CN104024308A - 制备包含活性剂的压敏粘合剂制品的方法 - Google Patents
制备包含活性剂的压敏粘合剂制品的方法 Download PDFInfo
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- CN104024308A CN104024308A CN201280061000.1A CN201280061000A CN104024308A CN 104024308 A CN104024308 A CN 104024308A CN 201280061000 A CN201280061000 A CN 201280061000A CN 104024308 A CN104024308 A CN 104024308A
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- base material
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- sensitive adhesive
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Abstract
本公开提供了一种方法,所述方法包括将活性组合物接触印刷到离型基材的表面上以形成经印刷表面。所述活性组合物自发地对离型基材的表面去湿以在离型基材的表面上形成活性沉积物。所述活性组合物包含溶解或分散在含水液体载体中的活性剂。在所述经印刷表面上设置压敏粘合剂层。
Description
技术领域
本公开广义地涉及压敏粘合剂制品及它们的制备方法。
背景技术
伤口护理制品如伤口敷料和开刀巾有多种设计以保护伤口和手术切口使之免于感染。这样的制品常常通过压敏粘合剂(PSA)层粘附到患者的皮肤。通常,PSA层被设置在基材如柔性膜、泡沫、织造材料、非织造材料或纱布上。为降低感染的风险,已与PSA层组合地使用抗微生物材料(例如,包含抗微生物化合物的材料)。
发明内容
在一个方面,本公开提供了一种制备压敏粘合剂制品的方法,所述方法包括:
将活性组合物接触印刷到离型基材的表面上以形成经印刷表面,由此,活性组合物自发地对离型基材的表面去湿以在离型基材的表面上形成活性沉积物,其中所述活性组合物包含溶解或分散在含水液体载体中的活性剂;以及
在所述经印刷表面上设置压敏粘合剂层。
根据本公开的方法可用来例如制备具有引入其中的活性剂的粘合剂制品。
由于问题如喷嘴堵塞和/或腐蚀,非接触方法如喷墨印刷对于一些流体溶液来说可能不可靠,并且可能较慢。
有利地,根据本公开的方法可有效地在压敏粘合剂上沉积生物活性组合物而无前述伴随喷墨印刷的问题。另外,它们可与薄的基材一起使用,此时,其它印刷方法可能没有效。
如本文所用:
术语“活性剂”指在哺乳动物的组织上局部地起作用以防止、减轻或治愈病症的化合物或化合物的组合。在一些实施例中,活性剂包含药理学上有效的化合物或化合物的组合。活性剂可或可不以药学上和/或临床上有效的量存在。
术语“含水”指包含至少5重量%的水。
术语“接触印刷”指其中组合物与印刷或计量元件及离型基材的表面同时接触并且被印刷或计量元件推向离型基材的表面的任何印刷或涂布方法。
术语“去湿”指发生在固-液界面的自发过程,并指离型基材的表面上薄液膜的收缩和/或破裂。该过程为液体在离型基材上的自发铺展的相反过程。
术语“可水合聚合物”指在20℃至40℃的范围内的温度下可水溶、可水溶胀和/或可水侵蚀的聚合物。
术语“离型基材”指以可脱开的方式粘附到压敏粘合剂材料并可易于从压敏粘合剂材料分离而无实质性的粘合剂转移的基材。
术语“圆化”指基本上成形为圆或球的形式;做成圆形。
在考虑具体实施方式以及所附权利要求书之后,将进一步理解本公开的特征和优点。
附图说明
图1为根据本公开的示例性方法的示意性工艺流程图;
图2为根据本公开的另一示例性方法的示意性工艺流程图;
图3为实例1d中使用的柔性版印刷板的显微照片;
图4为经印刷离型基材1d的显微照片;并且
图5为经印刷离型基材5的显微照片。
应当理解,本领域的技术人员可以设计出大量其他修改形式和实施例,这些修改形式和实施例也在本公开的原理的范围和精神内。附图可未按比例绘制。在所有附图中,相同参考标号可以用来表示相同部件。
具体实施方式
现在看图1,根据本公开的制备压敏粘合剂制品的一种示例性方法包括在接触印刷辊119上将活性组合物102接触印刷到离型基材110的表面112上。活性组合物102包含溶解或分散在含水液体载体中的活性剂。一旦被印刷,所述活性组合物将自发地对表面112去湿以在表面112上形成活性沉积物124而形成经印刷表面122。然后通过层合在经印刷表面122上设置承载于背衬150上的压敏粘合剂层140。经印刷表面122从压敏粘合剂层140的后续分离使得活性沉积物124转移到压敏粘合剂层140。
现在看图2,根据本公开的制备压敏粘合剂制品的另一示例性方法包括使用刮刀涂布机117将活性组合物102接触印刷到离型基材114的结构化表面113上。结构化表面113包括脊108。一旦被印刷,活性组合物102将自发地对结构化表面113去湿以形成被脊108包围的活性沉积物124(例如,在凹进区域109的角落和/或中心被脊108包围,具体取决于活性组合物的粘度)而形成经印刷表面123。接下来,将其上设置有压敏粘合剂层140的背衬150层合到经印刷表面123。经印刷表面123从压敏粘合剂层140的后续分离使得活性沉积物124转移到压敏粘合剂层140。
在其它实施例中,可通过溶剂涂布方法将压敏粘合剂层设置在经印刷表面上,然后将背衬层合到压敏粘合剂层上。
可用的接触印刷方法包括例如柔性版印刷、辊涂、刮涂、刮刀涂布和凹版辊涂布。在这些技术中,特别理想的是柔性版印刷。
与非接触印刷方法如喷涂或喷射方法相比,使用接触印刷的优点在于,在印刷装置附近存在的可吸入气载小滴(例如,含有生物活性剂)将大大减少或消除。
活性组合物可根据任何图案或图像接触印刷到离型基材的表面上。图案的例子包括包含点、正方形、菱形、线、圆、六边形、三角形和它们的组合的组合及阵列。例如,可使用如图3中所示的柔性版印刷板来印刷活性组合物,取决于组成,其在着墨区的收缩和干燥后产生活性沉积物的阵列,如例如图4或图5中所示。活性沉积物的印刷阵列的节距(或间距)可例如在0.1微米至1厘米的范围内或更大。
活性组合物包含活性剂和含水液体载体。在一些实施例中,活性组合物还包含可水合聚合物。可在活性组合物和活性沉积物中包含活性剂和/或可水合聚合物的组合。
示例性的可用活性剂(例如,治疗剂)包括:草药、抗炎药物、甾族(例如,泼尼松龙、曲安西龙)和非甾族(例如,萘普生、吡罗昔康);抗菌剂(例如,青霉素、先锋霉素、红霉素、四环素、庆大霉素、磺胺噻唑、呋喃妥因、三甲氧苄二氨嘧啶和喹诺酮(例如,诺氟沙星、氟甲喹和依巴沙星)、杆菌肽及其盐、新霉素及其盐、多粘菌素B)和防腐剂(例如,氯己定、葡糖酸氯己定、双胍啶、奥替尼啶、抗微生物的季铵表面活性剂如苯扎氯铵、西吡氯铵和十六烷基三甲基卤化物、酚、甲酚、三氯生、抗菌天然油、碘伏、季铵化合物、质子化的叔胺和仲胺化合物、某些金属离子(例如,银和铜)及它们的盐(例如,葡糖酸银、乳酸银和硫酸银)、双胍、三氯生和聚合物型抗菌剂(例如,聚六亚甲基双胍、具有质子化伯胺、仲胺和/或叔胺的聚合物、及聚季胺)、抗微生物类脂如美国公开专利申请No.2005/0089539A1(Scholz等人)中描述的那些,其包括C8-C12烷基单酯及甘油和丙二醇的单醚;抗原生动物药(例如甲硝唑);心血管药物(例如,苯磺酸氨氯地平、三硝酸甘油酯、尼非地平、氯沙坦钾、厄贝沙坦、盐酸地尔硫卓、硫酸氢氯吡格雷、地高辛、阿昔单抗、速尿、盐酸胺碘酮、贝前列素、茶碱、吡布特罗、沙美特罗、异丙去甲肾上腺素和维生素E烟酸酯);钙通道阻滞剂(例如硝苯啶、硫氮卓酮);酶抑制剂,如胶原酶抑制剂、蛋白酶抑制剂、弹性蛋白酶抑制剂、脂氧合酶抑制剂(例如,A64077)和血管紧张素转化酶抑制剂(例如,卡托普利、赖诺普利);其它抗高血压药(例如普萘洛尔);白三烯拮抗剂(例如,ICI204、219)抗溃疡药如H2拮抗剂;甾体激素(例如,孕酮、睾酮、雌二醇、乙羟基二降孕甾烯炔酮、霉酚酸酯和甲泼尼龙);抗病毒素和/或免疫调节剂(例如,1-异丁基-1H-咪唑[4,5-c]喹啉-4-胺、1-(2-羟基-2-甲基丙基)-1H-咪唑[4,5-c]喹啉-4-胺、阿昔洛韦);强心剂(例如洋地黄、地高辛);镇咳药(例如可待因、右美沙芬);抗组胺剂(例如苯海拉明、扑尔敏、特非那定);剥脱剂(例如,α-羟基酸或β-羟基酸);止痛药(例如,盐酸曲马多、芬太尼、安乃近、酮洛芬、硫酸吗啡、赖氨酸乙酰水杨酸、对乙酰氨基酚、酮咯酸氨丁三醇、吗啡、洛索洛芬钠和布洛芬);皮肤病学产品(例如,异维A酸和克林霉素磷酸酯);麻醉剂(例如,丙泊酚、盐酸咪唑二氮卓和盐酸利多卡因);偏头痛治疗剂(例如,麦角胺、褪黑激素、舒马曲坦、佐米曲坦和利扎曲坦);镇静剂和催眠药(例如,唑吡坦、酒石酸唑吡坦、三唑仑和丁溴东莨菪碱);成像组分(例如,碘海醇、锝、TC99M、司他比锝、碘美普尔、钆双胺、碘佛醇和碘普罗胺);肽激素(例如,人或动物生长激素LHRH);强心产品诸如心房肽;蛋白质产品(例如胰岛素);酶(例如,抗瘟疫酶、溶菌酶、葡聚糖酶)、抗恶心药(例如,东莨菪碱);抗痉挛药(例如,卡马西平);抑制免疫力剂(例如环孢菌素);精神治疗剂(例如,苯甲二氮卓、盐酸舍曲林、文拉法辛、盐酸安非他酮、奥氮平、盐酸丁螺旋酮、阿普唑仑、盐酸哌甲酯、马来酸氟伏沙明和甲磺酸二氢麦角碱);镇静剂(例如镇静安眠剂);抗凝血剂(例如肝素);止痛药(例如对乙酰氨基酚);抗偏头痛剂(例如,麦角胺、褪黑激素、舒马坦);降胆固醇剂(例如,阿托伐他汀、钙、洛伐他汀、苯扎贝特、环丙贝特和吉非贝齐);抗心律失常剂(例如氟卡尼);止吐剂(例如,甲氧氯普胺、昂丹司琼);血液调节剂(例如,阿法依泊汀、依诺肝素钠和抗血友病因子);抗关节炎组分(例如,塞来考昔、萘丁美酮、米索前列醇和罗非昔布);AIDS和AIDS相关药物(例如,拉米夫定、硫酸茚地那韦和司他夫定);糖尿病和糖尿病相关治疗剂(例如,盐酸二甲双胍、胰岛素、曲格列酮和阿卡波糖);生物制剂(例如,B型肝炎疫苗和A型肝炎疫苗);免疫应答调节剂(例如,嘌呤衍生物、腺嘌呤衍生物和CpGs);抗癌剂(例如,氨甲喋呤、紫杉醇、卡铂、枸橼酸他莫昔芬、多西他赛、盐酸表柔比星、醋酸亮丙瑞林、比卡鲁胺、醋酸戈舍瑞林植入剂、盐酸伊立替康、盐酸吉西他滨和沙格司亭);胃肠产品(例如,兰索拉唑、盐酸雷尼替丁、法莫替丁、盐酸昂丹司琼、盐酸格拉司琼、柳氮磺胺吡啶和英夫利昔单抗);呼吸治疗剂(例如,氯雷他定、盐酸非索非那定、盐酸西替利嗪、丙酸氟替卡松、沙美特罗和布地奈德);抑制免疫力剂(例如环孢菌素);神经剂如抗焦虑药;止血剂;抗肥胖剂;烟碱;杀藻剂;和前述的药学上可接受的盐和酯。
