CN110869482A - 洗涤剂添加剂 - Google Patents
洗涤剂添加剂 Download PDFInfo
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Abstract
一种洗涤剂添加剂,其包含:活性物质,所述活性物质包含四乙酰乙二胺和三乙酰乙二胺中的一者或两者;和互聚物络合物,所述互聚物络合物包含质子受体(共)聚合物和质子供体(共)聚合物两者。
Description
背景技术
通常通过使纺织品与洗涤剂配方接触来洗涤纺织品,如可穿戴织物,所述洗涤剂配方为洗涤剂组分和其它任选的活性物质(如漂白剂)的组合。为了易于使用,许多洗涤剂配方的用户更喜欢将洗涤剂和任选的活性物质并入到单个产品中的一体化产品。此外,相比于固体或颗粒状产品,许多用户更喜欢此产品为液体。
一种常见的洗涤剂活性物质为四乙酰乙二胺(TAED)。TAED充当过氧漂白活化剂和微生物控制剂。TAED已广泛地用于固体洗涤剂产品中。在部分地含有水的液体洗涤剂配方中,TAED将经历水解并且失去作为洗涤剂活性物质的效果,因为TAED反应形成N,N′二乙酰乙二胺(DAED),其无法作为洗涤剂活性物质生效。因此,当在不改性的情况下使用时,TAED作为水性洗涤剂配方的活性物质并不理想。三乙酰乙二胺(TriAED)为另一种洗涤剂活性物质。期望一种适用于含有水的液体洗涤剂配方中的洗涤剂添加剂,其含有TAED或TriAED中的一者或两者。
发明内容
一种洗涤剂添加剂,其包含:活性物质,所述活性物质包含四乙酰乙二胺或三乙酰乙二胺中的一者或两者;和互聚物络合物,所述互聚物络合物包含质子受体(共)聚合物和质子供体(共)聚合物两者。
具体实施方式
本公开描述一种改进的洗涤剂添加剂。在一个方面,本公开描述一种洗涤剂添加剂,其包含活性物质(例如四乙酰乙二胺(TAED))和互聚物络合物。所述互聚物络合物包括质子受体(共)聚合物和质子供体(共)聚合物两者。如本文所用,“(共)聚合物”是指聚合物或共聚物。本文所描述的洗涤剂添加剂的改进为TAED的水解稳定性提高,这在水性洗涤剂配方中提供增强的长期稳定性。在互聚物络合物中,质子供体(共)聚合物经由氢键结合与质子受体(共)聚合物缔合。互聚物网络定义本文所描述的添加剂的结构,其中添加剂封装活性物质。
质子供体(共)聚合物选自由以下组成的组:聚(甲基)丙烯酸、羧甲基纤维素、乙烯丙烯酸共聚物、果胶、黄原胶和海藻酸。如本文所用,“(甲基)丙烯酸”是指丙烯酸和甲基丙烯酸官能团两者。
质子受体(共)聚合物为选自由以下组成的组中的一或多者的均聚物或共聚物:聚环氧乙烷、聚乙二醇、聚丙二醇、聚环氧丙烷、环氧乙烷/环氧丙烷共聚物、聚乙烯醇和甲基纤维素。
质子供体(共)聚合物与质子受体(共)聚合物的比率可以是1∶10到10∶1摩尔。质子供体(共)聚合物与质子受体(共)聚合物的比率优选地是1∶5到5∶1摩尔。质子供体(共)聚合物与质子受体(共)聚合物的比率更优选地是1∶2到2∶1摩尔。质子受体(共)聚合物的重均分子量为1,000到10,000,000。质子受体(共)聚合物的重均分子量优选地为5,000到5,000,000。质子受体(共)聚合物的重均分子量更优选地为10,000到1,000,000。质子供体(共)聚合物的重均分子量为1,000到10,000,000。质子供体(共)聚合物的重均分子量优选地为10,000到5,000,000。质子供体(共)聚合物的重均分子量更优选地为100,000到1,000,000。
