硅氧烷類聚合物耐磨透明涂層的制備及其性能研究
發(fā)布時(shí)間：2019-05-29 05:59
【摘要】：有機(jī)硅高分子化合物因其特殊的化學(xué)結(jié)構(gòu)而擁有優(yōu)越的性能,應(yīng)用已遍及于各個(gè)領(lǐng)域,尤其是涂料行業(yè)。有機(jī)硅耐磨加硬涂層是其眾多應(yīng)用中應(yīng)用最廣泛的一種,作為光學(xué)塑料表面的保護(hù)涂層在改善光學(xué)塑料表面易被擦傷方面取得了突出效果,具有良好的經(jīng)濟(jì)效益和社會(huì)效益。本論文主要圍繞硅氧烷類耐磨涂層的制備及其性能開(kāi)展研究。(1)通過(guò)E 03型雙酚A環(huán)氧樹(shù)脂與丙烯酸反應(yīng)合成了雙酚A環(huán)氧丙烯酸樹(shù)脂,探究了不同摩爾比對(duì)反應(yīng)產(chǎn)率的影響；用硅烷偶聯(lián)劑MPS(Y-甲基丙烯酰氧丙基三甲氧基硅烷)對(duì)雙酚A環(huán)氧丙烯酸樹(shù)脂進(jìn)行改性,將所得產(chǎn)物均勻涂覆在PMMA(聚甲基丙烯酸甲酯)基材表面進(jìn)行固化,制備了硅烷偶聯(lián)劑MPS質(zhì)量分?jǐn)?shù)分別為10%、15%、20%、30%、40%和60%的耐磨加硬透明涂層,并對(duì)其物理性能、光學(xué)性能和耐磨性能等進(jìn)行測(cè)試,著重分析了硅烷偶聯(lián)劑MPS的含量對(duì)涂層各種性能的影響。觀察發(fā)現(xiàn)硅烷偶聯(lián)劑MPS含量為10%、15%、20%時(shí),涂層表面平整、光滑,通過(guò)對(duì)該三組涂層進(jìn)行性能測(cè)試發(fā)現(xiàn)：固化后的涂層透光率達(dá)到92%左右;鉛筆硬度最高達(dá)6H,附著力為1級(jí),而且提高了基材的抗刮性能和耐磨性能,表現(xiàn)為在相同擦拭次數(shù)下,涂覆涂層的PMMA基材的失重率明顯低于未涂覆涂層的PMMA基材的失重率；基于接觸角數(shù)據(jù)可以發(fā)現(xiàn),隨著硅烷偶聯(lián)劑MPS含量的增加,材料表面張力減小,表現(xiàn)為蒸餾水和乙二醇在耐磨涂層上的接觸角隨著硅烷偶聯(lián)劑MPS含量的增加而變大,賦予耐磨涂層表面比較低的表面自由能。(2)以正硅酸乙酯(TEOS)和Y-縮水甘油醚氧丙基三甲氧基硅烷(GPTMS)為反應(yīng)原料,利用溶膠-凝膠法制得了摩爾比分別為1.33、1.50、1.86、2.00、2.33、2.50、3.00和4.00的八組有機(jī)硅溶膠復(fù)合耐磨涂層,著重研究分析了不同的摩爾比組成對(duì)耐磨涂層物理性能、光學(xué)性能和耐磨性能等的影響。觀察發(fā)現(xiàn)摩爾比為2.33和4.00的兩組溶膠涂層表觀呈現(xiàn)起皺、破裂現(xiàn)象,而其余的六組樣品涂層表面平整、光滑且具有良好的儲(chǔ)存穩(wěn)定性。通過(guò)性能測(cè)試發(fā)現(xiàn)：涂層的鉛筆硬度和附著力等級(jí)隨著溶膠體系中TEOS含量的增加呈現(xiàn)先增大后減小的趨勢(shì),最大鉛筆硬度可達(dá)5H,附著力等級(jí)為1級(jí)。同時(shí)發(fā)現(xiàn)溶膠的陳化時(shí)間對(duì)涂層的硬度和附著力也有影響,隨著陳化時(shí)間的延長(zhǎng),溶膠涂層的鉛筆硬度和附著力隨之提高。制備的耐磨涂層具有很好的透光率,而且可以有效提高PMMA基材的抗刮性能和耐磨性能,表現(xiàn)為在相同擦拭次數(shù)下,涂覆涂層的PMMA基材的失重率明顯小于未涂覆涂層的PMMA基材的失重率,而且能夠使涂層表面產(chǎn)生明顯劃痕的最小砝碼質(zhì)量相比涂覆前有所增加�；诮佑|角數(shù)據(jù)可以發(fā)現(xiàn),隨著溶膠體系中TEOS含量的增加,材料表面張力減小,表現(xiàn)為蒸餾水和乙二醇在涂層上的接觸角隨著TEOS含量的增加而變大,賦予涂層表面比較低的表面自由能。(3)選擇了三種不同的光引發(fā)劑Irgacute 184、Irgacure MBF和Irgacure 907在紫外光下用硅烷偶聯(lián)劑MPS對(duì)雙酚A環(huán)氧丙烯酸樹(shù)脂進(jìn)行改性,同時(shí)添加分散劑、消泡劑和流平劑等助劑,制得了九組耐磨加硬涂層,探討了光引發(fā)劑的差別對(duì)耐磨涂層的物理性能、光學(xué)性能、耐磨性能及抗刮性能的影響。通過(guò)測(cè)定三種光引發(fā)劑的紫外吸收曲線發(fā)現(xiàn),在紫外光區(qū)內(nèi)三種光引發(fā)劑具有截然不同的紫外吸收峰。Irgacure184的吸收波長(zhǎng)在205 nm和248 nm,Irgacure 907的吸收波長(zhǎng)在204 nm、238 nm和305 am,而Irgacure MBF的吸收波長(zhǎng)在204 nm和256 nm。通過(guò)觀察不同光引發(fā)劑制備的九組耐磨涂層樣品發(fā)現(xiàn)涂料本身均一、透明且具有良好的穩(wěn)定性,涂層表面平整、光滑。通過(guò)對(duì)涂層進(jìn)行性能測(cè)試發(fā)現(xiàn)：所有涂層都具有良好的鉛筆硬度、附著力和透光率。同時(shí)發(fā)現(xiàn)Irgacure 907光引發(fā)劑制備的耐磨涂層相較于其他兩種光引發(fā)劑制備的耐磨涂層有著更好的鉛筆硬度、光學(xué)性能、耐磨性能和抗刮性能。
