CN108485587A - 一种聚氨酯型耐油密封胶及其制备方法和用途 - Google Patents
一种聚氨酯型耐油密封胶及其制备方法和用途 Download PDFInfo
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- CN108485587A CN108485587A CN201810266778.5A CN201810266778A CN108485587A CN 108485587 A CN108485587 A CN 108485587A CN 201810266778 A CN201810266778 A CN 201810266778A CN 108485587 A CN108485587 A CN 108485587A
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- polyurethane
- fluid sealant
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Classifications
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Abstract
本发明提供一种聚氨酯型耐油密封胶及其制备方法和应用,所述聚氨酯型耐油密封胶的制备原料包括80‑90重量份聚醚多元醇、20‑40重量份二异氰酸酯、15‑20重量份丁腈橡胶、10‑20重量份聚氯乙烯、10‑20重量份羟基封端聚氟硅氧烷、5‑10重量份重质碳酸钙、3‑5重量份二甲基硅油、3‑8重量份硅烷偶联剂、1‑4重量份扩链剂、1‑3重量份催化剂和1‑3重量份抗氧化剂。本发明的聚氨酯型耐油密封胶具有耐油性,耐水解性能良好,具有良好的稳定性,用于食品灌装密封胶,在接触食品时具有很低的迁移率,满足欧美国家食品卫生要求。
Description
技术领域
本发明属于密封胶技术领域,涉及一种聚氨酯型耐油密封胶及其制备方法和用途。
背景技术
聚氨酯密封胶是以聚氨酯橡胶以及聚氨酯预聚体为主要成分的密封胶。此类密封胶具有高的拉伸强度、优良的弹性、耐磨性、耐油性和耐寒性,广泛用于建筑物、公路、汽车制造、玻璃安装、单子密封等。然而其也存在一些缺陷,例如储存稳定性受包装以及外界影响较大,含有挥发性溶剂,固含量不够,而且用于食品包装例如金属瓶盖密封胶时,会存在迁移率较高,存在安全风险。
随着科技的发展以及人们对环保和健康意识的加强,全世界对于瓶盖密封胶的要求越来越高,不仅要求密封性好,而且还要求对食品和环境无污染,需要良好的控制密封胶的迁移性能,以达到满足欧美国家食品卫生要求。
CN101613587A公开了一种聚氨酯密封胶,由A组分和B组分组成,A组分和B组分的重量比为1:1-10,其中A组分为聚氨酯预聚体,B组分包含重量份如下的成分:聚醚多元醇16-30份,增塑剂2-15份,填料40-70份,催化剂0.1-2份,触变剂0.1-2份。虽然提高了聚氨酯密封胶的固含量,减少了挥发性溶剂以及其他小分子物质,但是其仍然无法克服在接触食品时会产生成分迁移的缺点。
在本领域中,期望得到一种具有低的迁移率能够满足欧美国家食品卫生要求的聚氨酯密封胶。
发明内容
针对现有技术的问题,本发明的目的在于提供一种聚氨酯型耐油密封胶及其制备方法和用途。本发明所述聚氨酯耐油密封胶,具有耐油性,耐水解,与食品接触时具有较低的迁移率,安全可靠,能够满足欧美国家食品卫生要求。
为达此目的,本发明采用以下技术方案:
一方面,本发明提供一种聚氨酯型耐油密封胶,所述聚氨酯型耐油密封胶的制备原料包括以下重量份的组分:
在本发明中,通过在聚氨酯制备原料中加入丁腈橡胶、聚氯乙烯、羟基封端聚氟硅氧烷以及二甲基硅油来调整材料的柔韧性以及耐油耐水解的性能,并且羟基封端聚氟硅氧烷通过羟基与二异氰酸酯的反应,将聚氟硅氧烷结构连接在聚氨酯结构中,增强聚氨酯材料的耐油性能,并且其与硅烷偶联剂配合可以更好地促进无机成分与有机成分良好地相容,使得无机成分的加入能够增强材料的硬度,各成分的整体配合使得材料的稳定性增强,耐油性以及耐水解性能提高,与食品接触时迁移率降低。
在本发明中,所述聚醚多元醇的用量可以为80重量份、81重量份、82重量份、83重量份、84重量份、85重量份、86重量份、87重量份、88重量份、89重量份或90重量份。
在本发明中,所述二异氰酸酯的用量可以为20重量份、22重量份、24重量份、26重量份、28重量份、30重量份、33重量份、35重量份、38重量份或40重量份。
在本发明中,所述丁腈橡胶的用量可以为15重量份、15.5重量份、16重量份、16.5重量份、17重量份、17.5重量份、18重量份、18.5重量份、19重量份、19.5重量份或20重量份。
