CN106009953B - 水性聚烯烃分散液涂层和制得方法 - Google Patents
水性聚烯烃分散液涂层和制得方法 Download PDFInfo
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- CN106009953B CN106009953B CN201610149880.8A CN201610149880A CN106009953B CN 106009953 B CN106009953 B CN 106009953B CN 201610149880 A CN201610149880 A CN 201610149880A CN 106009953 B CN106009953 B CN 106009953B
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- polyolefin
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- olefin
- melt
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- 229920000098 polyolefin Polymers 0.000 title claims abstract description 164
- 239000006185 dispersion Substances 0.000 title claims abstract description 93
- 238000000576 coating method Methods 0.000 title claims abstract description 71
- 239000011248 coating agent Substances 0.000 title claims description 59
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 124
- 239000000203 mixture Substances 0.000 claims abstract description 101
- 239000003381 stabilizer Substances 0.000 claims abstract description 54
- 239000011159 matrix material Substances 0.000 claims abstract description 51
- 239000007822 coupling agent Substances 0.000 claims abstract description 48
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 44
- 150000001336 alkenes Chemical class 0.000 claims abstract description 38
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 38
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 37
- 239000002530 phenolic antioxidant Substances 0.000 claims abstract description 34
- 239000002253 acid Substances 0.000 claims abstract description 31
- 239000000155 melt Substances 0.000 claims abstract description 26
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 23
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- 238000000034 method Methods 0.000 claims description 21
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
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- 229920001155 polypropylene Polymers 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 19
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- 239000004698 Polyethylene Substances 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 16
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 11
- 235000013305 food Nutrition 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 8
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- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 4
- YAPRWCFMWHUXRS-UHFFFAOYSA-N (2-hydroxyphenyl) propanoate Chemical compound CCC(=O)OC1=CC=CC=C1O YAPRWCFMWHUXRS-UHFFFAOYSA-N 0.000 claims description 3
- XMIIGOLPHOKFCH-UHFFFAOYSA-N 3-phenylpropionic acid Chemical group OC(=O)CCC1=CC=CC=C1 XMIIGOLPHOKFCH-UHFFFAOYSA-N 0.000 claims description 3
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 230000003472 neutralizing effect Effects 0.000 abstract description 8
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- 239000002585 base Substances 0.000 description 29
