CN115517980B - 一种婴儿手口湿巾及制备方法 - Google Patents
一种婴儿手口湿巾及制备方法 Download PDFInfo
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- CN115517980B CN115517980B CN202211290379.5A CN202211290379A CN115517980B CN 115517980 B CN115517980 B CN 115517980B CN 202211290379 A CN202211290379 A CN 202211290379A CN 115517980 B CN115517980 B CN 115517980B
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- fiber
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- sodium
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- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 229920002385 Sodium hyaluronate Polymers 0.000 claims abstract description 21
- 229940010747 sodium hyaluronate Drugs 0.000 claims abstract description 21
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical group [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims abstract description 21
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- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims abstract description 11
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- 159000000000 sodium salts Chemical class 0.000 description 3
- ANZUDYZHSVGBRF-UHFFFAOYSA-N 3-ethylnonane-1,2,3-triol Chemical compound CCCCCCC(O)(CC)C(O)CO ANZUDYZHSVGBRF-UHFFFAOYSA-N 0.000 description 2
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- MXOAEAUPQDYUQM-QMMMGPOBSA-N (S)-chlorphenesin Chemical compound OC[C@H](O)COC1=CC=C(Cl)C=C1 MXOAEAUPQDYUQM-QMMMGPOBSA-N 0.000 description 1
- 229940100555 2-methyl-4-isothiazolin-3-one Drugs 0.000 description 1
- NCZPCONIKBICGS-UHFFFAOYSA-N 3-(2-ethylhexoxy)propane-1,2-diol Chemical compound CCCCC(CC)COCC(O)CO NCZPCONIKBICGS-UHFFFAOYSA-N 0.000 description 1