活性剂可选自不与压敏粘合剂层和/或活性组合物的其它组分反应的那些,但可使用反应性活性剂。抗微生物活性剂通常基于实际使用中粘合剂制品将遭遇的微生物的类型来选择。通常,所述活性剂是非挥发性的,但这不是要求。活性剂可以任何量包含在活性组合物中。在一些实施例中,基于活性组合物的总重量计,活性剂可以至少10、20、30、40或甚至至少50重量%的量存在。
在一些实施例中,可能有利的是添加一种或多种用于向活性组合物输送透皮药物的赋形剂以产生透皮给药载体。赋形剂为用来帮助或延迟药物的扩散通过膜的化合物。赋形剂的例子包括:萜烯(例如,α-萜品醇、(+)-萜品烯-4-醇、1,3,3-三甲基-2-氧杂二环[2.2.2]辛烷、对-甲基异丙苯);醇,包括多元醇(例如,(S)-(+)-2,2-二甲基-1,-3-二氧戊环-4-甲醇、(R)-(-)-2,2-二甲基-1,3-二氧戊环-4-甲醇、1,2-丙二醇、丁烷-1,3-二醇、二乙二醇单乙基醚、四氢糠醇聚乙二醇醚、乙二醇、乙醇、丙醇、甘油);酯(例如,月桂酸丙二醇酯、肉豆蔻酸异丙酯、棕榈酸异丙酯、棕榈酸乙基己酯、十二烷酸丁酯、月桂酸月桂醇酯、丙酸2-羟基-十二烷基酯、亚油酸丁酯、月桂酸甲酯、十二烷酸甲酯、十二烷酸十二烷醇酯、月桂酸甲酯、十二烷酸甲酯、月桂酸乙酯、十二烷酸乙酯、油酸乙酯、L-乳酸(-)-甲酯、乳酸乙酯、乳酸月桂酯、乳酸丁酯);酰胺(例如,N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-月桂基吡咯烷酮、N-辛基吡咯烷酮、N-(2-羟乙基)吡咯烷酮、N-甲基吡咯烷酮、1-十二烷基氮杂环庚烷-2-酮和其它N-取代烷基氮杂环烷基-2-酮);卤代烃(例如,氯仿、二氯甲烷);脂肪酸(例如,月桂酸、油酸、异硬脂酸、亚油酸、癸酸、新癸酸);阳离子、阴离子和非离子表面活性剂(例如,十二烷基硫酸钠、聚乙氧基/聚丙氧基共聚物(polyoxamers));抗胆碱能剂(例如,苯咯溴铵、奥芬溴铵)、油(例如,茶树油、矿物油)、酮(例如,丙酮)、醚(例如,四氢呋喃);二甲亚砜;乙腈;水性溶剂(例如,水、缓冲盐水、乳酸林格氏液)以及它们的组合。
除挥发性共溶剂(例如,乙醇、异丙醇)外,基于活性组合物的总重量计,根据本公开的活性组合物通常包含约0.01至约100重量%的活性剂,更通常0.1至80重量%,但可使用其它量。就葡糖酸氯己定而言,基于活性组合物的总重量计,活性组合物通常包含约1至约70重量%的葡糖酸氯己定,但也可使用其它量。一般来说,待包含的活性剂的量受所选活性剂的活性及预期应用的影响。例如,活性沉积物可包含20至100%的活性剂,但也可使用其它量。
本公开中使用的可水合聚合物可以是阳离子的、非离子的、阴离子的或两性离子的,并可任选地经疏水基团改性。合适的可水合聚合物可以是线形的、支化的或交联的(例如,可水溶胀聚合物)。
轻度交联的可水合聚合物可能是可水溶胀的。如果以化学方式引入,则交联剂的浓度通常非常低,例如,基于干聚合物的重量计,低于约1000ppm或低于500ppm。可水溶胀聚合物也可使用化学交联剂来制备,和/或可使用电离辐射来交联。例如,当暴露于γ辐射时,包含N-乙烯基内酰胺如N-乙烯基吡咯烷酮的聚合物将增大分子量并可实际交联。
阳离子型可水合聚合物的例子包括永久荷电的季铵聚合物(包含季胺的那些聚合物,如聚季铵盐聚合物,特别是聚季铵盐4、7、10、24、32和37)以及已经合适的质子酸质子化的质子化伯胺、仲胺和叔胺官能聚合物二者。
质子化阳离子聚合物可用将不导致不适当的皮肤刺激的合适的酸质子化,如任选地被氧取代的C1-C10烷基羧酸(例如,乙酸、α-羟基酸如乳酸、葡萄糖酸等)、C1-C10烷基磺酸(例如,甲磺酸和乙磺酸)、C1-C10烷基硫酸氢盐(例如,甲基硫酸氢盐)和矿物酸(例如,盐酸、氢溴酸、硫酸和磷酸)。质子化阳离子聚合物上的电荷随pH变化。为此,为了确保聚合物充分质子化,必须适当地调节pH,并且应通常在5-9.5、理想地6.5-7.5的范围内。代表性的聚合物类别包括:阳离子多糖、衍生自丙烯酸和/或甲基丙烯酸的阳离子均聚物和共聚物、阳离子纤维素、瓜尔胶和其它胶树脂、二甲基二烯丙基氯化铵与丙烯酰胺和/或丙烯酸的阳离子共聚物、二甲基二烯丙基氯化铵的阳离子均聚物、阳离子聚亚烷基和乙氧基聚亚烷基亚胺以及它们的组合。
示例性的阳离子型可水合聚合物包括:阳离子瓜耳胶,如可以JAGUAR C-14-S和JAGUAR C-17得自新泽西州克兰伯里的罗地亚公司(Rhodia,Cranberry,New Jersey)的羟丙基三甲基铵瓜尔胶(密度0.11至0.22),此外,JAGUAR C-16,除上面指定的阳离子基团外,其还含有羟丙基取代基(密度0.8-1.1);季铵化羟乙基纤维素醚,可以UCARE POLYMER JR-30M和JR-400(新泽西州爱迪生的爱美高公司(Amerchol Corporation,Edison,New Jersey))及CELQUAT(新泽西州布里奇沃特的国家淀粉和化学品公司(National Starch andChemicals Corp.,Bridgewater,New Jersey))得到;其为多乙氧基化纤维素和二甲基二烯丙基氯化铵的共聚物,美国化妆品、盥洗用品和香水协会(Cosmetic,Toiletry and Fragrance Association,CTFA)命名为聚季铵盐-4。其它合适的阳离子聚合物有:二甲基二烯丙基氯化铵的均聚物,可以MERQUAT100获得(伊利诺伊州内珀维尔的纳尔科公司(Nalco Co.,Naperville,Illinois));甲基丙烯酸二甲氨基乙酯与丙烯酰胺的共聚物,可以商品名MERQUAT550和Merquat S商购获得(纳尔科公司(Nalco Co.));丙烯酸/二甲基二烯丙基氯化铵/丙烯酰胺共聚物,可以商品名MERQUAT3330获得(纳尔科公司(NalcoCo.));氨基醇的季铵化乙烯基吡咯烷酮丙烯酸酯或甲基丙烯酸酯共聚物;聚季铵盐11、23和28(乙烯基吡咯烷酮与甲基丙烯酸二甲基氨基乙酯的季铵化共聚物-GAFQUAT755N(新泽西州韦恩的国际特品公司(International Specialty Products,Wayne,New Jersey))和乙烯基吡咯烷酮与二甲基氨基乙基甲基丙烯酰胺的季铵化共聚物-HS-100);乙烯基吡咯烷酮/乙烯基咪唑甲氯化物共聚物,可以LUVIQUAT FC370获得(新泽西州弗伦翰帕克的巴斯夫公司(BASF Corp.,Florham Park,New Jersey));聚季铵盐2;聚亚烷基亚胺,如聚亚乙基亚胺和乙氧基化聚亚乙基亚胺,以及羟乙基纤维素和三甲基氯化铵取代环氧化物的烷基改性季铵盐,可以聚季铵盐24获得,可以QUATRISOFT LM-200自新泽西州爱迪生的爱美高公司(Corp.,Edison,New Jersey)获得。
示例性的非离子型可水合聚合物包括:聚氧化烯(例如,聚氧化乙烯、聚氧化丙烯及氧化乙烯、氧化丙烯和氧化丁烯的无规和嵌段共聚物,包括可以商品名POLYOX得自密歇根州米德兰的陶氏化学公司(Dow Chemical Co.,Midland,Michigan)的那些);纤维素塑料如羟乙基纤维素和羟丙基甲基纤维素、甲基羟丙基纤维素(例如,可以BENECEL MP943得自特拉华州威尔明顿的亚跨龙公司(Aqualon,Wilmington,Delaware))、羟丙基纤维素(例如,可以KLUCEL(LF,GF,MF,HF)得自亚跨龙公司(Aqualon))、羟丁基甲基纤维素(3.5%的羟丁基和30%的甲氧基,可得自纽约州安大略的科学聚合物产品公司(Scientific Polymer Products,Ontario,New York));聚丙烯酰胺;聚乙烯醇(例如,衍生自聚醋酸乙烯酯,40-100%、有利地85-100%水解,包括可以商品名POVAL得自日本东京可乐丽公司(Kuraray Co.,Tokyo,Japan)、以ELVANOL得自特拉华州威尔明顿的杜邦公司(E.I.du Pont de Nemours and Co.,Wilmington,Delaware)的那些);聚乙烯基吡咯烷酮(例如,可以商品名PVP-Kxx得自中国浙江的顶峰化学公司(Peakchem,ZheJiang,China)的那些,其中字母“K”后的“xx”编号指以1,000道尔顿表示的聚合物平均分子量,如PVP-K90和PVP-K30);淀粉、葡聚糖;黄原胶、亲水性聚氨酯如乙氧基化和磺化聚氨酯;甲基乙烯基醚与马来酸酐的共聚物(例如,可以商品名GANTREZ得自新泽西州韦恩的国际特品公司(International SpecialtyProducts,Wayne,New Jersey));植物分泌物如阿拉伯树胶、茄替胶和黄蓍胶;其它天然多糖聚合物如瓜耳胶、刺槐豆胶和黄原胶以及刺梧桐树胶。这些聚合物可任选地经疏水改性(例如,来自肯塔基州卡温顿的亚什兰公司(Ashland,Covington,Kentucky)的NATROSOLPLUS疏水改性羟乙基纤维素)。
