CN111819317A - 用阳离子粘合剂粘合的抗微生物非织造湿纸巾 - Google Patents
用阳离子粘合剂粘合的抗微生物非织造湿纸巾 Download PDFInfo
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- CN111819317A CN111819317A CN201880090157.4A CN201880090157A CN111819317A CN 111819317 A CN111819317 A CN 111819317A CN 201880090157 A CN201880090157 A CN 201880090157A CN 111819317 A CN111819317 A CN 111819317A
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- cationic
- nonwoven
- antimicrobial
- wet
- aqueous
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- YCUBDDIKWLELPD-UHFFFAOYSA-N ethenyl 2,2-dimethylpropanoate Chemical compound CC(C)(C)C(=O)OC=C YCUBDDIKWLELPD-UHFFFAOYSA-N 0.000 description 1
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- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
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- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
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- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
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- 235000011009 potassium phosphates Nutrition 0.000 description 1
- FRMWBRPWYBNAFB-UHFFFAOYSA-M potassium salicylate Chemical compound [K+].OC1=CC=CC=C1C([O-])=O FRMWBRPWYBNAFB-UHFFFAOYSA-M 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 229940082569 selenite Drugs 0.000 description 1
- MCAHWIHFGHIESP-UHFFFAOYSA-L selenite(2-) Chemical compound [O-][Se]([O-])=O MCAHWIHFGHIESP-UHFFFAOYSA-L 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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- HELHAJAZNSDZJO-OLXYHTOASA-L sodium L-tartrate Chemical compound [Na+].[Na+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O HELHAJAZNSDZJO-OLXYHTOASA-L 0.000 description 1
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- 239000001433 sodium tartrate Substances 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 235000011004 sodium tartrates Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- 235000002906 tartaric acid Nutrition 0.000 description 1
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- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
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Abstract
