CN104927589B - A kind of organic silicon wear resistant stiffened coating and preparation method thereof - Google Patents
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Abstract
本发明公开了一种有机硅耐磨加硬涂层及其制备方法，所述涂层由80‑90重量份的环氧树脂、10‑20重量份的硅烷偶联剂和0.2重量份的引发剂组成。涂料可以在室温下简单的设备中进行反应制备，易于运输、储存，达到了简化生产工艺、减少能源消耗、减少设备投入的目的，制成的涂层具有硬度高、耐磨性好、能在室温下长时间稳定存在的优点，同时该涂层在用于透明塑料基片如有机玻璃的浸涂时，不需要底涂就能直接浸涂固化。The invention discloses a silicone wear-resistant and hardened coating and a preparation method thereof. The coating consists of 80-90 parts by weight of epoxy resin, 10-20 parts by weight of silane coupling agent and 0.2 parts by weight of initiator agent composition. Coatings can be reacted and prepared in simple equipment at room temperature, easy to transport and store, and achieve the purpose of simplifying the production process, reducing energy consumption, and reducing equipment investment. The resulting coating has high hardness, good wear resistance, and can be used in It has the advantage of being stable for a long time at room temperature. At the same time, when the coating is used for dip coating of transparent plastic substrates such as plexiglass, it can be directly dip-coated and cured without primer.
Description
技术领域technical field
本发明涉及一种涂层，特别是涉及一种适用于有机玻璃及其他透明或不透明塑料表面保护，以及用于金属表面、金属镀件的防腐、耐磨涂层、电子元件的绝缘和防潮涂层、石质材料防风化涂层等的有机硅耐磨加硬涂层及其制备方法。The invention relates to a coating, in particular to a coating suitable for surface protection of plexiglass and other transparent or opaque plastics, as well as anti-corrosion and wear-resistant coatings for metal surfaces, metal plated parts, insulation and moisture-proof coatings for electronic components. Silicone wear-resistant and hardened coatings for layers, weatherproof coatings for stone materials, etc., and preparation methods thereof.
背景技术Background technique
与光学玻璃相比，光学塑料如聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)等，不仅有着许多突出的光学性能，同时具有低密度及高抗冲击性能。但是光学塑料的表面硬度低，易擦伤，日常使用过程中容易使其光学性能急剧下降，影响正常使用。耐磨涂层多为一些低分子量聚合物与硅烷偶联剂制得，而环保型的环氧丙烯酸树脂体系由于成本较高，限制了该类产品的普及应用。虽然市场上也有成本较低的涂料选用丙烯酸酯类作为助剂，但该类助剂与涂料基体树脂的相容性差，从而影响了涂层的应用性能。Compared with optical glass, optical plastics such as polymethyl methacrylate (PMMA) and polycarbonate (PC) not only have many outstanding optical properties, but also have low density and high impact resistance. However, the surface hardness of optical plastics is low, and it is easy to be scratched. During daily use, its optical performance is likely to drop sharply, affecting normal use. Wear-resistant coatings are mostly made of some low-molecular-weight polymers and silane coupling agents, and the high cost of environmentally friendly epoxy acrylic resin systems limits the popularization and application of such products. Although there are low-cost paints on the market that use acrylates as additives, these additives have poor compatibility with the paint matrix resin, thus affecting the application performance of the coating.
发明内容Contents of the invention
本发明的目的之一是要提供一种环氧丙烯酸树脂型透明耐磨涂层，以克服市场现有涂料对有机塑料表面附着力差、环保性差以及丙烯酸树脂体系制备成本过高导致其不能普及应用的弊端，同时也解决了选用常规的丙烯酸脂树脂体系对有机塑料表面进行透明涂装，所呈现的由于两者的相容性差而降低塑料表面涂层的透明效果的难题。One of the purposes of the present invention is to provide an epoxy acrylic resin type transparent wear-resistant coating, to overcome the poor adhesion of existing coatings on the organic plastic surface, poor environmental protection and the high cost of preparation of acrylic resin systems that cannot be popularized At the same time, it also solves the problem of reducing the transparent effect of the plastic surface coating due to the poor compatibility of the two when using a conventional acrylic resin system for transparent coating on the surface of organic plastics.
