CN113563708B - 一种应用于户外的聚碳酸酯实心板及其制备方法 - Google Patents
一种应用于户外的聚碳酸酯实心板及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种应用于户外的聚碳酸酯实心板及其制备方法，实心板表面含组合物薄膜层，组合物薄膜层主要包括异山梨醇基聚碳酸酯、含硅聚碳酸酯共聚物、光稳定剂、紫外线吸收剂、碳纳米管、纳米红外线吸收剂、抗氧剂、润滑剂和色粉。应用本发明的聚碳酸酯实心板具有长期的紫外线稳定性、耐水解、抗氧化，同时能阻隔紫外线、红外线、氧气和水气，具有出色的耐磨性能，在非常严苛的户外环境下，形成的薄膜层能保持厚度和性能的稳定，从而确保聚碳酸酯实心板长期保持颜色和机械性能稳定性。
Description
技术领域
本发明属于聚碳酸酯材料领域，特别涉及一种应用于户外的聚碳酸酯实心板及其制备方法。
背景技术
聚碳酸酯是一种性能非常优异的透明工程塑料，具有高达90％的可见光透光率和极高的清晰度，具有优异的抗冲性能，其冲击强度是玻璃的250倍以上，密度是玻璃的1/2，同时聚碳酸酯满足GB8624 B1、EN13501 Class B、ASTM E84等国内外的建筑阻燃标准，能在-40℃-120℃的温度范围内，保持性能稳定，其优异的综合性能，使其广泛应用于建筑采光、农业温室、交通隔音屏等行业。
众所周知，在户外环境下，紫外线、雨水、氧、热、风沙等因素会导致聚碳酸酯发生分子链重排、断裂，从而导致聚碳酸酯发生黄变和机械性能损失，影响产品使用寿命。通常应用于户外的聚碳酸酯实心板采用了共挤UV涂层的方式，使其有效使用寿命在10年-20年。专利CN108912372A采用了纳米紫外线吸收剂复合涂层共挤的方式，实现对紫外线的完全阻隔，但表面UV保护层的基材本体是普通的聚碳酸酯树脂，在长期的户外恶劣环境，特别是有风沙环境，UV保护层与风沙摩擦后，厚度会逐渐变薄，从而逐渐减弱保护基材的功能。专利CN112606502A采用了高耐候的聚氨酯作为保护层，通过模内熔融复合的工艺，实现三层共挤，保护UV层和基材，大幅度延长了产品的使用时间，但存在生产工艺复杂，产品成品率较低的缺点，合格成品率只有70％。现有技术普遍性的问题是均没有涉及如何阻隔水气、氧、热对材料的破坏。
为了克服现有技术的不足，进一步提高聚碳酸酯材料在户外的稳定性，有必要开发一种生产效率更高，同时使用寿命更长的聚碳酸酯产品。
发明内容
本发明所要解决的技术问题是提供一种应用于户外的聚碳酸酯实心板及其制备方法，使用的组合物薄膜层进一步提高聚碳酸酯材料在户外的稳定性。
本发明提供了一种应用于户外的聚碳酸酯实心板，所述实心板表面含组合物薄膜层；组合物薄膜层按质量百分比，由如下组分组成：
异山梨醇基聚碳酸酯是含异山梨醇重复单元的聚合物，可按照CN108727578A等公布的方法制备，可以是异山梨醇聚碳酸酯均聚物，也可以是异山梨醇-双酚的共聚物；聚合物的分子量采用渗透凝胶色谱测试，分子量Mw在10000-100000，优先Mw在15000-50000，最优选在15000-35000；聚合物中异山梨醇重复单元的摩尔比10％-100％，优选30-100％，最优选在50-100％；异山梨醇单元由于是饱和脂环式氧结构，相比双酚A型聚碳酸酯，具有更加优异的耐热、耐光和表面硬度；可选自三菱化学株式会社的DURABIO系列。
含硅聚碳酸酯共聚物是含有PDMS(聚二甲基硅氧烷)与BPA(双酚A)的共聚物，可按照CN108350263A等公布的方法制备，聚合物的分子量采用渗透凝胶色谱测试，分子量Mw在10000-100000，优先Mw在15000-50000，最优选在15000-35000；聚合物中聚硅氧烷重复单元的摩尔比0.5％-50％，优选2-30％，最优选在3-15％，相比双酚A型聚碳酸酯，具有更加优异的耐光、耐氧、耐水解、耐化学品腐蚀和耐磨性。比如PC-PDMS Copolymer"TARFLON NEO，LEXANTM_Copolymer_EXL系列。
所述光稳定剂为受阻胺光稳定剂HALS，为低碱性产品，能有效地捕捉自由基，阻断聚合物降解进程，同时不会导致产品降解。
