CN105754039B - A kind of poly(4-methyl-1-pentene) light diffusing agent and preparation method thereof - Google Patents
A kind of poly(4-methyl-1-pentene) light diffusing agent and preparation method thereof Download PDFInfo
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Abstract
本发明提供了一种聚4‑甲基‑1‑戊烯光扩散剂及其制备方法。在聚4‑甲基‑1‑戊烯颗粒表面,引入1,2‑环氧基‑5‑己烯,3,4‑环氧‑1‑丁烯,烯丙基缩水甘油醚参与聚合,升温至反应温度,待反应结束,离心,干燥。即得到光扩散剂产品。The invention provides a poly 4-methyl-1-pentene light diffusing agent and a preparation method thereof. On the surface of poly 4-methyl-1-pentene particles, introduce 1,2-epoxy-5-hexene, 3,4-epoxy-1-butene, allyl glycidyl ether to participate in polymerization, and heat up To the reaction temperature, after the reaction is completed, centrifuge and dry. That is, the light diffusing agent product is obtained.
Description
技术领域technical field
本发明涉及一种光扩散剂的制备方法,特别是一种聚4-甲基-1-戊烯光扩散剂及其制备方法。The invention relates to a preparation method of a light diffusing agent, in particular to a poly 4-methyl-1-pentene light diffusing agent and a preparation method thereof.
背景技术Background technique
光扩散广泛应用于照明、显示、投影成像、激光等领域,主要有无机型光扩散剂和有机型光扩散:无机光扩散剂主要有:纳米硫酸钡,碳酸钙,二氧化硅等,这些无机型光扩散剂,无机型光扩散剂从微观角度上讲是个实心微珠球,光线无法透过这个实心球体,会影响很多光线的透过,只有部分光线透过折射通过,因此影响亮度或透光。做灯管灯罩要求透光率50%之上的都不能选择无机光扩散剂;有机光扩散剂主要有压克力型,苯乙烯型,丙烯酸树脂型的等,这些树脂本身是透明或半透明,光线大部分可以通过,利用这些光扩散剂本身材质的折射率与基材的折射率的差异,光线多次折射后,通过基材的光线变得光亮柔和,且对材质的透光率影响较小,是做灯管灯罩等光学材料很好的选择。Light diffusion is widely used in lighting, display, projection imaging, laser and other fields. There are mainly inorganic light diffusing agents and organic light diffusing agents: inorganic light diffusing agents mainly include: nano barium sulfate, calcium carbonate, silicon dioxide, etc. These inorganic-type light diffusing agents, inorganic-type light diffusing agents are solid microspheres from a microscopic point of view, and light cannot pass through this solid sphere, which will affect the transmission of many light rays. Affects brightness or light transmission. Inorganic light diffusing agents cannot be selected for lampshades that require light transmittance above 50%; organic light diffusing agents mainly include acrylic type, styrene type, acrylic resin type, etc. These resins themselves are transparent or translucent , most of the light can pass through, using the difference between the refractive index of the material of these light diffusing agents and the refractive index of the substrate, after the light is refracted many times, the light passing through the substrate becomes bright and soft, and has an impact on the light transmittance of the material Smaller, it is a good choice for optical materials such as lampshades.
CN104059246公开了一种透光无机光扩散剂,其特征是:组成的各组分重量百分比为:冰晶石85-94%,叶腊石3-8%,高岭土2-5%,钾长石0.5-1%,水镁石0.2-1%,利用流化床包覆冰晶石,通过在旋流动态煅烧炉将粉状物料与加热的热空气混合,比表面达到瞬间煅烧熔融,球形化,在冰晶石表面包覆一层反光层,从而使冰晶石具备良好的透光性和反光性。CN104059246 discloses a light-transmitting inorganic light diffusing agent, which is characterized in that: the weight percentage of each component is: cryolite 85-94%, pyrophyllite 3-8%, kaolin 2-5%, potassium feldspar 0.5-1 %, brucite 0.2-1%, use the fluidized bed to coat the cryolite, and mix the powdery material with the heated hot air in the swirling flow dynamic calciner, and the specific surface can be instantly calcined, melted, and spheroidized. The surface is covered with a reflective layer, so that the cryolite has good light transmission and light reflection.