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 14
- 239000005977 Ethylene Substances 0.000 description 14
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 13
- 150000001412 amines Chemical class 0.000 description 12
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 12
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000004908 Emulsion polymer Substances 0.000 description 4
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
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- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 3
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- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 description 2
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- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明提供适用于金属涂层,如罐涂层的水性聚烯烃分散液组合物,其包含一种或多种聚烯烃基质聚合物;一种或多种至少部分中和的烯烃稳定剂,其酸值(AN)为80到250,优选聚烯烃稳定剂,如烯烃‑羧酸共聚物或两种此类聚合物的掺合物;任选的偶合剂,其酸值(AN)为10到70并且其熔融指数为500到5,000,000,其为在190℃下在10分钟内用装载有2.16kg的柱塞传送通过经加热的注射器或圆筒的聚合物熔体克数,所述偶合剂优选为聚合物;以及分散于所述聚烯烃分散液组合物中的含酯键受阻酚类抗氧化剂。所述含酯键受阻酚类抗氧化剂可以用聚烯烃基质聚合物、聚烯烃稳定剂或为聚合物的偶合剂母料化,与其余的聚烯烃组合物熔融混合并且随后与水性介质和中和剂一起分散以形成水性分散液。
Description
本发明涉及水性聚烯烃分散液涂层,如经涂布的金属物品、其对应的组合物和其制得方法,所述组合物包含一种或多种聚烯烃基质聚合物、一种或多种烯烃稳定剂、一种或多种偶合剂以及分散在其中的含酯键受阻酚类抗氧化剂。更确切地说,本发明涉及制得聚烯烃分散液的方法,其包含熔融掺合(i)包括抗氧化剂的所有材料或(ii)熔融掺合不为抗氧化剂的所有材料,并且单独地将抗氧化剂熔融掺合到选自聚烯烃基质聚合物、聚烯烃稳定剂、偶合剂或其混合物的聚烯烃中以制得抗氧化剂分散液(粒子或球粒),并且使来自(i)或(ii)的所有熔融掺合的材料分散到水性介质中以形成水性聚烯烃分散液。
聚烯烃分散液(POD)适用于金属包装(例如饮料和食品金属容器、喷雾罐)以及一般工业金属涂层应用。然而,如聚丙烯和聚乙烯的聚烯烃材料容易在形成涂层所需的170℃至375℃的高温下热降解。此类热降解是时间相关性的并且由涂层劣化证明,如耐溶剂性(MEK双重摩擦性能)的劣化或显示归因于氧化产物的峰值增长的涂层的红外(IR)光谱所示。
朗加德(Lundgard)等人的美国专利第8779053号公开用于金属涂层应用的聚烯烃分散液。抗氧化剂通过使其溶解于共溶剂中并且将其添加到水性分散液的连续相中来后添加到涂料配制品中。然而,由其得到的组合物并不维持金属涂层应用所需的热稳定性水平。
本发明人致力于解决提供金属涂层和其对应的组合物的问题,其使得能够提供在整个处理过程中和处理后具有极好的热稳定性的涂层或膜。
发明内容
1.根据本发明,水性聚烯烃分散液组合物包含以下各者的粒子作为分散相:一种或多种选自聚烯烃、羧酸官能聚烯烃以及羧酸酯官能聚烯烃的聚烯烃基质聚合物,优选聚烯烃,以聚烯烃分散液组合物的总固体计为1到40wt.%,或优选10到25wt.%;一种或多种至少部分中和的烯烃稳定剂,优选聚烯烃稳定剂,以聚烯烃分散液组合物的总固体计为0到50wt.%,或优选2到30wt.%,或更优选5wt.%或更多;一种或多种偶合剂,其酸值(AN)为10到70,或优选小于60,或优选为35到55,并且其熔融指数为500到5,000,000,优选1000或更大,其为在190℃下在10分钟内用装载有2.16kg的柱塞传送通过经加热的注射器或圆筒的聚合物熔体克数,或替代地,其粘度为75到10,000,优选150或更高,其为经由DIN 53019方法(2010),针对其中超过50wt.%的聚合物包含呈聚合形式的乙烯的聚合物在140℃下获取以及针对其中超过50wt.%的聚合物包含呈聚合形式的丙烯的聚合物在170℃下获取的mPa.s,所述偶合剂优选为顺丁烯二酸酐接枝的聚烯烃;以及分散于聚烯烃基质聚合物、聚烯烃稳定剂或为聚合物的偶合剂中的至少一种中的至少一种含酯键受阻酚类抗氧化剂。
2.根据上述项目1的组合物,其中所述抗氧化剂是包含至少一种羟苯基丙酸酯的酚类抗氧化剂。
3.根据上述项目1或2中的任一个的组合物,其中所述抗氧化剂是苯丙酸,3-(1,1-二甲基乙基)-β-[3-(1,1-二甲基乙基)-4-羟基苯基]-4-羟基-β-甲基-1,1′-(1,2-乙烷二基)酯。
4.根据上述项目1、2或3中的任一个的组合物,其进一步包含第二种或更多种抗氧化剂。
5.根据上述项目1、2、3或4中的任一个的组合物,其中含酯键受阻酚类抗氧化剂的总装载量在总聚烯烃分散液组合物固体的200ppm到10000ppm,或优选400或更大,或600到5,000ppm,或更优选800到3,000ppm范围内。
6.根据上述项目1、2、3、4或5中的任一个的组合物,其中所述一种或多种聚烯烃基质聚合物选自羧酸官能聚烯烃和羧酸酯官能聚烯烃,并且其熔融指数为0.3到50,或优选15或更少,其为针对其中超过50wt.%的聚合物包含呈聚合形式的乙烯的聚合物在190℃下用装载有2.16kg的柱塞以及针对其中超过50wt.%的聚合物包含呈聚合形式的丙烯的聚合物在230℃和2.16kg装载量下在10分钟内传送通过经加热的注射器或圆筒的聚合物熔体克数,并且其酸值(AN)为0.5到小于80,或优选1到20,或当组合物不包含偶合剂时优选为45-80。
7.根据上述项目1、2、3、4、5或6中的任一个的组合物,其中所述量的一种或多种至少部分中和的烯烃稳定剂具有80到250,或优选100或更大,或优选至多200,并且其中所述聚烯烃分散液组合物包含羧酸基团,其50%到300%经碱中和,或优选70%到200%经碱中和,所述碱优选为挥发性胺,或更优选为挥发性叔胺。
