CN109797539A - 复合银离子在柔软表面上的稳定性 - Google Patents
复合银离子在柔软表面上的稳定性 Download PDFInfo
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Abstract
一种水性组合物,其包含:(a)银离子;(b)包含至少10重量%的乙烯基咪唑聚合单元的聚合物;和(c)包含至少两个羟基、不包含羧基并且在25℃下的蒸气压不超过0.025Pa的氨基醇。乙烯基咪唑:银的摩尔比是至少3:1。
Description
本发明涉及一种包含络合银离子的组合物,所述组合物在柔软表面上是稳定的。
包含银离子和氨基醇的组合物公开于美国专利第8,637,088号中。然而,这一参考文献没有公开在柔软表面上稳定的组合物。
本发明所解决的问题是提供一种包含络合银离子的组合物,所述组合物在柔软表面上是稳定的。
发明内容
本发明是针对一种水性组合物,其包含:(a)银离子;(b)至少一种聚合物,其包含至少10重量%的乙烯基咪唑聚合单元;和(c)至少一种氨基醇,其包含至少两个羟基,不包含羧基并且在25℃下的蒸气压不超过0.025Pa;其中乙烯基咪唑:银的摩尔比是至少3:1。
本发明还针对一种用银离子处理柔软表面的方法;所述方法包含向所述柔软表面上施加水性组合物,所述水性组合物包含:(a)银离子;(b)至少一种聚合物,其包含至少10重量%的乙烯基咪唑聚合单元;和(c)至少一种氨基醇,其包含至少两个羟基,不包含羧基并且在25℃下的蒸气压不超过0.025Pa;其中乙烯基咪唑:银的摩尔比是至少3:1。
具体实施方式
除非另外说明,否则温度以摄氏度(℃)为单位,并且对百分比的引用是指重量百分比(重量%)。除非另外说明,否则所有操作在室温(20-25℃)下进行。聚合物的量按固体计,即不包括可与聚合物一起存在的任何水或溶剂。单体的量按固体聚合物计。术语“乙烯基咪唑”优选是指N-乙烯基咪唑。术语“银离子”是指Ag(I)离子。
优选地,水性组合物中所用的聚合物包含高达100重量%的乙烯基咪唑聚合单元;优选至少15重量%,优选至少20重量%,优选至少25重量%,优选至少30重量%,优选至少35重量%;优选不超过95重量%,优选不超过90重量%,优选不超过85重量%。优选地,聚合物还包含10到70重量%的极性单体;优选至少15重量%,优选至少20重量%;优选不超过60重量%,优选不超过50重量%,优选不超过45重量%。极性单体优选是具有至少一个羧基、磺酸基、磷酸基或具有环氧乙烷聚合单元的单体。优选的极性单体包括例如丙烯酸(AA)、甲基丙烯酸(MAA)、衣康酸、马来酸、富马酸、2-丙烯酰胺基-2-甲基丙磺酸和其钠盐、聚合环氧乙烷单元的(甲基)丙烯酸酯或混合的乙烯/环氧丙烷单元,其条件是环氧乙烷残基为乙烯/环氧丙烷残基以及其组合的至少50重量%(或者至少75%,或者至少90%)。优选地,环氧乙烷单元或混合的乙烯/环氧丙烷单元被单烷基化(例如,聚乙二醇单甲醚)并且Mn是至少150,优选至少300;优选不超过1000,优选不超过700,优选不超过600。优选地,聚合物是“丙烯酸聚合物”,即具有至少70重量%的丙烯酸单体,优选至少80重量%,优选至少90重量%,优选至少95重量%的聚合物。丙烯酸单体包括(甲基)丙烯酸、其盐和其C1-C22烷基或羟烷基酯;丁烯酸、衣康酸、富马酸、马来酸、马来酸酐、(甲基)丙烯酰胺、(甲基)丙烯腈以及丁烯酸、衣康酸、富马酸或马来酸的烷基或羟烷基酯。
在优选实施例中,聚合物还包含其它烯系不饱和单体的聚合单元,例如(甲基)丙烯酸酯、乙烯基酯、(甲基)丙烯酰胺。少量的疏水性单体,例如更高碳数(甲基)丙烯酸烷基酯(例如C-4和更高碳数)可在其不损害水溶性的程度下存在。在优选实施例中,聚合物包含0到70重量%的(甲基)丙烯酸烷基酯或(甲基)丙烯酸羟烷基酯的聚合单元;优选不超过60重量%,优选不超过55重量%;优选至少5重量%,优选至少10重量%。优选地,烷基是C1-C8烷基,优选是C1-C6烷基,优选是C1-C4烷基。优选地,羟烷基是C2-C8羟烷基,优选是C2-C6羟烷基,优选是C2-C4羟烷基。