CN102101971公开了一种光扩散剂,该光扩散剂含有聚氨酯丙烯酸酯、可聚合单体和有机粒子,所述聚氨酯丙烯酸酯的数均分子量为1000-10000,所述可聚合单体为至少两种多官能基的丙烯酸酯系单体,所述有机粒子的平均颗粒直径为1.8-30微米。CN102101971 discloses a light diffusing agent, which contains polyurethane acrylate, polymerizable monomers and organic particles, the number average molecular weight of the polyurethane acrylate is 1000-10000, and the polymerizable monomer is at least two The multifunctional acrylate monomer, the average particle diameter of the organic particles is 1.8-30 microns.
现有公知技术的光扩散剂在长时间光照下易老化,分解。需要进行表面处理以保证抗氧化性,以提高光分散性。The light diffusing agent in the prior art is easy to age and decompose under long-time light. Surface treatment is required to ensure oxidation resistance to improve light dispersion.
发明内容Contents of the invention
针对现有技术的不足,本发明提供了一种聚4-甲基-1-戊烯光扩散剂及其制备方法。Aiming at the deficiencies of the prior art, the invention provides a poly-4-methyl-1-pentene light diffusing agent and a preparation method thereof.
在聚4-甲基-1-戊烯颗粒表面,引入1,2-环氧基-5-己烯,3,4-环氧-1-丁烯,烯丙基缩水甘油醚参与聚合,升温至反应温度,待反应结束,离心,干燥。即得到光扩散剂产品。On the surface of poly-4-methyl-1-pentene particles, introduce 1,2-epoxy-5-hexene, 3,4-epoxy-1-butene, allyl glycidyl ether to participate in polymerization, and heat up To the reaction temperature, after the reaction is completed, centrifuge and dry. That is, the light diffusing agent product is obtained.
本发明提供一种4-甲基-1-戊烯光扩散剂及其制备方法,通过以下步骤实现:The invention provides a 4-methyl-1-pentene light diffusing agent and a preparation method thereof, which are realized through the following steps:
步骤1 水相的配制:Step 1 Preparation of aqueous phase:
按重量份计,在反应釜中内加入1000份水,0.5-2份十二烷基苯磺酸钠,搅拌均匀。In parts by weight, add 1000 parts of water and 0.5-2 parts of sodium dodecylbenzenesulfonate into the reactor, and stir evenly.
步骤2 油相的配制:Step 2 Preparation of oil phase:
按重量份计,在100份聚4-甲基-1-戊烯,占单体总量百分比含量0.05~0.5的1,2-环氧基-5-己烯,占单体总量百分比含量0.05~0.5的3,4-环氧-1-丁烯,参与聚合,再加入加入0.2-0.6份过氧化氢异丙苯、0.05-0.2份硫酸氢钠,搅拌均匀;In parts by weight, in 100 parts of poly-4-methyl-1-pentene, 1,2-epoxy-5-hexene, which accounts for 0.05 to 0.5 percent of the total amount of monomers, accounts for 0.5 percent of the total amount of monomers 0.05-0.5 of 3,4-epoxy-1-butene, participate in the polymerization, then add 0.2-0.6 parts of cumene hydroperoxide and 0.05-0.2 parts of sodium bisulfate, and stir evenly;
步骤3 聚合反应:Step 3 Polymerization:
将油相溶液加到步骤1中装有已配制水相的反应釜中,加入占单体总量百分比含量0.1~0.5的烯丙基缩水甘油醚,然后在50-80℃,反应1-4h,反应结束后过滤,烘干得到产品。Add the oil phase solution to the reaction kettle equipped with the prepared water phase in step 1, add allyl glycidyl ether with a percentage of 0.1 to 0.5 of the total amount of monomers, and then react at 50-80°C for 1-4h , filtered after the reaction, and dried to obtain the product.