本发明的目的之二是要提供一种制备环氧丙烯酸树脂型透明耐磨涂层的方法，从而能生产出制备工艺简单的环氧丙烯酸树脂型透明耐磨涂层。The second object of the present invention is to provide a method for preparing epoxy acrylic resin type transparent wear-resistant coating, so as to produce epoxy acrylic resin type transparent wear-resistant coating with simple preparation process.
本发明的目的是这样实现的：本发明有机硅耐磨加硬涂层及其制备方法，具体说来是设计一种以液体环氧丙烯酸树脂为主要基料的透明液体涂层及其制备方法。The object of the present invention is achieved like this: the organosilicon wear-resisting hard coating of the present invention and preparation method thereof, specifically design a kind of transparent liquid coating and preparation method thereof with liquid epoxy acrylic resin as main base material .
本发明的有机硅耐磨加硬涂层，由80-90重量份的环氧树脂、10-20重量份的硅烷偶联剂和0.2重量份的引发剂组成。The silicone wear-resistant and hardened coating of the invention consists of 80-90 parts by weight of epoxy resin, 10-20 parts by weight of silane coupling agent and 0.2 parts by weight of initiator.
进一步地，所述的环氧树脂为双酚A型环氧树脂。Further, the epoxy resin is bisphenol A type epoxy resin.
进一步地，所述的双酚A型环氧树脂为的E03型双酚A环氧树脂。Further, the bisphenol A type epoxy resin is E03 type bisphenol A epoxy resin.
进一步地，所述的硅烷偶联剂为γ-甲基丙烯酰氧丙基三甲氧基硅烷KH-570。Further, the silane coupling agent is γ-methacryloxypropyltrimethoxysilane KH-570.
进一步地，所述的引发剂为BPO(过氧化二苯甲酰)。Further, the initiator is BPO (dibenzoyl peroxide).
本发明的有机硅耐磨加硬涂层的制备方法，包括如下步骤：The preparation method of the organosilicon wear-resistant and hardened coating of the present invention comprises the following steps:
(1)双酚A型环氧丙烯酸树脂的制备：将双酚A型环氧树脂与丙烯酸按摩尔比1:2混合均匀，加入三苯基膦作催化剂，催化剂的重量为双酚A型环氧树脂与丙烯酸总重量的0.2％；80℃条件下反应4h制得双酚A型环氧丙烯酸树脂；(1) Preparation of bisphenol A type epoxy acrylic resin: Mix bisphenol A type epoxy resin and acrylic acid in a molar ratio of 1:2, add triphenylphosphine as catalyst, the weight of catalyst is bisphenol A type ring 0.2% of the total weight of epoxy resin and acrylic acid; under the condition of 80 ℃, react for 4h to prepare bisphenol A type epoxy acrylic resin;
(2)涂料的制备：将80-90重量份的双酚A型环氧丙烯酸树脂％、10-20重量份的KH-570硅烷偶联剂(γ-甲基丙烯酰氧丙基三甲氧基硅烷)混合均匀，以0.2重量份的BPO(过氧化二苯甲酰)作引发剂制备有机硅耐磨加硬涂料；(2) Preparation of coating: the KH-570 silane coupling agent (γ-methacryloyloxypropyltrimethoxy) of the bisphenol A type epoxy acrylic resin % of 80-90 weight parts, 10-20 weight parts Silane) is mixed evenly, and the BPO (dibenzoyl peroxide) of 0.2 weight part is used as initiator to prepare organosilicon wear-resistant and hardened coating;
(3)涂层的制备：将步骤(2)得到的涂料涂覆在PMMA基材表面，在通风处放置30分钟后放入烘箱中在80℃下固化8h，在PMMA基材表面获得有机硅耐磨加硬涂层。(3) Preparation of coating: coat the coating obtained in step (2) on the surface of the PMMA substrate, place it in a ventilated place for 30 minutes and then put it into an oven and cure it at 80°C for 8 hours to obtain organic silicon on the surface of the PMMA substrate. Wear-resistant hard coating.
