CN1133055A - 稳定的聚烯烃蜡的水分散体 - Google Patents

稳定的聚烯烃蜡的水分散体 Download PDF

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CN1133055A
CN1133055A CN94193719A CN94193719A CN1133055A CN 1133055 A CN1133055 A CN 1133055A CN 94193719 A CN94193719 A CN 94193719A CN 94193719 A CN94193719 A CN 94193719A CN 1133055 A CN1133055 A CN 1133055A
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wax
acid
weight
polyolefin
glyceryl ester
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M·W·米勒
P·克林格赫弗
S·怀斯
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Abstract

稳定的聚烯烃蜡水分散体，包括A)5-65％重量的具有平均颗粒大小为1-50μm的和酸值为小于5mgKOH/g蜡的聚乙烯蜡或聚丙烯蜡和B)0.5-20％重量的用1-50mol的具有2-4C原子的1，2-环氧烷转化了的甘油酯作为分散剂，该甘油酯为主要由乙烯性单不饱和或不饱和的C16-C22-一元羧酸所生成的酯，此酸还可以含有羟基。该分散体适用于制造地板蜡和石料上光剂、鞋油、汽车保护剂、印刷油墨、印染浆料、油漆、包装、润滑脂、凡士林、拉丝剂(drawing agent)、电器元件的密封材料和绝缘材料、水溶性木料清漆、热熔性涂层、化妆品和牙膏，用于塑料加工，用于造纸和用于防蚀，用于织物和纱线处理和皮革的加工以及有色金属的冷铸、压铸和离心铸造时作为分型剂。

