CN1846792A - 粘合剂制剂 - Google Patents
粘合剂制剂 Download PDFInfo
- Publication number
- CN1846792A CN1846792A CNA2006100736025A CN200610073602A CN1846792A CN 1846792 A CN1846792 A CN 1846792A CN A2006100736025 A CNA2006100736025 A CN A2006100736025A CN 200610073602 A CN200610073602 A CN 200610073602A CN 1846792 A CN1846792 A CN 1846792A
- Authority
- CN
- China
- Prior art keywords
- pressure sensitive
- adhesive layer
- sensitive adhesive
- adhesive formulation
- adhesive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Abstract
本发明涉及一种具有优良粘合性质的粘合剂制剂,其不容易剥离或脱落并且可以长时间粘附。粘合剂制剂10具有由织物制成的载体1和形成在载体1的一个表面上的压敏粘合剂层3,所述压敏粘合剂层包含压敏粘合剂和药物。载体1单位面积的质量(CW)和压敏粘合剂层3单位面积的质量(AW)的比率(CW/AW)为1.0-5.0,载体1没有粘合剂层的表面的静摩擦系数为0.25-0.75,并且在粘合剂制剂10的一个方向上的20%模量(AM)和垂直于所述方向的方向上的20%模量(EM)各为0.5-1.5N/cm,并且其比率(AM/EM)为0.5-2.0。
Description
技术领域
本发明涉及一种具有优良粘合性质的粘合剂制剂,其不容易剥离或脱落并且可以长时间粘附。
背景技术
近年来,包含主要由聚对苯二甲酸乙二醇酯和聚丙烯制成的塑料薄层膜作为载体和形成在载体一侧的包含粘合剂和药物的压敏粘合剂层的粘合剂制剂已经被广泛使用。至于粘合剂制剂,例如可以提及全身或局部透皮吸收性粘合剂制剂,含有炎性镇痛药的挠性橡皮膏等。但是,在一些透皮吸收性粘合剂制剂中,部分粘合剂由于冷流而从载体周边挤出,挤出的粘合剂在施用过程中可能附着并且污染衣服,并且粘合剂制剂经常在穿衣或脱衣过程中剥离。另外,在剥落过程中胶经常可能残留在沿着粘合剂制剂周边的皮肤上。另一方面,由于橡皮膏载体没有粘合剂层的表面摩擦高,粘合剂制剂可能令人不便地在穿衣/脱衣过程中剥离和脱落。此外,可能发生以下情况:橡皮膏在某一方向上具有足够的挠性和拉伸性但在与其垂直的方向上挠性和拉伸性差,从而反过来可能导致粘合过程中的异物感,以及橡皮膏由于弯曲部分的挠性和拉伸性不足而剥离或脱落。
为了改善常规粘合剂制剂的这种缺陷,提出了以下方法。例如,至于防止部分粘合剂由于冷流从载体周边挤出的方法,提出了:通过用活性物质使构成粘合剂的聚合物交联等限制流动性的方法(JP-B-2700835和JP-B-3014188),通过使用与粘合剂具有良好亲合力的载体膜来限制流动性的方法(JP-B-6-35381和JP-B-7-25665),通过将织物如无纺织物等层压在载体膜上形成物理无序而抑制流动性的方法(JP-B-3081858和JP-B-2886021),等。按照JP-B-2700835、JP-B-3014188、JP-B-6-35381、JP-B-7-25665、JP-B-3081858和JP-B-2886021中所述的方法,几乎可以解决部分粘合剂由于冷流从载体周边挤出的麻烦,但是由于使用拉伸性差的构件作为载体,在以下方面出现问题:对皮肤运动的随从性差,粘合过程中有相当大的异物感,和难以施用在弯曲部分,从而限制了粘合部位。
至于改善在某一方向上具有足够的挠性和拉伸性但在与其垂直的方向上挠性和拉伸性差的问题的方法,提出了:提供在一个方向上的50%模量为10-600g/cm的粘合剂制剂的方法(JP-A-5-238931);提供具有可拉伸载体和粘合剂层的粘合剂制剂的方法,其中长边方向和短边方向上50%伸长时的负载为0.98-14.71N/5cm(WO01/095889);提供在30%模量试验中纵向上强度为200g-3kg并且横向上强度为100g-600g的粘合剂制剂的方法,所述的30%模量试验是在伸长强度为200mm/min的测量条件下,使用通过将含有可拉伸聚酯机织织物作为载体的粘合片切割成50mm宽、200mm长的片而获得的试样(JP-B-3499247),等。但是,按照JP-A-5-238931和WO01/095889中所述的方法,粘合剂制剂拉长太多,不适合预测异物感并且在实际粘合过程中不舒服,而在JP-B-3499247中描述的粘合剂制剂根据粘合部位而产生异物感,因为其纵向和横向的30%模量不同。另外,至于减小载体的摩擦的方法,提出了:提供其中载体的静摩擦系数为0.5-2.5的粘合剂制剂的方法(WO02/100384)等。但是,当载体的静摩擦系数超过0.75时,摩擦变得过高并且粘合剂制剂由于与衣服的摩擦而可能剥离或者有时脱落。
发明内容
本发明考虑到这样的情况,并且旨在提供一种具有优良粘合性质的粘合剂制剂,其不容易剥离或脱落并且可以长时间粘附。
本发明的发明人进行了深入研究以试图解决上述问题,并且发现当完整包含载体和压敏粘合剂层的粘合剂制剂满足:载体和压敏粘合剂层的单位面积的某种质量比率,载体的不含粘合剂层的表面的某种静摩擦系数,以及在粘合剂制剂给定方向上的20%模量的某种水平及其某种比例时,可以解决上述问题,这导致本发明的完成。
因此,本发明提供以下内容:
(1)一种粘合剂制剂,其包含由织物制成的载体和形成在载体一个表面上的压敏粘合剂层,所述压敏粘合剂层包含压敏粘合剂和药物,其中
所述载体单位面积的质量(CW)和所述压敏粘合剂层单位面积的质量(AW)的比率(CW/AW)为1.0-5.0,
所述载体没有粘合剂层的表面的静摩擦系数为0.25-0.75,并且
在粘合剂制剂一个方向上的20%模量(AM)和垂直于所述方向的方向上的20%模量(EM)各为0.5-1.5N/cm,并且其比率(AM/EM)为0.5-2.0。
(2)上述(1)的粘合剂制剂,该粘合剂制剂的剪切粘合力为1.0-7.0N/cm2。
(3)上述(1)或(2)的粘合剂制剂,其中上述的织物是由合成纤维制成的。
(4)上述(1)至(3)中任何一项的粘合剂制剂,其中上述的织物是针织物。
(5)上述(1)至(4)中任何一项的粘合剂制剂,其中上述的织物是由聚对苯二甲酸乙二醇酯制成的。
(6)上述(1)至(5)中任何一项的粘合剂制剂,其中上述的压敏粘合剂包含丙烯酸类共聚物,所述丙烯酸类共聚物是通过包含作为主要组分的(甲基)丙烯酸烷基酯的单体混合物的共聚而获得的。
本发明的粘合剂制剂在粘合过程中很少引起异物感或痒感,并且提供舒服的粘合感觉。此外,由于载体的低摩擦,粘合和剥离过程中胶残余得到抑制。另外,由于粘合剂制剂在锻炼和日常生活中对粘合部位的拉伸的随从性高,其在穿衣和脱衣以及粘合过程中不剥离或脱落。此外,由于本发明的粘合剂制剂在粘合3天后不脱落,而是可以保持上面所述优良舒适的粘合感觉,它可以长期施用于粘合部位。
附图说明
图1是显示本发明粘合剂制剂一个实施方案的剖面图。
图2是显示本发明粘合剂制剂另一实施方案的剖面图。
具体实施方式
下面将参考优选实施方案详细解释本发明。在附图的解释中,相同的参考符号指的是相同的元件,并且省略重复解释。另外,出于方便目的,图中的大小比率不是必然与解释中的那些匹配。
图1是显示本发明粘合剂制剂一个实施方案的剖面图。粘合剂制剂10包含由织物制成的载体1和形成在载体1上的压敏粘合剂层3。图2是显示本发明粘合剂制剂一个优选实施方案的剖面图。粘合剂制剂20包含由织物制成的载体1、形成在载体1上的压敏粘合剂层3和形成在压敏粘合剂层3上的释放片5。在粘合剂制剂20中,将释放片5层压在压敏粘合剂层3上以防止压敏粘合剂层3在制造、运输和保存过程中粘附到仪器、容器等上,并且防止粘合剂制剂20的劣化。使用时,剥离释放片5以暴露压敏粘合剂层3并将其粘合剂表面粘附到皮肤上。以下,引用粘合剂制剂20进行解释。该解释同样适用于粘合剂制剂10。