洗涤剂添加剂可以通过质子供体(共)聚合物、质子受体(共)聚合物和活性物质的机械混合来制备。洗涤剂添加剂还可以通过将质子供体(共)聚合物和质子受体(共)聚合物的溶液喷雾干燥到活性物质的颗粒上来制备。在一些情况下,表面活性剂被包括于洗涤剂添加剂制剂中以增强封装效率和均一性。适合的表面活性剂的实例是非离子表面活性剂,包括脂肪族醇乙氧基化物、烷基苯酚乙氧基化物、脂肪酸酯乙氧基化物、烷基聚葡糖苷、环氧乙烷/环氧丙烷共聚物(包括无规和嵌段共聚物)、多元醇和乙氧基化多元醇。当选择非离子表面活性剂时,重要的是考虑表面活性剂的乙氧基化部分和疏水性部分两者与互聚物络合物的相互作用,以及与质子受体(共)聚合物竞争质子供体(共)聚合物的结合位点。
在制备互聚物络合物(IPC)期间,所制备的溶液的pH决定形成IPC的有效性。pH根据质子供体和质子受体(共)聚合物的类型、质子供体和质子受体(共)聚合物的分子量、质子供体(共)聚合物的中和程度、所存在的其它物质(如表面活性剂或无机盐)的类型和质子供体和质子受体(共)聚合物的比率和所选择的活性物质的量而变化。优选地,当活性物质为TAED或TriAED时,所制备的溶液的pH为2到4。在此pH范围内观测到不溶的IPC络合物的形成最大化。
洗涤剂添加剂为90重量%或更少的TAED和10重量%或更多的互聚物络合物。在一种情况下,洗涤剂添加剂为75重量%或更少的TAED和25重量%或更多的互聚物络合物。优选地,洗涤剂添加剂为50重量%或更少的TAED和50重量%或更多的互聚物络合物。
如本文中所描述,添加剂封装或部分封装活性物质。如本文所用,“经封装的”是指活性物质被结合或保持在互聚物络合物内。本文所描述的添加剂经设计以在触发事件期间释放活性物质(在本公开的上下文中,触发事件可能用于洗衣机中)。当提及活性物质被封装时,其是指在触发事件之前将活性物质保持在互聚物络合物内。根据本公开的方法制备的添加剂的封装效率为30到100%。优选地,根据本公开的方法制备的添加剂的封装效率为60到100%。更优选地,根据本公开的方法制备的添加剂的封装效率为90到100%。如本文所用,“封装效率”是指被封装在添加剂的互聚物络合物中的预期活性物质的百分比。
本文所描述的洗涤剂添加剂在水性系统中具有比单独的TAED更好的长期稳定性。当在洗衣机中使用洗涤剂添加剂时,TAED会从互聚物络合物中释放出来,从而使TAED可在洗涤系统中使用以执行其过氧漂白活化功能。
本文所描述的方法适合于制备其它类型的固体粉末系统。例如,本文中所描述的方法可以包括但不限于封装织物软化剂、洗涤剂活性物质、漂白活性物质、肥料、微量营养素、农药(杀真菌剂、杀细菌剂、杀虫剂、杀螨剂、杀线虫剂等)、杀生物剂、微生物控制剂、高分子润滑剂、阻燃剂、颜料、染料、脲抑制剂、食品添加剂、调味剂、药剂、组织、抗氧化剂、化妆品成分(芳香剂、香料等)、土壤改良剂(土壤排斥剂、土壤释放剂等)、催化剂、诊断剂和光保护剂(紫外阻隔剂等)。
实例
材料和实例制备
材料
TAED固体购自西格玛-奥德里奇(Sigma-Aldrich),并且使用80μm筛子将TAED固体研磨成粉末。POLYOX水溶性树脂WSR N-3000、WSR N-10和WSR-205购自陶氏化学公司(TheDow Chemical Company)。将WSR N-3000和WSR N10分别以7重量%的浓度溶解在去离子水中,而WSR-205则以5重量%的浓度溶解在去离子水中。重均分子量为250,000的35%聚丙烯酸(PAA)溶液购自西格玛-奥德里奇。从西格玛-奥德里奇获得数均分子量(Mn)为40K的甲基纤维素(MC),并且在室温下将其以2.5重量%的含量溶解在去离子(DI)水中。
实验程序
试剂和其用量概述于表1中。使用两种不同的程序进行封装。实例1描述基于掺合器的方案,而在搅拌烧瓶中制备其余的样品。
