CN105949624B - 咪唑盐成核剂及其制备方法及应用 - Google Patents

咪唑盐成核剂及其制备方法及应用 Download PDF

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CN105949624B
CN105949624B CN201610545207.6A CN201610545207A CN105949624B CN 105949624 B CN105949624 B CN 105949624B CN 201610545207 A CN201610545207 A CN 201610545207A CN 105949624 B CN105949624 B CN 105949624B
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nucleating agent
imidazole salts
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polypropylene
salts nucleating
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周颖
张凯
于杰
何敏
秦舒浩
何文涛
罗阳
张道海
李娟�
龙丽娟
向宇殊
张敬
付光
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Guizhou Material Industrial Technology Research Institute
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
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    • C07ORGANIC CHEMISTRY
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    • C07D233/00Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
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    • C07D233/56Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
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Abstract

本发明公开了一种咪唑盐成核剂及其制备方法及应用。本发明采用2’2‑亚甲基双(4,6‑二叔丁基苯基)磷酸酯与咪唑作为原料反应,制备获得的咪唑盐成核剂不仅与聚丙烯具有良好的相容性,而且能在聚丙烯中更好的分散。本发明材料来源广泛、制备方法简单、成本低廉,使用效果理想。

Description

咪唑盐成核剂及其制备方法及应用
技术领域
本发明涉及高分子材料技术领域,尤其是一种咪唑盐成核剂及其制备方法及应用。
背景技术
聚丙烯是一种价格低廉,性能优异,易加工的半结晶型热塑性塑料。通常在聚丙烯中添加少量的成核剂是改变聚丙烯结晶和透明性的有效办法。成核剂主要分为有机和无机两大类,而有机成核剂又分为山梨醇和有机磷酸盐两大类。无机成核剂在聚丙烯中分散性差,易导致局部应力集中,从而恶化聚丙烯制品的力学性能,而有机成核剂恰好能够弥补上述缺点。
因此,研究有机成核剂在聚丙烯加工中的应用,有机成核剂诱导聚丙烯结晶机理均成为研究的重要方向。
发明内容
本发明的目的是:提供一种咪唑盐成核剂及其制备方法及应用,它与聚丙烯有良好的相容性,在聚丙烯基体中分散性好,以克服现有技术的不足。
本发明是这样实现的:咪唑盐成核剂,它具有如下结构式:
咪唑盐成核剂的制备方法,将咪唑及2,2-亚甲基双(4,6-二叔丁基苯基)磷酸酯在有机溶剂中进行反应制得。
所述的有机溶剂可以为甲醇、乙醇、丙醇、四氢呋喃、苯、甲苯、氯仿或环己烷。
具体步骤如下:
1)在常温下将3-6质量份的2,2-亚甲基双(4,6-二叔丁基苯基)磷酸酯完全溶解在30-100体积份有机溶剂中;
2)再将0.4-0.8质量份的咪唑加入步骤1)的溶液中,搅拌至完全溶解;静置36-48小时,将溶液中产生的白色沉淀过滤后在70-100℃下烘干4-8小时,得产物咪唑盐成核剂,产率90-95%。
上述质量份与体积份的单位比是g/ml。
咪唑盐成核剂在聚丙烯加工中的应用,在以聚丙烯作为基体材料的加工中,加入占聚丙烯总质量的0.01-3%的咪唑盐成核剂。
由于采用了上述技术方案,与现有技术相比,本发明采用2’2-亚甲基双(4,6-二叔丁基苯基)磷酸酯与咪唑作为原料反应,制备获得的咪唑盐成核剂不仅与聚丙烯具有良好的相容性,而且能在聚丙烯中更好的分散。本发明材料来源广泛、制备方法简单、成本低廉,使用效果理想。
附图说明
附图1为本发明的产品的热分解曲线。
具体实施方式
本发明的实施例1:咪唑盐成核剂的制备方法,在常温下将5质量份的2,2-亚甲基双(4,6-二叔丁基苯基)磷酸酯完全溶解在70体积份四氢呋喃中;
2)再将0.6质量份的咪唑加入步骤1)的溶液中,搅拌至完全溶解;静置40小时,将溶液中产生的白色沉淀过滤后在80℃下烘干6小时,得产物咪唑盐成核剂,产率92%。
上述质量份与体积份的单位比是g/ml。
本发明的实施例2:咪唑盐成核剂的制备方法,在常温下将3质量份的2,2-亚甲基双(4,6-二叔丁基苯基)磷酸酯完全溶解在30体积份氯仿中;
2)再将0.8质量份的咪唑加入步骤1)的溶液中,搅拌至完全溶解;静置36小时,将溶液中产生的白色沉淀过滤后在100℃下烘干4小时,得产物咪唑盐成核剂,产率90%。
上述质量份与体积份的单位比是g/ml。
本发明的实施例3:咪唑盐成核剂的制备方法,在常温下将6质量份的2,2-亚甲基双(4,6-二叔丁基苯基)磷酸酯完全溶解在100体积份甲苯中;
2)再将0.4质量份的咪唑加入步骤1)的溶液中,搅拌至完全溶解;静置48小时,将溶液中产生的白色沉淀过滤后在70℃下烘干8小时,得产物咪唑盐成核剂,产率95%。
上述质量份与体积份的单位比是g/ml。
将上述实施例获得的咪唑盐成核剂进行检测分析,所有产品都具有如下结构式:
实施例4:咪唑盐成核剂在聚丙烯加工中的应用,取中国石油独山子石化公司生产的牌号为T30S的等规聚丙烯100重量份,制得的咪唑盐成核剂0.002重量份,混合均匀后,用CET-20型双螺杆挤出机挤出,挤出温度190-210℃,然后经130SeII型注塑机注塑,注塑温度220℃,制成试样标准样条和标准透明样板;将不加入成核剂的聚丙烯经同样处理,作为空白试样。对聚丙烯制品进行光学性能,力学性能,结晶性能等方面的测试。
将得到的样条按GB/T9341-2008测试标准进行弯曲弹性模量测试,按GB/T1040.1-2006测试标准进行拉伸强度测试。将得到的标准透明样板按GB2410-80测试标准进行光学性能测试。
表1成核剂对ipp结晶性能的改善
表2成核剂对ipp力学性能的改善
表3成核剂对ipp光学性能的改善
从表1、表2及表3可以看出,将本发明实施例制备的产品应用在聚合物改性加工中,得到的改性聚合物的结晶峰温度可提高14℃以上,得到的改性聚合物的弯曲模量可提高32%以上,得到的改性聚合物透光率可提高到69.5%。
从这些数据可以清楚的看出,使用本发明的产品,可以明显的改善聚合物的加工性能,特别是大幅度提高了聚合物透光率,弯曲模量和结晶峰温度。