在粘合剂制剂20中,载体1单位面积的质量(CW)和压敏粘合剂层3单位面积的质量(AW)的比率(CW/AW)为1.0-5.0,优选1.5-4.5。结果,即使当部分压敏粘合剂由于冷流而从载体1周边挤出时,部分挤出的压敏粘合剂随着使用时粘合剂制剂20从释放片5的剥离而粘附在载体1的部分边上。因此,可以防止在施用过程中附着的部分压敏粘合剂污染衣服,以及皮肤上的部分压敏粘合剂的残留。当载体1具有给定厚度时,可能暴露在粘合剂制剂20周边的压敏粘合剂不容易接触衣服。因此,可以防止由在穿衣/脱衣过程中压敏粘合剂与部分衣服的粘合造成的粘合剂制剂20的剥离或脱落。此外,构成载体1的织物自由地具有许多间隙。因此,部分压敏粘合剂由于冷流从载体1周边挤出的可能性变得更低。当CW/AW变得小于1.0时,载体1与压敏粘合剂层3的厚度比率趋向于变小。结果,载体1的边对于因冷流而挤出的部分压敏粘合剂而言可能不足够宽以将其粘附,部分压敏粘合剂可能在施用过程中附着在衣服上,或者部分压敏粘合剂可能在剥离过程中残留在皮肤上。另一方面,当CW/AW超过5.0时,载体1的厚度变得相当厚,其边变得容易被衣服缠住。另外,压敏粘合剂层3的厚度变得相对薄而皮肤粘合力下降。结果,随着身体的运动或者在穿衣/脱衣过程中粘合剂制剂20更易于剥离/脱落。
同时可以按照JIS L 1018:1990测量载体1的单位面积质量,其优选为60-160g/m2,更优选为80-130g/m2。当质量小于60g/m2时,悬垂性趋向于下降并且处理性趋向于劣化。当其超过160g/m2时,模量变高,并且拉伸性和透湿性趋向于劣化,这在经济上是不利的。载体1的厚度可以按照JIS L1085:1998测量,并且优选为150-750μm,更优选为200-700μm。当载体1的厚度小于150μm时,强度变得不足并且操作性也趋向于退化,还有压敏粘合剂渗出的担心。当其超过750μm时,挠性和拉伸性劣化,并且在粘合过程中由于厚度而可能有异物感。此外,透湿性趋向于劣化,这在经济上是不利的。
考虑到粘合性、药物的必要量和利用率等,压敏粘合剂层3单位面积的质量优选为10-150g/m2,更优选为30-100g/m2。当质量小于10g/m2时,不能获得足够的皮肤粘合力或不容易提供足够的药理学效果。当其超过150g/m2时,药物利用率可能下降并且生产成本趋向于增加。还可以按照JIS L 1018:1990测量压敏粘合剂层3的单位面积质量。适当设置载体1的单位面积质量和压敏粘合剂层3的单位面积质量,以满足1.0-5.0的(CW/AW)比率。压敏粘合剂层3的厚度优选为5-150μm,更优选为10-130μm。当压敏粘合剂层3厚度小于5μm时,不容易提供足够的皮肤粘合力,并且在施用过程中容易发生剥离和脱落。当其超过150μm时,压敏粘合剂容易从载体1周边挤出,这在粘合过程中可能引起强的皮肤刺激和异物感。压敏粘合剂层3的厚度也可以按照JIS L 1085:1998测量。
载体1没有压敏粘合剂层的表面的静摩擦系数为0.25-0.75,优选0.3-0.7。因此,可以赋予处理接触(handling tough)并且可以防止由与皮肤摩擦造成的剥离。当该静摩擦系数小于0.25时,在操作过程中表面变得滑溜,在粘合过程中可能引起不便。另外,与压敏粘合剂层3的锚定效果变得不足并且粘合剂制剂的完整性变低。当其超过0.75时,与衣服的摩擦增加,随着人体的运动或者在穿衣/脱衣过程中粘合剂制剂更易于剥离/脱落。此处,在本说明书中,“静摩擦系数”是通过JIS P 8147:1994中描述的试验方法(按照纸和纸板的摩擦系数试验方法)测量的值。
此外,粘合剂制剂20在任一方向上显示20%模量(AM)并且在垂直于该方向的方向上的20%模量(EM)各为0.5-1.5N/cm。其比率(AM/EM)为0.5-2.0,优选0.7-1.3。这具有粘合的舒服感和优良的皮肤随从性的效果。当AM和EM小于0.5 N/cm时,强度变得不足,粘合过程中趋向于发生因破损和破坏而导致的剥离,并且韧性降低造成操作困难。当其超过1.5时,对皮肤变形的随从性变得不足并且在粘合过程中有异物感。另外,粘合剂制剂20的周边在弯曲部分容易剥离。当AM/EM小于0.5或超过2.0时,粘合过程中出现异物感并且容易出现因弯曲造成的剥离和脱落。本说明书中,“20%模量”是指按照JIS Z 0237:2000中描述的试验方法(按照压敏粘合带-压敏粘合片的拉伸强度和伸长率试验方法)测量的值。通常用来评估拉伸性和挠性的50%模量对于精确测量本发明载体1的拉伸性是是不合适的,因为测量主要是在弹性消失的区域中进行的。
此外,考虑到减小在剥离过程中的物理刺激、降低在粘合过程中的异物感和弯曲部分的剥离困难,粘合剂制剂20的剪切粘合力优选为1.0-7.0N/cm,更优选为1.5-6.5N/cm。当剪切粘合力小于1.0N/cm时,周边趋向于在弯曲部分剥离。当其超过7.0N/cm时,粘合剂制剂20的剥离变得疼痛,物理刺激引起皮肤不适,并且粘合过程中皮肤伸长的抑制引起异物感。本说明书中,“剪切粘合力”是按照JIS Z 0237:1991中描述的试验方法(按照压敏粘合带-压敏粘合片试验方法的参考文献3的方法)测量的值。
粘合剂制剂20的透湿量优选为500-3000g/cm2·24小时,更优选为800-2000g/cm2·24小时,因为可以抑制剥离和因出汗产生的汗的郁积,以及由此造成的药理学效果不足和皮肤不适如皮肤刺激等,并且通过适宜的封闭敷裹技术(ODT)效果,可以获得治疗或预防效果。当透湿量小于500g/cm2·24小时时,出汗产生的湿气不能容易地从皮肤和压敏粘合剂层3表面之间蒸发,导致粘合剂制剂20的剥离和汗的郁积,这反过来容易降低药理效果并且引起皮肤不适如皮肤刺激等。另一方面,当透湿量超过3000g/cm2·24小时时,难以获得适宜的ODT效果,并且由药物导致的治疗或预防效果趋向于下降。可以根据以下因素适当地控制透湿量:载体1的单位面积质量,载体1的厚度,粘合剂制剂20的面积,形成压敏粘合剂层3的共聚物的单体组成比率,上述有机液体组分的种类和含量比率,压敏粘合剂层3的单位面积质量等。另外,织物本身的透湿量优选不小于5000g/m2·24小时,更优选不小于7000g/m2·24小时。当透湿量小于5000g/m2·24小时时,当压敏粘合剂层3层压时不能容易地获得足够的透湿性。此外,相对于构成载体1的织物固有的透湿量,适宜地将粘合剂制剂20的透湿量调节到5-25%,优选8-20%。当该比率超过25%时,不能容易地获得适当的ODT效果,并且由药物导致的治疗或预防效果趋向于下降。另一方面,当其小于5%时,不能明显利用织物的多孔性,并且不能容易获得充分效果。本说明书中,“透湿量”是按照JIS L 1099:1993值描述的方法(按照纤维产品透湿程度试验方法的氯化钙方法)测量的值。
考虑到减小剥离过程中的疼痛和物理刺激、降低粘合过程中的异物感和稳定的长期粘合方面,粘合剂制剂20与酚醛塑料板的粘合性优选为0.1-0.7N/24mm宽度,更优选为0.15-0.6N/24mm宽度。当粘合性小于0.1N/24mm宽度时,与皮肤的粘合力变得不足,并且在施用过程中可能出现剥离和脱落。当其超过0.7N/24mm宽度时,容易出现剥离时的疼痛造成的皮肤不适和物理刺激。尽管常规使用的粘合带大多数的粘合性比该值大,由于粘合剂制剂20,连同载体1和压敏粘合剂层3一起,能够跟随即使温和并且微小的变形,实际的皮肤粘合面积变大,并且可以获得良好的皮肤粘合。本说明书中,“粘合力”指的是按照JIS Z 0237:2000中描述的方法(按照压敏粘合带-压敏粘合片的粘合力试验方法)测量的值。即,将粘合剂制剂20切成宽24mm的样品带,粘附在酚醛塑料板(厚2mm,宽50mm,长130mm)上,并且通过辊(负载850g)往复一次按压。在按压粘合后,将粘合剂制剂于23℃放置20分钟,在相同的气氛下用TENSILON型拉伸试验机以300mm/分钟的速度在180度方向上剥离。此处作为释放力测量的值是上述的值。