本发明能适用于溶剂型塑料涂料技术领域，所述的有机硅耐磨加硬涂层可广泛应用于各种有机塑料板材表面，使之获得较好的防护修饰，它能较好地保护有机塑料表面，具有高透光率、良好的耐擦伤性、外观感强、符合环保要求、应用成本低的特点。The invention can be applied to the technical field of solvent-based plastic coatings. The wear-resistant and hardened silicone coating can be widely applied to the surface of various organic plastic plates, so that it can obtain better protective modification, and it can better protect organic The plastic surface has the characteristics of high light transmittance, good scratch resistance, strong appearance, meets environmental protection requirements, and low application cost.
本发明的主要改进体现在：创新性地先将双酚A环氧树脂与丙烯酸进行开环反应后再与硅烷偶联剂进行共聚的方式将硅氧烷类化合物引入环氧树脂体系中，提高制备的涂层与基材之间的结合力，提供一种各项性能良好的新型光学塑料耐磨加硬涂层。The main improvement of the present invention is reflected in: firstly carry out the ring-opening reaction of bisphenol A epoxy resin and acrylic acid and then carry out copolymerization with silane coupling agent to introduce siloxane compounds into the epoxy resin system, improve the The bonding force between the prepared coating and the base material provides a novel optical plastic wear-resistant and hardened coating with good various properties.
附图说明Description of drawings
图1是PMMA板涂膜前后的透光率图(a-空白，b-实施例一，c-实施例二，d-实施例三)；Fig. 1 is the light transmittance figure (a-blank, b-embodiment one, c-embodiment two, d-embodiment three) before and after PMMA plate coating film;
图2是PMMA板涂膜前后的耐磨性能变化图(a-空白，b-实施例一，c-实施例二，d-实施例三)；Fig. 2 is the wear resistance change figure (a-blank, b-embodiment one, c-embodiment two, d-embodiment three) before and after the coating film of PMMA plate;
图3是涂层表面水及乙二醇接触角随硅烷偶联剂含量的变化图。Figure 3 is a graph showing the variation of the contact angle of water and ethylene glycol on the surface of the coating with the content of the silane coupling agent.
具体实施方式detailed description
下面结合附图和具体实施例对发明作进一步详细说明。The invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.
实施例一：Embodiment one:
一种有机硅耐磨加硬涂层。首先是涂料的制备：双酚A型环氧丙烯酸树脂90重量份(E03型环氧树脂与丙烯酸按摩尔比1：2混合均匀，加入三苯基膦作催化剂，催化剂的重量为双酚A型环氧树脂与丙烯酸总重量的0.2％，80℃条件下反应4h制得双酚A型环氧丙烯酸树脂)；KH-570硅烷偶联剂(γ-甲基丙烯酰氧基丙基三甲氧基硅烷)10重量份。其次是基材的表面预处理：将有机玻璃(PMMA)板切割成：6×6cm2规格，依次经过NaOH/Na2CO3碱液清洗-超声振荡清洗-蒸馏水、无水乙醇交替清洗-异丙醇吹干，烘干备用。最后将90重量份双酚A型环氧丙烯酸树脂和10重量份KH-570硅烷偶联剂混合均匀，以0.2重量份的BPO(过氧化二苯甲酰)作引发剂制备有机硅耐磨加硬涂层，涂覆在PMMA板表面，在通风处放置30分钟后放入烘箱中于80℃下固化8h，在PMMA基材表面获得有机硅耐磨加硬涂层，并进行后期的涂层性能测试。A silicone wear-resistant hard coating. The first is the preparation of the coating: 90 parts by weight of bisphenol A type epoxy acrylic resin (E03 type epoxy resin and acrylic acid are mixed uniformly in a molar ratio of 1:2, and triphenylphosphine is added as a catalyst. The weight of the catalyst is bisphenol A type 0.2% of the total weight of epoxy resin and acrylic acid, react 4h under the condition of 80 ℃ to obtain bisphenol A type epoxy acrylic resin); KH-570 silane coupling agent (γ-methacryloxypropyl trimethoxy silane) 10 parts by weight. The second is the