对于实例1,按照表1中列出的配方,将聚合物溶液(如上文所描述制备的WSRN3000和PAA)组合在配备有机械搅拌器的塑料容器中并且以2500rpm搅拌10分钟,从而得到聚合物掺合物。将TAED粉末添加到设置成中等速度的金属掺合器中并将聚合物掺合物缓慢添加到其中。在添加了所有聚合物掺合物之后,混合物变成白色糊状物。继续搅拌30分钟。将内容物转移到铝盘中,并且在40℃下在减压下在真空烘箱中干燥16小时。所获得的材料为白色固体复合物。用具有干冰的金属掺合器将所述白色固体复合物研磨成精细粉末。
使用此段落中所描述的程序制备实例2-7。样品量概述在表1中。在配备有机械搅拌器的250ml 3颈烧瓶中称重TAED、PEO和甲基纤维素溶液。以2500rpm搅拌混合物2分钟,并且接着将搅拌速率降低到1000rpm再搅拌2分钟。将预定量的PAA溶液添加到20ml加料漏斗中并将漏斗连接到烧瓶上。在1000rpm搅拌下,将PAA溶液逐滴添加到烧瓶中。在添加了所有PAA溶液之后,将混合物再搅拌5分钟。通过离心分离产物且用去离子水洗涤3次。溶液的pH在2.5-2.8范围内。将产物在室温下干燥成薄层。所获得的材料为白色固体复合物。用具有干冰的金属掺合器将所述白色固体复合物研磨成精细粉末。
表1:实例(Ex)的配方处方
配方(g) | 实例1 | 实例2 | 实例3 | 实例4 | 实例5 | 实例6 | 实例7 | 实例8 |
7重量%WSR N10 | 0 | 0 | 0 | 0 | 0 | 100 | 0 | 0 |
5重量%WSR 205 | 0 | 0 | 0 | 0 | 0 | 0 | 100 | 0 |
7重量%WSR N3000 | 20.3 | 90 | 90 | 90 | 90 | 0 | 0 | 90 |
2.5%MC | 0 | 10 | 10 | 10 | 10 | 10 | 20 | 10 |
TAED | 6.0 | 11.5 | 9.4 | 17.3 | 11.5 | 14 | 10 | 0 |
35%PAA溶液 | 2.0 | 15 | 9 | 15 | 18 | 20 | 14.3 | 15 |
PAA:PEO g/g | 0.5 | 0.8 | 0.5 | 0.8 | 1.0 | 1.0 | 1.0 | 0.8 |
TAED/聚合物 | 3 | 1 | 1 | 1.5 | 1 | 1 | 1 | n/a |
材料表征
差示扫描量热法
差示扫描量热法(DSC)测量是使用TA Instruments的Q2000型差示扫描量热仪进行的。将5-10mg样品放置于气密密封的盘中并在-50-200℃下使用10℃/分钟扫描进行分析。与仅使用PEO、仅使用PAA、仅使用TAED和使用无TAED的IPC进行的比较测试相比,DSC测量产生的热流曲线通过证明PEO熔融吸热的消失而验证了IPC的形成。
pH对IPC形成的影响
对于pH对互聚物络合物的影响,使用针对实例2所描述的试剂比率。将配方分成三个部分,并且以与针对实例2-7所描述相同的方式对TAED进行封装,不同的是,在完全添加PAA之后使用氢氧化钠将反应混合物的pH调节到3、5和8。在pH=3的情况下,通过离心分离所得固体沉淀物,干燥并通过DSC分析。在更高的pH(pH=5和pH=8)下,所得固体为糊状的。将此聚集固体干燥并且也通过DSC分析。DSC分析仅展示pH=3的配方的PEO熔融吸热,而pH=5和pH=8的配方并未展示PEO熔融吸热。
不受理论限制,低pH有利于氢键结合,而当PAA去质子化(在此情况下作为钠盐)时,无法形成氢键。
用于测定TAED水解为二乙酰乙二胺(DAED)的HPLC分析
