CN113444243A - 一种聚醚-有机硅复合尼龙弹性体及其制备方法 - Google Patents
一种聚醚-有机硅复合尼龙弹性体及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种聚醚‑有机硅复合尼龙弹性体及其制备方法,将聚醚产物与有机硅聚合物引入尼龙合成反应过程中,制备成聚醚‑有机硅尼龙复合弹性体。本发明提出以机硅类为软段制备了新型尼龙弹性体,与传统聚醚为软段的弹性体相比,本发明制备的新型尼龙弹性体具有柔韧性更佳,断裂伸长率更高的优异性能。
Description
技术领域
本发明涉及一种聚醚-有机硅复合尼龙弹性体及其制备方法,属于尼龙材料合成领域。
背景技术
尼龙是一种高强度、高耐磨、高硬度的硬质材料,主要应用于对强度要求较高的工程塑料领域,在弹性体领域,尤其是在高柔性弹性体材料领域由于其较低的弹性限制了其应用。为进一步扩大其应用范围,尼龙弹性体是目前行业内研究较热,也是应用性较强的一类产品。
尼龙弹性体是一种嵌段共聚物,是由高熔点的结晶性尼龙硬段和非结晶性或者无定形聚酯或聚醚软段组成。它们的化学组成、片段长度和之间的比例决定了该类材料的物理和化学性质。尼龙弹性体强度高、韧性高、弹性好、比重低、耐弯曲疲劳性能好、耐磨性能好、低温性能好,可以广泛地应用于汽车、运动用品、医疗用品、密封件、机械零部件等方面。
现有的尼龙弹性体一般采用以尼龙为硬段、醚类为软段进行嵌段共聚反应聚合生产,产品兼具橡胶和热塑性塑料的特性,常用的尼龙弹性体由尼龙12和聚醚多元醇共聚而成,商业化的产品有法国Arkema公司的Pebax XX33系列产品,德国Envonik公司的VestamidE系列产品。但是,随着对尼龙弹性体的深入研究,以醚类为软段的产品存在断裂伸长率低、弹性低、耐温性低等问题。
发明内容
本发明克服了上述现有技术的不足,提供一种聚醚-有机硅复合尼龙弹性体及其制备方法,将聚醚产物与有机硅聚合物引入尼龙合成反应过程中,制备成聚醚-有机硅尼龙复合弹性体。
一种聚醚-有机硅复合尼龙弹性体,包括如下原料,按重量份计:
尼龙66盐50份、酸化剂10份、低粘度有机硅聚合物5-35份、低粘度聚醚产物5-35份、催化剂0.03-0.05份、增白剂0.03-0.05份、抗氧剂0.03-0.05份;
进一步的,上述的低粘度有机硅聚合物为黏度为500Mpa.s的端羟基聚二甲基硅氧烷。
进一步的,上述酸化剂为己二酸、戊二酸、十碳二元酸中的一种。
进一步的,上述低粘度聚醚产物为黏度为1000Mpa.s的聚丁二醇。
进一步的,上述催化剂为醋酸钾、二月桂酸二丁基锡、钛酸四丁酯中的一种或两种。
进一步的,上述增白剂为亚磷酸、次磷酸钠、亚磷酸三苯酯中的一种。
进一步的,上述抗氧剂为三[2.4-二叔丁基苯基]亚磷酸酯,N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺等中的一种或两种。
进一步的,上述聚醚-有机硅复合尼龙弹性体的制备方法,包括如下步骤:
1)取上述重量份的尼龙66盐加入软化水中,配制终浓度为50-70%的尼龙66盐溶液,加入上述重量份的酸化剂,获得酸化的尼龙66盐溶液;
2)取上述重量份的低粘度聚醚产物和低粘度有机硅聚合物混合获得共混软段物质;
3)将步骤2)制备的共混软段物质加到步骤1)制备的酸化的尼龙66盐溶液中,再加入上述重量份的催化剂、增白剂和抗氧剂,置于聚合釜中,保压至1.8-2.2Mpa,温度升至210-230℃,降压,当物料温度为260-280℃时出料,温水冷却,切粒制得聚醚-有机硅复合尼龙弹性体。
本专利以尼龙66为基础尼龙材料,成本低,硬度相对于长碳链尼龙较高,其关键就是有效降低尼龙66的硬度,增加其韧性。有机硅材料在经催化剂聚合后的韧性和柔软度远高于聚合后的聚醚,但有机硅聚合活性相比聚醚材料较弱,故本专利利用有机硅与聚醚复合软段材料。
有益效果:
(1)本发明提出以机硅类为软段制备了新型尼龙弹性体,与传统聚醚为软段的弹性体相比,本发明制备的新型尼龙弹性体具有柔韧性更佳,断裂伸长率更高的优异性能。
(2)本专利利用尼龙66盐溶液为基料,成本大大降低;成品大大改善尼龙66产品的硬度。
(3)本专利将聚醚类、有机硅类物质复合起来添加到尼龙66材料中,且对两种添加物的黏度有精确要求,可以有效降低产品聚合难度,成本大幅降低,且有效地解决了分子量大的有机硅类聚合物活性低,不易参与聚合的问题.