- TZZGHGKTHXIOMN-UHFFFAOYSA-N 3-trimethoxysilyl-n-(3-trimethoxysilylpropyl)propan-1-amine Chemical compound CO[Si](OC)(OC)CCCNCCC[Si](OC)(OC)OC TZZGHGKTHXIOMN-UHFFFAOYSA-N 0.000 description 1
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- AKGZDINYLOSBTE-UHFFFAOYSA-N [(e)-n'-(diaminomethylideneamino)carbamimidoyl]azanium;chloride Chemical compound Cl.NC(=N)NN=C(N)N AKGZDINYLOSBTE-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
本发明提供了一种婴儿手口湿巾及制备方法,湿巾包括湿巾液、载体,湿巾液包括如下原料中的两种或两种以上:山梨酸钾、脱氢乙酸钠、苯甲酸钠、葡萄糖酸内酯、柠檬酸钠,其余为纯净水,山梨酸钾、脱氢乙酸钠、苯甲酸钠至少含有一种;载体为双层结构非织造布,上层为接枝改性PET纤维,下层纤维原料为其他种类纤维,载体通过双层纤维原料分别梳理成网复合后,进行水刺加固得到;接枝改性PET纤维的接枝改性剂为透明质酸钠。通过酯化反应将透明质酸钠接枝到PET纤维的表面,并以接枝改性PET纤维作为载体的上层,其他纤维原料为下层原料制备载体,这种载体含液量高,在湿巾液组成简单,且满足对婴儿皮肤温和无刺激、毒理安全性良好、可入口的前提下,长期放置,抑菌率和溢液率的变化趋势较小。
Description
技术领域
本发明属于婴幼儿清洁产品技术领域,具体涉及一种婴儿手口湿巾及制备方法。
背景技术
湿巾是用来擦拭皮肤的湿润的纸巾,以无纺布、无尘纸或其他多孔或吸附性材料为载体,纯化水为生产用水,添加适量的保湿剂、香精、防腐剂等辅料而制成,对人体表面或物体表面有清洁作用的产品。婴儿手口湿巾指专门给婴儿手和嘴清洁用的湿巾,由于婴儿肌肤更娇嫩,对过敏源更敏感,婴儿手口湿巾既要具有基本的清洁的功能,又要满足湿巾中各成分为食品级可入口、且不会造成婴儿肌肤过敏。
专利CN201310014515.2公开了一种婴儿手口湿巾及其制备方法,湿巾复配液含有0.01-2.0%的防腐剂,防腐剂为Geogard Ultra防腐剂、苯扎氯铵、对羟基苯甲酸甲酯钠及其钠盐、对羟基苯甲酸乙酯及其钠盐、聚六亚甲基单胍、聚六亚甲基双胍盐酸盐、苯氧乙醇、甲基异噻唑啉酮、山梨酸钾、脱氢醋酸、苯甲醇、二氯苯甲醇、乙基己基甘油、辛二醇、辛甘醇中任意一种或几种的混合。专利CN201910167863.0公开了一种湿巾,所述湿巾浸泡液由以下重量百分比的组分组成:银离子0.000003%-0.0000049%,乙基己基甘油0-0.00049%,苯氧乙醇0-0.00049%,氯苯甘醚0-0.00049%,过氧化氢0-0.00049%,苯甲醇0-0.00049%,对羟基苯乙酮0-0.00049%,余量为去离子水;其中,乙基己基甘油、苯氧乙醇、氯苯甘醚、过氧化氢、苯甲醇、对羟基苯乙酮至少含有一种。
以上技术为较常见的具有清洁效果的婴儿手口湿巾配方,但其中有些成分对婴儿具有不良影响,如苯氧乙醇会导致发热、刺痛;尼泊金酯(对羟基苯甲酸甲酯、对羟基苯甲酸乙酯等)及其钠盐等化合物因生殖毒性在化妆品中已逐渐弃用,在婴儿手口湿巾中更不宜使用。并且为减少有机成分对婴儿产生不良影响,保湿剂用量很少或为零,加之原本水分含量多,制备的湿巾宜单片包装,若多片装,放置一段时间后受重力或外界压力影响会有液体溢出,大大降低清洁力。此外,多片装湿巾一经打开就必须在短时间内将剩余湿巾用完,否则水分挥发,清洁效果也会下降。
因此,开发一种湿巾液与载体有良好吸附力、不易分离,即湿巾保液量高,且对婴儿皮肤温和无刺激,护肤清洁性良好、毒理安全性良好,能入口的食品级的婴儿手口湿巾,对保护婴儿身体健康及推广湿巾在婴儿及婴儿用品领域的应用具有重要意义。