所述紫外线吸收剂为二苯甲酮类紫外线吸收剂、苯并三唑类紫外线吸收剂、三嗪类紫外线吸收剂、水杨酸类紫外线吸收剂中的一种或者几种。，优选分子量Mn≥300的，Tinuvin329、Tinuvin234、Uvinul 3030、Cyasorb UV-3638等，或同类分子结构产品，它能完全吸收紫外线，通过自身结构的可逆重排，将紫外线转化为无害的热能散发除去，同时保护表面层和中间的聚碳酸酯基材。
所述抗氧剂为位阻酚类抗氧剂、亚磷酸酯类抗氧剂、硫代酯类抗氧剂中的一种或几种。比如：1010，1076，168，S-9228等。抗氧剂能有效捕获自由基，并分解过氧化物，从而抑制聚合物的热氧老化进程，在组合物的制备、板材生产和长时间户外环境下，起到长效抗氧化的功能。
所述碳纳米管采用单壁或者多壁碳纳米管，碳纳米管具有优异的吸收全光谱光线的能力，碳纳米管由六边形组成的蜂窝状结构，具有出色的耐磨性和机械强度，能增强组合物的耐磨性能。碳纳米管采用市售的产品。
所述润滑剂为硬脂酸酯类润滑剂或硅氧烷化合物，如常见的PETS EBS硅酮粉等等。
所述纳米红外线吸收剂为氧化钨纳米分散体或钨酸盐纳米分散体。添加一定浓度的红外线吸收剂，屏蔽红外线对基材树脂的影响，可参考EP1847635公布的方法获取。
本发明还提供了一种应用于户外的聚碳酸酯实心板的制备方法，包括：
将碳纳米管、纳米红外线吸收剂、抗氧剂、润滑剂和部分含硅聚碳酸酯共聚物混合，通过熔融混炼设备挤出造粒，制得母粒；将母粒、异山梨醇基聚碳酸酯、另一部分含硅聚碳酸酯共聚物、光稳定剂、紫外线吸收剂、色粉混合，通过熔融混炼设备挤出造粒，制得组合物薄膜层；将组合物薄膜层涂覆于聚碳酸酯实心板基材上，即得。
所述聚碳酸酯实心板基材，采用普通的聚碳酸酯树脂制备，包括不限于芳香族聚碳酸酯，异山梨醇基聚碳酸酯、含硅聚碳酸酯共聚物，高耐热聚碳酸酯共聚物等；根据渗透凝胶色谱分析，分子量Mw 10000-100000优先选择Mw 15000-60000，最优先选择Mw15000-40000，依据ISO 1133-2011,300℃1.2Kg条件下，熔指范围1-15g/10min。
所述聚碳酸酯实心板基材，采用已知成熟的多层共挤实心板生产系统，模具出口为光滑的平面，组合物材料颗粒加入板材线1号挤出机配料系统，机筒温度200-300℃；组合物材料颗粒加入板材线2号挤出机配料系统，机筒温度200-300℃；主体层材料树脂颗粒加入板材线3号挤出机配料系统，机筒温度230-330℃；三种原料分别经过熔化后，通过三个独立流道，在模具中进行熔体的均匀复合，形成表面均为组合物覆盖的实心板。通过控制1号和2号挤出机的产量，调整表面薄膜层的厚度，薄膜层的厚度调整到80μm及以上。通过三辊压光机、牵引导辊、退火系统、除静电、覆膜、切割和码垛系统，制备实心板成品。
有益效果
(1)本发明的户外聚碳酸酯实心板具有长期的紫外线稳定性、耐水解、抗氧化，同时能阻隔紫外线、红外线、氧气和水气，同时具有出色的耐磨性能，在非常严苛的户外环境下，形成的薄膜层能保持厚度和性能的稳定，从而确保聚碳酸酯实心板长期保持颜色和和机械性能稳定性。
(2)本发明组合物采用了异山梨醇基聚碳酸酯，相比芳香族聚碳酸酯，提高产品的耐光性、耐刮擦性，避免了表面UV保护层厚度减薄；
(3)本发明组合物采用了含硅聚碳酸酯共聚物，由于含硅聚碳酸酯具有疏水的功能，减少了水气渗透，提升了产品的抗氧性、耐光性，耐水解性。同时提升了耐刮擦性，避免了表面UV保护层厚度减薄；
(4)本发明相对聚氨酯涂层提高表面耐刮擦性能，生产工艺更易实现，提高了生产效率，产品成品率达到95％；
(5)本发明通过碳纳米管、纳米红外线吸收剂、紫外吸收剂、光稳定剂、抗氧剂的有效组合，进一步提升了组合物的性能，提升了对聚碳酸酯基材的保护效能。
附图说明
图1为薄膜层厚度变化趋势；
图2为双85湿热老化后冲击强度变化趋势；
图3为氙灯老化后冲击强度变化趋势；
图4为氙灯老化后透光率变化趋势；
图5为氙灯老化后YI值变化趋势。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例和对比例中原料和来源如下：
异山梨醇基聚碳酸酯：DURABIOTM系列，如D7340R、D5380R，三菱化学株式会社；
