CN111117044A - 低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料及其制备方法 - Google Patents
低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料及其制备方法 Download PDFInfo
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Abstract
本发明公开一种低氟化物逸出辐照交联聚乙烯‑四氟乙烯共聚物绝缘料及其制备方法,由以下重量份的组分组成:聚乙烯‑四氟乙烯共聚物100份,滑石粉2~10份,三氧化二锑2~10份,氧化锌2~10份,硬脂酸锌1~5份,羟基‑2‑苯基‑3‑哒酮1~5份,甘油山嵛酸酯3~8份,N,N‑双[β‑(3,5‑二叔丁基‑4‑羟基苯基)丙酰]肼0.1~1份,3‑氨丙基三乙氧基硅烷1~4份,交联剂1~10份。本发明低氟化物逸出辐照交联聚乙烯‑四氟乙烯共聚物绝缘料,能迅速吸收辐照交联ETFE绝缘料经辐照后产生的HF,显著降低HF的逸出量,逸出量小于20ppm,提高辐照交联ETFE的安全、环保性,并且提高了共聚物绝缘料的力学性能。
Description
技术领域
本发明涉及电线电缆绝缘材料,尤其涉及一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料。
背景技术
乙烯-四氟乙烯共聚物(英文简称ETFE)又称F40,透明结晶料,熔点为255~280℃,是最强韧和最轻的氟塑料。ETFE具有优良的介电性、绝缘性能和力学性能,耐辐照,耐开裂,耐老化,耐各种化学溶剂,耐高低温,长期工作温度在-65℃到150℃之间,其比重为1.73g/cm3左右。而ETFE辐照交联后长期工作温度提高到200℃。通常用的辐照交联ETFE绝缘料挤制成线缆后,经过辐照会逸出氟化氢(HF),而HF是一种腐蚀性非常强的酸;在敷设的设备内经过长时间挥发,累积到一定量之后不仅降低设备元器件可靠性,而且会损害人体健康。常用的辐照交联ETFE线缆的氟化物逸出量普遍在200-300ppm, 而低氟化物逸出的辐照交联ETFE线缆氟化物逸出量要小于20ppm,因此低氟化物逸出的辐照交联ETFE绝缘料可以提高更安全、更环保,也是市场发展的主要趋势。
发明内容
本发明的目的是提供一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,能迅速吸收辐照交联ETFE绝缘料经辐照后产生的HF,显著降低HF的逸出量,提高辐照交联ETFE的安全、环保性,并且提高了共聚物绝缘料的力学性能。
为达到上述发明目的,本发明采用的技术方案是:一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,由以下重量份的组分组成:
聚乙烯-四氟乙烯共聚物 100份,
滑石粉 2~10份,
三氧化二锑 2~10份,
氧化锌 2~10份,
硬脂酸锌 1~5份,
羟基-2-苯基-3-哒酮 1~5份,
甘油山嵛酸酯 3~8份,
N,N - 双[β- (3,5-二叔丁基-4-羟基苯基)丙酰]肼 0.1~1份,
3-氨丙基三乙氧基硅烷 1~4份,
交联剂 1~10份。
上述技术方案进一步改进的技术方案如下:
1. 上述方案中,一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,由以下重量份的组分组成:
聚乙烯-四氟乙烯共聚物 100份,
滑石粉 2~5份,
三氧化二锑 2~6份,
氧化锌 1~5份,
硬脂酸锌 1~5份,
羟基-2-苯基-3-哒酮 2~4份,
甘油山嵛酸酯 5~7份,
N,N - 双[β- (3,5-二叔丁基-4-羟基苯基)丙酰]肼 0.1~1份,
3-氨丙基三乙氧基硅烷 1~4份,
交联剂 1~10份。
2. 上述方案中,所述滑石粉为超细滑石粉,所述滑石粉粒径在0.3微米~2微米。
3. 上述方案中,所述三氧化二锑粒径在0.3微米~1.5微米。
4. 上述方案中,所述氧化锌粒径在0.3微米~2微米。
5. 上述方案中,所述的交联剂由组分A和组分B混合而成,所述组分A:组分B的质量比为1:0.1~10,其中组分A符合下述结构通式(1):
其中X为乙烯基、烯丙基、甲代烯丙基或者炔丙基,n=2~15,组分A的重均分子量为600~5000;
所述组分B为三烯丙基异氰酸酯、三甲代烯丙基异氰酸酯、三烯丙基氰酸酯、三甲代烯丙基氰酸酯中的至少一种。
6. 上述方案中,所述交联剂中组分A:组分B的质量比为1:0.3~5。
7. 上述方案中,所述原料配方的辐照交联剂量为5~40兆拉德,优选为10~25兆拉德。