Description

稳定的聚烯烃蜡的水分散体
本发明涉及新的聚烯烃蜡的水分散体，它包含：A)5-65％重量的聚乙烯蜡或聚丙烯蜡，其平均颗粒大小为1-50μm，其酸值小于5mg KOH/g蜡，和
B)作为分散剂的0.5-20％重量的用1-50摩尔具有2-4个C-原子的1，2-环氧烷转化了的甘油酯，该甘油酯为主要由乙烯性单不饱和或多不饱和的C16-C22-一元羧酸生成的酯，此酸还可以另外含有羟基。
以聚乙烯或聚丙烯为基础的蜡的水分散体，原则上可以由两种途径制备：作为第一类分散体，是通过乙烯或丙烯在一种含有表面活性剂的水相里在加压和引发剂体系存在下聚合而得；而作为第二种分散体，是通过将可分散的粉末状的聚乙烯蜡或聚丙烯蜡借助一种适宜的分散剂体系进行分散而得。
对于可乳化的蜡通常可以理解为具有羧酸-、酮-或羟基官能化的低分子量的聚烯烃链。它们可以通过乙烯或丙烯与不饱和羧酸，如丙烯酸进行共聚而得，或者通过聚烯烃蜡在大气压下的氧化作用而得。
第一种分散体的颗粒大小通常在0.01-0.25μm范围内，而稳定的第二种分散体直到现在只能制备出平均颗粒大小为最多1μm。具有较大颗粒的分散体由于比较低的密度和聚烯烃蜡的疏水性而易出现相分离。
在这两种制备方法中，固含量通常只能达到大约35％重量以下。较高的蜡含量只有在很困难的情况下，通过使用适宜的助剂才能达到比较高的含量。
从US-A4 371 658中，已知用于制备聚酰胺纱线的纺纱助剂(spinning assistant)，该助剂是由各种乳化剂、酸值大约为14-32的氧化了的聚乙烯和碱金属氢氧化物在水乳浊液中形成的混合物。作为乳化剂组分，提及了用2-6摩尔环氧乙烷转化了的蓖麻子油(castor ail)。
本发明的任务是制备稳定的聚烯烃蜡的水分散体，根据所需的性能特性，该分散体平均颗粒大小明显大于1μm，并且实际上可以无限期存放。此外，这种分散体应该尽可能简单和用尽可能少的助剂进行制备。该分散体应该以未官能化，即不带起稳定作用的羧酸基团的聚烯烃蜡为基础。
为此，发现了开头阐明的聚烯烃蜡的水分散体。通过选择分散剂体系B，现在可通过简单地将适宜的细微的(微米级的)蜡粉末与分散剂一起在室温下于水中搅拌获得具有所希望性能的稳定的聚烯烃蜡分散体。在此，固含量可以达到最高65％重量。
在本发明所述的新分散体中，聚烯烃蜡A的平均颗粒大小为1-50μm，特别是3-20μm，尤其为5-15μm。平均颗粒大小最好用Coulter-法进行测定。
使用市售的未官能化的聚乙烯蜡，其重均分子量在500-10，000g/mol范围内，尤其是1,000-5,000g/mol，或者是聚丙烯蜡，其重均分子量在5,000-50,000g/mol范围之内，尤其是15,000-30,000g/mol，或者使用它们的混合物。聚乙烯或聚丙烯在这些蜡中的含量应大于99％重量。这些蜡采用常用的方法粉碎研细，以达到所需的颗粒大小。它们的酸值小于5，较好小于3，更好小于2，最好小于1mg KOH/g蜡，酸值表明作为杂质实质上存在于蜡中的酸成分。
按本发明所述的分散体，即或在高固含量时，倾倒和搅拌都不成问题，用Brookfield法测得的粘度通常为200-5,000，尤其是500-1,600mm2/s。
按本发明所述的分散体包括作为主要成分的5-65，较好的10-60，更好的20-55，最好的40-50％重量的蜡A和0.5-20，较好的1-15，更好的3-12，最好的4-10％重量的分散剂B。根据需要还可以添加普通的助剂，如：消泡剂，例如：有机磷酸盐、助溶剂，例如：N-甲基吡咯烷酮，流动改进剂，尤其在固含量大于50％重量时，生物杀伤剂、香料、颜料、防蚀剂等。
在烷氧基化的甘油酯B中的脂脂酸占优势地，也就是说，大于50％重量，较好的大于70％重量，更好的大于80％重量，是乙烯性单不饱和或多不饱和羧酸，优选为乙烯性单不饱和至三不饱和的C16-C22-一元羧酸，优选的为C18-一元羧酸，它们可以另外含有羟基。这类脂肪酸的例子为油酸、反油酸、亚油酸、亚麻酸、芥酸和12-羟基-9-顺式-十八烯酸(12-羟基油酸、蓖麻油酸)。在烷氧基化的甘油酯B中，作为次要成分可以加入饱和的脂肪酸，如：肉豆蔻酸、软脂酸、硬脂酸或蜡酸。甘油酯大多数或占优势地以甘油三酸酯形式存在，但也可能有带有未酯化羟基的甘油单酸酯和/或甘油二酸酯结构，甚至于该种结构是必需的，假如脂肪酸基团上不带有能与环氧烷进行反应的羟基时。
作为1，2-环氧烷首先要提到的是环氧乙烷，其次是环氧丙烷或环氧丁烷。也可以用上述环氧烷的混合物与甘油酯进行反应。烷氧化度为1-50，较好的为2-30，更好的为3-20，最好的为5-15mol环氧烷/1mol甘油酯。
在一个优选的实施方式里，作为B组分，使用以3-20mol环氧乙烷进行转化的甘油酯，该甘油酯主要是由乙烯性单不饱和至三不饱和的、至少部分还含有羟基的C18-一元羧酸生成。“至少部分”的意义是一元羧酸的一部分或全部，也就是说，通常50-10％重量的一元羧酸含有一个或多个羟基，较好的70-100％重量，更好的80-100％重量的一元羧酸含有一个或多个羟基。
特别优选的乙氧基化的甘油酯B为主要含有大于50％重量的，优选大于70％重量的，更优选大于80％重量的12-羟基-9-顺式-十八烯酸(蓖麻油酸)作为C18-一元羧酸的酯。
采用天然的蓖麻子油经过相应的乙氧基化所得到的产物作为B组分，可以达到特别好的结果。蓖麻子油通常含有80-85％重量的蓖麻油酸甘油酯，大约7％重量的油酸甘油酯，大约3％重量的亚油酸甘油酯，大约2％重量的软脂酸甘油酯和大约1％重量的硬脂酸甘油酯。
用5-15mol环氧乙烷转化的蓖麻子油在商业上名为EmulanELP(BASF公司的产品)，可以买到。Emulan ELP主要用作植物油的乳化剂，如：花生油、椰子油、亚麻油、玉米油、橄榄油、棕榈油、棕榈仁油、菜籽油、蓖麻子油，大豆油或葵花子油的乳化剂。
本发明的对象还在于应用转化了的甘油酯作为聚烯烃蜡的水分散体的分散剂，转化了的甘油酯是由1-50mol的具有2-4C-原子的1，2-环氧烷与主要为乙烯性单不饱和或多不饱和的、还可以带有羟基的C16-C22-一元羧酸转化而成的甘油酯，聚烯烃蜡的水分散体含有聚乙烯蜡或聚丙烯蜡，蜡的平均颗粒大小为1-50μm，其酸值小于5mg KOH/g蜡。
本发明所述的稳定的聚烯烃蜡的水分散体首先被用于制造地板蜡和石料上光剂(stone polish)、鞋油、汽车保护剂、印刷油墨、印染浆料、油漆、特别是水溶性漆、包装，例如食品包装、润滑脂、凡士林、拉丝剂(drawing agent)、电器元件的密封材料和绝缘材料、水溶性的木料清漆、热熔性涂层、化妆品和牙膏，用于塑料加工，用于造纸和用于防蚀、织物和纱线的处理，皮革的加工以及有色金属的冷铸、压铸和离心铸造时的分型剂。
本发明所述的蜡分散体在这里主要用于改善磨擦性能或耐磨擦性，因此由于它的特殊颗粒大小特别适合于此。
本发明所述的分散体在毒物学方面全然不用担心，因此可以毫无问题地用于生活用品方面和化妆品。从生态学角度它也同样是全然不用担心的，因为在这里涉及的乳化剂是以天然物质为基础的或者是类似天然的物质。
本发明所述的蜡分散体实际上是无限期稳定的，也就是说，经过数月或数年的存放，它本身不会沉积在容器壁上和底上。由于高的平均颗粒大小，带来了所希望的应用性能。本发明所述的分散体的制备方法简单、不成问题。并且高的固体浓度也有利于成品的存贮和运输。
实施例
将6.5g用5-15mol环氧乙烯转化了的蓖麻子油(EmulanELP，BASF公司产)事先置于43.5g彻底脱离子的水中，在强烈的搅拌下，将50g微细化了的聚乙烯蜡在20℃搅入其中，该蜡的重均分子量为3,000，酸值(按DIN 53 402)为＜0.1mg KOH/g(LuwaxAF30，BASF公司产)。该蜡的颗粒大小为大约8μm(用Coulter Counter法测定)。
得到的蜡分散体按Brookfield法测定的粘度为600mm2/S，无限期的稳定(无相分离)。