[Abstract]:The organosilicon polymer compound has excellent performance due to its special chemical structure and has been applied in various fields, especially in the coating industry. The organic silicon wear-resistant hardcoat is one of the most widely used in many applications, and the protective coating which is used as the surface of the optical plastic has the outstanding effect in improving the surface of the optical plastic, and has good economic and social benefits. This paper mainly studies the preparation and properties of the silicone-based wear-resistant coating. (1) The bisphenol A epoxy acrylic resin was synthesized by the reaction of the E 03 bisphenol A epoxy resin and the acrylic acid, and the effect of different molar ratios on the reaction yield was investigated. the bisphenol A epoxy acrylic resin is modified by using a silane coupling agent MPS (Y-methylpropylidene trimethoxy silane), the obtained product is uniformly coated on the surface of the PMMA (polymethyl methacrylate) substrate for curing, and the mass fraction of the silane coupling agent MPS is 10 percent, 15%,20%,30%,40% and 60% wear-resistant and hard transparent coatings, and the physical properties, optical properties and wear resistance of the coatings were tested, and the effects of the content of the silane coupling agent MPS on the various properties of the coatings were analyzed. when the content of the silane coupling agent is 10%,15% and 20%, the surface of the coating is flat and smooth, and the performance test of the three groups of coatings shows that the light transmittance of the cured coating reaches about 92%; the pencil hardness is up to 6 h and the adhesion force is grade 1, and the scratch resistance and the wear resistance of the base material are improved, the weight loss rate of the PMMA base material coated with the coating is obviously lower than the weight loss rate of the PMMA base material of the uncoated coating under the same wiping frequency, and based on the contact angle data, the content of the silane coupling agent MPS is increased, The surface tension of the material is reduced, the contact angle of the distilled water and the ethylene glycol on the wear-resistant coating is increased as the content of the silane coupling agent MPS is increased, and the surface free energy of the surface of the wear-resistant coating is relatively low. (2) an eight-group organic silica sol composite wear-resistant coating with the molar ratio of 1.33, 1.50, 1.86, 2.00, 2.33, 2.50, 3.00 and 4.00, respectively, is obtained by using the orthosilicate (TEOS) and the Y-glycidyl ether oxypropyltrimethoxysilane (GPTMS) as the reaction raw material, The effects of different molar ratios on the physical properties, optical properties and wear resistance of wear-resistant coatings were studied. The apparent wrinkling and cracking of two groups of sol coatings with a molar ratio of 2.33 and 4.00 were observed, while the remaining six groups of sample coatings were