本发明采用的方法技术方案是:一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料的制备方法,包括以下步骤:
第一步,将聚乙烯-四氟乙烯共聚物100份、滑石粉2~10份、三氧化二锑2~10份、氧化锌2~10份、硬脂酸锌1~5份、羟基-2-苯基-3-哒酮 1~5份、甘油山嵛酸酯3~8份、N,N - 双[β-(3,5-二叔丁基-4-羟基苯基)丙酰]肼 0.1~1份、3-氨丙基三乙氧基硅烷 1~4份、交联剂1~10份,按相应的重量份在高速混合机中混合均匀;
第二步,将上述步骤混合均匀的物料,在双螺杆挤出机中挤出造粒,烘干,挤出温度为250-300℃。
由于上述技术方案的运用,本发明与现有技术相比具有下列优点:
1、本发明的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其配方中在添加的滑石粉、氧化锌的基础上,添加了羟基-2-苯基-3-哒酮,能迅速吸收辐照交联ETFE绝缘料经辐照后产生的HF,显著降低HF的逸出量,逸出量小于20ppm,提高辐照交联ETFE的安全、环保性。
2、本发明的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其在绝缘料的羟基-2-苯基-3-哒酮基础上进一步添加甘油山嵛酸酯,能够提高本发明的滑石粉、氧化锌与ETFE树脂的相容性以及滑石粉、氧化锌本身的分散性,使得滑石粉、氧化锌能良好的分散在ETFE中,并且与ETFE结合的比较好,进一步提高了本发明绝缘料的强度。
具体实施方式
下面结合实施例对本发明作进一步描述:
实施例1~4:一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,由以下质量份的组分组成,如表1所示:
表1
实施例1~4中,所述交联剂中组分A与组分B的配比参见表2所示:
表2
一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料的制备方法,包括如下步骤:
第一步,将聚乙烯-四氟乙烯共聚物100份、滑石粉2~10份、三氧化二锑2~10份、氧化锌2~10份、硬脂酸锌1~5份、羟基-2-苯基-3-哒酮 1~5份、甘油山嵛酸酯3~8份、N,N - 双[β-(3,5-二叔丁基-4-羟基苯基)丙酰]肼 0.1~1份、3-氨丙基三乙氧基硅烷 1~4份、交联剂1~10份,按相应的重量份在高速混合机中混合均匀;
第二步,将上述步骤混合均匀的物料,在双螺杆挤出机中挤出造粒,烘干,挤出温度为250-300℃。
对比例1~2:一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,由以下质量份的组分组成,如表3所示:
对比例1~2中,所述交联剂中组分A与组分B的质量比为1:1,其中,组分A的结构通式(1)中的X为烯丙基,组分A的重均分子量为3100,组分B为三烯丙基异氰酸酯。对比例1~2的一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料的制备方法与实施例1~4的制备方法一致,此处不再说明。
将实施例1~4和对比例1~2的一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料进行力学性能测试,具体为:
将氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料粒子在平板硫化机上压片,压片温度290℃,得到的片子厚度为0.5mm。将片子进行辐照,辐照计量15Mrad。将片子进行密度、拉伸性能测试。片子的耐温测试如下:将片子制成标准哑铃片,然后挂在烘箱中,280℃、7个小时。然后拿出来,冷却,测其拉伸强度保留率。
将实施例1~4和对比例1~2的一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料进行氟化物逸出测试,将氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料粒子在平板硫化机上压片,压片温度290℃,得到的片子厚度为0.5mm。将片子进行辐照,辐照计量15Mrad。
将片子进行氟化物逸出测试,步骤如下:
1)取约0.5g左右的片子,长度不超过50mm,称重,精确至0.001g;
2)取一个聚苯乙烯试管(含盖子)也称重,并精确至0.1g。在聚苯乙烯试管内放入大约14mL蒸馏水,并再次称重。将称好的片子放入试管,并完全浸没水中,然后将试管盖盖紧。
3)将试管部分放入(70±2)℃的恒温水浴中,使恒温水浴水面与试管内液面平齐,试管需放置在恒温水浴中168h,并每隔一段时间进行检查,保证试样完全浸没于水中。结束后,将试管从水浴中取出并放置至室温。