8.根据上述项目1、2、3、4、5、6、或7中的任一个的组合物,其中所述一种或多种至少部分中和的烯烃稳定剂包含烯烃-羧酸共聚物,优选乙烯丙烯酸(EAA)或乙烯甲基丙烯酸(EMAA)。
9.根据上述项目1、2、3、4、5、7或8中的任一个的组合物,其中所述一种或多种聚烯烃基质聚合物是选自以下的聚烯烃:聚乙烯;聚丙烯;聚(α-烯烃)共聚物,如聚(乙烯丙烯)、聚(乙烯丁烯)或聚(乙烯辛烯);聚(α-烯烃)三元共聚物,如EPDM;以及其中的任一种的掺合物。
10.根据本发明的另一个方面,涂层包含衬底,在其上具有含以下各者的聚烯烃分散液组合物的一个或多个层或膜:一种或多种选自聚烯烃、羧酸官能聚烯烃以及羧酸酯官能聚烯烃的聚烯烃基质聚合物,以聚烯烃分散液组合物的总固体计为1到40wt.%,或优选10到25wt.%;一种或多种烯烃稳定剂,其酸值(AN)为80到250,或优选100或更大,或优选至多200,以聚烯烃分散液组合物的总固体计为0到50wt.%,或优选2到30wt.%,或更优选5wt.%或更大;一种或多种偶合剂,其酸值(AN)为10到70,小于60,或优选为35到55,并且其熔融指数为500到5,000,000,优选1000或更大,其为在190℃下在10分钟内用装载有2.16kg的柱塞传送通过经加热的注射器或圆筒的聚合物熔体克数,或替代地,其粘度为75到10,000,优选150或更高,其为经由DIN 53019方法(2010),针对其中超过50wt.%的聚合物包含呈聚合形式的乙烯的聚合物在140℃下测量以及针对其中超过50wt.%的聚合物包含呈聚合形式的丙烯的聚合物在170℃下测量获取的mPa.s,所述偶合剂优选为顺丁烯二酸酐接枝的聚烯烃;以及分散于聚烯烃分散液组合物中的至少一种含酯键受阻酚类抗氧化剂。
11.根据上述项目10的涂层,其中所述受阻酚类抗氧化剂包含至少一种羟苯基丙酸酯,优选为苯丙酸,3-(1,1-二甲基乙基)-β-[3-(1,1-二甲基乙基)-4-羟基苯基]-4-羟基-β-甲基-1,1′-(1,2-乙烷二基)酯或其与一种或多种第二抗氧化剂,如受阻酚类抗氧化剂的组合。
12.根据上述项目10或11中的任一个的涂层,其中含酯键受阻酚类抗氧化剂的总装载量在总聚烯烃分散液组合物固体的200ppm到10000ppm,或优选600到5,000ppm,或更优选800到3,000ppm范围内。
13.根据上述项目10、11或12中的任一个的涂层,其中所述量的一种或多种烯烃稳定剂包含烯烃-羧酸共聚物,优选乙烯丙烯酸(EAA)或乙烯甲基丙烯酸(EMAA)。
14.根据上述项目10、11、12或13中的任一个的涂层,其中所述一种或多种聚烯烃基质聚合物包含聚乙烯、聚丙烯、聚(α-烯烃)共聚物、聚(α-烯烃)三元共聚物以及其中的任一种的掺合物。
15.根据上述10、11、12、13、或14中的任一个的涂层,其中所述衬底是金属的,或优选金属容器、盖子以及封盖中的任一种,或更优选用于食品或饮料的金属容器或盖子以及封盖中的任一种。
16.根据上述10、11、12、13、14或15中的任一个的涂层,其中厚度为10微米的涂层展现根据ASTM D 5402-06,方法3(2011),使用每2.54cm×2.54cm正方形具有28×24根细线的漂厚棉布(级别50)以及906g(32盎司)圆头锤的100次双重摩擦或更多次,或优选150次或更多次,或更优选200次或更多次直到涂层被穿透并且衬底在任何区域中都变得可见为止的甲基乙基酮双重摩擦耐性,其中所述布用线固定到所述锤的平端并且抵着涂层跨过涂层来回摩擦,每25次双重摩擦将布再浸渍到MEK中。
17.根据本发明的另一个方面,制得上述1到9中的任一个的组合物的方法包含熔融掺合i)受阻酚类抗氧化剂、聚烯烃基质聚合物、烯烃稳定剂以及偶合剂(若存在),或(ii)熔融掺合(a)聚烯烃基质聚合物、偶合剂(若存在)和烯烃稳定剂,以及(b)单独地熔融掺合聚烯烃基质聚合物、聚烯烃稳定剂或为聚合物的偶合剂中的任一种中的含酯键受阻酚类抗氧化剂以形成抗氧化剂分散液,继而使用分散设备,优选挤压机或连续高剪切混合器,在水中连同所需量的一种或多种挥发性碱分散(i)的熔体或熔体(ii)(a)和(b)以形成水性分散液组合物。
18.根据本发明的又一个方面,制得上述10到16中的任一个的涂层的方法包含将以下各者的分散相粒子的水性聚烯烃分散液组合物施加到金属衬底上:一种或多种选自聚烯烃、羧酸官能聚烯烃以及羧酸酯官能聚烯烃的聚烯烃基质聚合物,以聚烯烃分散液组合物的总固体计为1到40wt.%,或优选10到25wt.%;一种或多种至少部分中和的烯烃稳定剂,优选为聚烯烃稳定剂,其酸值(AN)为80并且至多250,或优选100到200,以聚烯烃分散液组合物的总固体计为0到50wt.%,或优选2到30wt.%,或更优选5wt.%或更大;一种或多种偶合剂,优选地,其酸值(AN)为10到70,小于60,或为35到55,并且其熔融指数为500到5,000,000,优选1000或更大,其为在190℃下在10分钟内用装载有2.16kg的柱塞传送通过经加热的注射器或圆筒的聚合物熔体克数,或替代地,其粘度为75到10,000,优选150或更高,其为经由DIN 53019方法(2010),针对其中超过50wt.%的聚合物包含呈聚合形式的乙烯的聚合物在140℃下测量以及针对其中超过50wt.%的聚合物包含呈聚合形式的丙烯的聚合物在170℃下测量获取的mPa.s,所述偶合剂优选为顺丁烯二酸酐接枝的聚烯烃;并且具有分散于聚烯烃分散液组合物中的含酯键受阻酚类抗氧化剂;以及例如在170℃到375℃,或优选180℃到260℃下加热由此施加的组合物以形成涂层,优选例如在230℃到260℃下急骤固化5秒到2分钟的时间。
除非另外指示,否则所有温度和压力单位是室温和标准压力(STP)。
所有包含圆括号的短语都指示所包括的括号中的物质和其不存在中的任一者或两者。举例来说,在替代方案中短语“(甲基)丙烯酸酯”包括丙烯酸酯和甲基丙烯酸酯。
所列举的所有范围都是包括性的并且可组合。举例来说,10到70,小于60,或优选35到55的酸值(AN)的公开内容将包括10到70的AN、10到60的AN、60到70的AN、10到35的AN、10到55的AN、35到60的AN、35到70的AN以及55到60的AN、55到70的AN、60到70的AN,或优选35到55的AN。
如本文所使用,术语“酸值或AN”意指作为当通过滴定进行测量时中和酸官能团所需的以mg KOH/g聚合物计的KOH的量的数量并且根据ASTM D-1386(2010)测量。
如本文所使用,术语“ASTM”是指宾夕法尼亚州西康舍霍肯ASTM国际性组织(ASTMInternational,West Conshohocken,PA)的出版物。
如本文所使用,用以测量熔融温度、结晶温度和焓的术语“差示扫描热量测定或DSC”实验根据ASTM D-3418(2012)进行。
如本文所使用的术语“DIN”是指德国柏林的布斯出版公司(Beuth Verlag GmbH)(独家(Alleinverkauf))出版的德国语言材料说明书。