(4)本专利虽使用有机硅物质为添加份,但选用的端羟基聚二甲基硅氧烷为羟基封端,不再使用到硅烷偶联剂为链接剂。
具体实施方式
为了使本技术领域人员更好地理解本申请中的技术方案,下面结合实施例对本发明作进一步说明,所描述的实施例仅是本申请一部分实施例,而不是全部,本发明不受下述实施例的限制。
实施例一:
将5000g尼龙66盐以软化水溶解,溶液浓度调制65%,完全溶解后,加入1000g己二酸酸化,酸度调整好后,备用;均匀混合粘度为500Mpa.s的端羟基聚二甲基硅氧烷500g与粘度为1000Mpa.s的聚丁二醇3500g;将酸化好的尼龙66盐与混合好的端羟基聚二甲基硅氧烷与聚丁二醇混合均匀,再加入醋酸钾3g,钛酸四丁酯3g,亚磷酸3g,抗氧剂1098加入3g,投入聚合釜中,保温保压至215℃,2.0Mpa,随后逐步降压至常压,常压赶气1小时,维持真空度为-0.003Mpa,1小时,随后物料温度达到255℃出料,得尼龙66弹性体。
实施例二:
将5000g尼龙66盐以软化水溶解,溶液浓度调制65%,完全溶解后,加入1000g己二酸酸化,酸度调整好后,备用;均匀混合粘度为500Mpa.s的端羟基聚二甲基硅氧烷1000g与粘度为1000Mpa.s的聚丁二醇3000g;将酸化好的尼龙66盐与混合好的端羟基聚二甲基硅氧烷与聚丁二醇混合均匀,再加入醋酸钾3g,钛酸四丁酯3g,亚磷酸3g,抗氧剂1098加入3g,投入聚合釜中,保温保压至215℃,2.0Mpa,随后逐步降压至常压,常压赶气1小时,维持真空度为-0.003Mpa,1小时,随后物料温度达到255℃出料,得尼龙66弹性体。
实施例三:
将5000g尼龙66盐以软化水溶解,溶液浓度调制65%,完全溶解后,加入1000g己二酸酸化,酸度调整好后,备用;均匀混合粘度为500Mpa.s的端羟基聚二甲基硅氧烷1500g与粘度为1000Mpa.s的聚丁二醇2500g;将酸化好的尼龙66盐与混合好的端羟基聚二甲基硅氧烷与聚丁二醇混合均匀,再加入醋酸钾3g,钛酸四丁酯3g,亚磷酸3g,抗氧剂1098加入3g,投入聚合釜中,保温保压至215℃,2.0Mpa,随后逐步降压至常压,常压赶气1小时,维持真空度为-0.003Mpa,1小时,随后物料温度达到255℃出料,得尼龙66弹性体。
实施例四:
将5000g尼龙66盐以软化水溶解,溶液浓度调制65%,完全溶解后,加入1000g己二酸酸化,酸度调整好后,备用;均匀混合粘度为500Mpa.s的端羟基聚二甲基硅氧烷2000g与粘度为1000Mpa.s的聚丁二醇2000g;将酸化好的尼龙66盐与混合好的端羟基聚二甲基硅氧烷与聚丁二醇混合均匀,再加入醋酸钾3g,钛酸四丁酯3g,亚磷酸3g,抗氧剂1098加入3g,投入聚合釜中,保温保压至215℃,2.0Mpa,随后逐步降压至常压,常压赶气1小时,维持真空度为-0.003Mpa,1小时,随后物料温度达到255℃出料,得尼龙66弹性体。
实施例五:
将5000g尼龙66盐以软化水溶解,溶液浓度调制65%,完全溶解后,加入1000g己二酸酸化,酸度调整好后,备用;均匀混合粘度为500Mpa.s的端羟基聚二甲基硅氧烷2500g与粘度为1000Mpa.s的聚丁二醇1500g;将酸化好的尼龙66盐与混合好的端羟基聚二甲基硅氧烷与聚丁二醇混合均匀,再加入醋酸钾3g,钛酸四丁酯3g,亚磷酸3g,抗氧剂1098加入3g,投入聚合釜中,保温保压至215℃,2.0Mpa,随后逐步降压至常压,常压赶气1小时,维持真空度为-0.003Mpa,1小时,随后物料温度达到255℃出料,得尼龙66弹性体。
由以上实施例聚合生产的产品关键性能指标对比如下表:
表1实施例产品关键性能指标对比表
序号 | 冲击性能 | 硬度 | 断裂伸长率 |
实施例一 | 25JNB | 111A | 150% |
实施例二 | 25JNB | 102A | 240% |
实施例三 | 25JNB | 91A | 310% |
实施例四 | 25JNB | 79A | 390% |
实施例五 | 25JNB | 68A | 460% |
注:本专利检测标准:冲击性能(GB/T 1043-2008);硬度(GB/T 2411-2008);断裂伸长率(GB/T1040-2006)。