flat, smooth and have good storage stability. The performance test shows that the pencil hardness and the adhesion grade of the coating exhibit a tendency to decrease with the increase of the TEOS content in the sol system, and the maximum pencil hardness can be up to 5 H and the adhesion level is grade 1. At the same time, it is found that the aging time of the sol has an effect on the hardness and the adhesion of the coating, and the pencil hardness and the adhesion of the sol coating are improved as the aging time is prolonged. the prepared wear-resistant coating has good light transmittance and can effectively improve the scratch resistance and the wear resistance of the PMMA base material, But also an increase in the quality of the minimum weight of the coating surface that has a significant scratch. Based on the contact angle data, it can be found that with the increase of the content of TEOS in the sol system, the surface tension of the material is reduced, and the contact angle of the distilled water and the glycol on the coating increases with the increase of the TEOS content, giving a relatively low surface free energy to the coating surface. (3) Three different photo-initiators, Irgacute 184, Irgacure MBF and Irgacure 907, were selected to modify the bisphenol A epoxy acrylic resin with the silane coupling agent MPS under the ultraviolet light, and the addition of the additives such as the dispersing agent, the defoaming agent and the leveling agent were added. The effects of the difference of photoinitiator on the physical properties, optical properties, wear resistance and anti-scratch properties of the wear-resistant coatings were discussed. The UV-absorption curve of three kinds of photo-initiators showed that the three kinds of photo-initiators in the ultraviolet region had different ultraviolet absorption peaks. The absorption wavelength of Irgacure 184 was at 205 nm and 248 nm, and the absorption wavelength of Irgacure 907 was at 204 nm,238 nm and 305 am, while the absorption wavelength of Irgacure MBF was at 204 nm and 256 nm. The nine-group wear-resistant coating samples prepared by observing the different photo-initiators find that the coating itself is uniform, transparent and has good stability, and the surface of the coating is smooth and smooth. The performance test of the coating found that all the coatings had good pencil hardness, adhesion and light transmittance. At the same time, it is found that the wear-resistant coating prepared by the Irgacure 907 photoinitiator has better pencil hardness, optical performance, wear resistance and scratch resistance compared with the wear-resistant coating prepared by the other two photoinitiators.