如本文所使用,除非另外说明,否则术语“熔融指数”意指根据ASTM D-1238(2013)测定的值。熔融指数值定义为针对其中超过50wt.%的共聚物包含呈聚合形式的乙烯的聚乙烯聚合物在190℃和2.16kg装载量下以及针对超过50wt.%的共聚物包含呈聚合形式的丙烯时的聚丙烯聚合物在230℃和2.16kg装载量下装载的柱塞以dg/min(或g/10min)传送通过经加热的注射器的聚合物熔体的量。
如本文所使用,术语“熔点”意指通过DSC方法使用10℃/min的缓变率测定的值。
如本文所使用,术语“固体”或“总固体”是指一种或多种聚烯烃基质聚合物、一种或多种烯烃稳定剂、一种或多种偶合剂和一种或多种抗氧化剂以及(若存在)颜料、填充剂或增量剂和在本发明组合物的使用条件下不挥发的任何添加剂的固体的组合物的wt.%。举例来说,水、在本发明组合物的使用条件下挥发的添加剂,如聚结剂和溶剂或碱,如氨或低级烷基胺不被认为是固体。根据修改后的ASTM D2369方法(2011),使用OHAUS水分分析器,在干燥温度设定在150℃下的情况下测量固体值。
如本文所使用,术语“挥发性碱”意指在标准压力下在室温到250℃的温度下挥发的碱。
如本文所使用,术语“wt.%”是指重量%。
本发明组合物适用于制得用于金属容器的涂层,如符合食品接触顺应性要求并且不含有有意添加的双酚A的饮料和食品罐。根据本发明,组合物和涂层包含分散于水性聚烯烃分散液组合物中,即在聚合相中或与聚合相一起的受阻酚类抗氧化剂,尤其含酯键受阻酚类抗氧化剂的聚烯烃基质聚合物组合物。抗氧化剂的聚合物熔体掺合提供水性聚烯烃分散液,其中抗氧化剂并入分散相中。此使得能够更有效使用较少食品接触涂层的抗氧化剂并且避免在通过溶解于共溶剂中或其它已知方法将抗氧化剂添加到组合物中时产生的相不稳定性。此外,对于需要高温固化的金属涂层应用,如饮料和食品罐涂层,水性聚烯烃分散液和由其得到的涂层展现所需的热稳定性以耐受超过200℃的工艺温度。经由适当的处理步骤和选择抗氧化剂(AO)化学性质,本发明提供一种制备改良来自用于需要高温固化的金属涂层应用的聚烯烃分散液的涂层的热稳定性的分散液的新颖方式。
聚烯烃基质聚合物可以包含在固化条件下将形成膜的任何聚烯烃以制得根据本发明的涂层。一般来说,其选自聚烯烃、羧酸官能聚烯烃以及羧酸酯官能聚烯烃。
适合的聚烯烃可以选自一种或多种聚乙烯、聚丙烯聚(α-烯烃)共聚物、聚(α-烯烃)三元共聚物以及其中的任一种的掺合物。
适合的聚烯烃基质聚合物可以是熔点为至少60℃或至少90℃,或100℃或更大,或125℃或更大的任何聚合物。此类聚合物可以包括高密度聚乙烯(HDPE)、聚丙烯、乙烯-丙烯共聚物、乙烯-丁烯共聚物、乙烯-己烯共聚物、乙烯-辛烯共聚物、乙烯-丙烯酸乙酯共聚物、乙烯-丙烯-亚乙基降冰片烯三元共聚物、烯烃嵌段共聚物(如乙烯-丙烯和乙烯-辛烯嵌段共聚物)以及酸改性的聚烯烃,其熔融指数为0.3到50,或优选15或更小,其为针对其中超过50wt.%的聚合物包含呈聚合形式的乙烯的聚合物在190℃和2.16kg装载量下以及针对其中超过50wt.%的聚合物包含呈聚合形式的丙烯的聚合物在230℃和2.16kg装载量下装载的柱塞在10分钟内传送通过经加热的注射器的聚合物熔体克数,并且其酸值(AN)为0.5到小于80,或优选1到20,或当组合物不包含偶合剂时,优选45-80。
适合的聚乙烯可以选自聚乙烯、乙烯-共聚物、乙烯-丙烯-二烯三元共聚物以及其组合。示例性乙烯聚合物还可以包括如例如美国专利第3,645,992号中所描述的均质聚合物;如例如美国专利第4,076,698号中所描述的高密度聚乙烯(HDPE);有非均质分枝的线性低密度聚乙烯(LLDPE);有非均质分枝的超低线性密度聚乙烯(ULDPE);有均质分枝的线性乙烯/丙烯或乙烯/α-烯烃共聚物;有均质分枝的实质上呈线性的乙烯/丙烯或乙烯/α-烯烃聚合物,所述聚合物可以例如通过美国专利第5,272,236号和第5,278,272号中所公开的方法制备;以及高压自由基聚合的乙烯聚合物和共聚物,如低密度聚乙烯(LDPE)。
适合的聚合物的其它实例包括(但不限于)α-聚烯烃共聚物,如乙烯丙烯酸乙酯共聚物、乙烯丙烯酸甲酯、乙烯丙烯酸丁酯;乙烯-C4到C12烯烃共聚物,如乙烯-丁烯、乙烯-己烯或乙烯辛烯共聚物;乙烯-丙烯-丁烯三元共聚物;以及其组合。
聚烯烃基质聚合物可以包括衍生自丙烯聚合的单元和衍生自一种或多种α-烯烃共聚单体聚合的聚合单元。适合的共聚单体的实例是C2和C4到C10α-烯烃;例如C2、C4、C6和C8α-烯烃。聚烯烃基质聚合物可以包括1到40wt.%衍生自一种或多种α-烯烃共聚单体的单元,例如3wt.%,或7wt.%到35wt.%,或20wt.%。举例来说,基质聚合物可以包含1到35重量%衍生自一种或多种α-烯烃共聚单体的单元。
聚烯烃基质聚合物可以一方面包括60到100,优选80和99,或更优选85到99wt.%衍生自乙烯(例如高密度聚乙烯)或丙烯的聚合的单元,并且另一方面,其余单元衍生自至少一种其它α-烯烃的聚合。
聚烯烃基质聚合物可以具有大于0.88克/立方厘米(g/cm3)的密度。举例来说,包含聚烯烃的基质聚合物可以具有在0.88到1.1g/cm3、0.89到1.0g/cm3、0.90到0.98g/cm3或0.91到0.97g/cm3范围内的密度。举例来说,聚烯烃基质聚合物可以包含聚丙烯高密度聚乙烯、中密度聚乙烯、低密度聚乙烯或其组合。如本文所使用,“高密度聚乙烯”是指密度在0.93到0.97克/立方厘米(g/cm3)范围内的聚乙烯。
可获得的聚乙烯和α-聚烯烃共聚物包括(但不限于)作为VERSIFYTM DP-4000.01、VERSIFYTM 4200、VERSIFYTM 4000、VERSIFYTM 3200、VERSIFYTM 3000和VERSIFYTM3300可获得的聚合物(密歇根州米德兰市陶氏化学公司(The Dow Chemical Company,Midland,MI));ENGAGETM 8407聚合物(陶氏);INFUSETM 9807聚合物(陶氏);VISTAMAXXTM含丙烯弹性体(得克萨斯州休斯顿埃克森美孚化学公司(ExxonMobil Chemical,Houston,TX));可商购的高密度聚乙烯,如(但不限于)DMDA 8940NT 7(熔融指数44,密度0.951)、DMDA-8007NT 7(熔融指数8.3,密度0.965)、DMDC-8910NT7(熔融指数10,密度0.943)、DMDA-1210NT 7(熔融指数10,密度0.952)、HDPE 17450N(熔融指数17,密度0.950)、DMDA-8920NT 7(熔融指数20,密度0.954)、DMDA 8940NT 7(熔融指数44,密度0.951)、DMDA-8950NT 7(熔融指数50,密度0.942)、DMDA-8965-NT 7(熔融指数66,密度0.952)、DMDA-8940HDPE(熔融指数大致40-48g/10min),全部来自陶氏化学公司。