所述聚4-甲基-1-戊烯为市售产品,如日本三井化学有限公司生产的产品。所述3,4-环氧-1-丁烯为市售产品,如上海沪震实业有限公司生产的产品。所述1,2-环氧基-5-己烯为市售产品。如上海至鑫化工有限公司生产的产品。所述烯丙基缩水甘油醚为市售产品。如济南中维化工有限公司生产的产品。The poly-4-methyl-1-pentene is a commercially available product, such as a product produced by Mitsui Chemicals Co., Ltd., Japan. The 3,4-epoxy-1-butene is a commercially available product, such as a product produced by Shanghai Huzhen Industrial Co., Ltd. The 1,2-epoxy-5-hexene is a commercially available product. Such as the products produced by Shanghai Zhixin Chemical Co., Ltd. The allyl glycidyl ether is a commercially available product. Such as the products produced by Jinan Zhongwei Chemical Co., Ltd.
本发明的有益效果:Beneficial effects of the present invention:
现有的光扩散剂。需要进行表面处理以保证分散均匀,以提高光分散性。经过在骨架上引入含氧官能团,使光散射粒子耐氧化性能提高,不宜分解,老化,使透光率提高。Existing light diffusers. Surface treatment is required to ensure uniform dispersion to improve light dispersion. By introducing oxygen-containing functional groups into the skeleton, the oxidation resistance of the light-scattering particles is improved, and it is not suitable for decomposition and aging, so that the light transmittance is improved.
具体实施方式Detailed ways
以下实施例仅仅是进一步说明本发明,并不是限制本发明保护的范围。The following examples are only to further illustrate the present invention, but not to limit the protection scope of the present invention.
本发明提供一种聚4-甲基-1-戊烯光扩散剂及其制备方法,通过以下步骤实现:The invention provides a poly-4-methyl-1-pentene light diffusing agent and a preparation method thereof, which are realized through the following steps:
实施例1:Example 1:
步骤1.水相的配制Step 1. Preparation of water phase
在2000L高压反应釜中内加入1000Kg水,1Kg十六烷基苯磺酸钠,搅拌均匀。Add 1000Kg of water and 1Kg of sodium hexadecylbenzenesulfonate into a 2000L autoclave, and stir evenly.
步骤2.油相的配制Step 2. Preparation of oil phase
在500L反应釜中,将100Kg聚4-甲基-1-戊烯,0.3Kg1,2-环氧基-5-己烯,0.3Kg3,4-环氧-1-丁烯,加入0.4Kg过氧化氢异丙苯、0.1Kg硫酸氢钠搅拌均匀。In a 500L reactor, 100Kg poly 4-methyl-1-pentene, 0.3Kg1,2-epoxy-5-hexene, 0.3Kg3,4-epoxy-1-butene, 0.4Kg over Cumene hydrogen oxide and 0.1Kg sodium bisulfate were stirred evenly.
步骤3.聚合反应Step 3. Polymerization
将油相溶液加到步骤1中装有已配制水相的高压反应釜中,通入0.25Kg烯丙基缩水甘油醚,然后从70℃反应2h,反应结束后离心,干燥得到产品。编号为T-1。Add the oil phase solution to the autoclave equipped with the prepared water phase in step 1, pass through 0.25Kg allyl glycidyl ether, and then react at 70°C for 2 hours, centrifuge after the reaction, and dry to obtain the product. The number is T-1.
实施例2Example 2
步骤1.水相的配制Step 1. Preparation of water phase
在2000L高压反应釜中内加入1000Kg水,0.5Kg十六烷基苯磺酸钠,搅拌均匀。Add 1000Kg of water and 0.5Kg of sodium hexadecylbenzenesulfonate into a 2000L autoclave, and stir evenly.