在本发明中,所述聚氯乙烯的用量可以为5重量份、5.5重量份、6重量份、6.5重量份、7重量份、7.5重量份、8重量份、8.5重量份、9重量份、9.5重量份或10重量份。
在本发明中,所述羟基封端聚氟硅氧烷的用量可以为10重量份、11重量份、12重量份、13重量份、14重量份、15重量份、16重量份、17重量份、18重量份、19重量份或20重量份。
在本发明中,所述重质碳酸钙的用量可以为5重量份、5.5重量份、6重量份、6.5重量份、7重量份、7.5重量份、8重量份、8.5重量份、9重量份、9.5重量份或10重量份。
在本发明中,所述二甲基硅油的用量可以为3重量份、3.3重量份、3.5重量份、3.8重量份、4重量份、4.3重量份、4.5重量份、4.8重量份或5重量份。
在本发明中,所述硅烷偶联剂的用量可以为3重量份、3.5重量份、4重量份、4.5重量份、5重量份、5.5重量份、6重量份、6.5重量份、7重量份、7.5重量份或8重量份。
在本发明中,所述扩链剂的用量可以为1重量份、1.3重量份、1.5重量份、2重量份、2.5重量份、2.8重量份、3重量份、3.5重量份、3.8重量份或4重量份。
在本发明中,所述催化剂的用量可以为1重量份、1.3重量份、1.5重量份、1.8重量份、2重量份、2.3重量份、2.5重量份、2.8重量份或3重量份。
在本发明中,所述抗氧化剂的用量可以为1重量份、1.3重量份、1.5重量份、1.8重量份、2重量份、2.3重量份、2.5重量份、2.8重量份或3重量份。
优选地,所述二异氰酸酯为二甲基联苯二异氰酸酯与对苯二异氰酸酯的混合物。
优选地,所述二异氰酸酯中二甲基联苯二异氰酸酯与对苯二异氰酸酯的质量比为1:1-3,例如1:1、1:1.2、1:1.5、1:1.8、1:2、1:2.3、1:2.5、1:2.8或1:3。
优选地,所述硅烷偶联剂为六烷氧基硅烷偶联剂。多烷氧基硅烷偶联剂由于其端位具有多个烷氧基,相比与一般的偶联剂,该偶联剂可以提供更多的反应位点,可以更好的抓住无机组分碳酸钙、纳米二氧化硅以及纳米银,能够更好地将无机组分与有机成分进行牢固结合,提高产品的稳定性。
优选地,所述扩链剂为乙二醇、乙二胺、1,3-丙二醇、1,4-丁二醇或1,5-戊二醇中的任意一种或至少两种的组合。
优选地,所述催化剂为辛酸亚锡、二辛酸二丁锡或月硅酸二丁锡中的任意一种或至少两种的组合。
优选地,所述抗氧化剂为抗氧剂1010、抗氧剂1076、抗氧剂264、抗氧剂TPP或抗氧剂TNP中的任意一种或至少两种的混合物。
另一方面,本发明提供了如上所述的聚氨酯型耐油密封胶的制备方法,所述制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、羟基封端聚氟硅氧烷、扩链剂、催化剂和抗氧化剂混合,在搅拌条件下,真空脱水,而后在120-140℃(例如120℃、123℃、125℃、128℃、130℃、133℃、135℃或140℃)反应3-8h(例如3h、3.5h、4h、4.5h、5h、5.5h、6h、6.5h、7h、7.5h或8h);
(2)将步骤(1)的产物与丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,密炼,成型得到所述聚氨酯型耐油密封胶。
采用本发明所述的制备方法,使得在步骤(1)中合成聚氨酯,并且合成的聚氨酯结构上连接有聚氟硅氧烷,提高材料的抗油污性能,通过步骤(2)中与丁腈橡胶、聚氯乙烯、二甲基硅油以及硅烷偶联剂、重质碳酸钙等的混合密炼,使得进一步调整了材料的柔韧性以及耐油耐水解的性能,并且聚氟硅氧烷与硅烷偶联剂配合可以更好地促进无机成分与有机成分良好地相容,增强产品的稳定性,降低材料的迁移率。
优选地,步骤(1)所述搅拌的转速为80-120r/min;例如80r/min、85r/min、90r/min、95r/min、100r/min、110r/min、115r/min或120r/min。
优选地,步骤(1)所述真空脱水时的温度为70-90℃,例如可以是70℃、75℃、80℃、85℃或90℃。
优选地,步骤(1)所述真空脱水时的压力为-0.3~-0.1kPa,例如可以是-0.3kPa、-0.25kPa、-0.2kPa、-0.15kPa或-0.1kPa。
优选地,步骤(2)所述密炼的温度为80-100℃,例如80℃、85℃、90℃、95℃、98℃或100℃。
优选地,步骤(2)所述密炼的时间为1-5小时,例如1小时、1.5小时、2小时、2.5小时、3小时、3.5小时、4小时、4.5小时或5小时。
另一方面,本发明提供一种如上所述的聚氨酯型耐油密封胶作为金属瓶盖密封胶的应用。
