusing agent is the light diffusing agent provided in Example 1.
  • the light-diffusing PMMA material obtained in this example was tested using ASTM International Standard, and the results are shown in Table 4:
  • This comparative example provides a light diffusing PMMA material whose light diffusing agent is a commercially available silicone light diffusing agent, and the remaining components are the same as in Example 7 Consistent.
  • the light-diffusing PMMA material obtained in this comparative example was tested using ASTM International Standard. The results are shown in Table 5:
  • the present comparative example provides a light-diffusing PMMA material, the commercially available polysiloxane is used as the light diffusing agent, and the remaining components and the embodiment 8 Consistent.
  • This comparative example provides a light-diffusing PMMA material having the same composition as in Example 7, but the light diffusing agent does not contain a curing agent.

Abstract

PMMA光扩散剂，包含冷冻微粉碎聚硅氧烷颗粒、光散射剂1和2、固化剂和相容剂，其中相容剂为十六烷基三甲基溴化铵和乙酰乙酸乙酯的混合物，固化剂为过硫酸盐与四氢呋喃的混合物。

Description

一种高透光高雾度的PMMA光扩散剂及一种光扩散PMMA材料 技术领域
本发明涉及高分子材料技术领域，具体涉及一种高透光高雾度的PMMA光扩散剂及一种光扩散PMMA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。现有采用具有高雾度的PMMA材料（聚甲基丙烯酸甲酯）作为基体，以共混法将有机硅类光散射剂与之制备成用于LED照明产品的透光材料。该材料在透光率及折射率方面均有较好的表现，但材料的抗老化性能、抗冲击强度、热加工稳定性等指标均受到一定的影响。同时上述PMMA材料的透光率性能并不稳定，特别是应用于LED照明产品中，经长时间、高温、强光照工作后容易老化，最终导致透光率的下降。
发明内容
有鉴于此，本发明提供一种能够使 PMMA 材料具备稳定的高透光率及高雾化程度的光扩散剂。
本实用新型的目的通过以下技术方案实现，一种高透光高雾度的 PMMA 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 50 ～ 80 份；
光散射剂 1 1 ～ 2 份；
光散射剂 2 5 ～ 8 份；
固化剂 0.5-2.5 份；
相容剂 0.1-0.3 份；
所述光散射剂 1 为具有如下通式的物质
Figure YGHZ14016GMJ-appb-M000001
 ;
所述光散射剂 2 为具有如下通式的物质
Figure YGHZ14016GMJ-appb-M000002
 ；
所述相容剂为按重量计 0.01 ～ 0.07 份的十六烷基三甲基溴化铵以及 0.5 ～ 0.7 份的乙酰乙酸乙酯的混合物；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述的 R1 为酰氧基，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 2.5 μ m 的聚硅氧烷颗粒降温至 -10 ℃～ -20 ℃后，以 60 ～ 100KHz 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。上述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，可填补细小裂缝作为传导光线的介质，从而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。同时，本发明的光扩散剂 1 、光扩散剂 2 对 PMMA 有较高的亲和度，即二者的使用对 PMMA 本身的抗冲击强度、热加工稳定性等性质的影响较小。所述十六烷基三甲基溴化铵、乙酸乙酯、四氢呋喃均为市售产品。所述固化剂的作用是使上述光散射剂 1 、光散射剂 2 形成的混合体系能够长期、稳定地存在于聚硅氧烷颗粒中。具体而言，四氢呋喃在受到光照后产生的过氧化物与过硫酸盐可使所述光散射剂 1 、光散射剂 2 固着于聚硅氧烷颗粒，在加工过程中不易被降解或逃逸。