适用作聚烯烃基质聚合物的适合的聚丙烯可以包括(但不限于)6D43聚丙烯(宾夕法尼亚州费城布拉斯科(Braskem,Philadelphia,PA))。
可商购的羧酸官能聚烯烃基质聚合物的实例可以包括例如顺丁烯二酸酐官能化聚乙烯,包括以商品名AMPLIFYTM(密歇根州米德兰市陶氏化学公司)获得的那些,尤其如AMPLIFYTM GR-204聚合物。AmplifyTMGR-204是经2,5-呋喃二酮改性的乙烯/己烯-1聚合物。
适合的烯烃稳定剂可以是例如α-烯烃和具有不饱和键、含有任何羧酸、盐或酸酐基团的单体的任何经部分或完全中和的共聚物,其AN为80或更大,或110或更大,或140或更大并且至多250,如乙烯丙烯酸共聚物、乙烯甲基丙烯酸共聚物和/或酸改性的聚烯烃,如顺丁烯二酸酐接枝的聚烯烃以及/或其掺合物。
适合的烯烃稳定剂还可以包括例如具有14到45个碳,优选16到36个碳的长链线性羧酸,如线性脂肪酸,例如UnicidTM 350分散剂或二十二烷酸(C22)。
本发明的烯烃稳定剂可以包括一种或多种例如具有作为共聚单体或接枝单体的极性基团的极性聚烯烃。
烯烃稳定剂可以包括(但不限于)两亲性共聚物组合物,所述共聚物包括5到95wt.%一种或多种酸官能单体和5到95wt.%一种或多种可共聚烯系不饱和疏水性单体(如α烯烃)的反应产物。这些物质可以例如在中和之后是水可溶的和/或可乳化的,并且可以充当胶态稳定剂。
适用于产生烯烃稳定剂组合物的酸官能单体包括(但不限于)含有羧酸、膦酸、次膦酸、磺酸、磺酸基团的烯系不饱和单体以及随后水解的酸酐。适合的实例包括(甲基)丙烯酸、顺丁烯二酸、反丁烯二酸、衣康酸、乙烯基膦酸、(甲基)丙烯酸磷乙酯以及乙烯基磺酸。
烯烃稳定剂可以所任何经部分或完全中和的酸官能烯烃共聚物分散剂,如羧酸官能烯烃共聚物,如乙烯/(甲基)丙烯酸共聚物,如作为NucrelTM(杜邦(DuPont))或EscorTM(埃克森美孚)聚合物可获得的那些。
烯烃稳定剂可以包括内部表面活性剂。内部表面活性剂是在分散液制备期间会化学反应成聚烯烃的表面活性剂。
本发明的烯烃稳定剂经中和剂至少部分中和。中和剂的实例包括(但不限于)金属氢氧化物、碳酸酯、胺以及其组合,优选为胺,并且更优选为不是伯胺(例如不是氨)并且是仲胺或叔胺的挥发性胺。
本发明的烯烃稳定剂中的酸官能团在50%到300%,或优选70%到200%范围内经中和。如果酸官能团未充分中和,那么水性聚烯烃分散液粒度变得过大。如本文所使用,术语“中和%”是指所有聚烯烃分散液组合物中的酸基团的摩尔%。
烯烃稳定剂的实例包括(但不限于)至少部分中和的乙烯-丙烯酸和乙烯-甲基丙烯酸共聚物,其以用于制得含烯烃分散剂的单体的总重量计,包含12到25wt.%含酸基共聚单体。此类含烯烃分散剂的实例包括以商标PRIMACORTM可获得的那些,如PRIMACORTM 5980i或PRIMACORTM 5990i,两种都可购自陶氏化学公司;NUCRELTM聚合物(特拉华州威明顿市杜邦公司(E.I.DuPont de Nemours,Wilmington,DE));以及ESCORTM聚合物(埃克森美孚化学公司)以及美国专利第4,599,392号、第4,988,781号和第5,938,437号中所描述的那些。
本发明的偶合剂可以包括具有所需酸值(AN)和所需熔融指数的任何材料,所述熔融指数为500到5,000,000,优选1000或更大,其为在190℃下在10分钟内用装载有2.16kg的柱塞传送通过经加热的注射器或圆筒的聚合物熔体克数,或替代地,其粘度为75到10,000,优选150或更高,其为经由DIN 53019方法(2010),针对其中超过50wt.%的聚合物包含呈聚合形式的乙烯的聚合物在140℃下获取以及针对其中超过50wt.%的聚合物包含呈聚合形式的丙烯的聚合物在170℃下获取的mPa.s,所述偶合剂可以改良本发明的聚烯烃基质聚合物与烯烃稳定剂之间的相容性。偶合剂的熔融指数将明显高于针对聚烯烃基质聚合物和任何聚烯烃稳定剂的对应测量值,并且可以较高以使得粘度可以是定义偶合剂的较佳实际量度。
适合的聚合偶合剂可以包含酸官能改性的聚烯烃,优选为顺丁烯二酸酐聚烯烃共聚物、顺丁烯二酸酐接枝的聚烯烃或顺丁烯二酸酐改性的聚乙烯蜡或顺丁烯二酸酐改性的聚丙烯蜡。
偶合剂可以是具有10到70,小于60或35-55的酸值和500到5,000,000,优选1000或更大的熔融指数(其为在190℃下在10分钟内用装载有2.16kg的柱塞传送通过经加热的注射器或圆筒的聚合物熔体克数)或替代地具有75到10,000,优选150或更高的粘度(其为经由DIN 53019方法(2010),针对其中超过50wt.%的聚合物包含呈聚合形式的乙烯的聚合物在140℃下测量以及针对其中超过50wt.%的聚合物包含呈聚合形式的丙烯的聚合物在170℃下测量的mPa.s)的任何改性的聚烯烃。
本发明的聚合偶合剂可以包括酸或酸酐改性的聚烯烃。举例来说,偶合剂可以选自由以下组成的群组:酸官能化聚丙烯、酸官能化聚乙烯均聚物、已经用羧酸基改性的共聚物、已经用酸酐基团改性的共聚物以及其组合。
其它适合的偶合剂可以包括改性的聚烯烃接枝共聚物和/或嵌段共聚物,如丙烯-顺丁烯二酸酐接枝共聚物。
适用作偶合剂的改性的聚烯烃的特定实例可以包括例如顺丁烯二酸酐官能化聚乙烯、聚丙烯、乙烯和丙烯的共聚物以及其组合。实例包括(但不限于)顺丁烯二酸酐官能化聚乙烯,如高密度聚乙烯,也可以使用顺丁烯二酸酐官能化聚乙烯共聚物、三元共聚物和掺合物。顺丁烯二酸酐官能团可以通过接枝或其它反应方法并入聚合物中。接枝时,以聚合物的重量计,羧酸并入的水准低于10wt.%,如小于5wt.%。
可商购的适合的改性的聚烯烃的实例包括(但不限于)以商标名LICOCENETM或LICOLUBETM由科莱恩公司(Clariant Corporation)(新泽西州费尔劳恩市(Fair Lawn,NJ))出售的聚合物,如LICOCENETM 6452(例如LICOCENETM PP MA 6452)和LICOCENETM 4351(例如LICOCENETM PE MA 4351);以商标名A-CTM性能添加剂(新泽西州莫里斯敦哈尼威尔公司(Honeywell Corporation,Morristown,NJ))出售的聚合物,如AC575TM(其是乙烯顺丁烯二酸酐共聚物)和AC-392TM以及AC-395TM(其是高密度氧化聚乙烯);以及EPOLENETM聚合物(得克萨斯州休斯顿韦斯特莱克化学公司(Westlake Chemical Company,Houston,TX))。
除含酯键受阻酚类抗氧化剂外,还可以使用第二酚类抗氧化剂,例如季戊四醇四(3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯,其是可商购的,如可获自巴斯夫(BASF)的IRGANOXTM 1010。
可以使用任何熔体混合装置,如单螺杆挤压机或熔体反应器来制得本发明的抗氧化剂分散液,其是呈粒子、粉末或球粒形式的固体分散液。