示例性的阴离子型可水合聚合物包括俄亥俄州阿克伦的本·弗·古德里奇公司(B.F.Goodrich Co.,Akron,Ohio)以商品名CARBOPOL出售的丙烯酸/丙烯酸乙酯共聚物和羧乙烯基聚合物。这些树脂基本上由与0.75%至2.00%的交联剂如聚烯丙基蔗糖或聚烯丙基季戊四醇交联的丙烯酸的胶体状可水溶胀聚烯基聚醚交联聚合物构成。例子包括CARBOPOL934、CARBOPOL940、CARBOPOL950、CARBOPOL980、CARBOPOL951)和CARBOPOL981。CARBOPOL934为与约1%的蔗糖的聚烯丙基醚交联的丙烯酸的可水溶胀聚合物,所述蔗糖的聚烯丙基醚具有每个蔗糖分子平均约5.8个烯丙基基团。还合适的有具有两亲性质的丙烯酸的疏水改性交联聚合物,可以CARBOPOL1382、CARBOPOL1342和PEMULEN TR-1获得(CTFA名称:丙烯酸酯/10-30丙烯酸烷基酯交联聚合物,来自俄亥俄州威克利夫的路博润公司(Lubrizol,Wickliffe,Ohio))。阴离子聚合物也可形成为具有硫酸根或磺酸根基团如衍生自2-丙烯酰胺基-2-甲基丙磺酸(AMPS)的聚合物。阴离子聚合物也可基于天然聚合物如羧甲基纤维素和海藻提取物如海藻酸钠、海藻酸丙二醇酯和角叉菜胶钠。
两性离子型可水合聚合物的例子包括蛋白质如明胶、聚甜菜碱、polysultaines和聚氧化胺。
合适的可水合聚合物可具有宽的分子量范围,其中分子量和量通常强烈地影响活性组合物的粘度,从而决定产品性能。例如,如果聚合物分子量太高,则活性组合物可能太粘稠而不能使用选定的技术有效地印刷。或者,如果聚合物的分子量太低和/或可水合聚合物的量太小,则活性组合物可能不够粘稠而不能使用选定的技术在离型基材上有效地印刷。
基于活性组合物的总重量计,活性组合物中存在的可水合聚合物的总量通常在1至15重量%的范围内,更通常在1至10重量%的范围内,但也可使用更小和更大的量。一般来说,待包含的可水合聚合物的量受选择的印刷技术及一种或多种可水合聚合物的化学组成的影响。
含水液体载体包含至少5重量%的水,并可包含至少10、20、30、40、50、60或甚至70重量%的水或更多。含水液体载体还可包含与水形成单相的共溶剂。合适的共溶剂的例子包括可与水混溶的溶剂如甲醇、乙醇、异丙醇、乙二醇、丙二醇、丙酮、甘醇二甲醚、乙腈、二甘醇二甲醚、N,N-二甲基甲酰胺、二氧六环、甘油以及它们的组合。合适的可水溶、不可混溶的共溶剂的例子包括四氢呋喃、二甲亚砜和二乙二醇。所述共溶剂可以任何量使用,但通常选择为使得它们形成单一液相。一些高沸点溶剂如乙二醇、丙二醇、甘醇二甲醚、二甘醇二甲醚、N,N-二甲基甲酰胺、二氧六环和甘油也可用作增塑剂和/或溶胀剂。
活性组合物还可包含一种或多种其它添加剂如触变胶、增稠剂(包括无机增稠剂如硅胶、合成锂皂石和膨润土)、紫外光(UV)稳定剂、抗氧化剂、辅剂、芳香剂和着色剂。
合适的离型基材可包括例如适于与压敏粘合剂一起使用的那些离型基材。合适的离型基材的例子包括包含材料如聚酯膜、聚烯烃(例如,聚乙烯、聚丙烯)膜、纸或涂膜纸层合物如聚乙烯涂布纸的常规离型基材。这些离型基材可涂布以基于低表面能含氟聚合物的、基于有机硅的或基于丙烯酸类的聚合物涂层。通常,在其上印刷活性组合物的离型基材表面具有小于或等于线形聚乙烯的临界表面张力(或表面能)。可向一个或两个主表面施加低表面能涂层并可或可不交联。
离型基材可包括牛皮纸、聚乙烯、聚丙烯、聚酯或任何这些材料的复合物,其通常被涂布以离型剂如含氟化合物或有机硅。例如,美国专利No.4,472,480(Olson)描述了低表面能全氟化合物离型基材。市售有机硅涂布离型基材的例子包括得自威斯康星州哈蒙德的耐恒公司(Loparex LLC,Hammond,Wisconsin)的POLYSLIK有机硅离型纸和伊利诺伊州迪克森的道伯特化学公司(Daubert Chemical Co.,Dixon,Illinois)所供应的有机硅离型纸。虽然通常不必要,但预见到可移除根据本公开的方法的实施中使用的离型基材并更换以另一不同的离型基材。离型基材可包括例如片材、带、幅材或卷。
在一些实施例中,离型基材可包括结构化表面(即,结构化离型基材)。通常,微结构表面包含凸起的特征的重复图案或阵列。凸起的特征可包括例如直立棱柱(例如,三角形棱柱、正方形棱柱或六边形棱柱)、规则的棱柱、截顶正四棱锥、柱子、脊、凹槽或它们的组合。凸起的特征可包括高度和/或形状的组合。通常,凸起的特征的高度在5至500微米、更通常5至75微米的范围内,但也可使用其它高度。结构化离型基材是粘合剂领域中熟知的。在一些实施例中,活性组合物被印刷在凸起的特征上;例如通过辊涂。或者,在一些实施例中,活性组合物被印刷在设置于凸起的特征之间的低能表面(例如,平坦区域)的一个或多个区域上;例如,通过刮刀涂布或辊涂,然后刮走过量的活性组合物。
关于结构化离型基材的更多细节及它们的制造方法可见于例如美国专利申请公开No.2006/0127626A1(Fleming等人)、2007/0039271A1(Fleming等人)和2008/0083495A1(Sher等人)中。
通常,活性组合物具有足够大的表面张力以在接触印刷到离型基材的表面上后使得活性组合物相对于其与离型基材的初始接触面积而言收缩。这样的面积收缩可为至少10%、20%、30%、40%、50%、60%或70%或更大。在收缩过程中,油墨的轮廓变得更像滴。
离型基材的低能表面的任何部分或全部可被印刷以活性组合物。为了确保在接触离型基材的经印刷表面后压敏粘合剂层的充分粘附性质,活性沉积物可覆盖低能表面的总面积的不到15%、不到12%或不到7%,但也可使用其它覆盖量。为了取得活性剂的功效,活性沉积物通常覆盖低能表面的总面积的至少2%、至少3%、至少4%,但也可使用其它覆盖量。
就所得压敏粘合剂制品而论,活性沉积物可覆盖压敏粘合剂层的外主表面(即,与离型基材相背)的总面积的不到15%、不到12%或不到7%,但也可使用其它覆盖量。
在接触印刷到离型基材上后,活性组合物可通过液体载体的至少部分移除来经至少部分干燥(例如,基本上干燥或完全干燥),但这不是要求。在这样的干燥后,厚度和平均直径中的一者或多者通常可一定程度地减小,但活性沉积物保持圆化外观。干燥可通过任选地用加热蒸发来实现。热源的例子包括烘箱、经加热的辊和台板、以及红外加热器。
在典型的接触印刷工艺中,油墨和基材选择为使得油墨大体润湿基材以允许其停留在印刷过程中其所沉积于的地方。本公开通常涉及向离型基材的较低表面能(相对于活性组合物而言)表面印刷较高表面张力(和表面能)的含水活性组合物。因此,所述含水活性组合物通常不在离型基材的整个表面上自发地铺展(即,其不很好地润湿基材)。本公开人现已发现,此去湿往往使得初始经印刷图像(例如,与柔性版印刷板相对应)的精确图案随着图案化流体去湿而失去,使得活性沉积物可具有几乎均匀的尺寸并可根据受控的图案设置(例如,参见图4和5),具体取决于初始的印刷图案。不希望受理论束缚,但此受控的去湿的成功看起来受具有合适的粘度和表面张力的图案化流体的影响。在稠厚的粘度下,去湿仅缓慢地发生或根本不发生,而在非常稀薄的粘度下,接触印刷可能难以实现。一般来说,对如使用BROOKFIELD粘度计(型号DV-II+,马萨诸塞州米德波罗的布鲁克菲尔德工程实验室(Brookfield Engineering Laboratories,Middleboro,Massachusetts))在23℃下根据制造商的说明测得的粘度在50厘泊(cP)(50mPa-sec)至2500cP(2500mPa-sec)的范围内、理想地在100cP(100mPa-sec)至1000cP(1000mPa-sec)的范围内的活性组合物,观察到良好的印刷和去湿。
在接触印刷(和至少一部分含水液体载体的任选移除)后,所得活性沉积物的厚度和表面覆盖率通常取决于预期的用途。因此,对于应用如开刀巾,活性沉积物的厚度可在0.1至100微米的范围内,更通常在1至55微米的范围内,或甚至在10至50微米的范围内,但也可使用其它厚度范围。例如,活性沉积物的厚度可为至少0.1、0.5、1、2、5、10、15、20、25、30、40、50、60、75、100、150或甚至至少200微米或更大。
压敏层包含可用作压敏粘合剂的基料的聚合物。其理想地是皮肤病学上和药学上可接受的(例如,医疗级)并对所选活性剂是基本上化学惰性的。适合的聚合物的实例包括:丙烯酸酯如例如美国专利No.RE24,906(Ulrich)、3,389,827(Abere等人)、4,112,213(Waldman)、4,310,509(Berglund等人)、4,732,808(Krampe等人)、4,737,410(Kantner)、5,876,855(Wong等人)和7,097,853(Garbe等人)中公开的那些;聚异丁烯;聚异戊二烯;苯乙烯嵌段共聚物(例如,SEBS共聚物、SBS共聚物);和有机硅如美国专利No.5,232,702(Pfister)及PCT国际申请公开WO2010/056541A1(Liu等人)和WO2010/056543A1(Liu等人)中所公开的。也设想在所述压敏粘合剂中包含药剂或抗微生物剂;例如如美国专利No.4,310,509(Berglund等人)和4,323,557(Rosso等人)中所述。
丙烯酸类压敏粘合剂通常具有约-20℃或更低的玻璃化转变温度,并可包含100至80重量%的C3-C12烷基酯组分如例如丙烯酸异辛酯、丙烯酸2-乙基己酯和丙烯酸正丁酯以及0至20重量%的极性组分如例如丙烯酸、甲基丙烯酸、丙烯酰胺、乙烯-乙酸乙烯酯、N-乙烯基吡咯烷酮和苯乙烯大分子单体。在一些实施例中,丙烯酸类压敏粘合剂包含0至20重量%的丙烯酸和100至80重量%的丙烯酸异辛酯。某些活性剂(例如,CHG)可与丙烯酸反应,在这样的情况下,含丙烯酰胺或N-乙烯基吡咯烷酮而不是丙烯酸的压敏粘合剂可能是理想的。
压敏粘合剂层理想地以高于或等于人皮肤的速率传输湿气,但这不是要求。虽然这样的特性可通过选择适宜的粘合剂来获得,但也可使用获得高的湿气传输相对速率的其它方法;例如,在背衬上图案化涂布粘合剂,如美国专利No.4,595,001(Potter等人)中所述。可以连续或不连续的方式将粘合剂施加到背衬或离型基材的选定区域。
