CN107312456B - 一种液晶电路保护用组合物及其制备方法 - Google Patents
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Abstract
本发明涉及电路保护材料领域，公开了一种液晶电路保护用组合物及其制备方法。该液晶电路保护用组合物由以下重量份的组分组成：氢化苯乙烯‑丁二烯嵌段共聚物和石油树脂10～30份、氮化硼0.5～3.6份、环烷油10～20份、主溶剂和辅助溶剂60～70份、含氟助剂0.3～1份。制得的保护用组合物膜强度变大，具有很好的的拉伸性能，不易撕断，具有良好的阻隔性，能够提高薄膜的防潮性能，具有广阔的应用前景。
Description
技术领域
本发明涉及电路保护材料领域，具体地说是一种液晶电路保护用组合物及其制备方法。
背景技术
随着世界向信息社会的发展，显示器件作为人机对话的关键部件其重要性越来越高，液晶显示、等离子PDP显示、有机发光OLED显示等多种显示器正在蓬勃发展。异方性导电胶膜(Anisotropic Conductive Film；ACF)是以化学粘接的方式将显示器与驱动电路连接起来的材料，通过表面镀有金属层的高分子聚合物微球实现Z方向导电，X-Y方向绝缘，使用简单方便，易自动化操作，是目前柔性连接所不可缺少的关键材料。但是，目前国内厂家的产品的强度、涂膜性、防湿防潮性、粘附性和可剥离性较差，容易断裂，效果不理想。
发明内容
本发明旨在提供一种液晶电路保护用组合物。
本发明为实现上述目的，采取以下技术方案予以实现：
一种液晶电路保护用组合物，由以下重量份的组分组成：氢化苯乙烯-丁二烯嵌段共聚物和石油树脂(以下简称SEBS)10～30份、氮化硼0.5～3.6份、环烷油10～20份、主溶剂和辅助溶剂60～70份、含氟助剂0.3～1份。
优选地，所述含氟助剂为含氟硅氧烷偶联剂。本发明的液晶电路保护用组合物所形成的膜是不可湿润的，加入含氟硅氧烷偶联剂后可使总平均接触角迅速增大，从而大大地提高体系的疏水性能，从而增加了制成膜的可剥性。
优选地，所述辅助溶剂为三甲酮醇、丙烯酸羟丙酯中的一种或者两种混合物，所述主溶剂优选为所述主溶剂为甲基环己烷、环己烷或正己烷。加入三甲酮醇、丙烯酸羟丙酯后可使SEBS的甲基环己烷溶液的粘度下降明显，以改善操作性能。
优选地，所述液晶电路保护用组合物还包括不超过0.5重量份的蓝色染料。这样可以调节所制成的薄膜的颜色。
本发明的另一目的在于公开上述液晶电路保护用组合物的制备方法，包括以下步骤：
S 1：按所述重量份，将氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向辅助溶剂和主溶剂的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入其他原料，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
BN是一种人工合成的非氧化物陶瓷材料，它和C2是等电子体，因此和碳单质具有相似的晶体结构，BN特性也有很多，具有抗热振、耐高温、高导热率、抗氧化、高电阻率、高介电性能、自润滑、低密度、耐化学腐蚀、良好的加工性、与多种金属不浸润等优良的物理化学特性。将BN加入到复合材料中不仅可以充分发挥BN陶瓷的优势，同时可以弥补单相BN陶瓷材料机械性能偏低、抗雨蚀性差，得到具有优异综合性能的抗氧化涂层、导热耐热复合材料。
环烷油可以用于提高体系的透光性能，增加体系的透明度。加入增塑剂后可降低SEBS的熔融粘度，利于涂布工艺；增加SEBS的初粘性并改善低温柔软性；并降低成本。
石油树脂起到增粘作用。由于SEBS本身无粘接性，加入石油树脂后可提高内聚力、剥离强度和剪切强度，增加永久粘接强度，降低混合物的熔体粘度，提高被粘材料的浸润性，改善操作性能。
本发明的液晶电路保护用组合物所需原料易得，在均相物质中加入非均相的物质生产界面，该界面在受到外力冲击时会吸收能力，因此提高了强度，工艺流程简单，性价比高。所使用的溶剂跟助剂环保无毒，生产高效安全，边角余料可回收利用而不影响产品的性能，顺应绿色环保潮流。制得的保护用组合物膜具有以下优点：1、良好的成膜性、适度的柔韧性。2、机械强度优良，耐大气性能卓越。3、良好的阻隔性，制成的薄膜具有优越的防潮性能。
具体实施方式
本发明实施例中，氢化苯乙烯-丁二烯嵌段共聚物(SEBS)购自台橡(上海)实业有限公司，型号为Kraton G 1650；硅烷偶联剂购自广州市中杰化工科技有限公司，型号为KH-550；石油树脂购自青岛伊森化学有限公司，型号为LH100-1；甲基环己烷购自广州柏延化工有限公司；环烷油购自广州市彬豪化工有限公司。