优选地,在尽可能低的温度,如100℃到150℃,优选130℃或更低温度下将受阻酚类抗氧化剂熔融掺合成组分并且持续可能的最短掺合时间,如1到30分钟,或优选1到10分钟或更短时间。
适合的碱的实例包括挥发性碱。挥发性碱的实例包括(但不限于)N,N-二甲基乙醇胺、氨、肼、甲胺、乙胺、二乙胺、三乙胺、异丁胺、N,N-二异丙基乙胺、吗啉、哌嗪、乙二胺以及1,4-二氮杂双环[2.2.2]辛烷。酸基在碱挥发后,如在涂层的形成时(其中其可以帮助促进涂层粘合到衬底的表面)恢复到酸形式。
沸点低于250℃的胺可以用作碱。其它适合的碱可以包括例如胺,如单乙醇胺,或2-氨基-2-甲基-1-丙醇(AMP)。适用于本文所公开的实施例中的胺可以包括二乙醇胺、三乙醇胺和TRIS AMINOTM碱(伊利诺伊州布法罗格罗夫的安格斯(Angus,Buffalo Grove,IL))、NEUTROLTM TE碱(德国勒沃库森的巴斯夫(BASF,Leverkusen,DE)),以及三异丙醇胺和二异丙醇胺(陶氏化学公司)。其它适用的胺可以包括二甲胺、三甲胺、单正丙胺、丁胺、二丁胺、三丁胺、二甲基苯甲基胺、二甲基正丙胺、N-甲醇胺、N-氨基乙基乙醇胺、N-甲基二乙醇胺、单异丙醇胺、N,N-二甲基丙醇胺、2-氨基-2-甲基-1-丙醇、1,2-二氨基丙烷、三(羟甲基)-氨基甲烷、乙二胺、N,N,N′N′-四(2-羟丙基)乙二胺、3-甲氧基丙胺、亚氨基双-丙胺等。
可以使用胺的混合物。
碱可以是寡聚胺,例如二亚乙基三胺。
中和剂的其它适合的实例包括氢氧化物,如氢氧化钾、氢氧化锂以及氢氧化钠。碳酸盐的实例包括(但不限于)碳酸钠、碳酸氢钠、碳酸钾以及碳酸钙。
聚烯烃分散液组合物的水相可以是例如水;或在替代方案中,水相可以是大部分的水与小部分的一种或多种有机溶剂的混合物,例如一种或多种水可混溶溶剂。本发明的聚烯烃分散液组合物独立地包括以组合物的总重量计15到90wt.%水相。举例来说,水相含量可以在以组合物的总重量计,30到90,或35到85,或40到75wt%的范围内。
本发明的水性聚烯烃分散液组合物可以具有在8到12范围内的pH。
本发明的水性聚烯烃分散液组合物可以任选地在处理期间或之后与一种或多种交联剂掺合,所述交联剂如羟基烷基酰胺,如作为PRIMIDTM(瑞士多马特的EMS化学股份公司(EMS-Chemie AG,Domat/Ems,CH))可获得的那些、环氧基官能材料、多异氰酸酯、水可分散或水可溶酚类树脂、水可分散氨基塑料树脂或PCT公开案第WO/2011/011707号中所描述的那些。这些交联剂在本质上可以是有机或无机的(即,锌纳米粒子)。
本发明组合物也可以任选地在处理期间或之后与一种或多种添加剂或辅助聚合物掺合,如丙烯酸乳液聚合物、乙烯基丙烯酸乳液聚合物、苯乙烯丙烯酸乳液聚合物、乙酸乙烯酯乙烯乳液聚合物、环氧树脂、聚酯树脂、聚氨基甲酸酯树脂、聚酰胺树脂和其共聚物以及其组合中的一种或多种;一种或多种填充剂;一种或多种添加剂,如催化剂、湿润剂、消泡剂、助流剂、脱模剂、滑爽剂、防结块剂、遮掩硫染色的添加剂、颜料湿润剂/分散剂、抗沉降剂、UV稳定剂、粘着促进剂;一种或多种润滑剂,如脂肪酸酯蜡、含硅蜡、含氟蜡、聚乙烯或任何其它类似聚烯烃蜡、巴西棕榈蜡、羊毛脂蜡等;一种或多种腐蚀抑制剂,如铝和锌:一种或多种颜料,例如二氧化钛、硫酸钡、云母、碳酸钙、二氧化硅、氧化锌、磨碎玻璃、三水合铝、滑石、三氧化锑、飞灰和粘土等;一种或多种共溶剂,例如二醇、二醇醚、2,2,4-三甲基-1,3-戊二醇单异丁酸酯、醇、矿油精、芳香族溶剂和苯甲酸酯等;一种或多种分散剂,例如氨基醇和聚羧酸酯;一种或多种表面活性剂;一种或多种防腐剂,例如杀生物剂、杀霉剂、杀真菌剂、除藻剂以及其组合;一种或多种增稠剂,例如含纤维素增稠剂,如羟乙基纤维素、疏水改性碱可溶乳液(HASE增稠剂,如UCAR POLYPHOBE TR-116)和疏水改性乙氧基化氨基甲酸酯增稠剂(HEUR);或一种或多种其它中和剂,例如氢氧化物、胺、氨和碳酸盐;任选的一种或多种溶剂或聚结剂。
另外,本发明组合物可以与一种或多种其它分散液、乳液、悬浮液、胶态悬浮液等掺合。
本发明组合物可以通过所属领域的技术人员认可的多种方法形成。
制得任何聚烯烃分散液组合物的方法包含熔融掺合i)受阻酚类抗氧化剂、聚烯烃基质聚合物、烯烃稳定剂以及偶合剂(若存在),或(ii)(a)聚烯烃基质聚合物、任何偶合剂、烯烃稳定剂以及(b)单独地聚烯烃基质聚合物、聚烯烃稳定剂或为聚合物的偶合剂中的任一种中的含酯键受阻酚类抗氧化剂,以形成抗氧化剂分散液,继而使用分散设备,优选挤压机或均质机或高剪切混合器,在水中连同所需量的一种或多种挥发性碱一起分散(i)的熔体或(ii)(a)和(b)的熔体,优选熔体(ii)(a)和(b)两者以形成水性分散液组合物。
分散设备可以分批、半分批或连续模式操作。用于分散的混合器的实例包括转子-定子、微流化床、高压均质机、超声波、冲击射流、考雷司叶片(Cowles blade)、行星式混合器以及熔融捏合装置,如挤压机。
本发明的抗氧化剂分散液可以通过熔融掺合受阻酚类抗氧化剂和本发明组合物中的任何热塑性聚合组分,优选一种或多种聚烯烃稳定剂或为聚合物的偶合剂形成,与聚烯烃基质聚合物、烯烃稳定剂以及任何偶合剂的熔体掺合物的形成分开。
举例来说,(i)本发明的一种或多种聚烯烃基质聚合物、偶合剂、一种或多种烯烃稳定剂以及受阻酚类抗氧化剂的熔体掺合物可以通过在挤压机中连同水相(例如水)和任何适合的一种或多种挥发性碱熔融捏合在一起以就地形成具有本发明的水性聚烯烃分散液的抗氧化剂分散液来形成。
举例来说,(ii)(a)可以在挤压机中熔融捏合一种或多种聚烯烃基质聚合物、偶合剂、一种或多种烯烃稳定剂以及任何一种或多种挥发性碱以形成熔体聚烯烃分散液,以及单独地(b)可以在挤压机中熔融捏合本发明的受阻酚类抗氧化剂和选自聚烯烃基质聚合物、为聚合物的偶合剂、聚烯烃稳定剂或其组合的任何一种或多种聚合物以形成熔体抗氧化剂分散液,继而连同水相任何一种或多种挥发性碱(例如水)一起组合(a)和(b),以形成水性聚烯烃分散液组合物。
优选地,材料(i)一起或(ii)(a)和(b)单独地可以首先在无挥发性碱或水相的情况下混配,并且随后在挤压机中在水相(例如水)和挥发性碱存在下熔融捏合,从而形成水性分散液组合物。
分散液可以首先经稀释以含有1到20wt%,例如1到5wt%或1到3wt%的水相并且接着随后,进一步稀释以包含大于25wt%的水相。
进一步稀释可以经由水和/或如本文所提供的溶剂实现。
可以使用所属领域中已知的熔融捏合装置。举例来说,使用捏合机、班拍里混合器(BANBURY mixer)、单螺杆挤压机或多螺杆挤压机,例如双螺杆挤压机。适合的挤压机系统的一个实例提供于名称为“挤压机螺杆(Extruder Screw)”的PCT公开案WO 2011/068525中。