含硅聚碳酸酯共聚物：Lexan EXL系列，如1414T，1434T，1433T，SABIC-IP(SABICInnovative Plastics)制造；
光稳定剂：受阻胺光稳定剂HALS，科莱恩或者BASF；
紫外线吸收剂：Tinuvin 329、Tinuvin 234、Uvinul 3030，BASF SE；
抗氧剂：抗氧剂1010，抗氧剂168，BASF SE；
润滑剂：PETS，LONZA或者Faci；
碳纳米管：FT6000、FT7000、FT9000，江苏天奈科技；
纳米红外线吸收剂：纳米氧化钨，纳米氧化铟；
色粉：无机群青蓝。
组合物的制备方法包括：
将碳纳米管、纳米红外线吸收剂、抗氧剂、润滑剂和部分含硅聚碳酸酯共聚物在高混机中混合5分钟，采用失重式喂料系统下料，喂料速度为200kg/h，采用直径为52mm的双螺杆挤出机将混合物进行熔融挤出造粒，挤出机机筒各段温度为200-260℃，螺杆转速450rpm，真空度≤-0.6MPa，制得母粒；将母粒、异山梨醇基聚碳酸酯、另一部分含硅聚碳酸酯共聚物、光稳定剂、紫外线吸收剂、色粉混合，在高混机中混合5分钟，采用失重式喂料系统下料，喂料速度为200kg/h，采用直径为52mm的双螺杆挤出机将混合物进行熔融挤出造粒，挤出机机筒各段温度为210-270℃，螺杆转速450rpm，真空度≤-0.6MPa制得组合物薄膜层。
采用双酚A型聚碳酸酯作为基材，制备表面薄膜层分别为实施例和对比例组合物的实心板，厚度为8mm，薄膜层厚度调整为80μm厚度，制备方法包括：
采用三层共挤实心板生产系统制备三层共挤实心板，每层由独立的单螺杆挤出级输送熔体，熔体经过独立的流道，在T型开口的模具内部复合成三层结构。实心板两个表面分别为上表面和下表面，上表面和下表面材料，分别通过1号挤出机和2号挤出机输送，材料均为制备的组合物，螺杆直径为45mm，挤出机各段温度范围为220℃-260℃，螺杆转速为20rpm。实心板中间层通过3号挤出机输送，材料为双酚A型聚碳酸酯，螺杆直径为120mm，挤出机各段温度范围为230℃-270℃，螺杆转速为30prm。三层复合熔体从T型开口模具出口流出后，通过三辊压光机、牵引导辊、冷却退火装置、除静电装置、覆膜、切割和码垛，制备得实心板产品。
测试方法：
1.薄膜层厚度：采用高分辨率显微镜观察并测量表面层的厚度，精确到1μm，单位为μm；
2.耐化学品性能：依据ASTM D 543-95标准要求，采用1％NaOH溶液，弯曲应变1％，放置于50％RH、23℃的环境下，观察弯曲后实心板的变化情况，记录样条开裂时间；
3.冲击强度：依据ISO 179，采用实心板制备测试样条，使用简支梁冲击仪测试产品的冲击强度值；冲击强度保留率＝(老化后的冲击强度/初始冲击强度)×100％，冲击强度下降率＝(冲击强度保留率-1)×100％
4.拉伸强度：依据ISO 527，采用实心板制备测试样条，使用万能试验机测试拉伸强度和断裂伸长率；拉伸强度保留率＝(老化后的拉伸强度/初始拉伸强度)×100％，拉伸强度下降率＝(拉伸强度保留率-1)×100％
5.透光率：依据ASTM D1003，采用实心板制备测试样片，使用积分球式透光率雾度仪测试透光率；透光率下降值＝老化后的透光率-初始透光率
6.黄度指数YI值：依据ASTM E313-20标准，使用爱色丽分光光度仪，测试产品的黄度指数；YI值变化＝老化后的YI值-初始的YI值-
7.氙灯老化：依据ISO 4892标准，采用氙灯加速老化，采用Cycle 1的条件，连续老化10000h后观察表面层的情况，判断表层是否出现开裂、脱落等失效现象；
8.湿热老化：依据GB-T2423.3-2006，采用双85测试条件，在85％RH、85℃的恒温恒湿老化箱中老化1000h，观察外观，测试冲击强度、拉伸强度变化。
表1实施例和对比例材料配方
| 项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 对比例1 | 对比例2 | 对比例3 |
| 原料 | 配方1 | 配方2 | 配方3 | 配方4 | 配方5 | 配方6 | 配方7 | 配方8 |
| 异山梨醇基聚碳酸酯 | 26.35 | 51.35 | 66.35 | 66.05 | 65.35 | 96.35 | ||