本说明书中,“织物”指的是通过化学纤维或天然纤维的针织、机织、交织等形成的片状纤维束,其可以是针织织物、机织织物、无纺织物等中的任一种形式。这些当中,考虑到处理接触、挠性、弹性和均匀性,优选针织织物。尽管对形成针织织物的方法没有特别限制,只要可以维持拉伸性和弹性即可,但是优选经编,更优选圆筒形针织和纬编。
对用于载体1的织物没有特别限制,只要制剂满足上述预定数值范围内的上述单位面积质量、静摩擦系数和20%模量即可。例如,可以使用天然纤维如棉、麻、丝、毛等,再生纤维如粘胶人造丝、铜铵人造丝等,半合成纤维如普罗米克斯、二乙酸纤维素、三乙酸纤维素等,以及合成纤维如尼龙、维尼纶、亚乙烯基(vinylidene)、聚氯乙烯、聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、聚乙烯、聚丙烯、聚氨酯、苯甲酸酯、polycral等。考虑到稳定性、安全性、均匀性、经济方面、加工性、药物的不迁移等,优选合成纤维,更优选聚酯和聚烯烃,还更优选聚对苯二甲酸乙二醇酯。从通用性、经济方面和加工性考虑,优选纤维具有直径为10-30μm、更优选15-25μm的近似圆形横截面形状。另外,可以使用复合纤维。
压敏粘合剂层3优选由作为主要组分的医用粘合剂制成,所述医用粘合剂通常用作在施用到皮肤时不容易引起皮肤刺激等的压敏粘合剂。至于这样的医用粘合剂,可以提及丙烯酸类粘合剂、天然橡胶粘合剂、合成橡胶粘合剂、硅氧烷粘合剂、乙烯基酯粘合剂、乙烯基醚粘合剂等。其中,从稳定的质量、粘合性和粘合剂透湿性的易控制性方面考虑,优选丙烯酸类粘合剂。
优选丙烯酸类粘合剂含有通过(甲基)丙烯酸烷基酯(主要组分)与可共聚单体的共聚获得的共聚物。由于这种丙烯酸类共聚物可以被交联剂交联,因此可以抑制粘合性的下降或消失,粘合性的下降或消失是由施用于载体1后随着时间的流逝,共聚物通过针织线圈与纤维之间的间隙渗透造成的。至于(甲基)丙烯酸烷基酯,可以提及具有2-18个碳原子、优选4-12个碳原子的烷基的伯至叔醇与丙烯酸或甲基丙烯酸形成的酯。可以将一种或多种(甲基)丙烯酸烷基酯组合使用。
至于可以与(甲基)丙烯酸烷基酯共聚的单体,可以提及在分子中含有至少一个可加聚的不饱和双键并且在侧链上含有官能团的多官能单体,所述官能团如羧基、羟基、硫氧基(sulfoxyl group)、氨基、酰胺基、烷氧基等。至于含羧基的单体,可以提及(甲基)丙烯酸、衣康酸、马来酸、马来酸酐等。至于含羟基的单体,可以提及(甲基)丙烯酸羟基乙酯、(甲基)丙烯酸羟基丙酯等。至于含硫氧基的单体,可以提及苯乙烯磺酸、烯丙基磺酸、(甲基)丙烯酸磺基丙酯、(甲基)丙烯酰氧基萘磺酸、丙烯酰氨基甲基丙磺酸等。至于含氨基的单体,可以提及(甲基)丙烯酸氨基乙酯、(甲基)丙烯酸二甲基氨基乙酯、(甲基)丙烯酸叔丁基氨基乙酯等。至于含酰胺基的单体,可以提及(甲基)丙烯酰胺、二甲基(甲基)丙烯酰胺、N-丁基丙烯酰胺、N-羟甲基(甲基)丙烯酰胺、N-羟甲基丙烷(甲基)丙烯酰胺等。至于含烷氧基的单体,可以提及(甲基)丙烯酸甲氧基乙酯、(甲基)丙烯酸乙氧基乙酯、(甲基)丙烯酸甲氧基乙二醇酯、(甲基)丙烯酸甲氧基二甘醇酯、(甲基)丙烯酸甲氧基聚乙二醇酯、(甲基)丙烯酸乙氧基聚乙二醇酯、(甲基)丙烯酸四氢糠酯等。
此外,除上述之外的可共聚单体还可以提及,例如(甲基)丙烯腈、乙酸乙烯酯、丙酸乙烯酯、N-乙烯基-2-吡咯烷酮、N-乙烯基乙酰胺、甲基乙烯基吡咯烷酮、乙烯基吡啶、乙烯基哌啶酮、乙烯基嘧啶、乙烯基哌嗪、乙烯基吡嗪、乙烯基吡咯、乙烯基咪唑、乙烯基己内酰胺、乙烯基噁唑和乙烯基吗啉。这些可共聚单体的一种或多种可以组合使用。考虑到粘合性、凝结性、透湿性控制等,优选将含羧基的单体、含烷氧基的单体和含羟基的单体中的至少一种作为必要组分,和需要时的上面示例的其它单体共聚。
优选丙烯酸类共聚物含有比例不小于40质量%的(甲基)丙烯酸烷基酯,更优选由(甲基)丙烯酸烷基酯(50-99.5质量%,优选60-97质量%)与上述共聚单体(0.5-50质量%,优选2-10质量%)共聚获得的共聚物。具体地,可以提及(甲基)丙烯酸-2-乙基己酯与(甲基)丙烯酸的共聚物,以及(甲基)丙烯酸-2-乙基己酯(40-99.5质量%,,优选60-97质量%)、(甲基)丙烯酸(0.5-50质量%,优选2-10质量%)和N-乙烯基-2-吡咯烷酮(5-50质量%,优选10-40质量%)的共聚物。可以使用(甲基)丙烯酸烷基酯和上述的可共聚单体,通过已知的自由基聚合方法如溶液聚合法、乳液聚合法、本体聚合法、悬浮聚合法等合成丙烯酸类共聚物。
尽管压敏粘合剂可以由上述共聚物单独组成,但是其可以含有与所述共聚物相容的有机液体组分。有机液体组分通过增塑共聚物使压敏粘合剂层3具有柔性度而减小物理性的皮肤刺激,而且还能够控制透湿性。对有机液体组分没有特别限制,只要其在室温是液体,具有增塑作用并且与上述共聚物相容即可,其中优选改善药物的透皮吸收性和保存稳定性的有机液体组分。具体可以提及,由含有12-16个(优选12-14个)碳原子的高级脂肪酸和含有1-4个碳原子的低级一元醇获得的脂肪酸酯;含有8-10个碳原子的脂肪酸;二元醇类,如1,2-亚乙基二醇、二甘醇、三甘醇、聚乙二醇、丙二醇、聚丙二醇等;脂肪和油类,如橄榄油、蓖麻油、角鲨烯、羊毛脂等;有机溶剂,如乙酸乙酯、乙醇、二甲基癸基亚砜、甲基辛基亚砜、二甲亚砜、二甲基甲酰胺、二甲基乙酰胺、二甲基月桂酰胺、十二烷基吡咯烷酮、异山梨糖醇等;液体表面活性剂;常规已知的增塑剂,如己二酸二异丙酯、邻苯二甲酸酯、癸二酸二乙酯等;烃类,如液体石蜡等;以及乙氧基化硬脂醇、甘油脂肪酸酯(室温下为液体)、脱水山梨糖醇脂肪酸酯、肉豆蔻酸异丙酯、肉豆蔻酸异十三烷基酯、月桂酸乙酯、N-甲基-2-吡咯烷酮、油酸乙酯、油酸、己二酸二异丙酯、棕榈酸二异丙酯、棕榈酸辛酯、1,3-丙二醇、甘油等。这些有机液体组分可以一种或多种组合使用。
上述有机液体组分中,考虑到与共聚物的相容性、减小皮肤刺激、适当的皮肤粘合力、加热步骤中的不挥发性等,优选使用脂肪酸酯。至于构成脂肪酸酯的高级脂肪酸,优选月桂酸(C12)、肉豆蔻酸(C14)和棕榈酸(C16),特别优选肉豆蔻酸。至于低级一元醇,可以提及甲醇、乙醇、丙醇、丁醇等。这些不限于直链醇,还可以是支链醇。这些醇中,优选异丙醇作为低级一元醇。至于脂肪酸酯,最优选肉豆蔻酸异丙酯。有机液体组分的含量,相对于每100质量份的上述共聚物,优选为10-150质量份,更优选为50-120质量份。当含量小于10质量份时,压敏粘合剂层3未被充分增塑,可能不能充分减小物理性的皮肤刺激。当其超过150质量份时,即使共聚物的凝结是充分的,有机液体组分也可能不能充分保持在压敏粘合剂层3中,并且有机液体组分可能浮现在压敏粘合剂层3表面上从而降低粘合性。
压敏粘合剂层3可以与交联剂交联形成凝胶。这具有加入的脂肪酸酯不流出并且赋予内聚的作用。例如,可以使用交联剂如聚异氰酸酯化合物、有机过氧化物、有机金属盐、金属醇盐、金属螯合物、多官能化合物等,来进行交联处理。这些交联剂中,考虑到交联反应性和处理性质,优选三官能异氰酸酯和铝螯合物。这些交联剂具有非常优良的可使用性,因为它们在涂布和干燥之前几乎不使溶液增稠。对于每100质量份共聚物,交联剂含量通常为0.01-2质量份,优选0.05-1.5质量份。