用于生产根据本发明的组合物的方法不受特定限制。举例来说,将挤压机(在某些实施例中,例如为双螺杆挤压机)耦合到背压调节器、熔体泵或齿轮泵。示例性实施例还提供挥发性碱或中和剂储存器(碱储存器)和初始水相储存器,其中的每一个包括泵。分别从碱储存器和初始水相储存器提供所需量的挥发性碱和初始水相。可以使用任何适合的泵,例如在240巴的压力下提供150立方厘米/分钟(cc/min)的流速的泵可以用于提供碱和初始水相到挤压机。或,液体注入泵在200巴下提供300cc/min或在133巴下提供600cc/min的流速。
为了改进分散性,可以在预热器中预加热挥发性碱或中和剂和初始水相。
可以将呈球粒、粉末或薄片形式的任何聚烯烃基质聚合物从馈料机馈入基质聚合物进行熔融或混配的挤压机的入口。
含有受阻酚类抗氧化剂的聚烯烃基质聚合物、聚烯烃稳定剂或为聚合物的偶合剂(例如改性的聚烯烃)的任何母料或抗氧化剂分散液可以与聚烯烃基质聚合物和烯烃稳定剂和任何偶合剂同时经由馈料机或齿轮泵馈入到挤压机中。
聚烯烃稳定剂和(必要时)偶合剂可以混配到聚烯烃基质聚合物中,并且随后经由馈料机馈入挤压机中。
在一种方法中,聚烯烃稳定剂可以经由乳化区前的入口定量到包括聚烯烃基质聚合物的熔融化合物中。因此,聚烯烃稳定剂可以与聚烯烃基质聚合物一起添加或其可以单独地提供到挤压机。聚合物熔体随后从挤压机的混合与输送区传递到乳化区,在挤压机的乳化区中,经由入口从水相和碱储存器添加初始量的水相和碱。
在制得任何聚烯烃分散液时,可以将一种或多种偶合剂另外或专门添加到水相流。
可以在挤压机的稀释与冷却区中经由水相入口从水相储存器添加其它流体介质。典型地,在冷却区中将分散液稀释到至少30wt.%水相以形成经稀释的混合物。另外,经稀释的混合物可以稀释任何数目的次数直到达到所需的稀释水平为止。
任何分散液可以在退出挤压机或混合装置之后通过使用适合的热交换器而进一步冷却。
为了减少挤压机中的蒸气压(例如蒸汽压力)积聚并且在如转子定子混合器的第二混合装置中形成聚烯烃分散液,水相不添加到挤压机中但实际上在熔体已经从挤压机离开并且进入第二混合装置之后添加到含有熔体的物流中。
本发明组合物可以在不使用熔融捏合挤压机的情况下形成于连续高剪切混合器中。因此,包括一种或多种液体或熔融聚合物的第一物流从适合的液体泵(例如注射泵、齿轮泵或螺杆泵)供应到连续高剪切混合器。第一物流流经第一导管并且与流经第二导管的含有水相的第二物流持续合并。第一和第二物流在任何或全部烯烃稳定剂和偶合剂(各自独立地与挥发性碱或中和剂一起)存在下合并到分散设备中。这两种试剂可以添加到第一或第二物流中,或作为分离流。可以在分散设备下游添加包括水相(例如水)的第三物流。调节物流的流动速率以获得具有所需量的聚合物相和固体%的分散液。分散液可以在退出分散设备之后通过使用适合的热交换器而进一步冷却。
适合的分散设备可以是多种连续串联混合器中的任一种,例如IKA高剪切混合器、奥克斯(Oakes)转子定子混合器、罗斯混合器(Ross mixer)、希尔巴森混合器(Silversonmixer)、连续高剪切混合器或离心泵。分散器的转/分钟(rpm)设定可以用于帮助控制聚烯烃分散液中的分散相的粒度。可以加热系统以在对于泵送适合的粘度下提供聚合物和中和剂组分。经由在过程出口附近使用背压调节器、齿轮泵、计量泵或其它适合的装置控制压力来减少蒸汽形成。
单独地,辅助聚合物分散液或乳液可以用作分散液组合物的一部分水相。实例包括(但不限于)含有丙烯酸、环氧树脂、聚酯、聚氨基甲酸酯、聚烯烃、聚酰胺等的分散液、乳液、悬浮液、胶态悬浮液。
水性分散液组合物(例如其固体含量)可以具有在100到2000纳米(nm),或至多1750nm,或425到1800nm,或450到1750nm范围内的平均体积粒度直径。
在由本发明的聚烯烃分散液制备涂料组合物期间,可以在分散液配制过程之后将一种或多种填充剂、增量剂或颜料、一种或多种添加剂或辅助聚合物中的任一种添加到水性聚烯烃分散液中。
本发明组合物可以多种方法施加到衬底;例如经由滚涂、喷涂、粉末涂布、浸涂、电沉积涂布、印刷、洗涂、流涂、帘式涂布。
所得涂层的厚度可以在0.1微米(μm)到150μm,例如1μm到150μm、5μm或25μm的上限范围内。一个或多个涂层可以施加到衬底。
本发明组合物可以施加到金属衬底的至少一个表面并且随后可以经由习知干燥方法干燥以在等于100℃到375℃,或优选170℃到260℃范围内的烘箱设定点温度下形成涂层。
固化温度可以“峰金属温度或(PMT)”形式表示,意指具有涂层的金属衬底在烘箱中经固化时所应用的实际温度,其可以通过温度记录装置,如达塔帕克(Datapaq)烘箱校准器测量。涂层可以在100℃到260℃范围内的PMT下经固化。
干燥和固化温度是时间和方法相关性的。因此,在低于210℃(PMT)下,在烘箱中的固化可以耗时1-50分钟或4-15分钟。在使用急骤固化的应用,如卷材涂层中,涂层在210℃-260℃(PMT)下固化3秒到1分钟。
所使用的烘箱可以是气体燃烧烘箱、电烘箱或感应烘箱。此外,烘箱可以是多区域烘箱,其各区域温度可以独立地控制并且区域之间的停留时间可以不同。
适合的衬底可以包括例如金属衬底,例如铝、镀锡钢、无锡钢。实例包括金属、经预处理的金属,如经阳极化或经磷酸盐预处理的金属。衬底可以是用于食品或饮料容器或喷雾容器的任何衬底。
优选地,直接到金属涂层应用上制得涂层并且经涂布的金属可以用于食品/饮料金属包装。
实例:以下实例说明本发明。除非另外陈述,否则在所有以下实例中,温度是室温并且压力是大气压。
表1:聚烯烃分散液的原材料
1.德国勒沃库森(Leverkusen);2.密歇根州米德兰。
表1A:原材料
合成实例:聚烯烃分散液制备:原型分散液的固体组成保持相同,即,70wt.%聚烯烃基质聚合物/22.5%烯烃稳定剂/7.5wt%偶合剂。用以所存在的羧酸计150%理论值的二甲基乙醇胺(DMEA,安可乐斯有机物公司(Acros Organics),CAS 108-01-0)中和酸官能团(计算为聚烯烃分散液组合物中单独成分的所测量到的酸数的加权平均值)。除非另外指示,否则在以上表1或以下表2中,借助于进行转递和熔融的可控速率馈料机将包括任何母料的总树脂掺合物馈入25mm直径双螺杆挤压机中。挤压机温度分布逐渐升高到约160℃,之后添加初始水和DMEA,并且随后添加稀释水。挤压机速度为1200rpm。将胺中和剂和水混合在一起并且在初始水引入点馈入到挤压机。经由两个单独泵馈入稀释水,并且其在两个位置处引入到挤压机的稀释区中。初始水和稀释水物流经预加热到挤压机温度。在挤压机出口处,使用背压调节器来将挤压机筒内的压力调节到约300psig以减少运行温度下的蒸汽形成。冷却所得分散液并且经由800、200和50微米袋式过滤器,继而20微米筒式过滤器过滤。各组合物的不同组成显示于以下表2中。
表2:分散液组合物