优选地,乙烯基咪唑:银的摩尔比是至少3.5:1,优选是至少4:1,优选是至少5:1,优选是至少8:1;优选不超过100:1,优选不超过50:1,优选不超过20:1。优选地,聚合物的数均分子量(Mn)是1000到300,000;优选是至少5000,优选是至少10000;优选不超过200000,优选不超过100000,优选不超过50000。优选地,水性组合物中银离子的浓度是0.5到100ppm;优选是至少2ppm,优选是至少5ppm,优选是至少10ppm;优选不超过60ppm,优选不超过50ppm,优选不超过40ppm。优选地,银离子源是水溶性银盐,例如硝酸银、银/胺络合物和乙酸银。优选地,水性组合物中聚合物的浓度是0.0001到5重量%;优选是至少.001重量%,优选是至少.01重量%;优选不超过3重量%,优选不超过1重量%。
优选地,氨基醇具有四到十二个碳原子;优选不超过十个碳原子,优选不超过八个碳原子。优选地,氨基醇具有不超过两个氮原子,优选不超过一个氮原子。优选地,氨基醇是脂肪族的。优选地,氨基醇不具有羟基和氨基以外的官能团。优选地,氨基醇包含不超过五个羟基,优选不超过四个羟基。优选地,氨基醇的分子量不超过300,优选不超过250,优选不超过200。优选地,氨基醇在25℃下的蒸气压不超过0.020Pa,优选不超过0.018Pa。氨基醇不是二乙醇胺(25℃下的蒸气压为0.03Pa)。优选地,氨基醇不是三乙醇胺。特别优选的是二异丙醇胺(双(2-羟丙基)胺,25℃下的蒸气压为0.017Pa,“DIPA”)和三(羟甲基)氨基甲烷(25℃下的蒸气压为0.003Pa,“TRIS”)。优选地,氨基醇:银的摩尔比是至少1:1,优选是至少3:1,优选是至少10:1;优选不超过10000:1,优选不超过5000:1,优选不超过2000:1。优选地,水性组合物中的氨基醇的浓度是0.1到10重量%;优选是至少1重量%,优选是至少2重量%;优选不超过7重量%,优选不超过5重量%。
在本发明的方法中,柔软表面包括织物、纤维、泡沫、海绵、膜、海藻酸盐、水凝胶和亲水胶体。优选地,织物和纤维包括,例如丝、棉、羊毛、亚麻、毛皮、毛发、纤维素、苎麻、大麻、亚麻、皮革、合成皮革、木浆、聚烯烃,例如聚乙烯、聚丙烯和聚丁烯;卤代聚合物,例如聚氯乙烯;芳香族聚酰胺,例如聚对苯二甲酰对苯二胺(例如纤维)、聚间苯二甲酰对苯二胺(例如纤维);三聚氰胺和三聚氰胺衍生物(例如纤维);聚酯,例如聚对苯二甲酸乙二酯、聚酯/聚醚;聚酰胺,例如尼龙6和尼龙6,6;聚氨酯,例如可从诺誉(Noveon)获得的脂肪族热塑性材料聚氨酯;乙酸酯;人造丝丙烯酸树脂;以及其组合。优选的织物包括棉、聚酯、棉-聚酯掺合物和聚烯烃。可以任何方式将水性组合物施加到表面上,优选通过喷涂、刷涂、浸渍、涂布、浸轧和消耗;最优选是喷涂。
本发明的组合物可进一步包括二次气味吸收、捕获或抑制材料,包括例如金属氧化物、二氧化钛、环糊精、壳聚糖、沸石、分子筛、树脂、活性炭、银盐、铜盐、铁盐、锌盐、脂肪酸的锌盐、蓖麻醇酸锌、金属-聚合物络合物、硅胶、硅酸盐、结晶硅酸盐、无定形硅酸盐、粘土、蒙脱石、硅藻土、氧化剂、过氧化物、过氧化氢和碱性缓冲剂。
实例
材料:
碳酸氢钠,费希尔化学(Fisher Chemical)
聚乙烯吡咯烷酮(平均MW 360k),西格玛(Sigma)
羧甲基纤维素,钠盐,平均MW 250000-ACROS有机物(ACROS Organics)
2-羟乙基纤维素-Cellosize-陶氏化学公司(Dow Chemical)
聚(乙二醇),BioUltra,MW 4000
N,N-双(2-羟乙基)甘氨酸(二甘氨酸(BICINE)),西格玛
N-[三-(羟甲基)-甲基]-甘氨酸(麦黄酮(Tricine)),西格玛
方法:
织物处理
使用来自沃纳马西斯公司(Werner Mathis AG)的实验室规模轧染机(型号:CH-8155VFM28888)将精整化学品施加到织物样品上。