相对于现有技术,本发明具有以下有益效果:
本发明的聚氨酯型耐油密封胶具有耐油性,耐水解性能良好,具有良好的稳定性,可用于食品灌装密封胶,在接触食品时具有很低的迁移率,满足欧美国家食品卫生要求。
具体实施方式
下面通过具体实施方式来进一步说明本发明的技术方案。本领域技术人员应该明了,所述实施例仅仅是帮助理解本发明,不应视为对本发明的具体限制。
实施例1
在本实施例中,聚氨酯型耐油密封胶的制备原料包括以下重量份的组分:
其中,所述二异氰酸酯为质量比为1:3的二甲基联苯二异氰酸酯与对苯二异氰酸酯的混合物,硅烷偶联剂为六烷氧基硅烷偶联剂,扩链剂为1,3-丙二醇,催化剂为二辛酸二丁锡,抗氧剂为抗氧剂264。
所述制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、羟基封端聚氟硅氧烷、扩链剂、催化剂和抗氧化剂混合,在转速90r/min的搅拌条件下,于80℃、-0.2kPa的真空压力下真空脱水,而后在120℃反应5h;
(2)将步骤(1)的产物与丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,在90℃下密炼3小时,成型得到所述聚氨酯型耐油密封胶。
实施例2
在本实施例中,聚氨酯型耐油密封胶的制备原料包括以下重量份的组分:
其中,所述二异氰酸酯为质量比为1:1的二甲基联苯二异氰酸酯与对苯二异氰酸酯的混合物,硅烷偶联剂为六烷氧基硅烷偶联剂,扩链剂为乙二醇,催化剂为月硅酸二丁锡,抗氧剂为抗氧剂1010。
所述制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、羟基封端聚氟硅氧烷、扩链剂、催化剂和抗氧化剂混合,在转速100r/min的搅拌条件下,于90℃、-0.1kPa的真空压力下真空脱水,而后在130℃反应6h;
(2)将步骤(1)的产物与丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,在80℃下密炼4小时,成型得到所述聚氨酯型耐油密封胶。
实施例3
在本实施例中,聚氨酯型耐油密封胶的制备原料包括以下重量份的组分:
其中,所述二异氰酸酯为质量比为1:2的二甲基联苯二异氰酸酯与对苯二异氰酸酯的混合物,硅烷偶联剂为六烷氧基硅烷偶联剂,扩链剂为1,4-丁二醇,催化剂为二辛酸二丁锡,抗氧剂为抗氧剂TPP。
所述制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、羟基封端聚氟硅氧烷、扩链剂、催化剂和抗氧化剂混合,在转速120r/min的搅拌条件下,于70℃、-0.3kPa的真空压力下真空脱水,而后在140℃反应3h;
(2)将步骤(1)的产物与丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,在100℃下密炼1小时,成型得到所述聚氨酯型耐油密封胶。
实施例4
在本实施例中,聚氨酯型耐油密封胶的制备原料包括以下重量份的组分:
其中,所述二异氰酸酯为质量比为1:3的二甲基联苯二异氰酸酯与对苯二异氰酸酯的混合物,硅烷偶联剂为六烷氧基硅烷偶联剂,扩链剂为1,5-戊二醇,催化剂为辛酸亚锡,抗氧剂为抗氧剂1076。
所述制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、羟基封端聚氟硅氧烷、扩链剂、催化剂和抗氧化剂混合,在转速80r/min的搅拌条件下,于70℃、-0.1kPa的真空压力下真空脱水,而后在120℃反应8h;
(2)将步骤(1)的产物与丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,在80℃下密炼5小时,成型得到所述聚氨酯型耐油密封胶。
实施例5
在本实施例中,聚氨酯型耐油密封胶的制备原料包括以下重量份的组分:
其中,所述二异氰酸酯为质量比为1:1的二甲基联苯二异氰酸酯与对苯二异氰酸酯的混合物,硅烷偶联剂为六烷氧基硅烷偶联剂,扩链剂为乙二胺,催化剂为二辛酸二丁锡,抗氧剂为抗氧剂TNP。
所述制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、羟基封端聚氟硅氧烷、扩链剂、催化剂和抗氧化剂混合,在转速90r/min的搅拌条件下,于85℃、-0.2kPa的真空压力下真空脱水,而后在130℃反应5h;
(2)将步骤(1)的产物与丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,在95℃下密炼2小时,成型得到所述聚氨酯型耐油密封胶。
对比例1