进一步的，所述固化剂包括按重量计 1 ～ 3 份的过硫酸铵及 2 ～ 5 份四氢呋喃。
可变化的，所述固化剂包括按重量计 2 ～ 7 份的过硫酸钾及 8 ～ 11 份四氢呋喃。
经发明人测试，选用其他过硫酸盐，均会在一定程度上损伤光扩散剂的透光率。而过硫酸铵及过硫酸钾的这种影响作用最小。
特别的，光散射剂 1 可以为具有如下任一种结构式的物质
Figure YGHZ14016GMJ-appb-M000003
 ；
Figure YGHZ14016GMJ-appb-M000004
 ；
Figure YGHZ14016GMJ-appb-M000005
 。
特别优选的，光散射剂 1 可以是如下结构的物质：
Figure YGHZ14016GMJ-appb-M000006
。其为丙烯酸丁酯，可选用市售产品实现。
与之配合的，光散射剂 2 可优选为具有如下结构的物质：
Figure YGHZ14016GMJ-appb-M000007
。双丙酮丙烯酰胺，可采用市售产品实现。
经设计人测试，以上两种物质作为本发明的光散射剂 1 、光散射剂 2 ，二者具有较好的相容性，所形成的的体系更加稳定。特别是这一混合体系能够耐受较高的温度、较强的光照而不发生变性，对于维持 PMMA 材料的光学性质有促进作用。
本发明同时还提供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 ℃～ -20 ℃，保持 2min ～ 5min 后，采用频率为 60 ～ 100KHz 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 ；加入所述固化剂，在遮光条件下，于 5 ～ 8 ℃中采用旋转式摇床以 150 ～ 300 转 /min 的转速震荡 25 ～ 50min ；在 1500 ～ 3000lux 的光照条件下风干，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。同时，由于四氢呋喃对光敏感，光照有可能导致其提前发生反应，因此需在遮光、低温的条件下使其进入聚硅氧烷颗粒的体系中，再通过光照引发固化反应，完成对光散射剂 1 、光散射剂 2 的固化。
本发明还提供一种光扩散 PMMA 材料，其包含有上述的光扩散剂。
具体而言，其原料按重量份计包括以下组分：
PMMA 89-95 份；
扩散剂 0.1-0.6 份；
光扩散剂 0.9-1.5 份；
紫外线吸收剂 0.2-0.5 份；
增白剂 0.001 ～ 0.002 份。
特别的，所述扩散剂为 EBS 扩散剂；所述紫外线吸收剂为紫外线吸收剂 UV-531 ；所述增白剂为恶唑类增白剂。
本发明的 PMMA 材料可选用现有的任一种共混法制备。以上各组分均可采用市售产品实现。 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 PMMA 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 PMMA 材料中，并降低其极性的作用。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 PMMA 材料的外观，提高 PMMA 材料的白度。与光扩散剂协效，使 PMMA 材料能够进一步缓和 LED 发出的光线，使之更加柔和。
紫外线吸收剂 UV-531 可采用市售产品实现，其作用是增强所制得的 PMMA 材料的抗老化性能，使之不易发黄、脆化。
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 PMMA 材料中，可使 PMMA 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类光扩散剂对 PMMA 材料性能的影响，使本发明所制得的光扩散 PMMA 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 PMMA 材料能够保持较高的透光度。同时本发明对光散射剂 1 、光散射剂的种类限定为丙烯酸丁酯及双丙酮丙烯酰胺，二者在相容剂的作用下可形成均匀稳定的体系，使通过二者混合物的光线发生随机方向的多次折射，进一步提高了光扩散剂的雾化效果。而本发明设计的固化剂又可使上述体系稳定存在于光扩散剂中，不易于在加工或长期使用的过程中本分解、氧化或逃逸。
3. 本发明提供的光扩散 PMMA 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 PMMA 材料中，并是最终制得的光扩散 PMMA 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、抗老化性能等。
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
一种高透光高雾度的 PMMA 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 75 份；