surface pretreatment of the base material: cut the plexiglass (PMMA) plate into: 6×6cm 2 specifications, and then go through NaOH/Na 2 CO 3 lye cleaning-ultrasonic oscillation cleaning-distilled water, absolute ethanol alternate cleaning-iso Blow dry with propanol and dry for later use. Finally, 90 parts by weight of bisphenol A type epoxy acrylic resin and 10 parts by weight of KH-570 silane coupling agent are mixed evenly, and the BPO (dibenzoyl peroxide) of 0.2 parts by weight is used as initiator to prepare silicone wear-resistant coating Hard coating, coated on the surface of the PMMA board, placed in a ventilated place for 30 minutes, then placed in an oven and cured at 80°C for 8 hours, to obtain a silicone wear-resistant and hardened coating on the surface of the PMMA substrate, and perform subsequent coating Performance Testing.
采用该种方法制得的耐磨加硬涂层在有机玻璃上固化后铅笔硬度可达6H，附着力为1级。The wear-resistant and hardened coating prepared by this method can reach a pencil hardness of 6H after curing on the organic glass, and the adhesion is grade 1.
实施例二：Embodiment two:
一种有机硅耐磨加硬涂层。首先是涂料的制备：双酚A型环氧丙烯酸树脂85重量份(E03型环氧树脂与丙烯酸按摩尔比1：2混合均匀，加入三苯基膦作催化剂，催化剂的重量为双酚A型环氧树脂与丙烯酸总重量的0.2％，80℃条件下反应4h制得双酚A型环氧丙烯酸树脂)；KH-570硅烷偶联剂(γ-甲基丙烯酰氧基丙基三甲氧基硅烷)15重量份。其次是基材的表面预处理：将有机玻璃(PMMA)板切割成：6×6cm2规格，依次经过NaOH/Na2CO3碱液清洗-超声振荡清洗-蒸馏水、无水乙醇交替清洗-异丙醇吹干，烘干备用。最后将85重量份双酚A型环氧丙烯酸树脂和15重量份KH-570硅烷偶联剂混合均匀，以0.2重量份的BPO(过氧化二苯甲酰)作引发剂制备有机硅耐磨加硬涂层，涂覆在PMMA板表面，在通风处放置30分钟后放入烘箱中于80℃下固化8h，在PMMA基材表面获得有机硅耐磨加硬涂层，并进行后期的涂层性能测试。A silicone wear-resistant hard coating. The first is the preparation of the coating: 85 parts by weight of bisphenol A type epoxy acrylic resin (E03 type epoxy resin and acrylic acid are mixed uniformly in a molar ratio of 1:2, and triphenylphosphine is added as a catalyst. The weight of the catalyst is bisphenol A type 0.2% of the total weight of epoxy resin and acrylic acid, react 4h under the condition of 80 ℃ to obtain bisphenol A type epoxy acrylic resin); KH-570 silane coupling agent (γ-methacryloxypropyl trimethoxy silane) 15 parts by weight. The second is the surface pretreatment of the base material: cut the plexiglass (PMMA) plate into: 6×6cm 2 specifications, and then go through NaOH/Na 2 CO 3 lye cleaning-ultrasonic oscillation cleaning-distilled water, absolute ethanol alternate cleaning-iso Blow dry with propanol and dry for later use. Finally, 85 parts by weight of bisphenol A type epoxy acrylic resin and 15 parts by weight of KH-570 silane coupling agent are mixed evenly, and the BPO (dibenzoyl peroxide) of 0.2 parts by weight is used as initiator to prepare silicone wear-resistant coating Hard coating, coated on the surface of the PMMA board, placed in a ventilated place for 30 minutes, then placed in an oven and cured at 80°C for 8 hours, to obtain a silicone wear-resistant and hardened coating on the surface of the PMMA substrate, and perform subsequent coating Performance Testing.