一种抗微生物非织造湿纸巾包括:i)用由来自阳离子乙烯醇‑N‑乙烯基胺共聚物的组中的一种或多种阳离子保护胶体稳定的可交联VAE分散体粘合的纤维非织造基材,和ii)吸附于所述非织造基材中的包括一种或多种阳离子消毒剂的水性洗剂。所述抗微生物非织造湿纸巾中不存在阴离子表面活性剂。一种生产抗微生物非织造湿纸巾的方法包括:a)向非织造基材涂施包含由来自阳离子乙烯醇‑N‑乙烯基胺共聚物的组中的一种或多种阳离子保护胶体稳定的可交联VAE分散体的第一水性组合物;b)干燥所述组合物;和c)将第二水性组合物涂施于步骤b)的产物上。所述第一和第二水性组合物中的至少一种包括一种或多种阳离子消毒剂。
Description
技术领域
本发明涉及一种非织造湿纸巾(nonwoven wet wipe),该非织造湿纸巾包括非织造基材和水性抗微生物洗剂,其中所述非织造基材用阳离子粘合剂进行粘合。
背景技术
适用于气流成网(airlaid)非织造行业的自交联分散体粘合剂通常采用一定量的阴离子表面活性剂进行稳定。US 5,109,063 A公开了一种制备用于非织造粘合剂应用的乙酸乙烯酯乙烯N-羟甲基丙烯酰胺(NMA)共聚物乳液的方法。所述乳化系统由亚烷氧基聚(亚乙氧基)硫酸酯的盐组成。这种类型的粘合剂通常用于洗剂湿纸巾(lotionized wet wipe)应用,其中所述洗剂与用于为所述非织造制品提供完整性的自交联粘合剂的阴离子性质相容。
然而,如果所述洗剂含有带电荷的阳离子化合物,正如季铵盐消毒剂,通常称为季铵类消毒剂(quats),如苯扎氯铵的情况,则表面活性剂的阴离子性质往往会中和所述季铵消毒剂的功效,从而降低所述消毒剂的微生物杀灭力。因此,所述非织造制品需要用非离子或阳离子稳定的分散体粘合。US 2004/0137815 Al要求保护一种非织造抗微生物纸巾,其包含用非离子粘合剂粘合并包含阳离子消毒剂的纤维非织造基材。US 2002/0183233 A1公开了通过向所述洗剂中添加盐(阳离子释放剂)对抗微生物非织造纸巾的改进,其改善了所述阳离子消毒剂的释放。所述阳离子释放剂与阳离子季铵盐竞争所述纸巾基材中的阴离子位点。未使用非离子或阳离子粘合剂。US 2005/0025668 A1描述了用消毒剂浸洗的湿纸巾。所述非织造基材不含胶乳粘合剂,并且所述水性释放次卤酸盐组合物涂施于所述基材上。US 2002/0031486 A1公开了由水不溶性非织造基材和包含阳离子消毒剂和非离子表面活性剂的水性抗微生物清洁组合物组成的清洁巾。US 5,326,809描述了作为水性乳液聚合中的保护胶体的聚(乙烯醇)-共-(乙烯基胺)。却没有公开它用于抗微生物非织造湿纸巾的应用。
仍然需要一种简单且经济有效的方式用于改进湿纸巾组合物中阳离子消毒剂的功效。
发明内容
本发明提供了一种抗微生物非织造湿纸巾,其包括:i)用可交联乙酸乙烯酯乙烯(VAE)分散体粘合的纤维非织造基材,所述可交联乙酸乙烯酯乙烯(VAE)分散体采用一种或多种阳离子乙烯醇-N-乙烯基胺共聚物和可选的一种或多种非离子表面活性剂或非离子保护胶体进行稳定,和ii)吸附于所述非织造基材内的包括一种或多种阳离子消毒剂的水性洗剂。所述抗微生物非织造湿纸巾中不存在阴离子表面活性剂。
一种生产抗微生物非织造湿纸巾的方法包括:a)将包括用阳离子乙烯醇-N-乙烯基胺共聚物的组中的一种或多种阳离子保护胶体和可选的一种或多种非离子表面活性剂或非离子保护胶体稳定的可交联VAE分散体的第一水性组合物涂施于非织造基材上;b)干燥所述组合物;和c)将第二水性组合物涂施于步骤b)的产品。所述第一和第二水性组合物中的至少之一包括一种或多种阳离子消毒剂。
具体实施方式
本发明人发现,如果非织造湿纸巾中存在阴离子表面活性剂,则阳离子消毒剂,例如,季铵消毒剂的释放以及由此的功效就会减弱。阴离子表面活性剂通常用于稳定用作非织造基材粘合剂的乙酸乙烯酯乙烯共聚物(VAE)分散体。然而,本发明人发现,被乙烯醇-N-乙烯基胺共聚物的组中的一种或多种阳离子保护胶体阳离子性稳定的VAE分散体,与阴离子性稳定的或非离子性稳定的VAE粘合剂分散体相比,提供了所述湿纸巾组合物中阳离子消毒剂的改进功效。根据本发明的粘合剂组合物,以及由其生产的湿纸巾不含,或基本上不含,阴离子表面活性剂,从而避免干扰所述阳离子消毒剂的活性。
现在将详细讨论根据本发明的制备用非离子VAE粘合剂粘结的抗微生物非织造湿纸巾的组分和方法。除非上下文另外指出,否则本文列举的材料的百分比以重量计。
VAE共聚物
除非另有说明,否则本文提及的单体的重量百分比是基于用于制造VAE共聚物的聚合反应中所有单体的总重量,在每种情况下单体的重量百分数总计为100%。
根据本发明用作粘合剂的VAE共聚物包含乙酸乙烯酯、乙烯、N-羟甲基功能单体和(甲基)丙烯酰胺的聚合单元,即丙烯酰胺和/或甲基丙烯酰胺。乙酸乙烯酯通常以至少65wt%,或至少70%,而至多94.5wt%,或至多85%的量进行共聚。乙烯通常以至少5wt%,或至少10wt%,而至多30wt%或至多20wt%的量进行共聚。