步骤2.油相的配制Step 2. Preparation of oil phase
在500L反应釜中,将100Kg聚4-甲基-1-戊烯,0.05Kg1,2-环氧基-5-己烯,0.05Kg3,4-环氧-1-丁烯,加入0.2Kg过氧化氢异丙苯、0.05Kg硫酸氢钠,搅拌均匀。In a 500L reactor, add 100Kg poly-4-methyl-1-pentene, 0.05Kg1,2-epoxy-5-hexene, 0.05Kg3,4-epoxy-1-butene, add 0.2Kg Cumyl hydrogen oxide, 0.05Kg sodium bisulfate, stir evenly.
步骤3.聚合反应Step 3. Polymerization
将油相溶液加到步骤1中装有已配制水相的高压反应釜中,通入0.1Kg烯丙基缩水甘油醚,然后从50℃反应4h,反应结束后离心,干燥得到产品。编号为T-2。Add the oil phase solution to the autoclave equipped with the prepared water phase in step 1, pass through 0.1Kg allyl glycidyl ether, then react at 50°C for 4 hours, centrifuge after the reaction, and dry to obtain the product. The number is T-2.
实施例3Example 3
步骤1.水相的配制Step 1. Preparation of water phase
在2000L高压反应釜中内加入1000Kg水,2Kg十六烷基苯磺酸钠,搅拌均匀。Add 1000Kg of water and 2Kg of sodium hexadecylbenzenesulfonate into a 2000L autoclave, and stir evenly.
步骤2.油相的配制Step 2. Preparation of oil phase
在500L反应釜中,将100Kg聚4-甲基-1-戊烯,0.5Kg1,2-环氧基-5-己烯,0.5Kg3,4-环氧-1-丁烯,加入0.6Kg过氧化氢异丙苯、0.2Kg硫酸氢钠,搅拌均匀。In a 500L reactor, add 100Kg poly-4-methyl-1-pentene, 0.5Kg1,2-epoxy-5-hexene, 0.5Kg3,4-epoxy-1-butene, add 0.6Kg over Cumyl hydrogen oxide, 0.2Kg sodium bisulfate, stir evenly.
步骤3.聚合反应Step 3. Polymerization
将油相溶液加到步骤1中装有已配制水相的高压反应釜中,通入0.5Kg烯丙基缩水甘油醚,然后从80℃反应1h,反应结束后离心,干燥得到产品。编号为T-3。Add the oil phase solution to the autoclave equipped with the prepared water phase in step 1, pass through 0.5Kg allyl glycidyl ether, then react at 80°C for 1 hour, centrifuge after the reaction, and dry to obtain the product. The number is T-3.
对比例1Comparative example 1
不加入1,2-环氧基-5-己烯,其他同实施例1,产品编号为T-4。Without adding 1,2-epoxy-5-hexene, the others are the same as in Example 1, and the product number is T-4.
对比例2Comparative example 2
不加入烯丙基缩水甘油醚,其他同实施例1,产品编号为T-5。Allyl glycidyl ether is not added, the others are the same as in Example 1, and the product number is T-5.
对比例3Comparative example 3
不加入3,4-环氧-1-丁烯,其他同实施例1,产品编号为T-6。Without adding 3,4-epoxy-1-butene, the others are the same as in Example 1, and the product number is T-6.
实施例4Example 4
实施例1-3和对比例1-3中制得的光散射粒子1Kg,抗氧剂0.3Kg,与扩散剂进行预分散,加入PC粒子100Kg后,转移到低速混合机中搅拌,混合均匀后用双螺杆挤出机熔融共混、造粒,最后经注塑机注塑成型光扩散板。1Kg of light-scattering particles and 0.3Kg of antioxidant prepared in Example 1-3 and Comparative Example 1-3 were pre-dispersed with the diffusing agent. After adding 100Kg of PC particles, they were transferred to a low-speed mixer for stirring, and after mixing evenly A twin-screw extruder is used for melt blending and granulation, and finally an injection molding machine is used to form a light diffusion plate.
光学测试optical test
使用透光率/雾度测试仪(EEL57D,上海精密仪器有限公司),按GB/T2410-2008测试。Use a light transmittance/haze tester (EEL57D, Shanghai Precision Instrument Co., Ltd.), and test according to GB/T2410-2008.
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