可用的压敏粘合剂可还包含弹性体材料。合适的弹性体材料的例子包括线形、径向、星形和锥形苯乙烯-异戊二烯嵌段共聚物,如可得自德克萨斯州休斯顿的壳牌化学公司(Shell Chemical Co.,Houston,Texas)的KRATON D1107P和可得自德克萨斯州休斯顿的埃尼化工弹性体美洲公司(EniChem Elastomers Americas,Inc.,Houston,Texas)的EUROPRENE SOL TE9110;直链苯乙烯-(乙烯-丁烯)嵌段共聚物,如可得自壳牌化学公司(Shell Chemical Co.)的KRATON G1657;线形苯乙烯-(乙烯-丙烯)嵌段共聚物,如可得自壳牌化学公司(ShellChemical Co.)的KRATON G1657X;线形、径向和星形苯乙烯-丁二烯嵌段共聚物,如可得自壳牌化学公司(Shell Chemical Co.)的KRATON D1118X和可得自埃尼化工弹性体美洲公司(EniChemElastomers Americas,Inc)的EUROPRENE SOL TE6205;聚醚酯,如可得自杜邦公司(DuPont)的HYTREL G3548;和基于聚-a-烯烃的热塑性弹性体材料,如由式--(CH2CHR)所表示的那些,其中R为含2至10个碳原子的烷基基团,以及基于茂金属催化的聚-a-烯烃,如ENGAGE EG8200,一种可得自密歇根州米德兰的陶氏塑料公司(DowPlastics Co.,Midland,Michigan)的乙烯/聚-a-烯烃共聚物;天然橡胶,如CV-60(受控粘度级)和SMR-5(带肋烟片胶);丁基橡胶,如可得自埃克森化学公司(Exxon Chemical Co.)的EXXON BUTYL268;合成聚异戊二烯,如可得自荷兰的荷兰皇家壳牌集团(Royal DutchShell,Netherlands)的CARIFLEX IR309和可得自固特异轮胎橡胶公司(Goodyear Tire and Rubber Co.)的NATSYN2210;乙烯-丙烯;聚丁二烯;聚异丁烯,如可得自埃克森化学公司(Exxon Chemical Co.)的VISTANEX MM L-80;和苯乙烯-丁二烯无规共聚物橡胶,如可得自俄亥俄州阿克伦的本·弗·古德里奇公司(BF Goodrich of Akron,Ohio)的AMERIPOL1011A。
压敏粘合剂可以是自粘性或发粘的。对于丙烯酸类聚合物可用的增粘剂包括松香酯如可得自特拉华州威尔明顿的赫尔克里公司(Hercules,Inc.of Wilmington,Delaware)的FORAL85和芳族树脂如可得自赫尔克里公司(Hercules,Inc.)的PICCOTEX LC-55WK和可得自德克萨斯州休斯顿的埃克森化学公司(Exxon Chemical Co of Houston,Texas)的ESCOREZ1310LC。如果存在,增粘剂通常占压敏粘合剂的约5至75重量%。
可用的压敏粘合剂可以是交联的或非交联的。
压敏粘合剂可覆盖背衬的全部主表面或仅覆盖背衬的主表面的一部分,并且其可均匀地涂布以形成基本上无空隙的膜或者其可图案化涂布。可采用图案化涂布以例如提高湿气传输。
另外,可在压敏粘合剂层中包含其它添加剂如着色剂、填料、蜡、增塑剂和抗氧化剂。
通常,压敏层厚约10至600微米,更通常厚20至60微米,但也可使用其它厚度。丙烯酸类压敏粘合剂层可例如使用熔融挤出技术、涂布可聚合粘合剂前体材料并然后辐射固化(例如,电子束和/或紫外光)、通过层合或通过溶剂涂布设置在离型基材或背衬上。
背衬应能够支承所述压敏层。在一些实施例中,背衬具有基本上光滑的主表面,是柔性的并任选地是可适形的。可用的背衬的例子包括非织造织物、聚合物膜和金属箔。背衬可例如包括幅材、带、卷或片材。
可用的背衬包括例如柔性膜和非织造物。可用于柔性膜和非织造物中的材料的例子包括聚烯烃(例如,聚乙烯、聚丙烯、聚丁烯和茂金属聚烯烃,如可以商品名ENGAGE得到的聚烯烃弹性体和可以商品名AFFINITY得到的聚烯烃塑性体,二者均可得自密歇根州米德兰的陶氏化学公司(Dow Chemical Co.,Midland,Michigan))、聚酯(例如,可以商品名HYTREL得自特拉华州威尔明顿的杜邦公司(E.I.duPont de Nemours&Co.,Wilmington,Del.)的那些)、聚酰胺、苯乙烯/丁二烯共聚物(例如,可以商品名KRATON得自德克萨斯州休斯顿的科腾聚合物公司(Kraton Polymers,Houston Texas)的那些)和聚氨酯弹性体(例如,可以商品名ESTANE5701、ESTANE58309、ESTANE58237和ESTANE5702得到的那些聚氨酯弹性体);人造丝、氯丁二烯橡胶、乙丙橡胶、聚丁二烯橡胶、聚异戊二烯橡胶、天然或合成橡胶、丁基橡胶、有机硅橡胶或EPDM橡胶;以及它们的组合。在一些实施例中,背衬包括湿气高度可透过的膜;例如,如美国专利No.3,645,835(Hodgson)和4,595,001(Potter等人)中所述。在一些实施例中,背衬和压敏粘合剂层可作为复合制品(即,压敏层设置在背衬上)获得。一种可用的此类复合制品——在一侧上涂布了压敏粘合剂的聚氨酯弹性体膜,可以商品名TEGADERM自3M公司(3MCompany)商购获得。
背衬理想地易于适形于解剖学表面,但这不是要求。这样,当施加到解剖学表面时,即使在该表面移动时其也适形于该表面,并且可伸展和缩回。在一些实施例中,背衬包括弹性体聚氨酯膜、聚酯膜或聚醚嵌段酰胺膜。
在根据本公开的方法中,印刷了活性组合物的离型基材(即,经印刷离型基材)被抵靠通常设置于背衬(例如,膜或片材)上的压敏粘合剂层推动,任选地使用使得多个活性沉积物中的至少一部分变为至少部分地包埋在压敏粘合剂层中的足够的力。可通过任何合适的方法施加压力,例如使用冷辊层合机、压料辊、压机或手压。在一些实施例中,多个活性沉积物中的至少一部分变为完全包埋在压敏粘合剂中。完全包埋的活性沉积物可与压敏粘合剂层的外表面齐平或者包埋在压敏粘合剂层的外表面下方。在一些实施例中,多个活性沉积物中的至少一部分充分地包埋以致与背衬接触。
在其中背衬高度适形并且在幅材操作过程中易于损坏的实施例中,可或者将压敏粘合剂层设置在经印刷的离型基材上并然后在后续步骤中将所得组件层合到背衬。有利地,此方法通常对开刀巾的制造有效,开刀巾通常具有高度适形性并且难以操作背衬层。
虽然活性沉积物可与压敏粘合剂层的外主表面基本上齐平,但使得活性沉积物满出相应的凹进并且部分地设置于外表面上方也在本公开的范围内。同样,活性沉积物可仅部分地填充相应的凹进。
根据本公开的抗微生物压敏粘合剂制品是有用的。例如,可将它们施加到皮肤并用作开刀巾、胶带、伤口敷料(例如,包括封闭敷料和压力敷料)和透皮贴。就胶带而言,根据本公开的压敏粘合剂制品可具有设置于与粘合剂层相背的背衬主表面上的低粘附背胶,并且背衬和压敏粘合剂层(其上具有活性沉积物)可绕其自身卷绕形成卷。
通过以下非限制性实例进一步说明本公开的目的和优点,但这些实例中所述的具体材料及其用量,以及其它条件和细节不应视为对本公开进行不当限定。
实例
除非另外指明,否则在实例及本说明书的其余部分中的所有份数、百分数、比率等均为以重量计。
后面的实例中使用以下材料。
材料表
丙烯酸类离型基材的制备
将丙烯酸异十八烷基酯(NK ESTER ISA,日本大阪都大阪有机化学工业株式会社(Osaka Organic Chemical Industry Ltd.,Osaka,Japan))、丙烯酸十八烷基酯(NK ESTER STA,大阪有机化学工业株式会社(Osaka Organic Chemical Industry,Ltd.))和EBECRYL P36(新泽西州西帕特森的氰特工业公司(Cytec Industries,West Paterson,New Jersey))以50/50/0.4的单体比率悬浮在50:50的乙酸乙酯/庚烷共混物中至60重量%的固体含量。将该混合物加到反应器容器中。然后加入0.3份引发剂V-601(2,2'-偶氮双(2-甲基丙酸酯),日本大阪都和光纯药工业株式会社(Wako Pure Chemical Industries,Ltd.,Osaka,Japan)),然后用氮气吹扫容器的内容物10分钟。密封容器并置于保持在50℃的旋转恒温浴中。让反应进行24小时。
用甲苯/2-丁酮(50:50)的溶剂混合物将所得共聚物溶液稀释至2重量%,然后使用#4缠线棒将此经稀释的溶液涂布到2密耳(51微米)厚的聚酯膜(F7S,罗得岛州北金斯敦的东丽塑料美国公司(Toray Plastics America,North Kingstown,Rhode Island))上。然后通过在40fpm(12m/min)下,在氮气下,两次通过高压汞蒸气灯(H灯泡,130W/cm;马里兰州盖瑟斯堡的富讯系统公司(Fusion SystemsCorporation,Gaithersburg,Maryland))下使用506mJ/cm2的UVA能量密度辐照该涂膜来产生丙烯酸类离型基材膜。
实例1-9
印刷配方#1
通过在高温下搅拌PVA/水混合物数天来制备20%重量/重量的PVA(高分子量)水溶液。冷却后,将350克该溶液与150克20%的CHG溶液混合。加入0.1%的红色染料。该溶液在室温下的布氏粘度为140cP(140mPa-sec,#31转子,30-100rpm范围)。
印刷配方#2
将163克针对印刷配方#1描述的20%PVA(高分子量)溶液与163克20%的CHG溶液和174克水混合。加入0.1%的红色染料。该溶液在室温下的布氏粘度为190cP(190mPa-sec,#31转子,30-100rpm范围)。
印刷配方#3
将75克针对印刷配方#1描述的20%PVA(高分子量)溶液与176克20%的CHG溶液和250克水混合。加入0.1%的红色染料。该溶液在室温下的布氏粘度为200cP(200mPa-sec,#31转子,30-100rpm范围)。
印刷配方#4
将19%重量/重量的PVA(44-51%水解,Mn=93,000g/mol;Mw=400,000g/mol)(150克)/甲醇溶液与160克20%的CHG溶液和190克水混合。加入0.1%的红色染料。该溶液在室温下的布氏粘度为140cP(140mPa-sec,#31转子,30-100rpm范围)。
印刷配方#5
通过加热下搅拌混合物数天来制备5%重量/重量的瓜尔胶/水分散体。将164克该分散体与155克20%的CHG溶液和232克水混合。加入0.1%的红色染料。该溶液在室温下的布氏粘度为200cP(200mPa-sec,#31转子,10-50rpm范围)。
印刷配方#6