将0.5克未封装的原始TAED和上述实例中经封装的TAED粉末添加到20g allTMMighty PacTM洗涤剂中,并振荡10分钟。将1滴(约0.1g)每种混合物分别添加到10g的1∶3乙腈/H2O溶剂中,并超声处理15分钟以完全溶解TAED固体。使用具有四元泵和二极管阵列检测器的Agilent 1100高效液相色谱(HPLC)测量所制备的样品中DAED的浓度。HPLC方法的条件概述于表2中。
表2:HPLC测试条件
表3:DAED%的HPLC评估结果
首日(%) | 第2天(%) | 第7天(%) | 第20天(%) | |
未封装的TAED | 0 | 0.116 | 0.284 | 0.593 |
实例1 | 0 | 0.059 | 0.146 | 0.269 |
实例2 | 0 | 0.000 | 0.056 | 0.138 |
实例3 | 0 | 0.000 | 0.054 | 0.133 |
实例4 | 0 | 0.018 | 0.095 | 0.237 |
实例5 | 0 | 0.036 | 0.110 | 0.236 |
实例6 | 0 | 0.000 | 0.067 | 0.166 |
实例7 | 0 | 0.012 | 0.069 | 0.175 |
如表4所示,对于没有任何封装的TAED,DAED的浓度急剧增加,而对于其它用互聚物络合物封装的实例,DAED则缓慢增加。由于DAED是通过TAED水解生成的,因此DAED的缓慢释放曲线表明其封装效率良好。
另外,封装效率不受PEO的分子量的显著影响,如实例5(PEO Mw 400,000);实例6(PEO Mw 100,000)和实例7(PEO Mw 600,000)具有非常类似的DAED浓度。实例2和4以及实例1和3说明,即使增加TAED的量,它也被互聚物络合物有效地封装。改变PAA与PEO的比率,实例2、3和5也获得有效的封装。
Claims (9)
1.一种洗涤剂添加剂,其包含:
活性物质,所述活性物质包含四乙酰乙二胺或三乙酰乙二胺中的一者或两者;和
互聚物络合物,所述互聚物络合物包含质子受体(共)聚合物和质子供体(共)聚合物两者。
2.根据权利要求1所述的洗涤剂添加剂,其中所述质子供体(共)聚合物选自由以下组成的组:聚(甲基)丙烯酸、羧甲基纤维素、乙烯丙烯酸共聚物、果胶、黄原胶和海藻酸。
3.根据权利要求1到2中任一项所述的洗涤剂添加剂,其中所述质子受体(共)聚合物为选自由以下组成的组中一或多者的均聚物或共聚物:聚环氧乙烷、聚乙二醇、聚丙二醇、聚环氧丙烷、环氧乙烷/环氧丙烷共聚物、聚乙烯醇和甲基纤维素。
4.根据权利要求1到3中任一项所述的洗涤剂添加剂,其包含90重量%或更少的所述活性物质和10重量%或更多的所述互聚物络合物。
5.根据权利要求1到4中任一项所述的洗涤剂添加剂,其包含25重量%或更少的所述活性物质和75重量%或更多的所述互聚物络合物。
6.根据权利要求1到5中任一项所述的洗涤剂添加剂,其包含90重量%或更少的所述活性物质和10重量%或更多的所述互聚物络合物。
7.根据权利要求1到6中任一项所述的洗涤剂添加剂,其包含25重量%或更少的所述活性物质和75重量%或更多的所述互聚物络合物。
8.根据权利要求1到7中任一项所述的洗涤剂添加剂,其中所述洗涤剂添加剂的pH为2到4。
9.根据权利要求1到8中任一项所述的洗涤剂添加剂,其中所述添加剂中的所述活性物质的封装效率为60到100%。
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PCT/US2018/041370 WO2019027633A1 (en) | 2017-07-31 | 2018-07-10 | DETERGENT ADDITIVE |
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