对压敏粘合剂层3中含有的药物没有特别限制,只要其具有透皮吸收性即可,并且根据治疗对象而适当选择。药物的具体实例包括:镇静催眠药如阿普唑仑、地西泮、硝西泮、氟地西泮、苯巴比妥等,抗焦虑药,抗癫病药如苯妥英、三甲双酮、乙琥胺、唑尼沙胺、氯巴占等,退热药,消炎药和止痛药如水杨酸甲酯、水杨酸乙二醇酯、对乙酰氨基酚、甲芬那酸、吲哚美辛、酮洛芬、氟比洛芬、洛索洛芬、吡罗昔康等,抗帕金森病药如金刚烷胺、比哌立登、左旋多巴、司来吉兰、苯海索、培高利特、他利克索等,精神神经药如氯丙嗪、奋乃静、丙咪嗪、依替唑仑、哌罗匹隆、baroxetine、利他林、奥氮平、舒必利、卤呱啶醇等,局部麻醉药如利多卡因、奥昔卡因、普鲁卡因、地布卡因、布比卡因、甲哌卡因、robivacaine、苯佐卡因等,骨骼肌松弛药如氯唑沙宗、氯苯甘醚、琥珀胆碱、维库溴铵等,自主神经系统药如carpronium、贝胆碱、新斯的明、双环维林、吡斯的明等,解痉药如东莨菪碱、阿托品、罂粟碱、乙哌立松、替扎尼定、巴氯芬等,强心药如洋地黄毒苷、地高辛、氨茶碱、咖啡因、依替福林等,心律失常药如普鲁卡因胺、奎尼丁、阿替洛尔、普萘洛尔、吲哚洛尔等,利尿药如螺内酯、乙酰唑胺、呋塞米等,抗高血压药如肼屈嗪、利血平、咪达普利、依那普利、赖诺普利、可乐定、尼卡地平、特拉唑嗪、布尼洛尔等,血管收缩药如米多君等,血管扩张药如异山梨醇、地拉、地尔硫、尼可地尔、硝酸甘油、硝苯地平等,抗血脂药如氯贝胺、estase、普伐他汀、尼可莫尔、普罗布考等,镇咳药如麻黄碱、诺斯卡品、右美沙芬、福米诺苯、二甲啡烷等,镇咳祛痰药如可待因、双氢可待因、替培啶等,支气管扩张药如茶碱、特布他林、妥洛特罗、克仑特罗、沙丁胺醇、丙卡特罗等,胃溃疡药如西米替丁、雷尼替丁、尿囊素铝、哌仑西平、伊索拉定等,激素药如碘塞罗宁、左甲状腺素、氢化可的松、地塞米松、泼尼松龙、甲睾酮、炔雌醇等,催产药如麦角新碱等,泌尿生殖和肛门药如奥昔布宁、坦索洛新、黄酮哌酯、利托君等,维生素如α-calcidol、carcitriol、维生素B1、维生素B2、维生素B6、甲钴胺、维生素C、维生素E等,局部刺激药如辣椒碱、壬酸香草基酰胺、二氢辣椒碱、辣椒酯(capsiate)、薄荷醇、薄荷酮、樟脑、姜醇、姜酮等,肝病用药如葡醛内酯、氨基乙基磺酸等,解毒药如谷胱甘肽、曲恩汀、青霉胺等,经常性醉酒用药如氰酰胺、戒酒硫等,痛风用治疗药如秋水仙碱、丙磺舒、别嘌呤醇、苯溴马隆等,酶制剂如氯化溶菌酶、舍雷肽酶等,糖尿病药如乙酰苯磺酰环己脲(acetohexamide)、格列本脲、甲苯磺丁脲、阿卡波糖等,代谢药物如硫酸软骨素钠、硫唑嘌呤、环孢菌素、他克莫司、卡莫司他等,烷基化药如环磷酰胺、美法仑、卡波醌等,代谢拮抗剂如巯基嘌呤、替加氟、氟尿嘧啶等,源自植物的抗肿瘤制剂如依托泊苷等,抗肿瘤药如阿那曲唑、法倔唑、索布佐生、比卡鲁胺等,抗组胺药如苯海拉明、异丙嗪、美喹他嗪、氯苯那敏、氯马斯汀等,抗过敏药如异丁司特、氮 斯汀、奥沙米特、曲尼司特、酮替芬等,抗生素如克林霉素、弗氏霉素、阿莫西林、氨苄西林、头孢克洛、头孢氨苄、红霉素、米诺环素等,磺胺药如磺胺甲噁唑、磺胺甲二唑等,抗结核药如异烟肼、吡嗪酰胺、乙胺丁醇等,合成抗菌药如依诺沙星、氧氟沙星、萘啶酸、诺氟沙星等,抗病毒药如阿昔洛韦、更昔洛韦、去羟肌苷、拉米夫定等,化疗药如特比萘酚、伊曲康唑、咪康唑等,抗原生物药如奎宁、甲硝唑等,肠蠕虫药如麝香草酚、山道年、噻苯唑等,麻醉品如吗啡、乙基吗啡、可待因、羟考酮、芬太尼、舒芬太尼、瑞芬太尼、左洛啡烷等,古柯生物碱药如可卡因等,兴奋剂药如去氧麻黄碱等,等等。上述药物包括可以实质上制备的无机盐和有机盐。这些药物的一种或多种可以组合使用。
尽管压敏粘合剂层3中药物的含量是根据经皮吸收药的种类和给药对象适当确定的,但是优选为0.01-60质量%,更优选为0.1-30质量%。当含量小于0.01质量%时,不能预期药物以治疗有效量释放,而当含量超过60质量%时,不容易获得与含量相应的治疗或预防效果,这在经济上是不利的。
必要时,除了压敏粘合剂和药物外,压敏粘合剂层3可以含有已知的添加剂,如粘合力赋予剂(例如,松香,改性松香,石油树脂,聚萜烯树脂,聚苯乙烯树脂,聚丁烯树脂,液体聚异丁烯等),增塑剂(例如液体石蜡等),吸收促进剂,表面活性剂(例如,脱水山梨糖醇三油酸酯等),填料,抗氧化剂(例如,没食子酸丙酯,2-巯基苯并咪唑等)等。
对释放片5没有特别限制,只要其在使用期间可以容易地从压敏粘合剂层3剥离即可。例如,使用聚酯、聚氯乙烯、聚偏氯乙烯、聚对苯二甲酸乙二醇酯等的膜,其中与压敏粘合剂层3的接触表面用硅氧烷处理;高级纸或薄玻璃纸与聚烯烃的层压膜等。释放片5的厚度通常不大于1000μm,优选30-200μm。另外,可以适当切割释放片5以便于粘合操作。
对粘合剂制剂20的制备方法没有特别限制。例如,可以将丙烯酸类共聚物、上述有机液体组分、药物和交联剂依次溶解或分散在溶剂中,将获得的溶液或分散体涂布在保护性释放片上并且干燥,在释放片上形成压敏粘合剂层,将载体粘附在压敏粘合剂层上,将其在合适的温度加热给定时间以进行交联反应,使压敏粘合剂层3转变成凝胶,得到粘合剂制剂。尽管粘合剂制剂20的大小根据治疗用途和使用的对象而变化,其通常为10-300cm2,优选20-200cm2。必要时,边缘可以具有圆弧,所述的圆弧具有合适曲率半径。
尽管粘合剂制剂20的剂量根据患者的年龄、体重、症状等变化,但是优选通常将每次施用含有0.01-100mg药物的粘合剂制剂20施用在成年人的胸、腹、背、臂、腿、面等或粘膜上,在1~7天内施用约1或2次。
实施例
下面将参考实施例详细解释本发明,但是这些实施例不应理解为限制性的。
(共聚物A溶液的制备)
将丙烯酸-2-乙基己酯(95质量份)、丙烯酸(5质量份)、乙酸乙酯(100质量份)和过氧化苯甲酰(0.2质量份)在装备有回流冷凝器、搅拌器、温度计、滴液漏斗和氮气入口管的可拆式烧瓶中,在氮气气氛中于60℃反应15小时,得到共聚物A的溶液。
(共聚物B溶液的制备)
将丙烯酸-2-乙基己酯(72质量份)、N-乙烯基-2-吡咯烷酮(25质量份)、丙烯酸(3质量份)、乙酸乙酯(333质量份)和偶氮双异丁腈(0.2质量份)在装备有回流冷凝器、搅拌器、温度计、滴液漏斗和氮气入口管的可拆式烧瓶中,在氮气气氛中于60℃反应6小时,然后在76℃反应18小时,得到共聚物B的溶液。
(聚异丁烯溶液的制备)
高分子量聚异丁烯(28.5份,VISTANEX MML-80,粘均分子量990,000,由BASF制造)、低分子量聚异丁烯(43份,HIMOL 6H,粘均分子量60,000,由Nippon Petrochemicals Company,Limited制造)、聚丁烯(8.5份,HV-300,粘均分子量1,260,由Nippon Petrochemicals Company,Limited制造)和脂环族石油树脂(20份,ARKON P-100,软化点100℃;由Arakawa ChemicalIndustries,Ltd.制造)溶解在己烷中,得到聚异丁烯溶液。
(实施例1)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例2)
向上述共聚物B溶液,其固体含量相当于9g,加入肉豆蔻酸异丙酯(11g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.036g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例3)
向上述聚异丁烯溶液,其固体含量相当于16g,加入肉豆蔻酸异丙酯(3g)、水杨酸乙二醇酯(1g)和适量的用于调节浓度的己烷/四氢呋喃(1∶1)混合物,并且搅拌混合物,得到含有药物并且非溶剂浓度为20质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。此外,切割层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例4)
向上述共聚物A溶液,其固体含量相当于10g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约550μm厚的单位面积质量为150g/m2的圆形针织织物B上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例5)