Claims (8)

1.稳定的聚烯烃蜡的水分散体，包括
A)5-65％重量的平均颗粒大小为1-50μm及酸值小于5mg KOH/g蜡的聚乙烯蜡或聚丙烯蜡；和
B)作为分散剂的0.5-20％重量的用1-50mol的具有2-4C原子的1，2-环氧烷转化了的甘油酯，该甘油酯为主要由乙烯性单不饱和或多不饱和的C16-C22-一元羧酸所形成的酯，这类酸可以还含有羟基。
2.按权利要求1所述的稳定的聚烯烃蜡的水分散体，包括作为A组分的平均颗粒大小为3-20μm、酸值小于2mgKOH/g蜡的聚乙烯蜡或聚丙烯蜡。
3.按权利要求1或2所述的稳定的聚烯烃蜡的水分散体，包括
A)20-55％重量的A组分；和
B)3-12％重量的B组分。
4.按权利要求1-3之一所述的稳定的聚烯烃蜡的水分散体，包括作为B组分的用3-20mol环氧乙烷转化了的甘油酯，该甘油酯为由主要为乙烯性单不饱和至三不饱和的C18-一元羧酸形成的酯，这些酸的至少一部分还含有羟基。
5.按权利要求4所述的稳定的聚烯烃蜡的水分散体，其中乙氧基化了的甘油酯B主要含有12-羟基-9-顺式-十八烯酸(蓖麻油酸)作为C18-一元羧酸。
6.按权利要求5所述的稳定的聚烯烃蜡的水分散体，其中使用天然蓖麻子油的乙氧基化产物作为B组分。
7.用1-50mol具有2-4C原子的1，2-环氧烷转化了的甘油酯作为聚烯烃蜡水分散体的乳化剂之应用，该甘油酯由主要是乙烯性单不饱和或多不饱和的C16-C22-一元羧酸形成的酯，这类酸还可以含有羟基，聚烯烃蜡的水分散体含有平均颗粒大小为1-25μm且酸值小于5mg KOH/g蜡的聚乙烯蜡或聚丙烯蜡。
8.按权利要求1-6之一所述的稳定的聚烯烃蜡水分散体在以下方面的应用：用于制造地板蜡和石料上光剂、鞋油、汽车保护剂、印刷油墨、印染浆料、油漆、包装、润滑脂、凡士林、拉丝剂(drawing agent)、电器元件的密封材料和绝缘材料、水溶性木料清漆、热熔性涂层、化妆品和牙膏，用于塑料加工，用于造纸和用于防蚀，用于织物和纱线处理和皮革的加工以及有色金属的冷铸、压铸和离心铸造时作为分型剂。
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