本专利提供一种聚醚-有机硅复合类尼龙弹性体的制备,可见,50质量份的尼龙66盐,10质量份己二酸酸化剂,500Mpa.s的端羟基聚二甲基硅氧烷20质量份与粘度为1000Mpa.s的聚丁二醇20质量份可得到较符合需求和预期的产物,硬度低于80A,断裂伸长率接近400%,性能优异。
Claims (8)
1.一种聚醚-有机硅复合尼龙弹性体,其特征在于,包括如下原料,按重量份计:
尼龙66盐50份、酸化剂10份、低粘度有机硅聚合物5-35份、低粘度聚醚产物5-35份、催化剂0.03-0.05份、增白剂0.03-0.05份、抗氧剂0.03-0.05份。
2.如权利要求1所述的聚醚-有机硅复合尼龙弹性体,其特征在于,所述的低粘度有机硅聚合物为黏度为500Mpa.s的端羟基聚二甲基硅氧烷。
3.如权利要求1所述的聚醚-有机硅复合尼龙弹性体,其特征在于,所述的酸化剂为己二酸、戊二酸、十碳二元酸中的一种。
4.如权利要求1所述的聚醚-有机硅复合尼龙弹性体,其特征在于,所述的低粘度聚醚产物为黏度为1000Mpa.s的聚丁二醇。
5.如权利要求1所述的聚醚-有机硅复合尼龙弹性体,其特征在于,所述的催化剂为醋酸钾、二月桂酸二丁基锡、钛酸四丁酯中的一种或两种。
6.如权利要求1所述的聚醚-有机硅复合尼龙弹性体,其特征在于,所述的增白剂为亚磷酸、次磷酸钠、亚磷酸三苯酯中的一种。
7.如权利要求1所述的聚醚-有机硅复合尼龙弹性体,其特征在于,所述的抗氧剂为三[2.4-二叔丁基苯基]亚磷酸酯,N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺等中的一种或两种。
8.如权利要求1-7任一项所述的聚醚-有机硅复合尼龙弹性体的制备方法,其特征在于,包括如下步骤:
1)取上述重量份的尼龙66盐加入软化水中,配制终浓度为50-70%的尼龙66盐溶液,加入上述重量份的酸化剂,获得酸化的尼龙66盐溶液;
2)取上述重量份的低粘度聚醚产物和低粘度有机硅聚合物混合获得共混软段物质;
3)将步骤2)制备的共混软段物质加到步骤1)制备的酸化的尼龙66盐溶液中,再加入上述重量份的催化剂、增白剂和抗氧剂,置于聚合釜中,保压至1.8-2.2Mpa,温度升至210-230℃,降压,当物料温度为260-280℃时出料,温水冷却,切粒制得聚醚-有机硅复合尼龙弹性体。
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CN111349232A (zh) * | 2020-04-22 | 2020-06-30 | 建湖县兴隆尼龙有限公司 | 一种尼龙弹性体材料及其制备方法 |
CN111601852A (zh) * | 2018-01-15 | 2020-08-28 | 阿科玛法国公司 | 热塑性弹性体-有机硅组合物 |
CN112625248A (zh) * | 2020-09-30 | 2021-04-09 | 山东东辰瑞森新材料科技有限公司 | 一种有机硅尼龙弹性体及其制备方法 |
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CN1429253A (zh) * | 2000-07-26 | 2003-07-09 | 陶氏康宁公司 | 由相容化聚酰胺树脂制备的热塑性有机硅弹性体 |
DE10162968A1 (de) * | 2000-12-29 | 2002-07-11 | Hyundai Motor Co Ltd | Polyamidharz-Zusammensetzung und daraus hergestelltes synthetisches Harzprodukt |
CN111601852A (zh) * | 2018-01-15 | 2020-08-28 | 阿科玛法国公司 | 热塑性弹性体-有机硅组合物 |
CN111349232A (zh) * | 2020-04-22 | 2020-06-30 | 建湖县兴隆尼龙有限公司 | 一种尼龙弹性体材料及其制备方法 |
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