将75克针对印刷配方#5制备的5%瓜尔胶分散体与350克20%的CHG溶液和285克水混合。加入0.1%的红色染料。该溶液在室温下的布氏粘度为700cP(700mPa-sec,#31转子,10rpm)。
印刷配方#7
将350克针对印刷配方#1制备的PVA(高分子量)溶液与150克20%的CHG溶液混合并加入0.1%的红色染料以制备CHG/PVA储备溶液。用467克水稀释200克20%的CHG溶液并加入0.1%的红色染料以制备CHG储备溶液。将207克CHG/PVA储备溶液与84克CHG储备溶液混合以产生最终印刷配方。该溶液在室温下的粘度(诺克罗斯方法)为920cP(920mPa-sec)。
印刷配方#8
将10份印刷配方#7的样品用1份如针对印刷配方#7所述的CHG储备溶液稀释。该溶液在室温下的粘度(诺克罗斯方法)为640cP(640mPa-sec)。
印刷配方#9
将10份印刷配方#8的样品用1份如针对印刷配方#7所述的CHG储备溶液稀释。该溶液在室温下的粘度(诺克罗斯方法)为420cP(420mPa-sec)。
粘度测量
除非另外指明,否则使用BROOKFIELD粘度计(型号DV-II+,马萨诸塞州米德波罗的布鲁克菲尔德工程实验室(BrookfieldEngineering Laboratories,Middleboro,Massachusetts))测量印刷配方的粘度。该粘度计装配有#31转子或#21转子。测试在室温下完成。
使用诺克罗斯粘度测量杯(马萨诸塞州牛顿市的诺克罗斯公司(Norcross Corporation,Newton,Massachusetts))测量印刷配方7-9的粘度。对于印刷配方7和8,将5号诺克罗斯壳杯放置在大的塑料烧杯中,填充以所需的溶液并让静置数分钟以让任何空气泡逸散。然后提升该杯,让溶液排出。记录排出所花的时间并自诺克罗斯提供的标准化曲线图确定粘度。对于印刷配方9,按相同的程序进行,不同的是使用4号诺克罗斯杯。
实例1-9
对于印刷配方1a-1d(平行测定)和印刷配方2-9中的每一个,通过根据需要正好在刮刀前面手动添加印刷配方使网纹辊上保持印刷配方的滚动料堆。然后网纹辊将该溶液计量加到印刷辊上。印刷辊上的图案为凸起的正方形垫的正方形阵列,每个正方形垫的面积为约0.14mm2,如图3中所示。相邻正方形之间沿两个相互正交的正方形网格方向的中心到中心距离为大约0.7mm并且沿对角线为约1.0mm。
然后使用印刷辊来向硅化纸基材施加印刷配方,基材以10英尺每分钟运动。然后使带有湿图案的基材通过10英尺长的烘箱以干燥该图案。对于经印刷离型基材1的图案,干燥在四个不同的烘箱温度下进行,并且这四个试样在表1中被命名为经印刷离型基材1a-1d。用荧光显微镜对每个基材上经干燥的图案成像。图4示出了经印刷离型基材1d上经干燥图案的荧光显微照片。图5示出了经印刷离型基材5上经干燥图案的荧光显微照片。如图4和5所示,每个示例性的经印刷离型基材带有与CHG和聚合物的混合物的位置相对应的圆点图案。点的间距与印刷辊图案中特征的间距很好地匹配(即,正方形阵列中点之间为大约0.7mm)。分析这些图像,求出基材上图案的面积覆盖百分数和各个点的中值面积。在表1(下面)中,面积覆盖数取自图案的两个不同样品的图像,并且点的中值大小为来自两个图像的合并数据的中值。
表1
对CHG开刀巾配方的粘附力测试
用丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂手涂来自印刷配方1d、5、6和9的经印刷离型基材的试样。目标涂布量为大约11粒(0.713克)每155cm2。然后将经粘合剂涂布的试样在烘箱中于82℃下干燥大约3至5分钟。然后将每个经干燥试样层合到HYTREL4056无衬膜的片材。层合通过使带有粘合剂的基材与背衬一起通过未经加热的辊来进行,以粘合剂侧面向HYTREL4056膜。为评估这些试样,如下进行与钢的粘附。向开刀巾试样的HYTREL4056膜侧粘附书籍胶带(SCOTCH845书籍修补胶带,3M公司)。然后,从试样切割1.0英寸(2.5cm)宽且大约4至6英寸(10至15cm)长的条。从遮蔽胶带形成提拉把手,并附接到1.0英寸(2.5cm)条的一端。然后通过移除离型基材将该条粘附到经光亮退火的#302或304AISI不锈钢板(该不锈钢板刚用庚烷/异丙醇(1:1比率,重量/重量)清洁),仔细地铺展胶带条,并用4.5磅的辊上下滚动一次。按ASTM测试方法D1000-10“Standard Test Methods for Pressure-SensitiveAdhesive-Coated Tapes Used for Electrical and Electronic Applications(用于电气和电子设备应用的压敏粘合剂涂布胶带的标准测试方法)”在12英寸/分钟(30cm/min)的速度下进行180度剥离测试。记录平均剥离力。对每个试样,进行三个平行测试。
一些市售开刀巾的典型剥离力值略高于24oz/in宽度(0.27kg/cm宽度)。表2(下面)中的结果示出,实例1d、9、5和6表明粘合剂表面上的CHG图案化没有不利地影响剥离粘附力。
表2
抗微生物性能的时间杀灭测试
使上面的粘附力测试中使用的若干实例的试样也经受抗微生物性能测试。按如下进行5分钟时间杀灭研究。
采用0.5麦克法兰等价浊度标准(0.5McFarland EquivalenceTurbidity Standard),制备浓度为1×108CFU(菌落形成单位)每毫升(mL)的耐甲氧西林金黄色葡萄球菌(MRSA,ATCC#33592)/磷酸盐缓冲水(pbw)悬浮液。使用Eppendorf移液器以15-16个分开的小滴向粘合剂膜的2.5cm直径部分的粘合剂表面转移50μL该悬浮液。然后将这些接种试样在室温(23+/-2℃)下孵育5分钟。孵育后,将试样置于20mL的中和缓冲液中并声处理一分钟,然后剧烈涡旋两分钟。用pbw连续稀释所得溶液。将纯溶液和稀释液各接种到3MPETRIFILM需氧计数板(3M公司)上并孵育至少24小时。然后使用3M PETRIFILM板读取器(型号6499,3M公司)对3M PETRIFILM板计数。实例1d、5和9各表现出2至3的log减小。对于采用其它方面类似的非图案化基材的对照(安慰剂)试样,未发现log减小。
使用TEGADERM粘合剂配方的测试
从TEGADERM1624W透明敷料的试样移除离型基材。然后用辊将每个试样手动层合到选自表1中实例1d、5和6的CHG图案化基材。然后切割层合物至1624W敷料大小。使用这些层合物试样进行抗微生物抑菌圈(ZOI)测试及其它测试。
抗微生物抑菌圈(ZOI)测试
使用抑菌圈测试定量地确定抗微生物性能。
采用0.5麦克法兰浊度标准(0.5McFarland Turbidity Standard),制备表皮葡萄球菌和绿脓假单胞菌在Butterfield缓冲液中的溶液,浓度为大约1×108菌落形成单位每毫升。对于每个待测试试样,通过将无菌棉签在该溶液中浸一浸并在三个不同的方向上擦拭Mueller Hinton II板的干燥表面来制备菌苔。然后将从待测试粘合剂片材切割的8毫米(mm)直径盘置于该板上并压紧以确保与板的完全接触。将板在孵育箱中于35±2℃下保持24小时。然后测量每个样品周围观察到生长抑制和/或无生长的区域(包括8-mm直径样品盘之下的区域)的直径。以首要抑菌圈记录抑菌圈直径。首要抑菌圈定义为在其内未观察到生长的区域(包括8-mm直径样品盘之下的区域)的直径。结果报告于表3中。重复一些测试,并且在这些情况下,两个结果均示出。所有试样均呈现出抑菌圈。TEGADERM1624W透明敷料试样呈现出比类似的IOA/NVP试样略大的抑菌圈。实例1d中CHG浓度的大幅增加没有产生成比例地较大的抑菌圈值。PVA样品(实例1d和9)呈现出比瓜尔胶样品(实例5和6)略好的抑菌圈。
实例10-17
实例10-17示出了改变印刷板图案的效果。
印刷板图案1
印刷板图案1在每侧上具有一个一个单独的0.30mm正方形形状升高区域,这对应于约0.090mm2的升高垫面积。这些正方形区域以正方形阵列排列,中心到中心距离为0.63mm。
印刷板图案2
印刷板图案2在每侧上具有一个一个单独的0.29mm正方形形状升高区域,这对应于约0.084mm2的升高垫面积。这些正方形区域以正方形阵列排列,中心到中心距离为2.9mm。
印刷板图案3
印刷板图案3具有一个一个单独的0.18mm直径的圆形形状升高区域,这对应于约0.025mm2的升高垫面积。这些圆形区域以六边形阵列排列,中心到中心距离为0.24mm。
印刷板图案4
印刷板图案4具有一个一个单独的0.09mm直径的圆形形状升高区域,这对应于约0.006mm2的升高垫面积。这些圆形区域以六边形阵列排列,中心到中心距离为0.17mm。
实例10
通过使用热和数天的搅拌将25%重量/重量的PVA(低分子量)溶解在水中来制备印刷配方。将该PVA溶液(610克)与286.3克20%的CHG溶液和56.7克水混合并加入0.4%的红色颜料。所得印刷配方在室温下的布氏粘度为460cP(460mPa-sec,#31转子,50rpm)并且pH为5.2。使用印刷板图案1将其图案化到硅化纸基材上。所得图案的面积覆盖率为4.0%,图案化点之间的中值间距为约0.6mm,点的中值大小为约0.024mm2。
实例11
使用印刷板图案2将实例10中使用的印刷配方图案化到硅化纸基材上。所得图案的面积覆盖率为2.1%,图案化点之间的中值间距为约2.6mm,点的中值大小为约0.123mm2。
实例12
通过混合459克与实例1中相同的20%PVA(高分子量)溶液与351克20%的CHG溶液、24克PEG-4000和337克水来制备印刷配方。加入红色颜料(0.4%)。该印刷配方在室温下的布氏粘度为480cP(480mPa-sec,#31转子,50rpm)并且pH为4.8。使用印刷板图案1将其图案化到硅化纸基材上。所得图案的面积覆盖率为3.1%,图案化点之间的中值间距为约0.6mm,点的中值大小为约0.012mm2。
实例13
使用印刷板图案2将来自实例12的印刷配方图案化到硅化纸基材上。所得图案的面积覆盖率为0.9%,图案化点之间的中值间距为约2.7mm,点的中值大小为约0.030mm2。
实例14