所述共聚物中的N-羟甲基官能单体的份数通常为至少0.1wt%,或至少0.5%,1%或2wt%,并且通常为至多10.0wt%,或至多8wt%或5wt%,在每种情况下都基于聚合所用单体的总重量。N-羟甲基官能单体相对于N-羟甲基功能单体+(甲基)丙烯酰胺总量的合适用量为至少25wt%,或至少30wt%,35wt%,40wt%,45wt%,50wt%或55wt%。该用量至多85wt%,或至多80wt%,75wt%,70wt%,65wt%或60wt%。存在于所述共聚物中的N-羟甲基官能单体+(甲基)丙烯酰胺的总量为至少0.2wt%,或至少0.5wt%,1wt%,3wt%或5wt%,而至多5.0wt%,或至多8wt%,10wt%或15wt%。
用于制备所述共聚物的合适示例性N-羟甲基官能单体包括N-羟甲基丙烯酰胺(NMA)、N-羟甲基甲基丙烯酰胺、烯丙基N-羟甲基氨基甲酸酯和N-羟甲基丙烯酰胺、N-羟甲基-甲基丙烯酰胺或烯丙基N-羟甲基氨基甲酸酯的酯。N-羟甲基-丙烯酰胺和N-羟甲基-甲基丙烯酰胺是特别优选的。所述N-羟甲基官能单体与丙烯酰胺和/或甲基丙烯酰胺组合,优选与丙烯酰胺组合使用。最优选的是N-羟甲基丙烯酰胺和丙烯酰胺的共混物。这种共混物能够商购获得,例如,NMA和丙烯酰胺摩尔比1:1的48wt%水溶液,能够以商品名NMA-LF MONOMER(Cytec Industries,Woodland Park,NJ)商购获得,或含有28wt%的N-羟甲基丙烯酰胺和20wt%的丙烯酰胺的水溶液,能够以商品名NMA 2820(SNF Floerger,Andrezieux,法国)商购获得。可替代地,可以将NMA和丙烯酰胺分开添加到所述聚合进料中。
除NMA之外,所述VAE共聚物中还可以包含其他N-(C1-4)羟烷基(甲基)丙烯酰胺。也可以包括包含纤维素反应性部分的烯烃性不饱和单体,例如,含有醛、受保护醛和乙醇酸部分的那些。实例包括异丁氧基甲基丙烯酰胺、丙烯酰胺基乙醇酸、丙烯酰胺基丁醛和丙烯酰胺基丁醛的二烷基缩醛,其中所述烷基各自分别具有1-4个碳原子。
可选的是,通过在所述VAE共聚物中包括另外的单体可以扩展所述分散体中共聚物的可用性质的范围。通常而言,合适的共聚单体是具有单个可聚合烯基的单体。这种共聚单体的实例是具有3-18个碳原子的羧酸的乙烯基酯。优选的乙烯基酯是丙酸乙烯酯、丁酸乙烯酯,2-乙基己酸乙烯酯、月桂酸乙烯酯、乙酸1-甲基乙烯酯、新戊酸乙烯酯和具有9-11个C原子的α-支化一元羧酸的乙烯酯,实例有VEOVA9TM或VEOVA10TM酯(商购获自MomentiveSpecialty Chemicals,Houston,TX)。其他合适的共聚单体包括丙烯酸或甲基丙烯酸与具有1-15个C原子的直链或支链醇的酯。示例性的甲基丙烯酸酯或丙烯酸酯包括丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丙酯、甲基丙烯酸丙酯、丙烯酸正丁酯、甲基丙烯酸正丁酯、丙烯酸2-乙基己酯和丙烯酸降冰片基酯。其他合适的共聚单体包括乙烯卤化物如氯乙烯,或烯烃如丙烯。通常而言,基于用于聚合的单体的总重量,所述其它共聚单体以0.5wt%-30wt%,优选0.5wt%-20wt%的量进行共聚。
可选的是,基于用于聚合的单体的总重量,0.05wt%-10wt%的其他单体(辅助单体)可以另外共聚而形成分散体。辅助单体包括可聚合的烯基和至少一个另外官能团。辅助单体的实例包括丙烯腈以及富马酸和马来酸的二酯,例如,二乙基和二异丙基酯。通常而言,在用于制备VAE共聚物的每种单体中只有一个可聚合的烯基,尽管在某些情况下可以是更多个可聚合烯基。
另一方面,当用于制造根据本发明的湿纸巾时,包含羧酸、磺酸或磷酸或膦酸基团、其盐或水解成它们的基团的乙烯型不饱和单体通常排除于用作制备纸巾的粘合剂的VAE共聚物之外。具体的实例包括丙烯酸、甲基丙烯酸、富马酸、马来酸、马来酸酐、乙烯基磺酸和2-丙烯酰胺基-2-甲基丙磺酸。
单体的选择或单体重量比的选择优选以通常使共聚物具有合适的玻璃化转变温度(Tg)的方式进行。通常而言,Tg为至少-10℃,或至少-5℃,或至少0℃,而至多+20℃,或至多+15℃,或至多+10℃。共聚物的玻璃化转变温度Tg可以通过差示扫描量热法(DSC)按照根据ASTM D3418-82作为起始温度以每分钟10℃的加热速率的已知方式确定。Tg也能够近似地通过Fox方程预先计算。根据Fox T.G.,Bull.Am.Physics Soc.1,3,page 123(1956):1/Tg=xl/Tg1+x2/Tg2+…+xn/Tgn,其中xn是单体n的质量分数(wt%/100),Tgn是单体n均聚物的开氏(Kelvin)玻璃化转变温度。均聚物的Tg值提供于《聚合物手册》第二版,J.Wiley&Sons,纽约(1975)中(the Polymer Handbook 2nd Edition,J.Wiley&Sons,New York(1975))。
阳离子保护胶体
