CN104629366A - 一种有机硅增韧改性的聚苯硫醚材料及其制备方法 - Google Patents
一种有机硅增韧改性的聚苯硫醚材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种有机硅增韧改性的聚苯硫醚材料及其制备方法。该发明材料是一种经硅烷偶联剂KH-560接枝改性后的SiO2纳米粒子填充玻纤增强有机硅接枝聚苯硫醚体系的改性材料。制备该材料的技术工艺的创新性体现在：首先通过超声分散、搅拌反应、离心分离处理的方式将KH-560接枝在SiO2粒子表面，制备表面疏水的纳米SiO2，然后利用悬浮接枝与硅烷交联技术将有机硅单体接枝于聚苯硫醚上，进而与其它助剂组成配方体系通过双螺杆挤出机共混挤出，经牵条、冷却、切粒后得到增强增韧的改性聚苯硫醚材料。改性后的材料具有较高的拉伸强度、弯曲强度的同时，具有较高的冲击韧性，与纯PPS相比大大提高。
Description
技术领域
本发明涉及高分子材料领域，具体涉及一种有机硅增韧改性的聚苯硫醚材料及其制备方法，广泛用于电子电气工业、汽车工业、机械工业、军工国防领域。
背景技术
聚苯硫醚(PPS)是一种半结晶性热塑性特种工程塑料，它的分子主链是由苯环与硫原子交替排列，分子链的规整性强，苯环提供刚性，硫醚键提供柔顺性，由于分子主链具有刚柔兼备的特点，所以聚苯硫醚易于结晶，结晶度最高可达75%。聚苯硫醚树脂呈白色或近白色，是一种硬而脆的聚合物，吸湿率很低，只有0.03%。密度为1.34g/cm3，熔点为285℃，玻璃化转变温度在90℃左右，热稳定性突出，空气中在430℃～460℃以上才开始分解。在氮气中，500℃以下加热没有明显的质量损失。阻燃等级为U-94V-O级，200℃以下不溶于绝大多数有机溶剂，且电绝缘性非常好。
由于聚苯硫醚综合性能优异，在电子电气工业、汽车工业、机械工业、军工国防领域有这重要的应用，但其也存在不足之处，其力学强度不高，其拉伸强度、弯曲强度属中等水平，尤其聚苯硫醚的脆性较大，韧性较差，这会在一定程度上阻碍了该聚合物在市场上的广泛应用，解决聚苯硫醚的脆性问题是目前聚苯硫醚改性研究中最重要的目标。随着各行各业的不断发展以及高性能材料市场的不断开拓，对特种工程材料提出的要求会越来越高，尤其是一些尖端领域、国防军工等。因此，提高聚苯硫醚的韧性对于其今后在市场上更好更广泛地被使用具有十分重要的意义。
发明内容
本发明制备了一种有机硅增韧改性的聚苯硫醚材料，目的是在提高聚苯硫醚的拉伸强度、弯曲强度的同时，也具有较高的韧性。首先将硅烷偶联剂KH-560接枝在SiO2粒子表面，得到表面疏水的纳米SiO2，然后利用悬浮接枝与硅烷交联技术将有机硅单体接枝于聚苯硫醚上，进而与其它助剂组成配方体系通过双螺杆挤出机共混挤出，经牵条、冷却、切粒后得到增强增韧的改性聚苯硫醚材料。本发明的改性方法与传统的聚苯硫醚改性方法略有不同，是通过化学结构改性的方法制备出了一种韧性有所改善的新型聚苯硫醚材料，经硅烷偶联剂KH-560接枝处理过的SiO2纳米粒子表面存在Si-O基团能够与有机硅接枝改性的PPS表面的Si-O基团发生耦合，使制备的改性材料具有较高的拉伸强度、弯曲强度的同时，具有较高的冲击韧性。
技术方案：
步骤一：称取一定量纳米SiO2，加入一定体积的甲苯，常温超声波清洗器(300W)超声分散30min，得到均匀悬浮液，再向其中加入硅烷偶联剂KH-560，继续超声3～4min，转移到装有回流冷凝管、增力电动搅拌100mL四颈烧瓶中，于设定好的油浴温度中进行搅拌反应一定时间。反应后的浆液用台式高速冷冻离心机以12000r/min的速度常温离心分离,得到改性纳米SiO2。改性纳米SiO2超声分散、离心分离6次。将改性纳米SiO2置于真空干燥箱中，常温干燥8h～10h，得到制备好的改性纳米SiO2白色粉末。
步骤二：将已经干燥的PPS粉悬浮分散于二氯甲烷中进行预溶胀一段时间，在Al2O3的作用下，加入乙酰氯，待反应结束，将反应液移入冰盐酸中进行分解，抽滤，先用低浓度的NaOH溶液洗涤，之后用去离子水和乙醇反复洗涤，80～100℃真空干燥20～30h，得到乙酰化聚苯硫醚。在氮气保护下，将乙酰化聚苯硫醚分散于无水甲苯中，缓慢加入硅烷偶联剂，反应8～12h，抽滤，洗涤，并用乙醇溶液索式抽提20～30h，80～100℃下真空干燥至恒重，得到有机硅接枝改性的聚苯硫醚。最后将有机硅接枝改性的聚苯硫醚进行水解交联，抽滤，产物在80～100℃下真空干燥。
步骤三:将上述配方中的各组分按配比在高速混合机中混合均匀，将混合的物料加入到双螺杆挤出机中进行熔融挤出。
挤出温度范围为285～310℃；主机转速为400～600rpm；喂料转速为20～30rpm。
挤出的混合物经水冷、造粒后在真空干燥箱中烘干，然后将烘好的共混物在290～320℃下注塑成标准样条。
具体实例：
下面结合具体实施例对本发明进一步详细说明，但本发明并不局限于以下实施各例：