光散射剂 1 1.3 份；
光散射剂 2 6.5 份；
固化剂 2 份；
相容剂 0.2 份；
所述光散射剂 1 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000008
；
所述光散射剂 2 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000009
 ；
所述相容剂为按重量计 0.04 份的十六烷基三甲基溴化铵以及 0.3 份的乙酰乙酸乙酯；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2.5 μ m 的聚硅氧烷颗粒降温至 -17 ℃后，以 80KHz 的超声波粉碎获得的聚硅氧烷颗粒。
所述固化剂包括按重量计 2.8 份的过硫酸铵及 4.1 份四氢呋喃。
本实施例还提供一种上述光扩散剂的方法，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 70KHz 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 35min ；加入所述固化剂在遮光条件下，于 6 ℃中采用旋转式摇床以 200 转 /min 的转速震荡 45min ；在 2000lux 的光照条件下风干，制得所述光扩散剂。
实施例 2
一种高透光高雾度的 PMMA 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 80 份；
光散射剂 1 1 份；
光散射剂 2 8 份；
固化剂 0.5 份；
相容剂 0.3 份；
所述光散射剂 1 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000010
 ；
所述光散射剂 2 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000011
；
所述相容剂为按重量计 0.01 份的十六烷基三甲基溴化铵以及 0.5 ～ 0.7 份的乙酰乙酸乙酯；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2.5 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。
所述固化剂包括按重量计 3 份的过硫酸铵及 2 份四氢呋喃。
本实施例还提供一种上述光扩散剂的方法，包括以下工序：将聚硅氧烷颗粒降温至 -20 ℃，保持 2min 后，采用频率为 100KHz 的超声波将其粉碎 15min ，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 30 ；加入所述固化剂在遮光条件下，于 8 ℃中采用旋转式摇床以 150 转 /min 的转速震荡 50min ；在 1500lux 的光照条件下风干，制得所述光扩散剂。
实施例 3
一种高透光高雾度的 PMMA 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 50 份；
光散射剂 1 2 份；
光散射剂 2 5 份；
固化剂 2.5 份；
相容剂 0.1 份；
所述光散射剂 1 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000012
 ；
所述光散射剂 2 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000013
；
所述相容剂为按重量计 0.07 份的十六烷基三甲基溴化铵以及 0.5 份的乙酰乙酸乙酯；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2.5 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。
所述固化剂包括按重量计 3 份的过硫酸铵及 2 份四氢呋喃。
本实施例还提供一种上述光扩散剂的方法，包括以下工序：将聚硅氧烷颗粒降温至 -20 ℃，保持 2min 后，采用频率为 100KHz 的超声波将其粉碎 15min ，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 ；加入所述固化剂在遮光条件下，于 8 ℃中采用旋转式摇床以 150 转 /min 的转速震荡 50min ；在 3000lux 的光照条件下风干，制得所述光扩散剂。
实施例 4
一种高透光高雾度的 PMMA 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 80 份；
光散射剂 1 1.3 份；
光散射剂 2 5.5 份；
固化剂 0.7 份；
相容剂 2.5 份；
所述光散射剂 1 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000014
 ；
所述光散射剂 2 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000015