发明内容
针对上述技术问题,本发明提供了一种婴儿手口湿巾及制备方法,通过酯化反应将透明质酸钠接枝到PET纤维的表面,并以接枝改性PET纤维作为载体的上层,其他纤维原料为下层原料制备载体,这种载体含液量高,在湿巾液组成简单,在满足对婴儿皮肤温和无刺激、毒理安全性良好、可入口的前提下,还能显著提高湿巾的清洁能力。
一种婴儿手口湿巾,所述湿巾液包括如下原料中的两种或两种以上:山梨酸钾、脱氢乙酸钠、苯甲酸钠、葡萄糖酸内酯、柠檬酸钠,其余为纯净水,山梨酸钾、脱氢乙酸钠、苯甲酸钠至少含有一种;所述载体为双层结构非织造布,上层为接枝改性PET纤维,下层纤维原料为其他种类纤维,载体通过双层纤维原料分别梳理成网复合后,进行水刺加固得到;所述接枝改性PET纤维的接枝改性剂为透明质酸钠。
进一步地,所述湿巾液包括如下重量份的原料:0.05-0.5份山梨酸钾、0.03-0.3份脱氢乙酸钠、0.1-0.5份苯甲酸钠、0.1-1份葡萄糖酸内酯、0.1-1份柠檬酸钠,其余为纯净水,原料总和为100份,所述接枝改性PET纤维的接枝率为3-7.5wt%,优选5-7.5wt%。
所述透明质酸钠的重均分子量为10000以下。
所述接枝改性PET纤维通过包括如下步骤的方法制得:
1)将PET纤维浸泡入碱液中,升温至回流状态,恒温搅拌进行反应,反应结束后加入酸液中和至中性,过滤、洗涤、烘干,备用;
2)将步骤1)所得纤维浸泡于催化剂的水溶液,过滤、烘干;将烘干的纤维浸泡于透明质酸钠水溶液,过滤、烘干;洗涤、烘干即得接枝改性PET纤维。
步骤1)所述PET纤维的纤度为1-2dtex,长度为30-40mm;所述碱液种类没有特别的限制,本领域常用即可,包括但不限于氢氧化钠溶液、氢氧化钾溶液,所述碱液的浓度为10-20wt%,所述反应时间为0.5-1.5h;所述酸液没有特别的限制,本领域常用即可,包括但不限于盐酸溶液、醋酸溶液、硫酸溶液中的一种或两种及以上的组合;所述洗涤为用去离子水洗涤1-5次;
步骤2)所述催化剂为路易斯酸,选自FeCl3·6H2O、AlCl3·6H2O、SnCl4·5H2O、ZnCl2中的一种或两种及以上的组合,所述催化剂的水溶液中催化剂的浓度为3-7wt%,浸泡催化剂溶液的时间为5-15min,烘干温度为50-80℃、时间为1-3h;所述透明质酸钠溶液的浓度为6-15wt%,优选10-15wt%,浸泡于透明质酸钠溶液时间为10-30min,浸泡后的烘干温度为100-150℃,时间为20-60min;所述洗涤为用去离子水对纤维表面残留的催化剂和未反应的多羟基高分子进行冲洗去除,洗涤次数为1-5次,最后烘干温度为50-80℃,时间为6-12h。
步骤1)为PET纤维在碱性水溶液中水解反应,使纤维表面产生-COOH,步骤2)为纤维表面的-COOH在路易斯酸催化下与多羟基高分子上的-OH发生酯化反应,通过形成酯键将多羟基高分子接枝到PET纤维的表面,步骤2)酯化反应在无溶剂水的条件下进行以减少PET纤维的进一步水解。
所述载体的上、下层平方克重为20-50,所述载体的平方克重为40-100。
本发明还提供了上述多片装婴儿手口湿巾的制备方法,包括如下步骤:
将两层纤维原料分别经过开松,梳理成网,复合,预湿、压实,水刺加固,烘干,卷曲,杀菌,分切制备载体;将湿巾液经浸渍或喷涂工艺附着在载体上,包装,即得所述多片装婴儿手口湿巾。
所述包装为1-100片湿巾折叠封装入一个包装袋或包装盒中。
与现有技术相比,本发明的有益效果是:
本发明通过酯化反应将透明质酸钠接枝到PET纤维的表面,并以接枝改性PET纤维作为载体的上层,其他纤维原料为下层原料制备载体,这种载体含液量高,在湿巾液组成简单,且满足对婴儿皮肤温和无刺激、毒理安全性良好、可入口的前提下,能显著提高湿巾的清洁能力。
发明人还发现用透明质酸钠接枝改性的PET纤维,长期放置,抑菌率和溢液率的变化趋势较小,这是由载体结构和性能的改进所带来的。
具体实施方式
