CN102627812B - 一种溴化聚苯乙烯母粒及其制备方法 - Google Patents
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Abstract
本发明公开了一种溴化聚苯乙烯母粒及其制备方法。溴化聚苯乙烯母粒由如下质量百分比的组分所制成：溴化聚苯乙烯85～95％，载体3～14％，改性乙撑双脂肪酸酰胺0.1～5％。本发明制备的溴化聚苯乙烯母粒有效避免了粉体和粒料混合不均匀导致材料质量不稳定的情况；本发明采用密炼-挤出的连续生产工艺，生产效率高，生产成本低，生产清洁，分散效果好，大大提高溴化聚苯乙烯母粒的填充量，混合效果好；本发明制备的溴化聚苯乙烯母粒具有易分散、阻燃效率高、生产成本低的特点，对复合材料的物理机械性能、耐热性能、加工性能和表面色泽的影响都比溴化聚苯乙烯粉体要小。
Description
技术领域
本发明涉及一种溴化聚苯乙烯母粒及其制备方法。
背景技术
阻燃母粒也称阻燃母料、防火母粒。在国外称其为“浓缩物”，意之阻燃剂的浓缩。阻燃母粒产生已经有几十年历史，其最初主要是解决阻燃剂粉料使用过程中分散不均，扬尘污染严重的问题，经过多年的发展，大量科学手段和新型技术的应用，人们对阻燃母粒的研究已经不仅仅局限与分散、防止污染这些常规问题上了。其已经形成一个独立学科并发展成为一个独立的行业。大量的技术研究和应用使阻燃母粒成为高科技、高技术型的产品。
由于塑料中添加的阻燃剂大多为粉体，而且为了获得较佳的阻燃效果和力学性能，粉体的细度一般在800目以上，在称量、混合、造粒过程中容易产生大量的粉尘污染，恶化生产环境，对人体健康造成很大危害，而且会对加工设备造成一定程度的磨损。而如果生产过程中采用母粒做为添加助剂，则可以从根本上解决此问题。
溴化聚苯乙烯作为阻燃剂，具有阻燃性高，流动性好的优点，广泛应用在PBT、PET等工程塑料中。长期以来，关于溴化聚苯乙烯母粒的研究主要侧重于以下几个方面：①尽可能提高母粒中溴化聚苯乙烯的含量，使其能等量替换溴化聚苯乙烯粉体；②采用聚乙烯蜡或聚乙烯蜡和扩散油做为载体，使其能应用于多种通用塑料和工程塑料； ③采用高速搅拌机搅拌，然后经双螺杆挤出机造粒。目前的这些研究主要还存在以下不足：①阻燃母粒与阻燃剂粉体达到等效的情况下，需要增加阻燃母粒的添加量，而且阻燃母粒由于要经过挤出造粒的工序，所以成本较高；②目前采用的加工工艺在高速搅拌过程中依然存在扬尘的情况；③将高搅后的溴化聚苯乙烯粉体直接经双螺杆挤出造粒时由于粉体较细含量较高，下料困难，而且会对机筒和螺杆造成较大的磨损。
发明内容
本发明的目的在于克服现有技术的缺陷和不足，提供一种溴化聚苯乙烯母粒的制备方法。
一种溴化聚苯乙烯母粒，由如下质量百分比的组分所制成：
溴化聚苯乙烯85～95％
载体 3～14％
改性乙撑双脂肪酸酰胺0.1～5％。
其中载体是作为该阻燃母粒的载体，主要作用是把溴化聚苯乙烯粉体粘合起来，以得到颗粒状的溴化聚苯乙烯母料；改性乙撑双脂肪酸酰胺的作用一方面是减少物料与设备之间的磨损，另一方面是提高溴化聚苯乙烯粉体在载体中的分散效果，同时由于具有亲油、亲水性，可以增加溴化聚苯乙烯粉体和载体的相容性，从而提高其界面粘结力，增加复合材料的阻燃性能和物理机械性能。
在上述溴化聚苯乙烯母粒中，所述溴化聚苯乙烯是粉体，其平均粒径为0.03～0.1μm。
在上述溴化聚苯乙烯母粒中，所述载体为聚丙烯，包括均聚聚丙烯（PPH）、嵌段共聚聚丙烯（PPC）、无规共聚聚丙烯（PPR）、三元共聚聚丙烯的一种或两种混合，聚丙烯的熔融指数为10～50g/10min，230℃,2.16KG。
在上述溴化聚苯乙烯母粒中，所述改性乙撑双脂肪酸酰胺是以乙撑双脂肪酸酰胺（EBS）为基料，在催化剂的作用下，含有极性基团的反应性单体与EBS反应形成的BAB型共聚物。