向上述共聚物B溶液,其固体含量相当于9g,加入肉豆蔻酸异丙酯(11g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.036g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为40g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的质量为60g/m2的纺花边的(spunlaced)无纺织物圆形针织织物上,所述无纺织物由直径约5-10μm并且具有近似三角形截面的复合纤维制备,所述复合纤维由聚酯纤维(60%)和人造丝纤维(40%)制成。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例6)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、氟比洛芬(1g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATEHL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例7)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、辣椒碱(0.5g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATEHL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例8)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、辣椒碱(0.5g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATEHL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例9)
向上述的共聚物B溶液,其固体含量相当于10g,加入并混合酮洛芬(0.66g)、肉豆蔻酸异丙酯(12g)和异丙醇(20g)。向该溶液中加入5%异丙醇/乙酰乙酸乙酯(9/1(v/v))溶液形式的乙酰乙酸乙酯铝二异丙醇盐(0.3g),并且搅拌混合物,得到含有药物并且非溶剂浓度为25质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例10)
将以与实施例1相同的方式获得的含有药物的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为20g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例11)
将以与实施例1相同的方式获得的含有药物的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为40g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例12)
将以与实施例1相同的方式获得的含有药物的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为80g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约400μm厚的单位面积质量为105g/m2的圆形针织织物上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(实施例13)
将以与实施例1相同的方式获得的含有药物的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约550μm厚的单位面积质量为150g/m2的圆形针织织物上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例1)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在520μm厚的质量为85g/m2的纺花边的无纺织物上,所述无纺织物由直径约20μm并且具有近似圆形截面的聚酯皱缩纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例2)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在420μm厚的单位面积质量为100g/m2的纺花边的无纺织物上,所述无纺织物由直径约5-10μm并且具有近似三角形截面的复合纤维制备,所述复合纤维由聚酯纤维(60%)和聚丙烯纤维(40%)制成。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例3)
向上述聚异丁烯溶液,其固体含量相当于16g,加入肉豆蔻酸异丙酯(3g)、水杨酸乙二醇酯(1g)和适量的用于调节浓度的己烷/四氢呋喃(1∶1)混合物,并且搅拌混合物,得到含有药物并且非溶剂浓度为20质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约12μm厚的质量为16g/m2的单层聚酯膜上,用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例4)
向上述聚异丁烯溶液,其固体含量相当于16g,加入肉豆蔻酸异丙酯(3g)、水杨酸乙二醇酯(1g)和适量的用于调节浓度的己烷/四氢呋喃(1∶1)混合物,并且搅拌混合物,得到含有药物并且非溶剂浓度为20质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在通过层压约6μm厚的聚酯膜(质量9g/m2)于无纺织物(质量12g/m2)上获得的膜的无纺织物侧,所述无纺织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备,并且用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例5)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在约450μm厚的单位面积质量为110g/m2的圆形针织织物C上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例6)
将苯乙烯-异戊二烯-苯乙烯嵌段共聚物(12.5g,Kraton D-1107CU,由SHELL KAGAKU KK制造)、聚异丁烯(11.0g,Oppanol B80,由BASF制造)、氢化松香酯(6.0g,Steberite ester 7,由Rika Hercules制造)、液体石蜡(19.5g,Crystol J-352,由Esso Petroleum Co.,Ltd.制造)和没食子酸丙酯(0.5g)在氮气气氛于200℃加热下搅拌60分钟,得到压敏粘合剂溶液。向该溶液中,加入140℃(110-180℃)的水杨酸乙二醇酯,并且将混合物搅拌20分钟,得到含有药物的均匀压敏粘合剂溶液。随后,将该压敏粘合剂溶液浇铸在75μm厚的聚酯释放片上至单位面积质量为140g/m2。将如上制备的压敏粘合剂层转移并按压粘附在约450μm厚的单位面积质量为110g/m2的圆形针织织物C上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。切割该层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例7)