与实施例1不同之处仅在于,聚氨酯型耐油密封胶的制备原料中不包括羟基封端聚氟硅氧烷。
对比例2
与实施例1不同之处仅在于,聚氨酯型耐油密封胶的制备原料中不包括丁腈橡胶。
对比例3
与实施例1不同之处仅在于,聚氨酯型耐油密封胶的制备原料中不包括硅烷偶联剂。
对比例4
与实施例1不同之处仅在于,聚氨酯型耐油密封胶的制备原料中硅烷偶联剂为环氧基硅烷偶联剂。
对比例5
与实施例1不同的是聚氨酯型耐油密封胶的制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、扩链剂、催化剂和抗氧化剂混合,在转速90r/min的搅拌条件下,于80℃、-0.2kPa的真空压力下真空脱水,而后在120℃反应5h;
(2)将步骤(1)的产物与羟基封端聚氟硅氧烷、丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,在90℃下密炼3小时,成型得到所述聚氨酯型耐油密封胶。
对实施例1-5以及对比例1-5制备得到的聚氨酯型耐油密封胶进行耐温性、耐水解以及耐油性和稳定性的测定和评价,结果如表1所示。
表1
采用油脂性模拟物(正己烷、正庚烷、异辛烷以及橄榄油)对实施例1-5以及对比例1-5制备得到的聚氨酯型耐油密封胶进行了迁移性能的测试,其中,(1)正己烷1根据GB/T5009.67《食品包装用聚氯乙烯成型品卫生品标准的分析方法》标准进行测试;(2)正庚烷2根据§177.1210Closures with sealing gaskets for food containers标准进行测试;(3)异辛烷3与橄榄油4根据(EU)No 10/2011on plastic materials and articlesintended to come into contact with food标准进行测试,测试结果如表2所示。
表2
从表1和表2的数据可以看出,本发明制备的密封胶具有良好的耐温性、耐油污、耐水解性,产品稳定性好,可用于瓶装食品包装的瓶盖密封胶,具有较低的迁移率,能够满足欧美国家食品卫生要求。
本发明通过上述实施例来说明本发明的聚氨酯型耐油密封胶及其制备方法和应用,但本发明并不局限于上述实施例,即不意味着本发明必须依赖上述实施例才能实施。所属技术领域的技术人员应该明了,对本发明的任何改进,对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等,均落在本发明的保护范围和公开范围之内。
Claims (10)
1.一种聚氨酯型耐油密封胶,其特征在于,所述聚氨酯型耐油密封胶的制备原料包括以下重量份的组分:
2.根据权利要求1所述的聚氨酯型耐油密封胶,其特征在于,所述二异氰酸酯为二甲基联苯二异氰酸酯与对苯二异氰酸酯的混合物;
优选地,所述二异氰酸酯中二甲基联苯二异氰酸酯与对苯二异氰酸酯的质量比为1:1-3。
3.根据权利要求1或2所述的聚氨酯型耐油密封胶,其特征在于,所述硅烷偶联剂为六烷氧基硅烷偶联剂。
4.根据权利要求1-3中任一项所述的聚氨酯型耐油密封胶,其特征在于,所述扩链剂为乙二醇、乙二胺、1,3-丙二醇、1,4-丁二醇或1,5-戊二醇中的任意一种或至少两种的组合。
5.根据权利要求1-4中任一项所述的聚氨酯型耐油密封胶,其特征在于,所述催化剂为辛酸亚锡、二辛酸二丁锡或月硅酸二丁锡中的任意一种或至少两种的组合。
6.根据权利要求1-5中任一项所述的聚氨酯型耐油密封胶,其特征在于,所述抗氧化剂为抗氧剂1010、抗氧剂1076、抗氧剂264、抗氧剂TPP或抗氧剂TNP中的任意一种或至少两种的混合物。
7.根据权利要求1-6中任一项所述的聚氨酯型耐油密封胶的制备方法,其特征在于,所述制备方法包括以下步骤:
(1)将聚醚多元醇、二异氰酸酯、羟基封端聚氟硅氧烷、扩链剂、催化剂和抗氧化剂混合,在搅拌条件下,真空脱水,而后在120-140℃反应3-8h;
(2)将步骤(1)的产物与丁腈橡胶、聚氯乙烯、重质碳酸钙、二甲基硅油以及硅烷偶联剂混合,密炼,成型得到所述聚氨酯型耐油密封胶。
8.根据权利要求7所述的制备方法,其特征在于,步骤(1)所述搅拌的转速为80-120r/min;
优选地,步骤(1)所述真空脱水时的温度为70-90℃;
优选地,步骤(1)所述真空脱水时的压力为-0.3~-0.1kPa。
9.根据权利要求7或8所述的制备方法,其特征在于,步骤(2)所述密炼的温度为80-100℃;
优选地,步骤(2)所述密炼的时间为1-5小时。
10.根据权利要求1-6中任一项所述的聚氨酯型耐油密封胶作为金属瓶盖密封胶的应用。
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