 ；
所述相容剂为按重量计 0.07 份的十六烷基三甲基溴化铵以及 0.55 份的乙酰乙酸乙酯；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2.5 μ m 的聚硅氧烷颗粒降温至 -11 ℃后，以 90KHz 的超声波粉碎获得的聚硅氧烷颗粒。
所述固化剂包括按重量计 2 份的过硫酸铵及 5 份四氢呋喃。
本实施例还提供一种上述光扩散剂的方法，包括以下工序：将聚硅氧烷颗粒降温至 -15 ℃，保持 45min 后，采用频率为 100KHz 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 35 转 /min 的转速震荡 35min ；加入所述固化剂在遮光条件下，于 7 ℃中采用旋转式摇床以 200 转 /min 的转速震荡 40min ；在 3000lux 的光照条件下风干，制得所述光扩散剂。
实施例 5
一种高透光高雾度的 PMMA 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 1.5 份；
光散射剂 2 7 份；
固化剂 2.5 份；
相容剂 0.1 份；
所述光散射剂 1 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000016
；
所述光散射剂 2 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000017
；
所述相容剂为按重量计 0.03 份的十六烷基三甲基溴化铵以及 0.6 份的乙酰乙酸乙酯；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2.5 μ m 的聚硅氧烷颗粒降温至 -15 ℃后，以 100KHz 的超声波粉碎获得的聚硅氧烷颗粒。
所述固化剂包括按重量计 2 份的过硫酸铵及 4 份四氢呋喃。
实施例 6
一种高透光高雾度的 PMMA 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 2.5 份；
光散射剂 2 7 份；
固化剂 0.9 份；
相容剂 0.2 份；
所述光散射剂 1 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000018
 ；
所述光散射剂 2 为具有如下结构的物质
Figure YGHZ14016GMJ-appb-M000019
；
所述相容剂为按重量计 0.05 份的十六烷基三甲基溴化铵以及 0.6 份的乙酰乙酸乙酯；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述冷冻微粉碎聚硅氧烷颗粒是指将平均粒径为 2.5 μ m 的聚硅氧烷颗粒降温至 -13 ℃后，以 70KHz 的超声波粉碎获得的聚硅氧烷颗粒。
所述固化剂包括按重量计 2 份的过硫酸铵及 4 份四氢呋喃。
实施例 7
本实施例提供一种光扩散 PMMA 材料，其特征在于：其原料按重量份计包括以下组分：
PMMA 90 份；
EBS 扩散剂 0.4 份；
光扩散剂 1 份；
紫外线吸收剂 UV-531 0.4 份；
增白剂 OB-1 0.0015 份。
本实施例中，上述光扩散剂为实施例 1 所提供的光扩散剂。
使用 ASTM 国际标准对本实施例所得的光扩散 PMMA 材料进行测试，其结果如表 1 所示：
Figure YGHZ14016GMJ-appb-M000020
实施例 9
本实施例提供一种光扩散 PMMA 材料，其特征在于：其原料按重量份计包括以下组分：
PMMA 89 份；
EBS 扩散剂 0.6 份；
光扩散剂 0.9 份；
紫外线吸收剂 UV-531 0.5 份；
增白剂 OB-1 0.001 份。
本实施例中，上述光扩散剂为实施例 2 所提供的光扩散剂。
使用 ASTM 国际标准对本实施例所得的光扩散 PMMA 材料进行测试，其结果如表 2 所示：
Figure YGHZ14016GMJ-appb-M000021
实施例 10
本实施例提供一种光扩散 PMMA 材料，其特征在于：其原料按重量份计包括以下组分：
PMMA 95 份；
EBS 扩散剂 0.1 份；
光扩散剂 1.5 份；
紫外线吸收剂 UV-531 0.2 份；
增白剂 OB-1 0.002 份。
本实施例中，上述光扩散剂为实施例 1 所提供的光扩散剂。
使用 ASTM 国际标准对本实施例所得的光扩散 PMMA 材料进行测试，其结果如表 3 所示：
Figure YGHZ14016GMJ-appb-M000022
实施例 11
本实施例提供一种光扩散 PMMA 材料，其特征在于：其原料按重量份计包括以下组分：
PMMA 93 份；
EBS 扩散剂 0.2 份；
光扩散剂 1 份；
紫外线吸收剂 UV-531 0.4 份；
增白剂 OB-1 0.002 份。
本实施例中，上述光扩散剂为实施例 1 所提供的光扩散剂。
使用 ASTM 国际标准对本实施例所得的光扩散 PMMA 材料进行测试，其结果如表 4 所示：
Figure YGHZ14016GMJ-appb-M000023
对比例 1
本对比例提供一种光扩散 PMMA 材料，其光扩散剂为市售的有机硅光扩散剂，其余组分与实施例 7 一致。