上述溴化聚苯乙烯母粒的制备方法，包括如下步骤：
（1）将上述配方中的溴化聚苯乙烯、载体、改性乙撑双脂肪酸酰胺按配比准确称量；
（2）先将载体、改性乙撑双脂肪酸酰胺加入到加压式翻转密炼机中，控制密炼室内的温度为150～190℃，转子转速为20～80r/min，密炼时间为3～15min，待物料熔融后分三次将溴化聚苯乙烯粉体加入到密炼机中，每次投料间隔2～5min；物料全部加入后再密炼5～15min；
（3）上述密炼后的胶头经传输带输送到单螺杆挤出机的料斗里，经料斗里的切刀切成碎块，然后在重力作用下进入挤出机的机筒，经单螺杆熔融混炼挤出，经风冷磨面切粒制成溴化聚苯乙烯母粒。
在上述制备方法中，所述单螺杆挤出机的长径比为20～55；所述单螺杆挤出机的机筒温度为120～170℃；所述单螺杆挤出机的主机转速300～1000r/min。
本发明与现有技术相比，具有如下积极效果：（1）本发明采用的溴化聚苯乙烯由于其粒度小而具有特殊的延展性能，在阻燃性能方面比溴化聚苯乙烯粉体有了明显的提高，而且对复合材料的力学性能、热性能和各向异性的影响也比溴化聚苯乙烯粉体更小；（2）本发明制备的溴化聚苯乙烯母粒由于是颗粒状，和基础树脂的颗粒尺寸基本一致，所以物料混合均匀，有效避免了粉体和粒料混合不均匀导致材料质量不稳定的情况；（3）本发明选用的母粒载体主要是熔融指数较高的聚丙烯，由于其流动性较好，对粉体的包覆效果非常好，从而避免了切粒时易产生碎屑或粉末的现象，另一方面也提高了生产效率，降低了生产成本；（4）本发明采用密炼-挤出的连续生产工艺，相比传统的先高速搅拌，然后再经双螺杆挤出的工艺相比具有如下优点：一是密炼机和单螺杆挤出机的生产效率高，相同能耗和产量下，生产成本低；二是密炼机熔融共混过程在密闭的腔体中进行，不易扬尘，生产清洁，减少了对工人身体健康的危害，而且分散效果要比双螺杆要好；三是采用密炼机可大大提高溴化聚苯乙烯母粒的填充量，而且混合效果好。（5）本发明制备的溴化聚苯乙烯母粒具有易分散、阻燃效率高、生产成本低的特点，对复合材料的物理机械性能、耐热性能、加工性能和表面色泽的影响都比溴化聚苯乙烯粉体要小。
具体实施方式
实施例1
按以下质量百分比组成进行配比：溴化聚苯乙烯85％（山东寿光光大工贸有限责任公司），均聚聚丙烯（PPH）14％（牌号EP500N，中海壳牌石化公司），改性乙撑双脂肪酸酰胺(EBS)1％（成都同立助剂有限公司）。上述物料准确称量后将PPH、改性乙撑双脂肪酸酰胺加入到加压式翻滚密炼机中，控制密炼室内的温度为150℃，转子转速为40r/min，密炼时间为3min，待物料熔融后分三次将溴化聚苯乙烯粉体加入到密炼机中，每次投料间隔2min；物料全部加入后再密炼15min。上述密炼后的胶头经传输带输送到单螺杆挤出机的料斗里，经料斗内的切刀将胶头切成碎块，控制机筒各段温度为150℃，主机转速800r/min，经单螺杆熔融混炼挤出，然后经风冷磨面切粒制成溴化聚苯乙烯母粒。
实施例2
按以下质量百分比组成进行配比：溴化聚苯乙烯90％（山东寿光光大工贸有限责任公司），均聚聚丙烯（PPH）8.5％（牌号EP500N，中海壳牌石化公司），改性乙撑双脂肪酸酰胺1.5％（市购常规型号）。上述物料准确称量后将PPH、改性乙撑双脂肪酸酰胺加入到加压式翻滚密炼机中，控制密炼室内的温度为160℃，转子转速为40r/min，密炼时间为3min，待物料熔融后分三次将溴化聚苯乙烯粉体加入到密炼机中，每次投料间隔3min；物料全部加入后再密炼10min。上述密炼后的胶头经传输带输送到单螺杆挤出机的料斗里，经料斗内的切刀将胶头切成碎块，控制机筒各段温度为160℃，主机转速700r/min，经单螺杆熔融混炼挤出，然后经风冷磨面切粒制成溴化聚苯乙烯母粒。
实施例3