通过在室温下搅拌过夜将100克PVP HMW溶解在400克20%的CHG溶液中来制备印刷配方。加入红色染料(0.1%)。所得印刷配方在室温下的布氏粘度为160cP(160mPa-sec,#21转子,3-12rpm范围)并且pH为4.8。使用印刷板图案3将其图案化到硅化聚合物基材1752上。所得图案的面积覆盖率为2.6%,图案化点之间的中值间距为约0.24mm,点的中值大小为0.0019mm2。
实例15
使用印刷板图案4将来自实例14的印刷配方图案化到1752硅化膜基材上。所得图案的面积覆盖率为2.9%,图案化点之间的中值间距为约0.17mm,点的中值大小为0.0006mm2。
实例16
通过在室温下搅拌过夜将17.5克羟丙基纤维素溶解在487.5克20%的CHG溶液中来制备印刷配方。加入红色染料(0.1%)。其在室温下的布氏粘度为210cP(210mPa-sec,#21转子,12rpm)并且pH为4.6。使用印刷板图案3将其图案化到1752硅化膜基材上。所得图案的面积覆盖率为1.5%,图案化点之间的中值间距为约0.24mm,点的中值大小为0.0005mm2。
实例17
使用印刷板图案4将来自实例16的印刷配方图案化到硅化纸基材上。所得图案的面积覆盖率为1.5%,图案化点之间的中值间距为约0.17mm,点的中值大小为0.0004mm2。
实例18-30
实例18-30示出了进一步改变印刷配方和基材的效果。
制备实例18-30的方法
使用双面涂布胶带将图3中所示印刷板安装到114mm直径、51mm宽度的黄铜盘上。使用20号迈耶棒(Meyer rod)(纽约州韦伯斯特的RD精化公司(RD Specialties,Webster,New York))在玻璃板上涂布一层印刷配方。将带印刷板的黄铜盘辊压过涂布玻璃,然后立即辊压到离型基材上。将基材于100℃烘箱中放置1至5分钟。
实例18
通过混合8.2克与实例1中相同的20%PVA(高分子量)溶液与0.4克LAURICIDIN、0.8克BRIJ78、0.03克苯甲酸和10.6克水来制备印刷配方。加入0.4%的红色颜料,并于室温下搅拌溶液。如上所述将其涂布到硅化纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾(部件号70-2004-1797-3,3M公司)上。从硅化纸基材剥离粘合剂,转印到粘合剂的图案覆盖4.0%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.019mm2。
实例19
通过混合8.2克与实例1中相同的20%PVA(高分子量)溶液与0.4克SENSIVA SC50、0.8克BRIJ78、0.03克苯甲酸和10.6克水来制备印刷配方。加入0.4%的红色颜料,并于室温下搅拌溶液。如上所述将其涂布到硅化纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从硅化纸基材剥离粘合剂,转印到粘合剂的图案覆盖2.8%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.012mm2。
实施例20
通过混合8.2克与实例1中相同的20%PVA(高分子量)溶液与6克COSMOCIL CQ和5.8克水来制备印刷配方。加入0.4%的红色颜料,并于室温下搅拌溶液。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖2.6%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.010mm2。
实施例21
通过混合8.2克与实例1中相同的20%PVA(高分子量)溶液与0.2克氯化十六烷基吡啶和11.6克水来制备印刷配方。加入0.4%的红色颜料,并于室温下搅拌溶液。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖1.8%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.010mm2。
实施例22
通过混合8.2克与实例1中相同的20%PVA(高分子量)溶液与0.2克RITA PCMX和11.6克水来制备印刷配方。加入0.4%的红色颜料,并于室温下搅拌溶液。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖0.9%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.005mm2。
实施例23
通过混合8.2克与实例1中相同的20%PVA(高分子量)溶液与0.4克奥替尼啶-HCl和11.4克水来制备印刷配方。加入0.4%的红色颜料,并于室温下搅拌溶液。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖7.6%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.022mm2。
实施例24
通过在真空下在圆底烧瓶中于60℃油浴中将50克20%的CHG溶液机械搅拌30分钟来制备印刷配方,在此期间,溶液重量减至23.7克。在相似的热和真空下将23.0克该溶液再搅拌10分钟,在此期间,重量减至16.4克。用1.2克水稀释14.8克该溶液。该溶液的布氏粘度为400cP(400mPa-sec,#31转子,4rpm)。加入红色颜料(0.4%)。如上所述将该印刷溶液涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖6.2%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.024mm2。
实施例25
通过熔融90.75克LAURICIDIN并然后加入20克羟丙基纤维素在297.5克乙醇中的溶液来制备印刷配方。然后加入112.5克20%的CHG溶液,然后加入红色染料(0.1%)。该溶液在室温下的布氏粘度为170cP(170mPa-sec,#21转子,6rpm)。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖4.5%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.016mm2。
实例26
通过在高温下搅拌PVA/水混合物数天来制备20%重量/重量的PVA(高分子量)水溶液。冷却后,将150克该溶液与350克20%的CHG溶液混合。加入0.1%的红色染料。该溶液在室温下的布氏粘度为230cP(230mPa-sec,#21转子,6rpm)并且pH为4.7。
向上述溶液的15g份中加入磷酸溶液(0.05g,85%)。测得该溶液的pH为4.16。如上所述将该溶液涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖4.3%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.017mm2。
实例27
向实例26的第一段中所述溶液的15g份中加入葡萄糖酸溶液(0.45g,大约50%)。测得该溶液的pH为3.88。如上所述将该溶液涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖4.8%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.019mm2。
实例28
通过在搅拌板上混合12.50g20%的CHG/水、37.46g水和0.24gSOFTCAT SK-MH聚合物来制备印刷配方。然后将样品置于罐状辊(jar roller)上两天,然后使用Brookfield DV-I+粘度计用小样品适配器套件sc4-31测量粘度,为280cP(280毫帕-秒)。然后将一部分该溶液与等量的乙醇混合并加入0.05%(重量/重量)的红色染料。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖0.5%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.002mm2。
实例29
通过在搅拌板上混合12.50g COSMOSIL CQ PHMB/水、37.57g水和0.24g SOFTCAT SK-MH聚合物来制备印刷配方。然后将样品置于罐状辊上两天,然后使用Brookfield DV-I+粘度计用小样品适配器套件sc4-31测量粘度(350cP)。然后将一部分该溶液与等量的乙醇混合并加入0.05%(重量/重量)的红色染料。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖0.7%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.003mm2。
实例30
通过在搅拌板上混合0.50g CAPMUL PG-8单辛酸丙二醇酯(俄亥俄州哥伦布的阿比泰克公司(Abitec Corp.Columbus,Ohio))、1.50gTWEEN20(MP生物医药公司(MP Biomedicals))、0.25g2-苯氧基乙醇(威斯康星州密尔沃基的奥德里奇化学公司(Aldrich Chemical Co.,Milwaukee,WI))、0.20g ARISTOFLEX HMB于47.55g水中来制备印刷配方。然后将样品置于罐状辊上两天,然后使用Brookfield DV-I+粘度计用小样品适配器套件sc4-31测量粘度,为420cP(420mPa-sec)。然后将一部分该溶液与0.1%(重量/重量)的红色染料混合。如上所述将其涂布到纸基材的硅化表面上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖0.9%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.003mm2。
抗微生物活性测试(实例28-30)