4)将试管表面的水分擦拭干净,对试管(含盖)、水和试样进行称重以确定水量损失。如果水质量损失超过0.5g,须重新进行测试。
5)从试管中取5mL水,通过离子色谱仪测试氟化物离子含量,氟化物离子含量应换算成ppm。
空白测试:同绝缘料片子的测试,但是不加入绝缘料片子。仅对试管和蒸馏水进行测试。含片子试样的氟离子测试结果中应减去空白试样测试结果。
F(氟化物逸出量) =C(氟离子净浓度)*W水(水原始重量)/W试(试样重量)
结果如表4。
表4
从表4中性能可以看出,对比例1的氟化物逸出比较低,为11ppm,但其拉伸强度、拉伸强度保留率要比实施例1要低,断裂伸长率比实施例1高;对比例2的氟化物逸出比较高,为65ppm,但其拉伸强度、拉伸强度保留率要比实施例1要低,断裂伸长率比实施例1高。
可见,本发明的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其配方中在添加的滑石粉、氧化锌的基础上,添加了羟基-2-苯基-3-哒酮,能迅速吸收辐照交联ETFE绝缘料经辐照后产生的HF,显著降低HF的逸出量,逸出量小于20ppm,提高辐照交联ETFE的安全、环保性。本发明的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其在绝缘料的羟基-2-苯基-3-哒酮基础上进一步添加甘油山嵛酸酯,能够提高本发明的滑石粉、氧化锌与ETFE树脂的相容性以及滑石粉、氧化锌本身的分散性,使得滑石粉、氧化锌能良好的分散在ETFE中,并且与ETFE结合的比较好,进一步提高了本发明绝缘料的强度。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于,由以下重量份的组分组成:
聚乙烯-四氟乙烯共聚物 100份,
滑石粉 2~10份,
三氧化二锑 2~10份,
氧化锌 2~10份,
硬脂酸锌 1~5份,
羟基-2-苯基-3-哒酮 1~5份,
甘油山嵛酸酯 3~8份,
N,N - 双[β- (3,5-二叔丁基-4-羟基苯基)丙酰]肼 0.1~1份,
3-氨丙基三乙氧基硅烷 1~4份,
交联剂 1~10份。
2.根据权利要求1所述的一种低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于,由以下重量份的组分组成:
聚乙烯-四氟乙烯共聚物 100份,
滑石粉 2~5份,
三氧化二锑 2~6份,
氧化锌 1~5份,
硬脂酸锌 1~5份,
羟基-2-苯基-3-哒酮 2~4份,
甘油山嵛酸酯 5~7份,
N,N - 双[β- (3,5-二叔丁基-4-羟基苯基)丙酰]肼 0.1~1份,
3-氨丙基三乙氧基硅烷 1~4份,
交联剂 1~10份。
3. 根据权利要求1所述的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于:所述滑石粉为超细 滑石粉,所述滑石粉粒径在0.3微米~2微米。
4.根据权利要求1所述的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于:所述三氧化二锑粒径在0.3微米~1.5微米。
5.根据权利要求1所述的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于:所述氧化锌粒径在0.3微米~2微米。
7.根据权利要求6所述的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于:所述交联剂中组分A:组分B的质量比为1:0.3~5。
8.根据权利要求1所述的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于:所述原料配方的辐照交联剂量为5~40兆拉德。
9.根据权利要求8所述的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料,其特征在于:所述原料配方的辐照交联剂量为10~25兆拉德。
10.一种用于权利要求1的低氟化物逸出辐照交联聚乙烯-四氟乙烯共聚物绝缘料的制备方法,其特征在于,包括以下步骤:
第一步,将聚乙烯-四氟乙烯共聚物100份、滑石粉2~10份、三氧化二锑2~10份、氧化锌2~10份、硬脂酸锌1~5份、羟基-2-苯基-3-哒酮1~5份、甘油山嵛酸酯3~8份、N,N - 双[β- (3,5-二叔丁基-4-羟基苯基)丙酰]肼 0.1~1份、3-氨丙基三乙氧基硅烷 1~4份、交联剂1~10份,按相应的重量份在高速混合机中混合均匀;
第二步,将上述步骤混合均匀的物料,在双螺杆挤出机中挤出造粒,烘干,挤出温度为250-300℃。
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