【學(xué)位授予單位】：浙江大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB306
本文編號(hào)：2487707
[Abstract]:The organosilicon polymer compound has excellent performance due to its special chemical structure and has been applied in various fields, especially in the coating industry. The organic silicon wear-resistant hardcoat is one of the most widely used in many applications, and the protective coating which is used as the surface of the optical plastic has the outstanding effect in improving the surface of the optical plastic, and has good economic and social benefits. This paper mainly studies the preparation and properties of the silicone-based wear-resistant coating. (1) The bisphenol A epoxy acrylic resin was synthesized by the reaction of the E 03 bisphenol A epoxy resin and the acrylic acid, and the effect of different molar ratios on the reaction yield was investigated. the bisphenol A epoxy acrylic resin is modified by using a silane coupling agent MPS (Y-methylpropylidene trimethoxy silane), the obtained product is uniformly coated on the surface of the PMMA (polymethyl methacrylate) substrate for curing, and the mass fraction of the silane coupling agent MPS is 10 percent, 15%,20%,30%,40% and 60% wear-resistant and hard transparent coatings, and the physical properties, optical properties and wear resistance of the coatings were tested, and the effects of the content of the silane coupling agent MPS on the various properties of the coatings were analyzed. when the content of the silane coupling agent is 10%,15% and 20%, the surface of the coating is flat and smooth, and the performance test of the three groups of coatings shows that the light transmittance of the cured coating reaches about 92%; the pencil hardness is up to 6 h and the adhesion force is grade 1, and the scratch resistance and the wear resistance of the base material are improved, the weight loss rate of the PMMA base material coated with the coating is obviously lower than the weight loss rate of the PMMA base material of the uncoated coating under the same wiping frequency, and based on the contact angle data, the content of the silane coupling agent MPS is increased, The surface tension of the material is reduced, the contact angle of the distilled water and the ethylene glycol on the wear-resistant coating is increased as the content of the silane coupling agent MPS is increased, and the surface free energy of the surface of the wear-resistant coating is relatively low. (2) an eight-group organic silica sol composite wear-resistant coating with the molar ratio of 1.33, 1.50, 1.86, 2.00, 2.33, 2.50, 3.00 and 4.00, respectively, is obtained by using the orthosilicate (TEOS) and the Y-glycidyl ether oxypropyltrimethoxysilane (GPTMS) as the reaction raw material, The effects of different molar ratios on the physical properties, optical properties and wear resistance of wear-resistant coatings were studied. The apparent wrinkling and cracking of two groups of sol coatings with a molar ratio of 2.33 and 4.00 were observed, while the remaining six groups of sample coatings were flat, smooth and have good storage stability. The performance test shows that the pencil hardness and the adhesion grade of the coating exhibit a tendency to decrease with the increase of the TEOS content in the sol system, and the maximum pencil hardness can be up to 5 H and the adhesion level is grade 1. At the same time, it is found that the aging time of the sol has an effect on the hardness and the adhesion of the coating, and the pencil hardness and the adhesion of the sol coating are improved as the aging time is prolonged. the prepared wear-resistant coating has good light transmittance and can effectively improve the scratch resistance and the wear resistance of the PMMA base material, But also an increase in the quality of the minimum weight of the coating surface that has a significant scratch. Based on the contact angle data, it can be found that with the increase of the content of TEOS in the sol system, the surface tension of the material is reduced, and the contact angle of the distilled water and the glycol on the coating increases with the increase of the TEOS content, giving a relatively low surface free energy to the coating surface. (3) Three different photo-initiators, Irgacute 184, Irgacure MBF and Irgacure 907, were selected to modify the bisphenol A epoxy acrylic resin with the silane coupling agent MPS under the ultraviolet light, and the addition of the additives such as the dispersing agent, the defoaming agent and the leveling agent were added. The effects of the difference of photoinitiator on the physical properties, optical properties, wear resistance and anti-scratch properties of the wear-resistant coatings were discussed. The UV-absorption curve of three kinds of photo-initiators showed that the three kinds of photo-initiators in the ultraviolet region had different ultraviolet absorption peaks. The absorption wavelength of Irgacure 184 was at 205 nm and 248 nm, and the absorption wavelength of Irgacure 907 was at 204 nm,238 nm and 305 am, while the absorption wavelength of Irgacure MBF was at 204 nm and 256 nm. The nine-group wear-resistant coating samples prepared by observing the different photo-initiators find that the coating itself is uniform, transparent and has good stability, and the surface of the coating is smooth and smooth. The performance test of the coating found that all the coatings had good pencil hardness, adhesion and light transmittance. At the same time, it is found that the wear-resistant coating prepared by the Irgacure 907 photoinitiator has better pencil hardness, optical performance, wear resistance and scratch resistance compared with the wear-resistant coating prepared by the other two photoinitiators.
【學(xué)位授予單位】：浙江大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TB306
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