使用直接时间杀灭法(ASTM2315-03(2008年重新批准))测量实例28-30的抗微生物活性,该方法将在下文描述。按如下进行90分钟时间杀灭研究。
采用0.5麦克法兰等价浊度标准(0.5McFarland EquivalenceTurbidity Standard),制备浓度为大约1×108CFU(菌落形成单位)每毫升(mL)的金黄色葡萄球菌(ATCC#25923)/磷酸盐缓冲水(PBW)悬浮液。使用Eppendorf连续移液器以16个分开的小滴向粘合剂膜的25mm直径部分的粘合剂表面转移50μL该悬浮液。平均种菌为6.11log细菌。然后将这些接种试样在加盖的培养皿中于35℃(+/-2℃)下孵育90分钟。孵育后,将试样置于20mL的Dey/Engley中和肉汤(DE)中并声处理一分钟,然后剧烈涡旋两分钟。在PBW中连续稀释所得溶液。将纯溶液和稀释液各接种到胰酶大豆琼脂(TSA)中并孵育40小时。实例28和29各表现出99.99%的微生物减少。实例30表现出78.75%的减少。对于采用其它方面类似的非图案化基材的对照(STERI-DRAPE2)试样,发现log减小极小。
表4
实例31A和31B
通过混合500克20%重量/重量的PVA(高分子量)溶液与366克20%的CHG溶液和354克水并然后加入0.4%的红色颜料来制备印刷配方。如上所述将其涂布到丙烯酸类离型基材上。所得图案具有6.4%的面积覆盖率。点之间的中值距离为约0.6mm,并且点的中值大小为约0.024mm2。
将一片此经印刷离型基材涂布以50微米厚的丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂(实例31A),另一片涂布以50微米厚的丙烯酸异辛酯/丙烯酰胺IOA/ACM(97/3)粘合剂(实例31B)。将这些粘合剂涂布片材与2SAB聚酯膜层合。
比较例A1和A2
将一片无印刷物的丙烯酸类离型基材涂布以50微米厚的丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂(比较例A1),另一片无印刷物的丙烯酸类离型基材涂布以50微米厚的丙烯酸异辛酯/丙烯酰胺IOA/ACM(97/3)粘合剂(比较例A2)。将这些粘合剂涂布片材与2SAB聚酯膜层合。
实例32A和32B
如上所述将实例31中所述的印刷配方图案化到1720硅化膜基材上。所得图案具有3.6%的面积覆盖率。点之间的中值距离为约0.6mm,并且点的中值大小为约0.013mm2。将一片此经印刷离型基材涂布以50微米厚的丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂(实例32A),另一片涂布以50微米厚的丙烯酸异辛酯/丙烯酰胺IOA/ACM(97/3)粘合剂(实例32B)。将这些粘合剂涂布片材与2SAB聚酯膜层合。
比较例B1和B2
将一片无印刷物的1720硅化膜基材涂布以50微米厚的丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂(比较例B1),另一片无印刷物的1720硅化膜基材涂布以50微米厚的丙烯酸异辛酯/丙烯酰胺IOA/ACM(97/3)粘合剂(比较例B2)。将这些粘合剂涂布片材与2SAB聚酯膜层合。
实例33A和33B
如上所述将来自实例31A的印刷配方图案化到1752硅化膜基材上。所得图案具有4.8%的面积覆盖率。点之间的中值距离为约0.6mm,并且点的中值大小为约0.19mm2。将一片此经印刷离型基材涂布以50微米厚的丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂(实例33A),另一片涂布以50微米厚的丙烯酸异辛酯/丙烯酰胺IOA/ACM(97/3)粘合剂(实例33B)。将这些粘合剂涂布片材与2SAB聚酯膜层合。
比较例C1和C2
将一片无印刷物的1752硅化膜基材涂布以50微米厚的丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂(比较例C1),另一片无印刷物的1752硅化膜基材涂布以50微米厚的丙烯酸异辛酯/丙烯酰胺IOA/ACM(97/3)粘合剂(比较例C2)。将这些粘合剂涂布片材与2SAB聚酯膜层合。
对CHG开刀巾配方的离型测试
使用刮刀涂布机对来自实例31、32和33的经印刷离型基材的试样涂布以丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂或丙烯酸异辛酯/丙烯酰胺IOA/ACM(97/3)粘合剂。目标涂布厚度为50微米。然后将经粘合剂涂布的试样在烘箱中于80℃干燥5分钟。让所得样品冷却,然后与2密耳聚酯膜3SAB的底漆侧层合。层合通过使带有粘合剂的基材与背衬一起通过未经加热的辊来进行,以粘合剂侧面向2SAB膜的底漆侧。
然后对这些试样评估经印刷活性组合物和粘合剂自基材的离型表面的离型性。将所得试样在如表5中所指定的常温下热老化一段时间。在所需的老化期后将样品切割成宽1.27cm、长大约15cm的测试条。使用施加到测试试样的离型衬垫侧的2.54cm宽双面涂布粘合剂纸带(可自明尼苏达州圣保罗的3M公司(3M company,St.Paul,MN)以商品名3M DOUBLE COATED PAPER TAPE410B商购获得)将测试条附接到滑动/剥离测试仪(型号SP2000,得自俄亥俄州斯特朗斯维尔的仪器公司(Instrumentors,Inc.,Strongsville,Ohio))的工作台板。用2kg橡胶滚筒将附接的测试条在工作台板上滚轧一次。然后通过在180度的角度下以2.3米每分钟(90英寸每分钟)的速率剥离而从基材的表面移除带聚酯背衬的粘合剂(也称粘合剂胶带),并在五秒的数据采集时间内测量从离型衬垫移除粘合剂所需的力。所有释放测试均在恒定温度(23℃)和恒定相对湿度(50%)的设施中进行。对每个样品进行至少两次测量,并且将数据记录为所有测量的平均值。测量值单位为克-力/0.5"并换算为克-力/英寸。
测量后续粘附力的测试方法
在从经印刷表面剥离带聚酯背衬的粘合剂(也称粘合剂胶带)后,通过将刚剥离的粘合剂胶带(无离型基材)粘附到浮法玻璃测试面板来测量粘合剂胶带的后续(180度剥离)粘附力,以胶带的具有粘合剂的一侧与面板接触。首先使用拇指轻压然后使用2kg辊将粘附的粘合剂胶带按平在测试面板上。然后使用上述仪器和测试参数测量胶带的后续粘附力值。进行这些测量来确定是否因CHG配方的印刷而发生粘附力值的下降。后续的粘附力测试也在23℃和50%相对湿度下进行。对每个样品进行至少两次测量,并且将数据记录为所有测量的平均值。测量值单位为盎司-力/0.5英寸并换算为盎司-力/英寸。结果报告于(下面的)表5中。
表5
实例34-38
实例34-38证实具有纹理化表面的基材作为图案化印刷物的替代物的用途。
对含聚合物、CHG和红色染料的溶液评估粘度及涂布聚对苯二甲酸乙二醇酯结构化基材(压印或微复制)的能力。制备若干溶液并使用Brookfield粘度计测量粘度。溶液粘度在700至5000cP(700至5000mPa-sec)的范围内。然后使用聚碳酸酯刮刀将样品涂布到基材上,移除过量的。将样品置于150℉(65.5℃)烘箱中并让干燥10分钟。让样品冷却,然后层合到TEGADERM1624W透明敷料以进一步测试。显微镜法结果表明,溶液回缩并在凹进区域中形成聚合物/CHG盘。当使用2600cP(2.6Pa-sec)的粘度时获得最佳涂布。
实例34
制备在水中含CHG(6%)、聚乙烯醇(12.6%,高分子量)和红色染料(0.1%)的涂布溶液。其粘度为5000cP(5000mPa-sec)。将其涂布到结构化基材1上。将结构化图案层合到TEGADERM1624W透明敷料(3M公司,部件号8333-1626-05)。在从基材剥离粘合剂时,转印到粘合剂的图案的面积覆盖率为7.7%。
实例35
制备在水中含CHG(6%)、聚乙烯醇(11.2%,高分子量)和红色染料(0.1%)的涂布溶液。其粘度为2600cP(2600mPa-sec)。将其涂布到结构化基材1上。将结构化图案层合到TEGADERM1624W透明敷料。在从基材剥离粘合剂时,转印到粘合剂的图案的面积覆盖率为6.2%。
实例36
涂布溶液在水中包含CHG(6%)、瓜尔胶(1.9%,高分子量)和红色染料(0.1%)。其粘度为700cP(700mPa-sec)。将其涂布到结构化基材1上。将结构化图案层合到TEGADERM1624W透明敷料。基材1。在从基材剥离粘合剂时,转印到粘合剂的图案的面积覆盖率为7.0%。
实例37
涂布溶液在乙醇/水中包含CHG(4.5%)、羟丙基纤维素(4%)、甘油单月桂酸酯(14.8%)和红色染料(0.1%)。其粘度为170cP(5000mPa-sec)。将其涂布到基材2上。将结构化图案层合到TEGADERM1624W透明敷料。在从基材剥离粘合剂时,转印到粘合剂的图案的面积覆盖率为8.9%。
实例38
制备在水中含CHG(2%)、聚乙烯基吡咯烷酮(1.25%)、羟丙基瓜尔胶(1.5%,法国巴黎的罗地亚公司(Rhodia S.A.,Paris,France))和聚甘油-3(55%,CAS#56090-54-1,德国莱茵贝格的苏威英特罗斯公司(Solvay Interox,Rheinberg,Germany))的涂布溶液。让该溶液静置过夜。使用前,用50ml去离子水和3克异丙醇稀释10g等分试样,然后涂布到结构化基材1上。15-30分钟后,将结构化图案层合到一片TEGADERM1624W透明敷料的粘合剂面。在从基材剥离粘合剂时,转印到粘合剂的图案的面积覆盖率为40-50%。
实例39和40
实例39和40示意有机硅粘合剂的使用。通过在混合辊装置上合并100份OHX-4070(密歇根州米德兰的道康宁公司(Dow Corning,Midland,MI))与60份Wacker-Belsil TMS803(四烷氧基硅烷与三甲基乙氧基硅烷的共水解产物)(德国慕尼黑的瓦克化学公司(WackerChemie,Munich,Germany))直至获得澄清溶液来制备有机硅粘合剂。然后使用设置为4密耳(100微米)间隙的刮刀涂布机将该溶液涂布到2CL PET5100/5100含氟有机硅涂布聚对苯二甲酸乙二醇酯离型基材(伊利诺伊州威洛布鲁克的耐恒公司(Loparex,Willowbrook,Illinois))上。然后用6Mrads在300keV下将经涂布试样电子束固化。然后如下将固化试样层合到ESTANE58237聚氨酯膜(可得自俄亥俄州威克利夫的路博润公司(Lubrizol Corp.,Wickliffe,Ohio))。移除基材并通过用手辊压将带膜的粘合剂试样层合到来自实例1和6的印刷图案上,分别产生实例39和40。