将苯乙烯-异戊二烯-苯乙烯嵌段共聚物(13.0g,Kraton D-1107CU,由SHELL KAGAKU KK制造)、聚异丁烯(10.5g,Oppanol B80,由BASF制造)、氢化松香酯(5.5g,Ester Gum H,由Arakawa Chemical Industries,Ltd.制造)、液体石蜡(19.0g,Crystol J-352,由Esso Petroleum Co.,Ltd.制造)、N-甲基-2-吡咯烷酮(2.5g)和没食子酸丙酯(0.5g)在氮气气氛于200℃加热下搅拌60分钟,得到压敏粘合剂溶液。向该溶液中,加入140℃(110-180℃)的水杨酸乙二醇酯,并且将混合物搅拌20分钟,得到含有药物的均匀压敏粘合剂溶液。随后,将该压敏粘合剂溶液浇铸在75μm厚的聚酯释放片上至单位面积质量为210g/m2。将如上制备的压敏粘合剂层转移并按压粘附在约450μm厚的单位面积质量为110g/m2的圆形针织织物C上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。切割该层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例8)
将苯乙烯-异戊二烯-苯乙烯嵌段共聚物(12.5g,Kraton D-1107CU,由SHELL KAGAKU KK制造)、聚异丁烯(11.0g,Oppanol B80,由BASF制造)、氢化松香脂(5.5g,Steberite ester 7,由Rika Hercules制造),液体石蜡(19.0g,Crystol J-352,由Esso Petroleum Co.,Ltd.制造)和没食子酸丙酯(0.5g)在氮气气氛于200℃加热下搅拌60分钟,得到压敏粘合剂溶液。向该溶液中,加入140℃(110-180℃)的酮洛芬(1.5g),并且将混合物搅拌20分钟,得到含有药物的均匀压敏粘合剂溶液。随后,将该压敏粘合剂溶液浇铸在75μm厚的聚酯释放片上至单位面积质量为140g/m2。将如上制备的压敏粘合剂层转移并按压粘附在约450μm厚的单位面积质量为110g/m2的圆形针织织物C上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。切割该层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例9)
将苯乙烯-异戊二烯-苯乙烯嵌段共聚物(13.0g,Kraton D-1107CU,由SHELL KAGAKU KK制造)、聚异丁烯(10.5g,Oppanol B80,由BASF制造)、氢化松香酯(5.5g,Ester Gum H,由Arakawa Chemical Industries,Ltd.制造)、液体石蜡(19.0g,Crystol J-352,由Esso Petroleum Co.,Ltd.制造)、N-甲基-2-吡咯烷酮(2.5g)和没食子酸丙酯(0.5g)在氮气气氛于200℃加热下搅拌60分钟,得到压敏粘合剂溶液。向该溶液中,加入140℃(110-180℃)的双氯芬酸钠(1.5g),并且将混合物搅拌20分钟,得到含有药物的均匀压敏粘合剂溶液。随后,将该压敏粘合剂溶液浇铸在75μm厚的聚酯释放片上至单位面积质量为210g/m2。将如上制备的压敏粘合剂层转移并按压粘附在约450μm厚的单位面积质量为110g/m2的圆形针织织物C上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。切割该层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例10)
向上述聚异丁烯溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(1g)和适量的用于调节浓度的己烷/四氢呋喃(1∶1)混合物,并且搅拌混合物,得到含有药物并且非溶剂浓度为25质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并按压粘附在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。此外,切割该层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例11)
将苯乙烯-异戊二烯-苯乙烯嵌段共聚物(12.5g,Kraton D-1107CU,由SHELL KAGAKU KK制造)、聚异丁烯(11.0 g,Oppanol B80,由BASF制造)、氢化松香脂(6.0 g,Steberite ester 7,由Rika Hercules制造)、液体石蜡(19.5g,Crystol J-352,由Esso Petroleum Co.,Ltd.制造)和没食子酸丙酯(0.5g)在氮气气氛于200℃加热下搅拌60分钟,得到压敏粘合剂溶液。向该溶液中加入140℃(110-180℃)的双氯芬酸钠(1.5g),并且将混合物搅拌20分钟,得到含有药物的均匀压敏粘合剂溶液。随后,将该压敏粘合剂溶液浇铸在75μm厚的聚酯释放片上至单位面积质量为140g/m2。将如上制备的压敏粘合剂层转移并按压粘附在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。此外,切割该层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例1 2)
将苯乙烯-异戊二烯-苯乙烯嵌段共聚物(13.0g,Kraton D-1107CU,由SHELL KAGAKU KK制造)、聚异丁烯(10.5g,Oppanol B80,由BASF制造)、氢化松香酯(5.5g,Ester Gum H,由Arakawa Chemical Industries,Ltd.制造)、液体石蜡(19.0g,Crystol J-352,由Esso Petroleum Co.,Ltd.制造)、N-甲基-2-吡咯烷酮(2.5g)和没食子酸丙酯(0.5g)在氮气气氛于200℃加热下搅拌60分钟,得到压敏粘合剂溶液。向该溶液中加入140℃(110-180℃)的双氯芬酸钠(1.5g),并且将混合物搅拌20分钟,得到含有药物的均匀压敏粘合剂溶液。随后,将该压敏粘合剂溶液浇铸在75μm厚的聚酯释放片上至单位面积质量为210g/m2。将如上制备的压敏粘合剂层转移并按压粘附在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备。切割该层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例1 3)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(2g)、作为交联剂的三官能异氰酸酯(0.0108g,CORONATE HL,由Nippon Polyurethane Industry Co.,Ltd.制造)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并层压在400μm厚的单位面积质量为100g/m2的纺花边的无纺织物上,所述无纺织物由聚酯纤维(60%)和聚丙烯纤维(40%)制成的并且具有近似三角形的截面(底面积5μm,高10μm)的复合纤维制备,并且用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
(比较例14)
向上述共聚物A溶液,其固体含量相当于12g,加入肉豆蔻酸异丙酯(8g)、水杨酸乙二醇酯(2g)和适量的用于调节浓度的乙酸乙酯,并且搅拌混合物,得到含有药物并且非溶剂浓度为30质量%的均匀压敏粘合剂溶液。将获得的压敏粘合剂溶液涂敷在75μm厚的聚酯释放片上至干燥后的单位面积质量为60g/m2,并且干燥得到交联的凝胶状压敏粘合剂层。将如上制备的压敏粘合剂层转移并按压粘附在约400μm厚的单位面积质量为105g/m2的圆形针织织物A上,所述针织织物由直径约20μm并且具有近似圆形截面的聚酯纤维制备,并且用铝层压膜包装上述层压材料并且在70℃老化48小时。此外,切割老化后的层压片,得到粘合剂制剂(长10cm,宽14cm,边缘是曲率半径为1cm的圆弧)。