本实施方式均使用科倍隆双螺杆挤出机和海天注塑机，主要原料聚苯硫醚，工业级（四川得阳）；GF，工业级（巨石集团）；硅烷偶联剂使用KH-560，工业级（市售）；二氧化硅（比表面积150m2/g，广州吉必时科技事业有限公司）；甲苯（AR，天津市大茂化学试剂厂）；抗氧剂包括1010、168（利安隆）。
双螺杆挤出机料筒温度一区温度：260～275℃，二区温度：280～290℃，三区温度：280～290℃；四区温度：280～290℃；五区温度：280～290℃；六区温度：280～290℃，压力为10～16MPa，螺杆长径比35～40，主机转速400～600r/min。KH-560的浓度为0.2%，反应温度为90℃，搅拌反应时间为6h。
将各组分按配比混合均匀置于双螺杆挤出中，经熔融混合挤出造粒。所得粒料再经120℃鼓风干燥8～10h，在注塑机上注塑成标准的性能测试样条。
表1 各实施例对应的配方
表2 各实施例样品对应的物理性能
Claims (3)
1.有机硅增韧的聚苯硫醚改性材料的配方组成如下所示：
预处理PPS 60～70%
GF 30～40%
纳米SiO2 0.1～0.5%
助剂 0.1～3%。
2.根据权利要求1所述有机硅增韧的聚苯硫醚改性材料，其特征在于：所述SiO2纳米粒子，经过超声分散，搅拌反应、离心分离处理，使得KH-560接枝在SiO2粒子表面，得到表面疏水的纳米SiO2，SiO2纳米粒子的用量为0.1%～0.5%，KH-560的浓度为0.1%～3%，反应温度为60℃～90℃，搅拌反应时间为6h～10h。
3.根据权利要求1所述有机硅增韧的聚苯硫醚改性材料，其特征在于：所述预处理PPS采用悬浮接枝与硅烷交联技术将有机硅单体（3-氨基丙基三乙氧基硅烷）接枝在聚苯硫醚表面而得。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109423048A (zh) * | 2017-09-04 | 2019-03-05 | 四川鑫达企业集团有限公司 | 一种有机硅增韧改性的聚苯硫醚材料及其制备方法 |
| CN110964321A (zh) * | 2019-12-11 | 2020-04-07 | 西北师范大学 | 一种聚苯硫醚-二氧化硅超疏水复合材料及其制备方法 |
| CN114573984A (zh) * | 2022-03-16 | 2022-06-03 | 四川中科兴业高新材料有限公司 | 一种液体硅胶接枝改性增韧聚苯硫醚及其制备方法 |
| CN117402358A (zh) * | 2023-10-13 | 2024-01-16 | 现代纺织技术创新中心(鉴湖实验室) | 一种改性硅基聚苯硫醚树脂及聚苯硫醚薄膜的制备方法 |
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| CN101717580A (zh) * | 2009-12-30 | 2010-06-02 | 四川华通特种工程塑料研究中心有限公司 | 高性能聚苯硫醚绝缘复合材料及其制备方法 |
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| CN101717580A (zh) * | 2009-12-30 | 2010-06-02 | 四川华通特种工程塑料研究中心有限公司 | 高性能聚苯硫醚绝缘复合材料及其制备方法 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109423048A (zh) * | 2017-09-04 | 2019-03-05 | 四川鑫达企业集团有限公司 | 一种有机硅增韧改性的聚苯硫醚材料及其制备方法 |
| CN110964321A (zh) * | 2019-12-11 | 2020-04-07 | 西北师范大学 | 一种聚苯硫醚-二氧化硅超疏水复合材料及其制备方法 |
| CN110964321B (zh) * | 2019-12-11 | 2022-03-11 | 西北师范大学 | 一种聚苯硫醚-二氧化硅超疏水复合材料及其制备方法 |
| CN114573984A (zh) * | 2022-03-16 | 2022-06-03 | 四川中科兴业高新材料有限公司 | 一种液体硅胶接枝改性增韧聚苯硫醚及其制备方法 |
| CN114573984B (zh) * | 2022-03-16 | 2023-11-03 | 四川中科兴业高新材料有限公司 | 一种液体硅胶接枝改性增韧聚苯硫醚及其制备方法 |
| CN117402358A (zh) * | 2023-10-13 | 2024-01-16 | 现代纺织技术创新中心(鉴湖实验室) | 一种改性硅基聚苯硫醚树脂及聚苯硫醚薄膜的制备方法 |
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