合适的阳离子保护胶体是阳离子乙烯醇-N-乙烯基胺共聚物,在本文中也称为阳离子聚(乙烯醇)-共-(乙烯胺)。乙烯醇-N-乙烯基胺共聚物能够商购获自Sekisui。这些共聚物的合成在本领域中是众所周知的,并且例如,描述于EP 0339371 A2或WO 2006/082157A1中。在制备的第一步中,将乙酸乙烯酯和N-乙烯基甲酰胺共聚生成乙酸乙烯酯-N-乙烯基甲酰胺共聚物。在第二步中,乙酸乙烯酯-N-乙烯基甲酰胺共聚物通过酸或碱催化皂化成乙烯醇-N-乙烯基胺共聚物。在第三步中,用酸或碱催化将乙烯醇-N-乙烯基甲酰胺共聚物水解为乙烯醇-N-乙烯基甲酰胺共聚物。水解后,乙烯醇-N-乙烯胺共聚物优选由0-15mol%的乙酸乙烯酯单元、50mol%-99mol%的乙烯醇单元、0-10mol%的乙烯基甲酰胺单元和1mol%-25mol%的乙烯基胺单元组成,并且数据以mol%计,在每种情况下总计100mol%。通常而言,乙烯醇-N-乙烯基胺共聚物的重均分子量Mw为10,000-200,000,优选Mw为15,000-130,000。通常而言,乙烯醇-N-乙烯胺共聚物在4%浓度的水溶液中具有1-30mPas的粘度(霍普勒(Hoeppler)粘度,根据DIN 53015在20℃下测定)。一般而言,在VAE共聚物的乳液聚合期间引入乙烯醇-N-乙烯胺共聚物的阳离子电荷,这通常在低于6的pH下进行。
另外,能够使用一种或多种非离子保护胶体稳定乳液聚合反应期间和之后的VAE分散体。合适的非离子保护胶体包括聚乙烯醇(PVOH)和非离子纤维素衍生物,例如,羟乙基纤维素。其他实例包括聚乙烯吡咯烷酮,带有环氧乙烷或聚环氧乙烷取代基的PVOH和乙酰乙酰基化PVOH。另外,可以使用PVOH的共聚物。实例包括乙烯醇的乙烯和/或N-乙烯基吡咯烷酮共聚物。聚乙烯醇是特别有用的。合适的PVOH包括部分水解的聚乙烯醇,其水解度为80mol%-99mol%,优选85mol%-99mol%,并且在4%浓度的水溶液中的粘度为1-30mPas,优选3-6mPas(霍普勒(Hoeppler)粘度,根据DIN 53015在20℃下测定)。这样的PVOH能够商购获得或可通过技术人员已知的方法获得。
阳离子乙烯基醇-N-乙烯基胺共聚物,以及可选的其他保护性胶体,例如,聚乙烯醇,通常将以至少0.1wt%,或至少0.2wt%或0.5wt%的水平存在。通常而言,该水平为至多10wt%,或至多5wt%或1wt%。这些百分比表示保护胶体相对于用于聚合的所有单体的总重量的含量。
除了阳离子乙烯醇-N-乙烯胺共聚物外,在可交联的VAE分散体中能够可选地存在非离子表面活性剂(乳化剂)。优选的非离子表面活性剂是乙氧基化的支链或非支链脂族醇,特别是具有3-80个环氧乙烷单元和C5-C36烷基的乙氧基化度。优选的非离子表面活性剂还包括具有3-30个环氧乙烷单元的乙氧基化度的C13-C15羰基化醇乙氧基化物(C13-C15oxo-process alcohol ethoxylate),以及具有乙氧基化度11-80个环氧乙烷单元的乙氧基化度的C16-C18脂族醇乙氧基化物。特别优选的是具有3-30个环氧乙烷单元的乙氧基化度的C12-C14脂族醇乙氧基化物,以及具有至少10wt%的环氧乙烷的最低含量的环氧乙烷和环氧丙烷共聚物。这些表面活性剂优选不包含烷基酚乙氧基化物结构。
每种情况下基于单体总重量,表面活性剂的总量通常为0.5wt%-5wt%,优选1wt%-3wt%。
乳液聚合方案
在VAE共聚物的聚合期间,聚合混合物用一种或多种乙烯醇-N-乙烯基胺共聚物和可选的一种或多种非离子表面活性剂或非离子保护胶体进行稳定。VAE分散体可以通过乳液聚合,通常在40℃-100℃,更通常50℃-90℃,最通常60℃-80℃的温度下制备。聚合压力取决于乙烯进料通常为10-100bar(巴),更通常而言25-90bar,特别是45-85bar。聚合混合物的pH要调节至pH<5,优选pH调节至3-5。
聚合使用氧化还原引发剂组合,如乳液聚合常规的组合进行引发。氧化还原引发剂系统可以用于制备适合本发明使用的VAE分散体。引发剂可以是产生甲醛的氧化还原引发系统,如甲醛次硫酸钠(sodium formaldehyde sulfoxylate)。然而,在某些实施方式中,最小化分散体中的甲醛水平是合乎需要的。在这种情况下,使用不产生甲醛的氧化还原引发系统是合乎需要的。通常而言,用于氧化还原对的合适的不产生甲醛还原剂包括,作为非限制性实例,基于本领域中已知的抗坏血酸、亚硫酸氢盐、异抗坏血酸盐或酒石酸化学品的那些,和由德国海尔布隆(Heilbronn)的布鲁格曼化学公司(Bruggeman Chemical)制造的称为FF6M的商业还原剂。也可以使用非氧化还原引发剂,如过氧化物和偶氮类引发剂,所有这些都是本领域众所周知的。
所有单体可以构成初始进料,或所有单体可以形成进料,或部分单体可以形成初始进料,而其余的可以在引发聚合之后形成进料。进料可以是分开的(在空间上和时间上),或可以在预乳化后进料全部或部分组分。一旦聚合过程结束,可以使用已知方法进行后聚合(post-polymerization)而除去残留单体,合适方法的一个实例是由氧化还原催化剂引发的后聚合。挥发性残留单体也可以通过蒸馏,优选在低于大气压下,以及在合适的情况下,通过使惰性夹带气体如空气、氮气或水蒸气穿过或越过该材料而除去。