如以上表2中所示,通过熔融掺合制备具有不同指示抗氧化剂装载量的聚丙烯(PP)聚烯烃基质聚合物的母料。含POD抗氧化剂通过组合指示量的含有抗氧化剂的母料制备。举例来说,为了达到HostanoxTMO3抗氧化剂(AO)的600ppm含量水平和IrganoxTM3114AO的750ppm含量水平,制备7000g PP球粒混合物,其由3500g 42.9%具有50ppm HostanoxTMO3AO的PP母料与57.1%具有2060ppm HostanoxTM O3AO(母料)的PP母料的混合物以及3500g23.4%具有126ppm IrganoxTM 3114AO的PP母料与76.6%具有1920ppm Irganox 3114AO(母料)的PP母料的混合物组成。向球粒混合物中添加2250g聚烯烃稳定剂和750g偶合剂1。用机械搅拌器组合球粒混合物以均匀地分布球粒组分。制备这10kg批料中的一些并且馈入到乳化挤压机以制备如上文所描述的POD。
熔融掺合聚烯烃中的抗氧化剂分散液或提供撒布在抗氧化剂上的聚烯烃以用于制得水性分散液。通过以10wt.%浓度在1/1丁基溶纤剂/正丁醇混合物中溶解所指示的抗氧化剂并且将溶液与分散液混合进行抗氧化剂的后添加,而无任何其它配制步骤。
涂层制备:用绕线刮涂棒将所有涂料施加到铝罐体储备液(X1178591212澄清铝罐储备液(俄亥俄州克利夫兰的全箔公司(All Foils Inc.,Cleveland,OH)),以7-10微米的干燥涂层厚度为目标。在225℃下在VWR 1640强制空气对流烘箱(宾夕法尼亚州拉德诺的VWR(VWR,Radnor,PA))中进行涂层固化4分钟。
测试方法:
MEK双重摩擦:根据ASTM D 5402-06方法3(2011)2011),在根据涂层制备制得的涂层上,使用每2.54cm×2.54cm正方形具有28×24根细线的漂厚棉布(级别50)和906g(32盎司)圆头锤进行MEK双重摩擦测试,其中所述布用线固定到所述锤的平端并且抵着涂层跨过涂层来回摩擦,每25次双重摩擦将布再浸渍到MEK中。将所述布再定位到新区域或在每组后替换。以上表2中所报告的数目是来回摩擦循环直到涂层被穿透并且衬底在任何区域中都变得可见为止的总次数。可接受的MEK双重摩擦结果是100次摩擦或更多次。
如以上表2中所示,实例2到6中包含母料或含酯键受阻酚类抗氧化剂的抗氧化剂分散液的所有涂料组合物都产生良好的MEK双重摩擦结果,指示由其形成的涂层具有良好耐热性。当以聚丙烯中的抗氧化剂分散液形式形成时,实例1并不具有足够的抗氧化剂。然而,实例6以与聚合偶合剂中的抗氧化剂分散液相同的分散的受阻酚类抗氧化剂的量产生极好的结果。这些实例指示,用于形成抗氧化剂分散液的优选聚合物是具有一定水分散性和与抗氧化剂的相容性的偶合剂或聚烯烃稳定剂。实例4指示,抗氧化剂分散液可以有效地包含第二不含酯键酚类抗氧化剂并且降低组合物中含酯键受阻酚类抗氧化剂的所需量。所有比较实例都未能包括抗氧化剂分散液,不管以母料形式还是分散于聚烯烃中。另外,比较实例1、8、9和10都不合格,部分因为其未能包含含酯键受阻酚类抗氧化剂。
Claims (11)
1.一种包含衬底的涂层,在所述衬底上具有含以下各者的聚烯烃分散液组合物的一个或多个层或膜:一种或多种选自聚烯烃、羧酸官能聚烯烃以及羧酸酯官能聚烯烃的聚烯烃基质聚合物,以所述聚烯烃分散液组合物的总固体计为1到40wt.%;一种或多种烯烃稳定剂,其酸值(AN)为80到250,以所述聚烯烃分散液组合物的总固体计为0到50wt.%;一种或多种偶合剂,其酸值(AN)为10到70,并且其熔融指数为500到5,000,000,其为在190℃下在10分钟内用装载有2.16kg的柱塞传送通过经加热的注射器或圆筒的聚合物熔体克数;以及分散于所述聚烯烃基质聚合物、为聚合物的所述烯烃稳定剂或为聚合物的所述偶合剂中的至少一种中的至少一种含酯键受阻酚类抗氧化剂。
2.根据权利要求1所述的涂层,其中所述含酯键受阻酚类抗氧化剂包含至少一种羟苯基丙酸酯或其与一种或多种第二抗氧化剂的组合。
3.根据权利要求2所述的涂层,其中所述含酯键受阻酚类抗氧化剂是苯丙酸,3-(1,1-二甲基乙基)-β-[3-(1,1-二甲基乙基)-4-羟基苯基]-4-羟基-β-甲基-1,1'-(1,2-乙烷二基)酯。
4.根据权利要求1所述的涂层,其中含酯键受阻酚类抗氧化剂的总装载量在总聚烯烃分散液组合物固体的200ppm到10000ppm范围内。
5.根据权利要求1所述的涂层,其中所述量的所述一种或多种烯烃稳定剂包含烯烃-羧酸共聚物或两种此类聚合物的掺合物。
6.根据权利要求1所述的涂层,其中以所述聚烯烃分散液组合物的总固体计,所述一种或多种偶合剂构成2到30wt.%。
7.根据权利要求1所述的涂层,其中所述一种或多种偶合剂是顺丁烯二酸酐接枝的聚烯烃。
8.根据权利要求1所述的涂层,其中所述一种或多种聚烯烃基质聚合物包含聚乙烯、聚丙烯、聚(α-烯烃)共聚物、聚(α-烯烃)三元共聚物以及其中的任一种的掺合物。
9.根据权利要求1所述的涂层,其中所述衬底是用于食品或饮料的金属容器、盖子以及封盖。
10.根据权利要求1所述的涂层,其中厚度为10微米的涂层展现根据ASTM D5402-06,方法3,2011,使用每2.54cm×2.54cm正方形具有28×24根细线的级别50的漂厚棉布以及906g圆头锤的100次双重摩擦或更多次,直到所述涂层被穿透并且所述衬底在任何区域中都变得可见为止的甲基乙基酮双重摩擦耐性,其中所述布用线固定到所述锤的平端并且抵着所述涂层跨过所述涂层来回摩擦,每25次双重摩擦将所述布再浸渍到MEK中。
11.一种制得水性分散液组合物的方法,所述组合物用于制得根据权利要求1所述的涂层,所述方法包含i)熔融掺合所述含酯键受阻酚类抗氧化剂、所述聚烯烃基质聚合物、所述烯烃稳定剂和任选的聚烯烃稳定剂以及任何偶合剂或(ii)(a)熔融掺合所述聚烯烃基质聚合物、任何偶合剂以及所述烯烃稳定剂,以及(b)单独地熔融掺合聚烯烃基质聚合物、聚烯烃稳定剂或为聚合物的任何偶合剂中的任一种中的所述受阻酚类抗氧化剂以形成抗氧化剂分散液;继而在水中连同足够量的一种或多种挥发性碱分散(i)的熔体或(ii)(a)和(b)两者的熔体以中和所述聚烯烃分散液组合物中50摩尔%到300摩尔%的羧酸,从而形成水性分散液。
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JP2016186071A (ja) | 2016-10-27 |
US20160280951A1 (en) | 2016-09-29 |
BR102016005699B1 (pt) | 2021-03-09 |
JP6788312B2 (ja) | 2020-11-25 |
CN106009953A (zh) | 2016-10-12 |
US10221327B2 (en) | 2019-03-05 |
EP3072925A1 (en) | 2016-09-28 |
SG10201600773QA (en) | 2016-10-28 |
BR102016005699A2 (pt) | 2017-01-24 |
EP3072925B1 (en) | 2017-11-15 |
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