然后从粘合剂移除基材。观察到CHG图案已转印到粘合剂。当用于抑菌圈实验时,样品还表现出抗微生物活性。
实例41
通过混合150克20%重量/重量的PVA(高分子量)溶液与350克20%的CHG溶液并然后加入0.1%的红色染料来制备印刷配方。其布氏粘度为230cP(室温,6rpm,转子S21)并且pH为4.7。使用实例18的方法将其涂布到SILFLU M117膜(含氟有机硅涂布聚酯膜,来自伊利诺伊州芝加哥的矽利康美国公司(Siliconature,USA,LLC,Chicago,Illinois))上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖3.4%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.012mm2。
实例42
使用实例18中描述的方法将来自实例41的印刷配方涂布到SBOPP9741离型衬垫(3M SCOTCHPAK9741RELEASE LINER,来自明尼苏达州圣保罗的3M公司(3M,St.Paul,MN55144))上。将所得经印刷表面层合到一张STERI-DRAPE1050开刀巾上。从基材剥离粘合剂,转印到粘合剂的图案覆盖7.0%的面积。点之间的中值距离为约0.6mm,并且点的中值大小为约0.025mm2。
实例43
使用实例18中描述的方法将来自实例41的印刷配方涂布到通过涂布有机硅丙烯酸酯制得的膜的低粘附背胶处理表面上。向经印刷图案上涂布厚0.02mm大体根据美国专利No.5,032,460(Kantner等人)中的公开内容制得的丙烯酸异辛酯/N-乙烯基吡咯烷酮(IOA/NVP,91/9)粘合剂。然后将膜卷到自身上使得粘合剂表面接触膜的未经背胶处理表面。24小时后,展开样品,粘合剂已转移到膜的未经背胶处理表面。然后使印刷图案暴露在粘合剂的表面上,面积覆盖率为7.4%。点之间的中值距离为约0.6mm,并且点的中值大小为约0.030mm2。
本公开的精选实施例
在第一个实施例中,本公开提供了一种制备压敏粘合剂制品的方法,所述方法包括:
将活性组合物接触印刷到基材的表面上以形成经印刷表面,由此,活性组合物自发地对基材的表面去湿以在基材的表面上形成活性沉积物,其中所述活性组合物包含溶解或分散在含水液体载体中的活性剂;以及
在所述经印刷表面上设置压敏粘合剂层。
在第二个实施例中,本公开提供了根据第一个实施例所述的方法,其中随着最初与基材的表面接触,活性组合物接触基材的表面的第一区域,并且其中活性沉积物接触基材的表面的第二区域,并且其中所述第二区域小于或等于第一区域的50%。
在第三个实施例中,本公开提供了根据第一或第二个实施例所述的方法,其中所述活性组合物还包含可水合聚合物。
在第四个实施例中,本公开提供了根据第一至第三个实施例中任一项所述的方法,其中所述活性剂包含至少一种非挥发性组分。
在第五个实施例中,本公开提供了根据第一至第四个实施例中任一项所述的方法,其中所述活性剂包含抗微生物剂、局部防腐剂或阳离子防腐剂中的至少一个。
在第六个实施例中,本公开提供了根据第一至第五个实施例中任一项所述的方法,其中所述活性剂包含葡糖酸氯己定。
在第七个实施例中,本公开提供了根据第五或第六个实施例所述的方法,其中所述活性剂包含聚合物。
在第八个实施例中,本公开提供了根据第一至第七个实施例中任一项所述的方法,其中所述基材的表面包含有机硅聚合物、含氟聚合物或丙烯酸类聚合物中的至少一个。
在第九个实施例中,本公开提供了根据第一至第八个实施例中任一项所述的方法,其中所述基材的表面是微结构化的。
在第十个实施例中,本公开提供了根据第一至第九个实施例中任一项所述的方法,其中所述活性沉积物以阵列排列于所述基材的表面上。
在第十一个实施例中,本公开提供了根据第一至第十个实施例中任一项所述的方法,其中所述接触印刷包括柔性版印刷。
在第十二个实施例中,本公开提供了根据第一至第十一个实施例中任一项所述的方法,其中所述接触印刷包括辊涂。
在第十三个实施例中,本公开提供了根据第一至第十二个实施例中任一项所述的方法,其中所述接触印刷包括刮涂或刮刀涂布。
在第十四个实施例中,本公开提供了根据第一至第十三个实施例中任一项所述的方法,所述方法还包括在将活性组合物接触印刷到基材的表面上之后,但在经印刷表面上设置压敏粘合剂层之前,从活性组合物移除液体载体的至少一部分。
在第十五个实施例中,本公开提供了根据第一至第十四个实施例中任一项所述的方法,其中在接触基材的表面之前,将压敏粘合剂设置在背衬上。
在第十六个实施例中,本公开提供了根据第一至第十五个实施例中任一项所述的方法,其中所述压敏层通过在经印刷表面上涂布压敏粘合剂组合物来形成。
在第十七个实施例中,本公开提供了根据第一至第十六个实施例中任一项所述的方法,其中所述背衬的至少一部分是透明或半透明的。
在第十八个实施例中,本公开提供了根据第一至第十七个实施例中任一项所述的方法,其中所述背衬的至少一部分和所述压敏粘合剂层的至少一部分是透明或半透明的。
本文所提及的所有专利和出版物据此全文以引用方式并入本文。在不脱离本公开的范围和精神的条件下,本领域的技术人员可对本公开进行各种修改和更改,并且应当理解,本公开不应不当地受限于本文所述的示例性实施例。
Claims (18)
1.一种制备压敏粘合剂制品的方法,所述方法包括:
将活性组合物接触印刷到离型基材的表面上以形成经印刷表面,由此,所述活性组合物自发地对所述离型基材的所述表面去湿以在所述离型基材的所述表面上形成活性沉积物,其中所述活性组合物包含溶解或分散在含水液体载体中的活性剂;以及
在所述经印刷表面上设置压敏粘合剂层。
2.根据权利要求1所述的方法,其中随着最初与所述离型基材的所述表面接触,所述活性组合物接触所述离型基材的所述表面的第一区域,并且其中所述活性沉积物接触所述离型基材的所述表面的第二区域,并且其中所述第二区域小于或等于所述第一区域的50%。
3.根据权利要求1所述的方法,其中所述活性组合物还包含可水合聚合物。
4.根据权利要求1所述的方法,其中所述活性剂包含至少一种非挥发性组分。
5.根据权利要求1所述的方法,其中所述活性剂包含抗微生物剂、局部防腐剂或阳离子防腐剂中的至少一个。
6.根据权利要求1所述的方法,其中所述活性剂包含葡糖酸氯己定。
7.根据权利要求1所述的方法,其中所述活性剂包含聚合物。
8.根据权利要求1所述的方法,其中所述离型基材的所述表面包含有机硅聚合物、含氟聚合物或丙烯酸类聚合物中的至少一个。
9.根据权利要求1所述的方法,其中所述离型基材的所述表面是微结构化的。
10.根据权利要求1所述的方法,其中所述活性沉积物以阵列排列于所述离型基材的所述表面上。
11.根据权利要求1所述的方法,其中所述接触印刷包括柔性版印刷。
12.根据权利要求1所述的方法,其中所述接触印刷包括凹版辊涂布。
13.根据权利要求1所述的方法,其中所述接触印刷包括刮涂或刮刀涂布。
14.根据权利要求1所述的方法,还包括在将所述活性组合物接触印刷到所述离型基材的所述表面上之后,但在所述经印刷表面上设置所述压敏粘合剂层之前,从所述活性组合物移除所述液体载体的至少一部分。
15.根据权利要求1所述的方法,其中在接触所述离型基材的所述表面之前,将所述压敏粘合剂设置在背衬上。
16.根据权利要求1所述的方法,其中所述压敏层通过在所述经印刷表面上涂布压敏粘合剂组合物来形成。
17.根据权利要求1所述的方法,其中所述背衬的至少一部分是透明或半透明的。
18.根据权利要求1所述的方法,其中所述背衬的至少一部分和所述压敏粘合剂层的至少一部分是透明或半透明的。
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US61/569,954 | 2011-12-13 | ||
PCT/US2012/068757 WO2013090191A2 (en) | 2011-12-13 | 2012-12-10 | Method of making pressure-sensitive adhesive article including active agent |
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EP (1) | EP2791216B1 (zh) |
JP (1) | JP6120873B2 (zh) |
KR (1) | KR20140101416A (zh) |
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Also Published As
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WO2013090191A2 (en) | 2013-06-20 |
EP2791216A2 (en) | 2014-10-22 |
WO2013090191A3 (en) | 2013-11-07 |
IN2014CN04311A (zh) | 2015-09-04 |
US20140363564A1 (en) | 2014-12-11 |
JP2015507036A (ja) | 2015-03-05 |
CN104024308B (zh) | 2015-11-25 |
US9592161B2 (en) | 2017-03-14 |
EP2791216B1 (en) | 2015-09-23 |
JP6120873B2 (ja) | 2017-04-26 |
KR20140101416A (ko) | 2014-08-19 |
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