本发明实施例中，粘度测试按照国标GB12005.1-89进行；力学性能的测定按照国标GB/T528-2009进行；扭矩测试为对样品进行压膜制样后用扭矩测试仪进行；红外光谱分析按照GBT21186-2007傅立叶变换红外光谱仪进行。
以下结合具体实施例来对本发明作进一步的说明。
实施例1
将SEBS溶于甲基环己烷，制成2g/dl的溶液，测得流出时间t0＝147.50s，取出0.01ml，共取10份，向各份中分别滴加乙酸乙酯、乙酸异丁酯、三甲酮醇、甲苯、丙烯酸羟丙酯、丙烯酸丁酯6种不同溶剂，每种溶剂由0.01mL滴加到0.07mL，每次增加0.01mL，测得到各组溶液的平均流出的时间，并根据下式求出溶液的流出时间变化量，其中，
为平均流出时间，t0为147.50s，r为流出时间的变化量。结果如表1所示。
<表1>
可以得出，在SEBS的甲基环己烷溶液中加入三甲酮醇或者丙烯酸羟丙酯后，溶液的粘度下降明显，说明这三种液体适合作为该体系的溶剂；而乙酸乙酯、乙酸异丁酯或者丙烯酸丁酯加入后，混合体系粘度变化不大，不适合作为基础溶液的溶剂；另外，加入甲苯后，混合体系粘度反而增大，起不到降粘作用，更加说明这几类溶液不适合作为基础溶液的溶剂。
实施例2
将石油树脂以不同的比例加入SEBS的甲基环己烷溶液中，测试制得的溶液成膜后的力学性能，结果如表2所示。可以得出，随着石油树脂用量的增大，样品断裂总伸长率增大，拉伸强度减小，弹性模量减小，最大拉伸应力减小。一方面是石油树脂的相对分子质量相对橡胶较低，石油树脂分子夹杂在橡胶分子链间起润滑作用，易于链的伸展和运动；另一方面是由于树脂分子链为线形，受到外力易于伸展取向。SEBS与石油树脂共混后变得软而韧，该种混合物成膜以后具有柔韧性强，抗刮性能好和易于整体剥离等优良性能。
<表2>
实施例3
将环烷油以不同的比例加入SEBS的甲基环己烷溶液中，测试制得的溶液成膜后的力学性能，结果如表3所示。可以得出，加入环烷油后，弹性模量、最大拉伸应力、拉伸强度、断裂总伸长率均减小。当环烷油的加入量从0增大到25％时，SEBS的最大拉伸应力，拉伸强度，弹性模量下降的幅度较大，断裂总伸长率缓慢下降；当环烷油的加入量大于25％时，SEBS的断裂总伸长率从9.3％骤降到6.09％，最大拉伸应力、弹性模量跟拉伸强度呈缓慢下降趋势。
<表3>
实施例4
本实施例的液晶电路保护用组合物由以下步骤制得：
S1：将10g氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向40g三甲酮醇和30g甲基环己烷的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入16g石油树脂、10g环烷油、0.3g KH-550型硅烷偶联剂、0.5g氮化硼，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
实施例5
本实施例的液晶电路保护用组合物由以下步骤制得：
S1：将10g氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向30g丙烯酸羟丙酯和30g环己烷的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入20g石油树脂、20g环烷油、1g KH-550型硅烷偶联剂、1.7g氮化硼，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
实施例6
本实施例的液晶电路保护用组合物由以下步骤制得：
S1：将10g氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向35g三甲酮醇和30g环己烷的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入14g石油树脂、15g环烷油、0.6g KH-550型硅烷偶联剂、2.6g氮化硼、0.5g蓝色染料，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
实施例7
本实施例的液晶电路保护用组合物由以下步骤制得：