对实施例1-5和比较例1-7中获得的粘合剂制剂进行以下试验。试验结果示于表1中。
(1)载体的单位面积质量(CW)和含有药物的压敏粘合剂层的单位面积质量(AW)是按照JIS L 1018:1990测量的,并且计算CW/AW。
(2)没有压敏粘合剂层的载体表面较短尺寸方向上的静摩擦系数是按照JIS P 8147:1994测量的。
(3)粘合剂制剂较短尺寸方向上的20%模量(AM)和粘合剂制剂较长尺寸方向上的20%模量(EM)是JIS Z 0237:2000测量的,并且计算AM/EM。
(4)粘合剂制剂较短尺寸方向上的剪切粘合力是按照JIS Z 0237:1991测量的(N=3),并且计算平均值。
表1
单位面积质量(g/m2) | CW /AW | 静摩擦系数(tanθ) | 20%模量(N/cm) | AM/EM | 剪切粘合力(N/cm2) | |||
CW | AW | AM | EM | |||||
实施例1 | 105 | 60 | 1.7 | 0.69 | 0.9 | 0.8 | 1.1 | 3.0 |
实施例2 | 105 | 60 | 1.7 | 0.68 | 0.9 | 0.8 | 1.1 | 2.8 |
实施例3 | 105 | 60 | 1.7 | 0.69 | 1.0 | 0.9 | 1.1 | 2.0 |
实施例4 | 150 | 60 | 2.5 | 0.66 | 1.2 | 1.2 | 1.0 | 3.6 |
实施例5 | 60 | 40 | 1.5 | 0.38 | 0.6 | 0.5 | 1.2 | 2.5 |
比较例1 | 85 | 60 | 1.4 | 0.82 | 2.1 | 0.6 | 3.5 | 3.7 |
比较例2 | 100 | 60 | 1.7 | 0.83 | 12.6 | 9.0 | 1.4 | 10.1 |
比较例3 | 16 | 60 | 0.3 | 0.21 | 不可测量 | 不可测量 | - | 15.2 |
比较例4 | 21 | 60 | 0.4 | 0.23 | 不可测量 | 不可测量 | - | 14.2 |
比较例5 | 110 | 60 | 1.8 | 0.65 | 1.4 | 0.5 | 2.8 | 3.4 |
比较例6 | 110 | 140 | 0.8 | 0.65 | 1.6 | 0.6 | 2.7 | 4.2 |
比较例7 | 110 | 210 | 0.5 | 0.64 | 1.7 | 0.6 | 2.8 | 2.0 |
使用实施例1-5和比较例1-7中获得的粘合剂制剂,由5名志愿者对皮肤粘合进行功能评估。具体而言,将切成长7cm、宽10cm(边缘是曲率半径为1cm的圆弧)的相同样品的粘合剂制剂粘附在志愿者的胸部48小时(可以淋浴,但是尽可能使制剂不被弄湿),并且对(1)粘合过程中的异物感、(2)粘合过程中的痒感、(3)粘合过程中的状态和(4)剥离后的胶残余按照以下标准进行评估并且测定平均值。评估结果示于表2中。
(1)粘合过程中的异物感
粘合过程中的异物感基于志愿者的功能评估分级成0、1、2、3、4和5点的六个水平,其中“显著感觉”为0,而“根本没有感觉”为5。
(2)粘合过程中的痒感
粘合过程中的痒感基于志愿者的功能评估分级成0、1、2、3、4和5点的六个水平,其中“显著感觉”为0,而“根本没有感觉”为5。
(3)粘合过程中的状态
在22小时后对粘合过程中的状态进行分级,其中“剥离小于5%”为5点,“剥离大于等于5%并且小于10%”为4点,“剥离大于等于10%并且小于30%”为3点,“剥离大于等于30%并且小于60%”为2点,“剥离大于等于60%并且小于100%”为1点,而“脱落”为0点。
(4)剥离后的胶残余
22小时后对剥离后的胶残余进行分级,其中“周边没有胶残余”为5点,“周边的胶残余小于周长的5%”为4点,“周边的胶残余大于等于周长的5%并且小于周长的20%”为3点,“周边的胶残余大于等于周长的20%并且小于周长的50%”为2点,“周边的胶残余大于等于周长的50%并且小于周长的100%”为1点,而“所有周长上都有胶残余”为0点。
表2
粘合过程中的异物感(平均值) | 粘合过程中的痒感(平均值) | 粘合过程中的状态(平均值) | 剥离后的胶残余(平均值) | |
实施例1 | 5.0 | 4.8 | 5.0 | 5.0 |
实施例2 | 4.8 | 4.8 | 5.0 | 5.0 |
实施例3 | 4.8 | 4.0 | 4.4 | 5.0 |
实施例4 | 4.8 | 4.6 | 5.0 | 5.0 |
实施例5 | 5.0 | 4.8 | 5.0 | 4.8 |
比较例1 | 3.4 | 4.4 | 3.0 | 4.8 |
比较例2 | 0.8 | 4.0 | 2.2 | 4.8 |
比较例3 | 0.4 | 1.6 | 0.6 | 0.4 |
比较例4 | 0.6 | 2.6 | 0.8 | 0.6 |
比较例5 | 2.8 | 4.0 | 4.0 | 4.4 |
比较例6 | 2.4 | 2.6 | 4.2 | 4.8 |
比较例7 | 2.0 | 1.8 | 4.4 | 4.8 |
将实施例1、8-13和比较例10-14中获得的粘合剂制剂用铝层压膜包装,在25℃和60%相对湿度下保存3个月,并且进行以下试验。试验结果示于表3中。
(1)按照JIS L 1099:1993测量透湿量。
(2)实施例1、8-13和比较例10-14中使用的织物的固有透湿量取作11420g/m2·24小时,比较例13中使用的织物的固有透湿量取作9700g/m2·24小时,并且计算粘合剂制剂制造后剩余的透湿量。
(3)一个方向上的20%模量按照JIS Z 0237:2000测量。
(4)与酚醛塑料板的粘合力按照JIS Z 0237:2000测量。
(5)按照JIS Z 0237:2000测量剪切粘合力(N=3),并且确定平均值。
表3
透湿量(g/m2·24小时) | 透湿量剩余比率(%) | 20%模量(N/cm) | 与酚醛塑料板的粘合力(N/24mm宽度) | 剪切粘合力(N/cm2) | |
实施例1 | 1250 | 11 | 与表1相同 | 0.48 | 3.0 |
实施例8 | 1300 | 11 | 0.83 | 0.43 | 2.8 |
实施例9 | 1470 | 13 | 0.77 | 0.51 | 3.3 |
实施例10 | 1880 | 16 | 0.72 | 0.29 | 2.2 |
实施例11 | 1520 | 13 | 0.73 | 0.37 | 2.4 |
实施例12 | 990 | 9 | 0.84 | 0.55 | 3.7 |
实施例13 | 1110 | 10 | 1.22 | 0.50 | 3.2 |
比较例10 | 未测量 | - | 0.85 | 不可测量 | 不可测量 |
比较例11 | 220 | 2 | 1.15 | 0.96 | 4.2 |
比较例12 | 120 | 1 | 0.88 | 0.29 | 2.0 |
比较例13 | 1020 | 11 | 7.76 | 0.69 | 10.0 |
比较例14 | 未测量 | - | 0.83 | 不可测量 | 不可测量 |
表3中,“不可测量”是指不能进行测量,因为压敏粘合剂层渗入织物中,在表面上不留下压敏粘合剂,导致粘合性的消失。
使用实施例1、9、13和比较例11-13中获得的粘合剂制剂,由5名志愿者对保存3月后对皮肤的粘合进行功能评估。具体而言,将切成长7cm、宽10cm(边缘是曲率半径为1cm的圆弧)的相同样品的粘合剂制剂粘附在志愿者的胸部72小时(可以淋浴,但是尽可能使制剂不被弄湿),对(1)粘合过程中的异物感、(2)粘合过程中的痒感、(3)脱落与否和(4)剥离时的疼感按照以下标准进行评估并且测定平均值。评估结果示于表4中。