按以下质量百分比组成进行配比：溴化聚苯乙烯95％（山东寿光光大工贸有限责任公司），无规共聚聚丙烯（PPR）4.5％（牌号EP500N，中海壳牌石化公司），改性乙撑双脂肪酸酰胺0.5％（市购常规型号）。上述物料准确称量后将PPR、改性乙撑双脂肪酸酰胺加入到加压式翻滚密炼机中，控制密炼室内的温度为160℃，转子转速为45r/min，密炼时间为5min，待物料熔融后分三次将溴化聚苯乙烯粉体加入到密炼机中，每次投料间隔5min；物料全部加入后再密炼10min。上述密炼后的胶头经传输带输送到单螺杆挤出机的料斗里，经料斗内的切刀将胶头切成碎块，控制机筒各段温度为160℃，主机转速600r/min，经单螺杆熔融混炼挤出，然后经风冷磨面切粒制成溴化聚苯乙烯母粒。
对本发明制备的溴化聚苯乙烯母粒的效果进行以下对比实验：
表1 材料配方
| 树脂及含量（%） | 玻璃纤维含量（%） | 溴化聚苯乙烯粉体（%） | 溴化聚苯乙烯母粒（实施例1制得）（%） | 溴化聚苯乙烯母粒（实施例3制得）（%） | 三氧化二锑 | |
| 配方1 | PA66-EPR27，41 | 35 | 18 | 6 | ||
| 配方2 | PA66-EPR27，41 | 35 | 18 | 6 | ||
| 配方3 | PA66-EPR27，43 | 35 | 18 | 4 | ||
| 配方4 | PBT1100，57 | 30 | 10 | 3 | ||
| 配方5 | PBT1100，57 | 30 | 10 | 3 | ||
| 配方6 | PBT1100，58 | 30 | 10 | 2 |
表2 阻燃材料性能对比表
从表2的测试结果可以看出，使用等量的本发明制备的溴化聚苯乙烯母粒与溴化聚苯乙烯粉体相比，复合材料的冲击强度、拉伸强度、弯曲强度和模量都略有提升，而且材料的阻燃性能均可以达到UL94V0级，在配方3和配方6中，使用比溴化聚苯乙烯粉体含量低的溴化聚苯乙烯母粒，材料的阻燃性能依然可达V0级，从而降低了材料成本，减少了添加剂对材料综合物理性能的影响。
Claims (3)
1.一种溴化聚苯乙烯母粒，其特征在于由如下质量百分比的组分所制成：
溴化聚苯乙烯85 ～ 95％
载体 3 ～ 14％
改性乙撑双脂肪酸酰胺0.1 ～ 5％；
所述载体为均聚聚丙烯、嵌段共聚聚丙烯、无规共聚聚丙烯、三元共聚聚丙烯的一种或两种混合，聚丙烯的熔融指数为10 ～ 50g/10min，230℃ ,2.16KG；
所述溴化聚苯乙烯母粒通过如下步骤制备得到：
（1）将上述配方中的溴化聚苯乙烯、载体、改性乙撑双脂肪酸酰胺按配比准确称量；
（2）先将载体、改性乙撑双脂肪酸酰胺加入到加压式翻转密炼机中，控制密炼室内的温度为150 ～ 190℃，转子转速为20 ～ 80r/min，密炼时间为3 ～ 15min，待物料熔融后分三次将溴化聚苯乙烯粉体加入到密炼机中，每次投料间隔2 ～5min ；物料全部加入后再密炼5 ～ 15min；
（3）上述密炼后的胶头经传输带输送到单螺杆挤出机的料斗里，经料斗里的切刀切成碎块，然后在重力作用下进入挤出机的机筒，经单螺杆熔融混炼挤出，经风冷磨面切粒制成溴化聚苯乙烯母粒；
所述单螺杆挤出机的长径比为20 ～ 55；
所述单螺杆挤出机的机筒温度为120 ～ 170℃；所述单螺杆挤出机的主机转速300 ～ 1000r/min。
2.如权利要求1 所述的溴化聚苯乙烯母粒，其特征在于，所述溴化聚苯乙烯是粉体，其平均粒径为0.03 ～ 0.1μm。
3.如权利要求1 所述的溴化聚苯乙烯母粒，其特征在于，所述改性乙撑双脂肪酸酰胺是以乙撑双脂肪酸酰胺为基料，在催化剂的作用下，含有极性基团的反应性单体与EBS 反应形成的BAB 型共聚物。
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