S1：将10g氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向30g三甲酮醇和35g正己烷的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入10g石油树脂、13g环烷油、0.7g KH-550型硅烷偶联剂、1.5g氮化硼、0.08g蓝色染料，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
实施例8
本实施例的液晶电路保护用组合物由以下步骤制得：
S1：将10g氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向32g三甲酮醇和35g正己烷的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入15g石油树脂、18g环烷油、0.9g KH-550型硅烷偶联剂、3.6g氮化硼、0.08g蓝色染料，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
对比例1
本实施例的液晶电路保护用组合物由以下步骤制得：
S1：将10g氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向30g丙烯酸羟丙酯和30g环己烷的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入20g石油树脂、20g环烷油、1g KH-550型硅烷偶联剂、搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
对比例2
本实施例的液晶电路保护用组合物由以下步骤制得：
S1：将10g氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向30g丙烯酸羟丙酯和30g环己烷的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入20g石油树脂、20g环烷油、1g KH-550型硅烷偶联剂、1.7g硅酸铝(Al2SiO5)，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
效果实施例
将实施例5、对比例1和对比例2的组合物制成薄膜，然后封住装有变色硅胶的瓶子，放置150天，观察瓶中变色硅胶的颜色变化，结果如表4所示。
表4无机填料对保护膜水蒸气阻隔性的影响
通过表4可以看出，未增强的SEBS薄膜对自然条件下的水蒸气阻隔性较差，30天内，已有少量水蒸气透过薄膜进入瓶内，硅胶颜色由深蓝变为蓝，90天后，进入瓶内的水蒸气增多，硅胶变为浅蓝色，到150天时，硅胶由原来的深蓝变为浅紫红，说明薄膜的水蒸气透过性好，不利于起到阻隔保护的作用。当加入填料增强后，薄膜的水蒸气阻隔性明显变好，加入硅酸铝后，经过90天，硅胶颜色才由深蓝变为蓝，150天后变为浅蓝，与原来相比，硅胶颜色变化时间增加，说明大大提升了材料的阻隔性；而当加入氮化硼后，薄膜的阻隔性得到了更为显著的提升，硅胶从深蓝变为蓝，经过了150天的长时间跨度，效果比前两者都要好。这主要得益于氮化硼特殊的纳米片状结构，经表面化学修饰改性后，加入到体系中与SEBS进行有机-无机杂化，依靠其片层结构所表现出来的阻隔性大大降低材料对湿气的透过率。由于氮化硼的直径非常小，达到纳米级别，填充到高聚物材料中会利用其纳米效应提高材料的综合性能。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内限制本发明之权利范围。
Claims (3)
1.一种液晶电路保护用组合物，其特征在于包括以下重量份的组分：氢化苯乙烯-丁二烯嵌段共聚物和石油树脂10～30份、氮化硼0.5～3.6份、环烷油10～20份、主溶剂和辅助溶剂60～70份、含氟助剂0.3～1份，所述含氟助剂为含氟硅氧烷偶联剂，所述主溶剂为甲基环己烷、环己烷或正己烷，所述辅助溶剂为三甲酮醇、丙烯酸羟丙酯中的一种或者两种混合物。
2.根据权利要求1所述的一种液晶电路保护用组合物，其特征在于：所述液晶电路保护用组合物还包括不超过0.5重量份的蓝色染料。
3.根据权利要求1或2所述的一种液晶电路保护用组合物的制备方法，其特征在于包括以下步骤：
S1：将氢化苯乙烯-丁二烯嵌段共聚物在65～75℃下干燥4小时以上；
S2：搅拌下向辅助溶剂和主溶剂的混合溶剂中加入经步骤S1处理的氢化苯乙烯-丁二烯嵌段共聚物；
S3：向步骤S2制得混合物中加入其他原料，搅拌至均匀；
S4：滤去不溶物，脱泡后分装。
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