(1)粘合过程中的异物感
粘合过程中的异物感基于志愿者的功能评估分级成0、1、2、3、4和5点的六个水平,其中“显著感觉”为0,而“根本没有感觉”为5。
(2)粘合过程中的痒感
粘合过程中的痒感基于志愿者的功能评估分级成0、1、2、3、4和5点的六个水平,其中“显著感觉”为0,而“根本没有感觉”为5。
(3)脱落与否
将制剂是否脱落分级,其中“制剂粘合72小时后不脱落”为5点,“制剂粘合48小时后不脱落”为4点,“制剂粘合24小时后不脱落”为3点,“制剂粘合12小时后不脱落”为2点,“制剂粘合6小时后不脱落”为1点,而“制剂在粘合6小时内脱落”为0点。
(4)剥离时的痛感
剥离时的痛感基于志愿者的功能评估分级成0、1、2、3、4和5点的六个水平,其中“显著感觉”为0而“根本没有感觉”为5。当制剂在粘合72小时内脱落时,从评估对象上除去制剂。
表4
粘合过程中的异物感(平均值) | 粘合过程中的痒感(平均值) | 脱落与否(平均值) | 剥离时的痛感(平均值) | |
实施例1 | 4.8 | 4.8 | 5.0 | 4.8 |
实施例9 | 4.6 | 4.8 | 5.0 | 4.6 |
实施例13 | 4.8 | 4.6 | 5.0 | 4.6 |
比较例11 | 4.0 | 2.2 | 3.4 | 1.0(一个志愿者的制剂脱落) |
比较例12 | 3.6 | 1.8 | 3.3 | 1.5(一个志愿者的制剂脱落) |
比较例13 | 0.8 | 4.4 | 4.6 | 3.0 |
上述结果证实,实施例1-13的粘合剂制剂具有优良的粘合舒服感,因为在粘合过程中几乎没有相伴的异物感和痒感,并且因为载体的摩擦小而很少发生粘合过程中的胶残余和剥离。此外,粘合剂制剂在穿衣/脱衣过程中和粘合过程中不剥离或脱落。而且,还证实它们即使在粘合3天后也不脱落,并且可以长时间粘附。
本申请基于在日本提交的专利申请No.2005-116081,其内容通过引用结合在此。
Claims (6)
1、一种粘合剂制剂,其包含由织物制成的载体和形成在载体一个表面上的压敏粘合剂层,所述压敏粘合剂层包含压敏粘合剂和药物,其中
所述载体单位面积的质量(CW)和所述压敏粘合剂层单位面积的质量(AW)的比率(CW/AW)为1.0-5.0,
所述载体没有粘合剂层的表面的静摩擦系数为0.25-0.75,并且在粘合剂制剂一个方向上的20%模量(AM)和垂直于所述方向的方向上的20%模量(EM)各为0.5-1.5N/cm,并且其比率(AM/EM)为0.5-2.0。
2、权利要求1所述的粘合剂制剂,该粘合剂制剂的剪切粘合力为1.0-7.0N/cm2。
3、权利要求1或2所述的粘合剂制剂,其中所述的织物是由合成纤维制成的。
4、权利要求1至3中任何一项所述的粘合剂制剂,其中所述的织物是针织物。
5、权利要求1至4中任何一项所述的粘合剂制剂,所述的织物是由聚对苯二甲酸乙二醇酯制成的。
6、权利要求1至5中任何一项所述的粘合剂制剂,其中所述的压敏粘合剂包含丙烯酸类共聚物,所述丙烯酸类共聚物是通过包含作为主要组分的(甲基)丙烯酸烷基酯的单体混合物的共聚而获得的。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2005116081 | 2005-04-13 | ||
JP2005116081A JP2006288887A (ja) | 2005-04-13 | 2005-04-13 | 貼付製剤 |
Publications (1)
Publication Number | Publication Date |
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CN1846792A true CN1846792A (zh) | 2006-10-18 |
Family
ID=36950207
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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CNA2006100736025A Pending CN1846792A (zh) | 2005-04-13 | 2006-04-13 | 粘合剂制剂 |
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Country | Link |
---|---|
US (1) | US7501358B2 (zh) |
EP (1) | EP1716850B1 (zh) |
JP (1) | JP2006288887A (zh) |
KR (1) | KR20060108511A (zh) |
CN (1) | CN1846792A (zh) |
CA (1) | CA2542688C (zh) |
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- 2005-04-13 JP JP2005116081A patent/JP2006288887A/ja active Pending
-
2006
- 2006-04-10 CA CA 2542688 patent/CA2542688C/en not_active Expired - Fee Related
- 2006-04-10 EP EP20060007496 patent/EP1716850B1/en not_active Not-in-force
- 2006-04-12 US US11/402,004 patent/US7501358B2/en not_active Expired - Fee Related
- 2006-04-12 KR KR1020060033053A patent/KR20060108511A/ko active IP Right Grant
- 2006-04-13 CN CNA2006100736025A patent/CN1846792A/zh active Pending
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CN101313896B (zh) * | 2007-06-01 | 2012-11-14 | 日东电工株式会社 | 贴片和贴片制剂 |
CN111016313A (zh) * | 2019-11-07 | 2020-04-17 | 广东中晨电子科技有限公司 | 一种菲林保护膜 |
CN111040416A (zh) * | 2019-12-23 | 2020-04-21 | 广西通祥投资有限公司 | 高性能聚氨酯冷库保温板及其制备方法 |
CN116172303A (zh) * | 2023-04-21 | 2023-05-30 | 比音勒芬服饰股份有限公司 | 一种具有三角梅形态的防滑耐磨eva鞋底 |
Also Published As
Publication number | Publication date |
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CA2542688C (en) | 2013-06-18 |
US7501358B2 (en) | 2009-03-10 |
CA2542688A1 (en) | 2006-10-13 |
EP1716850A1 (en) | 2006-11-02 |
KR20060108511A (ko) | 2006-10-18 |
US20060234581A1 (en) | 2006-10-19 |
EP1716850B1 (en) | 2012-05-23 |
JP2006288887A (ja) | 2006-10-26 |
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