所制备的合适VAE共聚物分散体的固体含量通常处于45wt%-75wt%的范围内。如果稀释至25%固含量水平,则分散体通常具有至少5mPas或至少10、20或30mPas的粘度。该粘度通常为至多800mPas,或至多700、600或500mPas。粘度使用具有#3转子的布鲁克菲尔德(Brookfield)粘度计LVD型以60rpm和25℃下进行测定。
纤维非织造基材
纤维非织造基材可以是天然纤维,例如(但不限于)纤维素纤维或木浆,或合成纤维,其包括,但不限于,通过干法(气流成网(airlaid),梳理成网(carded),朗多(rando)成网)或湿法成网(wet laid)工艺处理的聚酯、聚乙烯、聚丙烯和聚乙烯醇或粘胶纤维或任何这些的组合中的一种或多种。在用阳离子粘合剂组合物处理之前,纤维非织造基材的基重通常为至少10g/m2或至少45g/m2,并且通常最多150g/m2或最多120g/m2。
水性消毒洗剂
在粘合的非织造基材中吸收的水性洗剂包括一种或多种阳离子消毒剂。这些通常是季铵消毒剂化合物。苯扎氯铵(Benzalkonium chloride)是一个具体的实例,尽管本领域已知的任何其他阳离子消毒剂可以代替或另外使用。一些阳离子消毒剂可以溶解于所述洗剂的水相中,而另一些则吸附于非织造基材的纤维表面上。优选所述阳离子消毒剂每个分子仅包含一个阳离子部分。
该水性洗剂还可以可选地包含不是阳离子消毒剂的盐。可以包括任何类型的盐,例如,有机盐、无机盐和包含有机阴离子和金属、非消毒剂季铵盐阳离子,或非季铵盐阳离子,即NH4 +或质子化的伯、仲或叔胺的盐。非限制性实例包括乙酸盐、乙炔化物(acetylide)、铵盐(不包括季铵盐类)、砷酸盐、砹化物(astatide)、叠氮化物、双卤盐、碳酸氢盐,双硫化物、硼化物、硼氢化物、硼卤化物、碳酸盐、柠檬酸盐、氰酸盐、氰化物、甲酸盐、锗酸盐(germanate)、甘氨酸盐、卤酸盐、卤化物、氢化物、氢硒酸盐、氢硫化物(hydrosulphide)、氢氧化物、酰亚胺、偏铌酸盐、偏钽酸盐、偏钒酸盐、硝酸盐、氮化物、亚硝酸盐、氧化物、高氯酸盐、磷酸盐、鏻盐、硒化物、亚硒酸盐、硒酸盐、硫化物、硫酸盐、三元盐、非消毒剂四烷基铵盐、碲化物、硫氰酸盐和/或钒酸盐。具体实例包括柠檬酸钾,柠檬酸钠,酒石酸钠,酒石酸钾,乳酸钾,乳酸钠,钠和/或钾水杨酸盐,硫酸镁,氯化钠,氯化铵和/或氯化钾。然而,可以排除除阳离子消毒剂以外的任何一种或多种上述盐或所有盐。
该水性洗剂还可以包含有机溶剂,如果存在,则有机溶剂通常将占所述洗剂组合物至多10wt%,或至多5wt%、2wt%或1wt%。实例包括C1-6链烷醇、C1-6二醇、亚烷基二醇的C1-10烷基醚、C3-24亚烷基二醇醚和/或聚亚烷基二醇。特定类型的溶剂包括烷醇如甲醇、乙醇、正丙醇、异丙醇、丁醇、戊醇和/或己醇及其各种位置异构体;丙酮;和二醇醚如乙二醇单丙醚、乙二醇单丁醚、乙二醇单己醚、丙二醇正丙醚、丙二醇单丁醚、丙二醇叔丁醚、二甘醇单乙基或单丙基或单丁基醚、二-或三聚丙二醇的甲基或乙基或丙基或丁基醚、乙二醇醚的乙酸酯和/或丙酸酯。然而,可以排除任何一种或多种上述溶剂,或所有溶剂。
制作抗微生物非织造湿纸巾
阳离子VAE粘合剂组合物通常通过喷涂、饱和、凹版印刷或发泡而施涂施于非织造基材上。该粘合剂组合物可以可选地包含催化剂,例如,酸性化合物或其铵盐。一个实例是氯化铵。
该粘合剂组合物中可以包含润湿添加剂,以辅助不仅润湿该基材上的所配制的粘合剂,而且还润湿随后的成品纤维非织造基材。润湿添加剂应该是非离子型或阳离子型润湿表面活性剂,才能避免降低作为洗剂添加到所粘合的非织造基材上的阳离子消毒剂的功效。一个实例是这是一种由Air Products销售的非离子型乙氧基化炔二醇(nonionic ethoxylated acetylenic diol)。基于干聚合物的重量,该湿润剂可以以0.1-3干份(dry parts)的水平包括于该粘合剂组合物中,但是更典型地配制成0.5-2份。
该组合物通常以0.5wt%-30wt%的固含量涂施,这要取决于所述基材上的所需负载量。通常而言,基于未处理基材的重量,粘合剂以干重计的用量将为至少5wt%,或至少10%或15%。它通常为至多50wt%,或至多40%或30%。
在该粘合剂组合物涂施于基材上之后,干燥所述基材。通常在120℃-160℃的温度范围内进行,但可以使用更高或更低的温度。之后,就可以涂施包含阳离子消毒剂的水性洗剂。
可替代的是,该阳离子消毒剂可以包括于VAE粘合剂组合物中,而不是如上所述将其分开添加至所述洗剂中。在那种情况下,在已经涂施并干燥所述粘合剂组合物之后,可以将水和任何其他洗剂组分,例如,溶剂,添加到所述基材中,并且应当理解的是,某些或全部阳离子消毒剂可以溶解于该水中。或者,可以使用两种添加阳离子消毒剂的方式。在任何一种这些方式中,每100份粘合的基材(干基),所述水性洗剂通常将以至少50份洗剂(湿基)或至少150、200或250份的量存在。每100份基材,洗剂的量通常最多500份,或最多400或350份。在所有情况下,都可以用有效最小化或避免变干的任何方式包装所获得的湿纸巾。