| 含硅聚碳酸酯共聚物 | 70 | 45 | 30 | 30 | 30 | 96.35 | ||
| 双酚A型聚碳酸酯 | 93.35 | |||||||
| 抗氧剂1010 | 0.15 | 0.15 | 0.15 | 0.15 | 0.15 | 0.15 | 0.15 | 0.15 |
| 抗氧剂168 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| 润滑剂PETS | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| 紫外线吸收剂 | 2 | 2 | 2 | 2 | 2 | 2 | 2 | 2 |
| HALS | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| 碳纳米管 | 0.3 | 0.3 | 0.3 | 0.3 | 1 | 0.3 | 0.3 | 0.3 |
| 纳米红外线吸收剂 | 0.2 | 0.2 | 0.2 | 0.5 | 0.5 | 0.2 | 0.2 | 0.2 |
| 无机群青蓝 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
表2实心板数据对比
实施例和对比例经过多项对比测试，可以明显看出采用本发明中的组合物薄膜层作为表面层材料，可以大幅度提升产品的性能稳定性。
Claims (8)
1.一种应用于户外的聚碳酸酯实心板，其特征在于：所述实心板表面含组合物薄膜层；组合物薄膜层按质量百分比，由如下组分组成：
异山梨醇基聚碳酸酯 26.35%；
含硅聚碳酸酯共聚物 70%；
光稳定剂 0.2%-3%；
紫外线吸收剂 0.2%-15%；
抗氧剂 0.1%-1%；
润滑剂 0.1%-1%；
碳纳米管 0.1%-5%；
纳米红外线吸收剂 0.1%-5%；
色粉 0.001%-0.1%。
2.根据权利要求1所述的实心板，其特征在于：所述异山梨醇基聚碳酸酯的分子量Mw在10000-100000，其中异山梨醇重复单元的摩尔比为10%-100%；所述含硅聚碳酸酯共聚物的分子量Mw在10000-100000，其中聚硅氧烷重复单元的摩尔比0.5%-50%。
3.根据权利要求1所述的实心板，其特征在于：所述光稳定剂为受阻胺光稳定剂HALS。
4.根据权利要求1所述的实心板，其特征在于：所述紫外线吸收剂为二苯甲酮类紫外线吸收剂、苯并三唑类紫外线吸收剂、三嗪类紫外线吸收剂、水杨酸类紫外线吸收剂中的一种或者几种。
5.根据权利要求1所述的实心板，其特征在于：所述抗氧剂为位阻酚类抗氧剂、亚磷酸酯类抗氧剂、硫代酯类抗氧剂中的一种或几种。
6.根据权利要求1所述的实心板，其特征在于：所述润滑剂为硬脂酸酯类润滑剂或硅氧烷化合物。
7.根据权利要求1所述的实心板，其特征在于：所述纳米红外线吸收剂为氧化钨纳米分散体或钨酸盐纳米分散体。
8.一种如权利要求1所述的应用于户外的聚碳酸酯实心板的制备方法，包括：
将碳纳米管、纳米红外线吸收剂、抗氧剂、润滑剂和部分含硅聚碳酸酯共聚物混合，通过熔融混炼设备挤出造粒，制得母粒；将母粒、异山梨醇基聚碳酸酯、另一部分含硅聚碳酸酯共聚物、光稳定剂、紫外线吸收剂、色粉混合，通过熔融混炼设备挤出造粒，制得组合物薄膜层；将组合物薄膜层涂覆于聚碳酸酯实心板基材上，即得。
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Denomination of invention: A polycarbonate solid board for outdoor use and its preparation method Granted publication date: 20230505 Pledgee: Societe Generale Bank Co.,Ltd. Qingpu Branch of Shanghai Pledgor: Shanghai Pincheng Holding Group Co.,Ltd. Registration number: Y2024980016352 |