Claims (5)

1.一种咪唑盐成核剂,其特征在于:它具有如下结构式:
2.一种如权利要求1所述的咪唑盐成核剂的制备方法,其特征在于:将咪唑及2,2-亚甲基双(4,6-二叔丁基苯基)磷酸酯在有机溶剂中进行反应制得。
3.根据权利要求2的所述的制备方法,其特征在于:所述的有机溶剂可以为甲醇、乙醇、丙醇、四氢呋喃、苯、甲苯、氯仿或环己烷。
4.根据权利要求2或3的所述的制备方法,其特征在于:具体步骤如下:
1)在常温下将3-6质量份的2,2-亚甲基双(4,6-二叔丁基苯基)磷酸酯完全溶解在30-100体积份有机溶剂中;
2)再将0.4-0.8质量份的咪唑加入步骤1)的溶液中,搅拌至完全溶解;静置36-48小时,将溶液中产生的白色沉淀过滤后在70-100℃下烘干4-8小时,得产物咪唑盐成核剂,产率90-95%;
上述质量份与体积份的单位比是g/ml。
5.一种如权利要求1所述的咪唑盐成核剂在聚丙烯加工中的应用,其特征在于:在以聚丙烯作为基体材料的加工中,加入占聚丙烯总质量的0.01-3%的咪唑盐成核剂。
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CN108329590A (zh) * 2018-02-08 2018-07-27 贵州省材料产业技术研究院 一种双峰结晶聚丙烯复合材料及其制备方法
CN110982120B (zh) * 2019-11-20 2024-07-30 贵州省材料技术创新基地 一种复配型咪唑盐成核剂及其聚烯烃复合材料
CN113429767B (zh) * 2021-07-13 2022-08-02 湖南玥昇杰科技有限责任公司 一种含咪唑型成核剂的聚乳酸组合物及其制备方法
CN114773731A (zh) * 2022-04-29 2022-07-22 苏州润佳高分子材料有限公司 一种抗静电的聚丙烯塑料及其制备方法

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