实施例
Tg的测量
共聚物的玻璃化转变温度(Tg)通过差示扫描量热法(DSC)使用Mettler-ToledoDSC1动态差示扫描量热仪根据ASTM D3418-82作为起始温度以每分钟10℃的加热速率进行测定。在第二加热循环中评价玻璃化转变的开始。
粘度的测量-布鲁克菲尔德(Brookfield)
除非另有说明,否则都使用具有#3转子(spindle)的Brookfield粘度计LVD型以60rpm在25℃下测定共聚物分散体和粘合剂组合物的布氏(Brookfield)粘度。聚乙烯醇的粘度是按照DIN 53015在20℃下测得的4wt%水溶液的霍普勒(Hoeppler)粘度。
制备并测试了以下与NMA和丙烯酰胺共聚的乙酸乙烯酯乙烯分散体:
比较实施例1:
将以下组分混合至一起:3.200kg 10%水溶液(聚乙烯醇,平均水解水平为98mol%-99mol%,4wt%水溶液粘度为5.5-6.5mPa.s,商购获自Sekisui)、3.200kgTLA 3040(十三烷醇乙氧基化物表面活性剂的40wt%溶液,每个十三烷醇具有约30个环氧乙烷单元,商购获自Solvay)、1.600kgF68(环氧乙烷/环氧丙烷嵌段共聚物,商购获自BASF Chemical Corp.)、0.640kgL64(环氧乙烷/环氧丙烷嵌段共聚物,商购获自BASF Chemical Corp.)和40.0g磷酸二氢铵溶解于27.100kg去离子水中。用40.0g磷酸(85%)调节该混合物pH至3.8,并且然后向该混合物中加入1.7g硫酸亚铁铵。将该混合物加入已用氮气吹扫的三十五加仑(132.5L)压力反应器中,并在搅拌(350rpm)下加入54.372kg乙酸乙烯酯。用乙烯吹扫反应器,将搅拌保持于350rpm,并将9.595kg乙烯加入所述反应器中。然后将温度升至35℃,并将118.0g 4.8wt%异抗坏血酸钠水溶液(用85%磷酸将pH调节至4.5)加入该反应器中。使反应器内容物达到平衡,而此时的压力为392psi(27bar)。4.0wt%叔丁基过氧化氢水溶液和4.8wt%异抗坏血酸钠水溶液(用85%磷酸将pH调节至4.5)分别以10.0g/min和16.7g/min的速率连续进料至该反应器中。在温度上升1℃之后,在60分钟内使反应器温度升至75℃。另外,在180分钟内将11.440kg NMA-LF水溶液(NMA 2820,约28wt%N-羟甲基丙烯酰胺和20wt%丙烯酰胺的水性混合物,商购获自SNF Floerger)进料到该反应器中,并且然后将NMA-LF的进料管线用另外0.375kg水冲洗到该反应器中。在这3个小时的延迟时间内,NMA-LF的添加速率大致恒定。
叔丁基过氧化氢和异抗坏血酸钠进料的流速保持于约1:1.7的比率,并调节流速而保持75℃的反应温度。在反应过程期间测量未反应的乙酸乙烯酯,并发现1小时后为46.6%,2小时后为26.1%,3小时后为7.6%,3.2小时后为4.7%。在3.5小时结束时,停止叔丁基过氧化氢和异抗坏血酸钠进料,将反应冷却至50℃,并将所述反应混合物转移至脱气机中而除去未反应乙烯。用2.300kg水冲洗反应器,该水也转移到脱气机中,并加入35.0gDF540消泡剂(商购获自Solvay)和110.0g水的混合物以抑制泡沫形成。为了将未反应乙酸乙烯酯单体减少到低于0.1wt%,在40分钟内加入0.740kg 8.0wt%异抗坏血酸钠水溶液和0.740kg 6.30wt%叔丁基过氧化氢水溶液。最后,在30分钟内加入溶于215g 7.01wt%过氧化氢水溶液中的18.9g十二烷基胍盐酸盐。
固含量、粘度和Tg列于表1中。
实施例2:
将以下成分混合至一起:811.5g 10%聚乙烯醇-共-乙烯胺水溶液(88:12的乙烯醇:乙烯胺摩尔比,4wt%水溶液粘度为4-6mPa.s)和100.0g去离子水。使用33.8g 50wt%磷酸水溶液将该混合物pH调节至3.5,并且随后将2.1g 5wt%硫酸亚铁铵水溶液加入到该混合物中。将该混合物加入到已经用氮气吹扫的一加仑(3.8L)不锈钢压力反应器中,并在搅拌(200rpm)下加入1100g乙酸乙烯酯。
用乙烯吹扫反应器,将搅拌增加到1000rpm,并将245g乙烯加入到反应器中。然后将温度升高至32℃,并将7.3g 4.75wt%异抗坏血酸钠水溶液(用50%磷酸将pH调节至4.5)加入该反应器中。将1.50wt%过氧化氢水溶液和4.75wt%异抗坏血酸钠水溶液分别以0.2g/min的速率连续进料到该反应器中。温度升高1℃后,将反应器温度在80分钟内升至85℃。