首先确定吸湿率(WPUR),以计算在经干燥的织物上实现目标银装载所需的抗微生物配制物溶液的浓度。辊压力最初设定为3巴(404kPa)。然后称出12”×10”(30×25cm)的织物样片。将样片浸泡在去离子水浴中3到8秒直到其完全吸收水分。紧接着,将湿织物在3巴压力设定下通过旋转辊。然后重新称重织物以确定由于吸水而增加的重量。用经过辊后湿织物的重量与经干燥的织物重量差除以经干燥的织物重量来计算WPUR。如果吸湿率与期望值不匹配,则可以向上或向下调节轧染辊的压力以达到所需的值。
其次,制备施加用浴液以处理每个纺织样片。浴中的银浓度基于初始浓缩溶液和吸湿率计算。抗微生物配制物的浴液浓度计算是通过将目标银水平除以抗微生物配制物中的活性物装载量,然后除以吸湿率进行计算的。举例来说,对于使用具有1000ppm银的抗微生物配制物以100%吸湿率的棉织物上理论30ppm银为目标,将需要30ppm Ag目标/配制物中1000ppm Ag/1.00WPUR*100%,或100g中3.0g抗微生物配制物。
通过称量3.0克抗微生物配制物并且将其混合入97.0克去离子水中简单地配制用于棉的30ppm银目标织物装载。
最后,使用以上确定的压力设定值在轧染机中对每种织物进行处理,以获得每种织物样片的所需吸湿率。处理之前,将每种银溶液倒入轧染机的槽中。随后将织物样品浸入银溶液中3到8秒直到浸透。紧接着,湿织物随后通过辊以获得所需的吸湿重量。随后将织物放在一台可以拉伸绷紧织物的装置上,并且在150℃的对流烘箱中干燥2分钟。
织物风化
将所有织物在气候室(型号:KBWF 720气候室,宾德公司(Binder Company)中陈化以加速颜色变化。将12”×10”处理过的织物样片纵向切成两半以产生6”×10”(15×25)的两条。将一条水平放置在室中用于陈化,并且另一条置于环境黑暗条件下。然后将室设定为30℃并且如下进行循环湿度:30%相对湿度4小时,2小时从30%过渡到90%,在90%保持4小时,2小时从90%过渡到30%并且重复。重复这一风化循环直到去除样品。光源是在风化过程中保持打开的LUMILUX Cool Daylight(欧司朗(OSRAM)L36w/865照明灯泡)。
颜色测量
风化后织物的颜色使用Hunterlab分光光度计(型号:Labscan XE)测量,用脉冲氙弧光源照明,0度照明角度和45度观察角,测量区域为13mm(0.5”)。测量在使用标准白色瓷砖作为背衬的2层实验织物上进行。使用未处理的标准棉作为对照织物,所有实验织物样品与之进行比较,以评估总的颜色变化(ΔE*ab)。较大的ΔE*ab对应于较大的织物颜色变化。ΔE*ab的计算基于L、a和b的测量,其描述了浅/深、红/绿和蓝/黄的坐标空间。ΔE*ab值计算为测量的样品值与对照样品之间平方差总和的平方根。
下标0表示对照样品值,并且i表示单个样品测量值。每个织物样片在三个位置测量,并且在ΔE*ab计算中使用L、a和b的平均值。
ΔE*ab低于约1.3的值是优选的。
顶空气相色谱
使用顶空进样结合气相色谱与接近体温(37°℃)的质量选择性检测(HS-GC-MS)分析每个样品瓶的顶空挥发物。仪器是配备有Perkin Elmer TurboMatrix 40Trap顶空进样器的Agilent GC-MS型号6890/5973。仪器参数列于下表中。如下所述在双瓶气味捕获测试和散装材料气味吸附部分中制备样品。校准标准物(如上所述)包括在每个序列,以及几个空气空白中。标准物的顶空分析以完全蒸发模式进行,以消除静态顶空进样中可能发生的基质效应。在这一模式中,使用小的样品尺寸(约15-20mg),并且顶空瓶温度设定得足够高以允许受关注的挥发物完全蒸发。对于这一分析,在取样之前将标准样品加热到150℃持续10分钟。然后使用来自所述化合物的校准曲线的线性最小二乘方程确定样品顶空中每种校准化合物的ppm体积/体积(v/v)浓度(峰面积对v/v浓度,方程式1)。
方程式1