使用 ASTM 国际标准对本对照例所得的光扩散 PMMA 材料进行测试，其结果如表 5 所示：
Figure YGHZ14016GMJ-appb-M000024
对比例 2
本对比例提供一种光扩散 PMMA 材料，其光扩散剂选用市售的聚硅氧烷，其余组分与实施例 8 一致。
使用 ASTM 国际标准对本对照例所得的光扩散 PMMA 材料进行测试，其结果如表 7 所示：
Figure YGHZ14016GMJ-appb-M000024
对比例 3
本对比例提供一种光扩散 PMMA 材料，其组分与实施例 7 一致，但其光扩散剂不含固化剂。
采用 GB/T 2410 - 2008 对实施例 7-11 、对比例 1-3 的雾度、透光率进行测试，其结果如表 6 所示。
Figure YGHZ14016GMJ-appb-M000025
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 PMMA 材料板，使 LED 光源的光线垂直照射在厚度为 h 的 PMMA 材料板上，测量 PMMA 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 7-11 、对比例 1-3 的雾度的折射角进行测试，其结果如表 7 所示。
Figure YGHZ14016GMJ-appb-M000026
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 2.5 μ m 聚硅烷颗粒进行测试，其结果如表 8 所示。
Figure YGHZ14016GMJ-appb-M000027
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 (8)

  1. 一种高透光高雾度的 PMMA 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 50 ～ 80 份；
    光散射剂 1 1 ～ 2 份；
    光散射剂 2 5 ～ 8 份；
    固化剂 0.5-2.5 份；
    相容剂 0.1-0.3 份；
    其中，所述光散射剂 1 为具有如下通式的物质
    Figure YGHZ14016GMJ-appb-M000028
    ；
    所述光散射剂 2 为具有如下通式的物质
    Figure YGHZ14016GMJ-appb-M000029
    ；
    所述相容剂为按重量计 0.01 ～ 0.07 份的十六烷基三甲基溴化铵以及 0.5 ～ 0.7 份的乙酰乙酸乙酯的混合物；所述固化剂为过硫酸盐与四氢呋喃的混合物；所述的 R1 为酰氧基，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 2.5 μ m 的聚硅氧烷颗粒降温至 -10 ℃～ -20 ℃后，以 60 ～ 100KHz 的超声波粉碎获得的聚硅氧烷颗粒。
  2. 根据权利要求1所述的高透光高雾度的PMMA光扩散剂，其特征在于：所述固化剂包括按重量计1～3份的过硫酸铵及2～5份四氢呋喃。
  3. 根据权利要求1所述的高透光高雾度的PMMA光扩散剂，其特征在于：所述固化剂包括按重量计2～7份的过硫酸钾及8～11份四氢呋喃。
  4. 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60～100KHz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；加入所述固化剂在遮光条件下，于5～8℃中采用旋转式摇床以150～300转/min的转速震荡25～50min；在1500～3000lux的光照条件下风干，制得所述光扩散剂。
  5. 一种光扩散PMMA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。
  6. 根据权利要求5所述的光扩散PMMA材料，其特征在于：其原料按重量份计包括以下组分：
    PMMA 89-95份；
    扩散剂 0.1-0.6份；
    光扩散剂 0.9-1.5份；
    紫外线吸收剂 0.2-0.5份；
    增白剂 0.001～0.002份。
  7. 根据权利要求6所述的光扩散PMMA材料，其特征在于：所述扩散剂为EBS扩散剂；所述紫外线吸收剂为紫外线吸收剂UV-531；所述增白剂为恶唑类增白剂。
  8. 根据权利要求 1 所述的高透光高雾度的 PMMA 光扩散剂，其特征在于：光散射剂 1 为具有如下结构式的物质
    Figure YGHZ14016GMJ-appb-M000030
    ；
    所述光散射剂 2 为具有如下结构式的物质
    Figure YGHZ14016GMJ-appb-M000031
    。
PCT/CN2014/084049 2014-06-27 2014-08-10 一种高透光高雾度的pmma光扩散剂及一种光扩散pmma材料 WO2015196532A1 (zh)

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