过氧化氢和异抗坏血酸钠的进料保持相等的流速并经过调节而保持85℃的反应温度。在反应过程期间测量未反应的乙酸乙烯酯,并发现0.5小时后为23.5%,1.5小时后为9.2%,2.5小时后为1.0%。在2.5小时结束时,停止过氧化氢和异抗坏血酸钠进料,将反应冷却至60℃,并将该反应混合物转移至脱气机中而除去未反应的乙烯。加入1.0gFoamaster VF消泡剂(商购获自Solvay)和5g水的混合物以抑制泡沫形成。为了将未反应的乙酸乙烯酯单体降低至低于0.1wt%,在15分钟内加入25.0g 8wt%异抗坏血酸钠水溶液和20.0g 8.0wt%叔丁基过氧化氢水溶液,而同时将温度保持于30℃或以上。
固含量、粘度和Tg列于表1中。
实施例3:
将以下组分混合在一起:33.895kg 10wt%聚乙烯醇-共-乙烯胺水溶液(88:12乙烯醇:乙烯胺摩尔比,4wt%水溶液的粘度为4-6mPa.s)和1.959kg去离子水。使用834g的磷酸(85%)将该混合物的pH调节至4.0,并且然后将4.4g硫酸亚铁铵加入到该混合物中。将该混合物加入已用氮气吹扫的三十五加仑(132.5L)压力反应器中,使用2.300kg去离子水冲洗该初始进料到反应器中,并在搅拌(375rpm)下添加45.948kg乙酸乙烯酯。
用乙烯吹扫该反应器,搅拌保持于375rpm,并将10.235kg乙烯加入到该反应器中。然后将温度升至32℃,并将246.0g 2.9wt%异抗坏血酸钠水溶液(用85wt%磷酸将pH调节至4.5)加入到该反应器中。使反应器内容物平衡。将1.5wt%过氧化氢水溶液和2.9wt%异抗坏血酸钠水溶液(用85wt%磷酸将pH调节至4.5)分别以6.7g/min和6.8g/min的速率连续进料至该反应器中。温度升0.5℃后,使反应器温度在90分钟内升至77℃。另外,将5.367kg7.63wt%NMA-LF活性水溶液(NMA 2820,约28wt%N-羟甲基丙烯酰胺和20wt%丙烯酰胺的水性混合物,商购获自SNF Floerger)在180分钟内进料到该反应器中,并将NMA-LF的进料管线用另外0.375kg去离子水冲洗至该反应器中。在这3个小时的延迟时间内,NMA-LF的添加速率大致恒定。
过氧化氢和异抗坏血酸钠进料的流速保持于约1:1的比率,并调节流量而使反应温度保持于77℃。在反应过程期间测量未反应的乙酸乙烯酯,并发现在1小时后为36.7%,在2小时后为18.4%,在3小时后为7.5%,在4小时后为2.0%。在4.0h结束时,停止过氧化氢和异抗坏血酸钠进料,将反应冷却至50℃,并将该反应混合物转移至脱气机中而除去未反应的乙烯。用2.300kg去离子水冲洗该反应器,也将其转移到脱气机中,并加入63.0gFoamaster M02185消泡剂(商购获自BASF)和415.0g水的混合物以抑制泡沫形成。为了将未反应的乙酸乙烯酯单体降低至低于0.1wt%,在45分钟内加入1.044kg 8.0wt%异抗坏血酸钠水溶液和0.836kg 8.0wt%叔丁基过氧化氢水溶液。最后,在30分钟内加入0.609kg7.0wt%过氧化氢水溶液。
固含量、粘度和Tg列于表1中。
测试与结果:
证明非织造基材中阳离子消毒剂功效的改进的测试和测量遵循以下步骤:
1.粘合剂涂施于非织造物:
本研究中使用的非织造基础基材(base substrate)经由气流成网工艺方法(airlaid process)生产,并由88wt%纤维素纤维和12wt%由聚乙烯外皮和聚酯芯组成的合成双组分纤维制成。气流成网的基础基材(base)基重为约90g/m2。表1中所列的粘合剂按照表2中所示进行配制,并作为20wt%固体水性组合物喷涂于气流成网基材的两侧以获得20wt%聚合物添加量(在干燥的基材上干燥),并在Mathis中通过气流烘干器在150℃下干燥3分钟。在涂施季胺之前,将粘合的基材置于70°F(21℃)和50%相对湿度的恒温湿室中。这些与所列粘合剂粘合的基材的物理性能如表3中所示。根据ASTM方法D 5035-95进行干和湿拉伸断裂强度测试。
2.季铵盐涂施于非织造基材上:
将上述步骤1中形成的非织造基材用378ppm苯扎氯铵(季胺)水溶液以300%湿苯扎氯铵溶液的水平润湿(针对非织造基材的干重)。然后将所处理过的基材放置于塑料袋中并密封以防止蒸发。将密封于袋子中的处理过的基材静置42小时,然后根据所使用的粘合剂从所述纸巾中将苯扎氯铵溶液提取到单个棕色瓶中,并且然后对每个瓶加盖。
3.苯扎氯铵分析:
从所述处理过的纸巾中提取的苯扎氯铵溶液用进一步用市售净水器纯化的去离子水按照1:10的比例稀释。使用Sigma-Aldrich的苯扎氯铵标准溶液制备水性标准溶液。使用浓度范围为0.5ppm-45ppm的标准溶液创建四点外标线性校准曲线。相关系数的平方(R2)为0.999905。然后将所稀释的测试苯扎氯铵溶液进行高压液相色谱(HPLC)分离,该分离使用乙腈/磷酸钾流动相,采用Waters Alliance系统和Surfactant Plus色谱柱完成。Waters PDA检测器用于峰检测。峰下的面积表示存在的苯扎氯铵的量。表1中显示了分析的结果(苯扎氯铵功效,以ppm为单位)。
4.粘合的气流成网基材的物理强度测量:
使用ASTM方法D 5035-95,在Instron拉伸试验机上测量经处理的气流成网非织造基材的横向(CD)湿和干拉伸断裂强度。使用5.1cm×25.4cm(2英寸×10英寸)模切机将所粘合的基材进行模切(die cut),以制备用于测定拉伸强度的样品。将条带放置于Instron机械拉伸试验机的钳口中。为了进行干拉伸测定,将所述模切样品垂直放置于试验机的钳口中并开始测试。拉伸试验机提供断裂时获得的最大拉伸的统计数据。使用十字头速度为15.2cm/min(6英寸/分钟),设置标距长度为20.3cm(8英寸),进行干拉伸测定。进行了多次测试,并且计算并报告平均值。
除了将样品放入包括充水容器的Finch Cup设备中之外,类似地测定湿拉伸测量。将样品绕于金属棒上,然后浸入水中并保持15秒钟。然后开始拉伸测试。由于拉伸条带的环圈效应(loop effect),使用了5.1cm(2英寸)的标距长度。最大湿强度由拉伸试验机进行测定。试验进行数次,并计算出平均值。
粘合的气流成网基材的物理强度测量结果如表3中所示。
表1:季胺功效试验和结果
*Wacker Chemie AG的192是一种市售的自交联VAE分散体,含有4.8wt%的NMA和丙烯酰胺1:1摩尔共混物,用相对于该聚合物2.5wt%的阴离子表面活性剂系统进行稳定,并且该分散体的固含量为52.3%。
苯扎氯铵消毒剂在湿纸巾组合物中的功效测试结果表明,阳离子粘合剂相比于非离子粘合剂的功效高两倍至三倍,而相比于阴离子粘合的基材,功效高十倍以上。
表2:粘合剂配方
表3:横向(CD)干和湿拉伸断裂强度
使用作为对照比较,作为单独实验运行表3中所示的比较分散体样品实验。由于基础气流成网基材的变化和正常实验误差,进行了单独实验。这些变化导致每次实验之间采用192粘合的基材拉伸值产生差异。因此,重要的是显示每个实施例如何与其相应的192对照物进行比较。
即使可交联的NMA未进行共聚(实施例2)或即使仅八分之一的NMA进行了共聚(实施例3),采用实施例2和3的阳离子粘合剂粘合的抗微生物非织造物显示出与阴离子或非离子粘合非织造物相似的机械强度。根据实验数据,按照实施例2作出的实施方式在干非织造物上添加1.0%-25.0%干分散体会提供250克力/5厘米宽-5000克/5厘米宽度的干非织造物拉伸强度和250克力/5厘米宽度-3000克/力/5厘米宽度的湿拉伸强度。根据实施例3作出的实施方式在干非织造物上添加1.0%-25.0%干分散体会提供250克力/5cm宽-5000克/5cm宽的干非织造物拉伸强度和250克力/5厘米宽-3000克/力/5cm宽的湿拉伸强度。因此,低得多的NMA含量会提供甲醛释放量的显著降低。
采用阳离子粘合剂粘合的基材的吸收率,尽管较慢,但不会妨碍流体(如用于抗微生物应用的洗剂)完全吸收至基材中。
Claims (10)
1.一种抗微生物非织造湿纸巾,包括
i)用由来自阳离子乙烯醇-N-乙烯基胺共聚物的组中的一种或多种阳离子保护胶体稳定的可交联VAE分散体粘合的纤维非织造基材,和
ii)吸附于所述非织造基材中的包括一种或多种阳离子消毒剂的水性洗剂,
其中所述抗微生物非织造湿纸巾中不存在阴离子表面活性剂。
2.根据权利要求1所述的抗微生物非织造湿纸巾,其中所述可交联VAE分散体另外用一种或多种非离子保护胶体进行稳定。
3.根据权利要求1所述的抗微生物非织造湿纸巾,其中所述可交联VAE分散体另外用一种或多种非离子表面活性剂进行稳定。
4.根据前述权利要求中任一项所述的抗微生物非织造湿纸巾,其中所述乙烯醇-N-乙烯基胺共聚物由50mol%-99mol%的乙烯醇单元、0-10mol%的乙烯基甲酰胺单元和1mol%-25mol%的乙烯基胺单元构成。
5.根据前述权利要求中任一项所述的抗微生物非织造湿纸巾,其中所述一种或多种阳离子消毒剂包括季铵消毒剂。
6.根据前述权利要求中任一项所述的抗微生物非织造湿纸巾,其中所述一种或多种阳离子消毒剂包括苯扎氯铵。
7.一种生产前述权利要求中任一项所述的抗微生物非织造湿纸巾的方法,包括:
a)将包含用由来自阳离子乙烯醇-N-乙烯基胺共聚物的组中的一种或多种阳离子保护胶体稳定的可交联VAE分散体的第一水性组合物涂施于非织造基材上;
b)干燥所述组合物;和
c)将第二水性组合物涂施于步骤b)的产物上;
其中所述第一水性组合物和第二水性组合物中的至少一种包含一种或多种阳离子消毒剂。
8.根据权利要求7所述的方法,其中所述第一水性组合物包含一种或多种所述阳离子消毒剂。
9.根据权利要求7所述的方法,其中所述第二水性组合物包含一种或多种所述阳离子消毒剂。
10.根据权利要求7所述的方法,其中用以1.0%-25%的量干添加于干非织造物上的阳离子乙烯醇-N-乙烯基胺共聚物胶体稳定的所述乙酸乙烯酯-乙烯分散体粘合的所述抗微生物非织造湿纸巾提供使用ASTM方法D 5035-95在Instron拉伸测试仪上测定的250克力/5厘米宽度-5000克/5cm宽度的干非织造拉伸强度和250克/5厘米宽度-3000克/5厘米宽度的湿拉伸强度。
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