与没有添加化学品的小瓶中的酸的顶空浓度(3个的平均值)相比,计算减少百分比。
实例1:筛选用于控制气味的碱性试剂
使用气相色谱-质谱法筛选多种化学品以捕获挥发性脂肪酸的能力。将化学品(100mg)加入22ml气相色谱(GC)小瓶中。将2mL液相色谱(LC)小瓶插入GC小瓶中。使用气密注射器,将5μL含有1%丁酸和1%异戊酸在纯乙醇中的标准物加入LC小瓶中,消除了气味捕获化学品与挥发性脂肪酸之间的直接接触。将小瓶卷曲,形成气密密封,并且在37℃下培养24小时。如上所述测量酸的顶空浓度。
实例2:用银盐和气味控制剂处理的织物
用硝酸银和气味控制添加剂将处理浴溶液制备到最终浓度是30ppm的银和1%的气味控制添加剂。使用上文所描述的方法浸轧处理溶液,其中吸湿重量为100%+/-10%。将处理过的织物放入粘合剂室中4天,并且如上所描述通过ΔE*ab测量颜色变化。
实例3:用银盐、气味控制剂和银结合聚合物处理的织物
用商业含银抗微生物剂SILVADURTM 930(VI:银摩尔比3.6:1)和气味控制添加剂制备处理浴溶液到最终浓度是30ppm银和1%气味控制添加剂。使用上文所描述的方法浸轧处理溶液,其中吸湿重量为100%+/-10%。将处理过的织物放入粘合剂室中4天,并且如上所描述通过ΔE*ab测量颜色变化。
实例4:聚合物合成
使用US7390774B2或US7927379B2中概述的方法合成含乙烯基咪唑的聚合物。
实例5:用银盐、气味控制剂和亲水性聚合物处理的织物
用各种亲水性聚合物(195ppm聚合物固体)、硝酸银(30ppm银)和TRIS(1:1摩尔比TRIS:Ag)制备处理浴溶液。使用上文所描述的方法浸轧处理溶液,其中吸湿重量为100%+/-10%。将经处理的织物放在粘合剂室中1天,并且如上所描述通过ΔE测量颜色变化。
实施例6:喷雾制剂
在商业上可获得的喷雾瓶中形成气味控制喷雾制剂,其中3ppm银与以VI:银比率为3.6的聚合物2一起和2%的气味中和盐递送。将溶液喷到棉样片上,使吸湿重量为100%+/-10%。使样片风干。对于所需数量的应用重复所述过程。将经处理的织物放在粘合剂室中7天,并且如上所描述通过ΔE测量颜色变化。
Claims (10)
1.一种水性组合物,其包含:(a)银离子;(b)至少一种聚合物,其包含至少10重量%的乙烯基咪唑聚合单元;和(c)至少一种氨基醇,其包含至少两个羟基,不包含羧基并且在25℃下的蒸气压不超过0.025Pa;其中乙烯基咪唑:银的摩尔比是至少3:1。
2.根据权利要求1所述的水性组合物,其中所述聚合物包含至少20重量%的乙烯基咪唑聚合单元。
3.根据权利要求2所述的水性组合物,其中所述氨基醇是脂肪族的并且具有四到二十个碳原子。
4.根据权利要求3所述的水性组合物,其中乙烯基咪唑:银的摩尔比是至少3.5:1。
5.根据权利要求4所述的水性组合物,其中所述水性组合物包含0.5到100ppm的银离子。
6.根据权利要求5所述的水性组合物,其中所述聚合物还包含10到70重量%的极性单体。
7.一种用银离子处理柔软表面的方法;所述方法包含向所述柔软表面施加水性组合物,所述水性组合物包含:(a)银离子;(b)至少一种聚合物,其包含至少10重量%的乙烯基咪唑聚合单元;和(c)至少一种氨基醇,其包含至少两个羟基,不包含羧基并且在25℃下的蒸气压不超过0.025Pa;其中乙烯基咪唑:银的摩尔比是至少3:1。
8.根据权利要求7所述的方法,其中所述聚合物包含至少20重量%的乙烯基咪唑聚合单元。
9.根据权利要求8所述的方法,其中所述氨基醇是脂肪族的并且具有四到十二个碳原子。
10.根据权利要求9所述的方法,其中乙烯基咪唑:银的所述摩尔比是至少3.5:1,所述水性组合物包含0.5到100ppm的银离子。
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EP3485731B1 (en) | 2022-02-23 |
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