采用该种方法制得的耐磨涂层在有机玻璃上固化后铅笔硬度可达5H，附着力为1级。After the wear-resistant coating prepared by this method is cured on the plexiglass, the pencil hardness can reach 5H, and the adhesion is grade 1.
实施例三：Embodiment three:
一种有机硅耐磨加硬涂层。首先是涂料的制备：双酚A型环氧丙烯酸树脂80重量份(E03型环氧树脂与丙烯酸按摩尔比1：2混合均匀，加入三苯基膦作催化剂，催化剂的重量为双酚A型环氧树脂与丙烯酸总重量的0.2％，80℃条件下反应4h制得双酚A型环氧丙烯酸树脂)；KH-570硅烷偶联剂(γ-甲基丙烯酰氧基丙基三甲氧基硅烷)20重量份。其次是基材的表面预处理：将有机玻璃(PMMA)板切割成：6×6cm2规格，依次经过NaOH/Na2CO3碱液清洗-超声振荡清洗-蒸馏水、无水乙醇交替清洗-异丙醇吹干，烘干备用。最后将80重量份双酚A型环氧丙烯酸树脂和20重量份KH-570硅烷偶联剂混合均匀，以0.2重量份的BPO(过氧化二苯甲酰)作引发剂制备有机硅耐磨加硬涂层，涂覆在PMMA板表面，在通风处放置30分钟后放入烘箱中于80℃下固化8h，在PMMA基材表面获得有机硅耐磨加硬涂层，并进行后期的涂层性能测试。A silicone wear-resistant hard coating. The first is the preparation of the coating: 80 parts by weight of bisphenol A type epoxy acrylic resin (E03 type epoxy resin and acrylic acid are mixed uniformly in a molar ratio of 1:2, and triphenylphosphine is added as a catalyst. The weight of the catalyst is bisphenol A type 0.2% of the total weight of epoxy resin and acrylic acid, react 4h under the condition of 80 ℃ to obtain bisphenol A type epoxy acrylic resin); KH-570 silane coupling agent (γ-methacryloxypropyl trimethoxy silane) 20 parts by weight. The second is the surface pretreatment of the base material: cut the plexiglass (PMMA) plate into: 6×6cm 2 specifications, and then go through NaOH/Na 2 CO 3 lye cleaning-ultrasonic oscillation cleaning-distilled water, absolute ethanol alternate cleaning-iso Blow dry with propanol and dry for later use. Finally, 80 parts by weight of bisphenol A type epoxy acrylic resin and 20 parts by weight of KH-570 silane coupling agent are mixed evenly, and the BPO (dibenzoyl peroxide) of 0.2 parts by weight is used as an initiator to prepare silicone wear-resistant coating Hard coating, coated on the surface of the PMMA board, placed in a ventilated place for 30 minutes, then placed in an oven and cured at 80°C for 8 hours, to obtain a silicone wear-resistant and hardened coating on the surface of the PMMA substrate, and perform subsequent coating Performance Testing.
采用该种方法制得的耐磨涂层在有机玻璃上固化后铅笔硬度可达6H，附着力为1级。After the wear-resistant coating prepared by this method is cured on the plexiglass, the pencil hardness can reach 6H, and the adhesion is grade 1.
表1涂层的铅笔硬度及附着力与硅烷偶联剂含量的关系Table 1 The relationship between the pencil hardness and adhesion of the coating and the content of the silane coupling agent
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