下面结合具体实施例对本发明作进一步的说明,但并不局限于说明书上的内容。若无特殊说明,本发明实施例中所述“份”均为重量份。所用试剂均为本领域可商购的试剂。
透明质酸钠购自上海诗梵生物科技有限公司,重均分子量为8000。
PET纤维购自中石化仪征化纤有限公司,纤度为1.56dtex,长度为38mm。
粘胶纤维购自唐山三友集团兴达化纤有限公司,纤度为1.67dtex,长度为38mm。
制备接枝改性PET纤维
制备例b1
1)将PET纤维浸泡入浓度为18wt%的氢氧化钠溶液中,升温至回流状态,恒温搅拌进行反应1h,反应结束后滴加15wt%的稀盐酸中和至中性,过滤、用去离子水洗涤3次、60℃烘干6h至恒重,备用;
2)将步骤1)所得纤维浸泡于AlCl3·6H2O浓度为7wt%的水溶液中10min,过滤、60℃烘干3h;将烘干的纤维浸泡于透明质酸钠浓度为15wt%的水溶液中,过滤、150℃烘干60min;去离子水洗涤3次、60℃烘干12h即得接枝改性PET纤维。
制备例b2
其余与实施例1相同,不同之处在于步骤2)透明质酸钠水溶液浓度为10wt%。
制备例b3
其余与实施例1相同,不同之处在于步骤2)透明质酸钠水溶液浓度为5wt%。
对比制备例b1
其余与实施例1相同,不同之处在于用羟乙基纤维素替代透明质酸钠。
制备多片装婴儿手口湿巾
实施例1
将制备例b1制备的接枝改性PET纤维开松,交叉铺叠形成梳理成网,纤维网的平方克重为20;
将粘胶纤维开松,交叉铺叠形成梳理成网,纤维网的平方克重为20;
按从上至下顺序,将上层接枝改性PET纤维网与下层粘胶纤维纤维网复合,复合网经预湿装置预湿、压实,在水刺机内经过三道正反面水刺加固,水刺压力分别为75bar、110bar、75bar,使上、下层纤维网之间相互缠结并复合为一体,120℃烘干至恒重、自然冷却至室温,卷曲,紫外杀菌,分切为140mm×185mm尺寸得到水刺非织造载体;
将0.1份山梨酸钾、0.1份脱氢乙酸钠、0.5份苯甲酸钠、1份葡萄糖酸内酯、1份柠檬酸钠,纯净水补全使湿巾液为100份;载体浸渍湿巾液至吸附饱和,取出,将80片浸液的载体折叠封装入一个包装袋中,即得多片装婴儿手口湿巾。
实施例2-3
其余与实施例1相同,不同之处在于,接枝改性PET纤维网的原料分别对应于由制备例b2-b3制备。
实施例4
其余与实施例1相同,不同之处在于,0.2份山梨酸钾代替0.1份山梨酸钾、0.1份脱氢乙酸钠。
实施例5
其余与实施例1相同,不同之处在于,湿巾液中脱氢乙酸钠的用量为0.2份,山梨酸钾用量为0。
对比实施例1
其余与实施例1相同,不同之处在于上层为未经改性的PET纤维。
对比实施例2
其余与实施例1相同,不同之处在于,接枝改性PET纤维网的原料对应于由对比制备例b1所制备。
将制备例b1-3、对比制备例b1制备的接枝改性PET纤维进行以下性能测试:
接枝率:按下式计算接枝率,
G=(m1-m0)/m0×100%
式中,m1为接枝改性PET纤维的质量,m0为PET纤维的质量。
将上述实施例1-5级对比实施例1-2制备的多片装婴儿手口湿巾进行以下性能测试:
平均溢液量:将实施例或对比实施例制备的多片装婴儿手口湿巾静置一周,然后取出堆垛最上部20片和最下部20片进行称重,按下式进行计算每包湿巾的溢液量,每实施例或对比实施例批次湿巾随机取3包,称量计算溢液量的平均值作为该批次的平均溢液量,
Bi=(Wi-Wi0)/Wi0×100%
式中,Bi为第i包湿巾的溢液量,i=1、2、3;Wi为第i包湿巾最下部20片湿巾重,g;Wi0为第i包湿巾最上部20片湿巾重,g。
湿巾的防腐效能测试:测试方法参考《欧洲药典》EP 10.0,5.1.3,检测菌种为:金黄色葡萄球菌(ATCC 6538)、大肠杆菌(ATCC 8739)、绿脓杆菌(ATCC 9027)、白色念珠菌(ATCC 10231)、巴西曲霉(ATCC 16404),将数量级为108这5种菌种接种到湿巾上,经过28天观察湿巾对这些菌种的杀灭率以评判此湿巾的防腐效能,欧洲药典的标准要求为:接种三种细菌(金黄色葡萄球菌、大肠杆菌、绿脓杆菌)后,经过14天,细菌对数减少值至少为3(即细菌数量至少减少103),经过28天细菌不增长(即细菌数量减少值不少于14天的减少数量);接种两种真菌(白色念珠菌、巴西曲霉)后,经过14天,真菌对数减少值至少为1(即真菌数量至少减少10),经过28天真菌不增长(即真菌数量减少值不少于14天的减少数量);
表1
项目 | 接枝率wt% |
制备例b1 | 7.5 |
制备例b2 | 5.1 |
制备例b3 | 4.0 |
对比制备例b1 | 7.5 |
表2
将实施例制得的湿巾进行一次完整皮肤刺激试验:结果显示,制得的湿巾对皮肤无刺激,充分体现了食品级防腐剂在湿巾产品中的安全性,符合消毒技术规范的要求。由表2可以看出本发明制备的湿巾具有良好的防腐稳定性。此外发明人还发现用透明质酸钠接枝改性的PET纤维能显著减少湿巾溢液量,防止湿巾长时间放置,溶液因重力影响持续下沉,导致上层湿巾溶液少非常干,而下层湿巾溶液多,严重影响体验感,解决了目前常规湿巾普遍存在的问题。由抑菌性能测试可以看出抑菌率的变化趋势与平均溢液量近似,说明本发明湿巾的抑菌性能受湿巾液的流失影响较大。
上述详细说明是针对本发明其中之一可行实施例的具体说明,该实施例并非用以限制本发明的专利范围,凡未脱离本发明所为的等效实施或变更,均应包含于本发明技术方案的范围内。
Claims (7)
1.一种婴儿手口湿巾,所述湿巾包括湿巾液、载体,其特征在于,所述湿巾液包括如下重量份的原料:0.05-0.5份山梨酸钾、0.03-0.3份脱氢乙酸钠、0.1-0.5份苯甲酸钠、0.1-1份葡萄糖酸内酯、0.1-1份柠檬酸钠,其余为纯净水,原料总和为100份;所述载体为双层结构非织造布,上层为接枝改性PET纤维,下层纤维原料选自粘胶纤维、PET纤维、木浆纤维、竹纤维中的一种或两种及以上的组合,所述载体通过双层纤维原料分别梳理成网复合后,进行水刺加固得到;所述接枝改性PET纤维的接枝改性剂为透明质酸钠,接枝率为3-7.5wt%;
所述接枝改性PET纤维通过包括如下步骤的方法制得:
1)将PET纤维浸泡入碱液中,升温至回流状态,恒温搅拌进行反应,反应结束后加入酸液中和至中性,过滤、洗涤、烘干,备用;
2)将步骤1)所得纤维浸泡于催化剂的水溶液,过滤、烘干;将烘干的纤维浸泡于透明质酸钠水溶液,过滤、烘干;洗涤、再烘干即得接枝改性PET纤维;
步骤2)所述催化剂为路易斯酸,选自FeCl3•6H2O、AlCl3•6H2O、SnCl4•5H2O、ZnCl2中的一种或两种及以上的组合。
2.权利要求1所述婴儿手口湿巾,其特征在于,所述透明质酸钠的重均分子量为10000以下。
3.权利要求1所述婴儿手口湿巾,其特征在于,步骤1)所述PET纤维的纤度为1-2dtex,长度为30-40mm;所述碱液的浓度为10-20wt%,所述反应的时间为0.5-1.5h。
4.权利要求1所述婴儿手口湿巾,其特征在于,步骤2)所述催化剂的水溶液浓度为3-7wt%,浸催化剂水溶液的时间5-15min,浸催化剂水溶液后烘干温度为50-80℃、时间为1-3h;所述透明质酸钠水溶液的浓度为6-15wt%,浸透明质酸钠水溶液后的时间为10-30min,浸催化剂水溶液后烘干温度为100-150℃,时间为20-60min。
5.权利要求1所述婴儿手口湿巾,其特征在于,所述载体的上层平方克重为20-50,下层的平方克重为20-50,所述载体的平方克重为40-100。
6.权利要求1-5任一项所述婴儿手口湿巾的制备方法,其特征在于,包括如下步骤:
将两层纤维原料分别经过开松,梳理成网,复合,预湿、压实,水刺加固,烘干,卷曲,杀菌,分切制备载体;将湿巾液经浸渍或喷洒工艺附着在载体上,包装,即得所述婴儿手口湿巾。
7.权利要求6所述婴儿手口湿巾的制备方法,其特征在于,所述包装为1-100片湿巾折叠封装入一个包装袋或包装盒中。
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