CN107419434B - 一种无防腐剂无纺布面膜的制备方法 - Google Patents
一种无防腐剂无纺布面膜的制备方法 Download PDFInfo
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- CN107419434B CN107419434B CN201710701178.2A CN201710701178A CN107419434B CN 107419434 B CN107419434 B CN 107419434B CN 201710701178 A CN201710701178 A CN 201710701178A CN 107419434 B CN107419434 B CN 107419434B
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- Prior art keywords
- woven fabrics
- facial mask
- preparation
- fabrics facial
- alginate fibre
- Prior art date
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- 239000000835 fiber Substances 0.000 claims abstract description 101
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical class O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims abstract description 50
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- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 claims abstract description 11
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- BIVBRWYINDPWKA-VLQRKCJKSA-L Glycyrrhizinate dipotassium Chemical compound [K+].[K+].O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@H]1CC[C@]2(C)[C@H]3C(=O)C=C4[C@@H]5C[C@](C)(CC[C@@]5(CC[C@@]4(C)[C@]3(C)CC[C@H]2C1(C)C)C)C(O)=O)C([O-])=O)[C@@H]1O[C@H](C([O-])=O)[C@@H](O)[C@H](O)[C@H]1O BIVBRWYINDPWKA-VLQRKCJKSA-L 0.000 claims abstract description 7
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- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims description 5
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 4
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- 238000011068 loading method Methods 0.000 claims description 2
- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 claims 1
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- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 7
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- 229920000742 Cotton Polymers 0.000 description 2
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
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- KCIDZIIHRGYJAE-YGFYJFDDSA-L dipotassium;[(2r,3r,4s,5r,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl] phosphate Chemical compound [K+].[K+].OC[C@H]1O[C@H](OP([O-])([O-])=O)[C@H](O)[C@@H](O)[C@H]1O KCIDZIIHRGYJAE-YGFYJFDDSA-L 0.000 description 2
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- 244000146553 Ceiba pentandra Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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Classifications
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/54—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/203—Unsaturated carboxylic acids; Anhydrides, halides or salts thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
- D06M13/21—Halogenated carboxylic acids; Anhydrides, halides or salts thereof
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Abstract
本发明属于面膜材料技术领域,具体涉及一种无防腐剂无纺布面膜的制备方法。本发明采用聚酯纤维、改性壳聚糖纤维和改性海藻纤维作为无纺布面膜基材配合由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成的柔软剂和由野菊维素和甘草酸二钾按质量比4:1组成的抗敏剂制备的无纺布面膜,并在常温常压、氧化性气体介质和低辐照吸收剂量的条件下进行辐照灭菌。本发明的技术优势在于:本发明无纺布面膜具有高吸湿性、透气性和低刺激性,对无纺布面膜进行辐照灭菌能有效降低菌种的繁殖力从而有利于无纺布面膜的保存,同时免除防腐剂的添加对人体皮肤的潜在危害。
Description
技术领域
本发明属于面膜材料技术领域,具体涉及一种无防腐剂无纺布面膜的制备方法。
背景技术
面膜是成年女性生活中必不可少的美白用品,面膜的材质有多种,其中无纺布由于价格较低,应用非常广泛。无纺布作为面膜、卸妆纸、湿巾等产品的基材,要求其具有高度的吸湿性和湿态下的韧性。对于面膜高端产品来说,还要具有相当的通透性以及与皮肤的贴合性。市场上流行的面膜布多为30-70g厚度的混纺无纺布,此种方法制成的面膜布因缺乏回复性,产品表面硬挺,不能和脸部紧密贴合。由于涤纶纤维、粘胶纤维制成的面膜布松软易变形,湿水经美容液浸泡后面膜易变形。另外由于生产无纺布的工厂多为纺织企业,车间环境卫生条件较差,无纺布的含菌量较高,一般化妆品生产企业在无纺布制成脸部形状后需要先进性杀菌处理,通常采用射线辐照,而在膜液和无纺布罐装后一般不宜用射线辐照,因为γ射线会使一些营养成分变色,无纺布面膜的最大问题是敷在脸上有刺痛感,一般是由防腐剂引起,所以而膜内液中要加入一些抗刺激的成分,如红没药醇,更有效的可能是一些天然植物提取液,在防腐剂的选择上要考究,不能一味强调抑菌。
中国专利申请CN1298972A公开了一种甲壳质纤维水刺无纺布及其生产方法,其选用甲壳素纤维和其他基础纤维,经称重、开松、机械梳理、杂乱成网、水刺缠结等工序,使其形成具有一定强力和致密度的三维空间结构,再在一定温度下烘干而成,该甲壳素无纺布具有抗菌消炎的功效,不易脱水收缩,缺点是强度太低面膜布容易扯烂。
中国专利申请CN102493124A公开了一种绢丝棉混纺水刺无纺布的生产方法,其采用盖板式梳棉机取代无纺生产线传统使用的梳理机,通过对纤维进行充分梳理后,进行预湿、水刺缠结。存在的问题是:充分处理后生产的无纺布在湿态下的韧性和贴肤性不高,制成的面膜在使用时,使用者的面部必须保持静止,一旦有面部张弛动作,就会造成面膜脱离皮肤;制造出的无纺布的通透性不高,不能满足面膜中美容液的高渗透的要求。
发明内容
为解决现有无纺布面膜存在添加防腐剂对人皮肤产生刺激、吸湿-保湿和透气性差的问题,本发明提供一种无防腐剂无纺布面膜的制备方法。
本发明一种无防腐剂无纺布面膜的制备方法,包括以下步骤:
S1、取聚酯纤维30-40份、改性壳聚糖纤维10-20份和改性海藻纤维20-30份装入40-60℃的高速混料机中共混10-20min后,通过120-240℃的双螺杆挤出机加热熔融30-50min,拉伸成丝后铺设成网并热轧成型,得网布;
S2、将柔软剂、抗敏剂和水按质量比1:4:20配制后搅拌并加热至50-70℃,均匀涂在步骤S1得到的网布上,烘干得无纺布粗品;
S3、将步骤S2得到的无纺布粗品放入纸箱,在常温常压下用60Co-γ射线在含氧气体中进行辐照处理,辐照吸收剂量为2-3kGy;
S4、将步骤S3辐照处理后的无纺布面膜经过分切机分切包装,即得。
优选的,步骤S1所述的改性壳聚糖纤维的制备方法为:
(1)取壳聚糖120-180g和聚乙烯醇70-80g,溶于400-500ml水中,加入氧化海藻酸钠20-30g搅拌均匀,真空脱泡16-20h后在凝固浴中30-40℃下纺丝,得壳聚糖纤维;
(2)将步骤(1)得到的壳聚糖纤维加入到质量浓度为3-5%的2,3-环氧丙基三甲基氯化铵的乙醇溶液中,于80-90℃下反应5-7h后洗涤烘干,即得。
优选的,步骤S1所述的改性海藻纤维的制备方法为:
1)取海藻纤维200-400g加入800-1000ml质量分数为25%的氢氧化钠溶液中,浸泡15-25min后取出海藻纤维并挤干,得碱化处理的海藻纤维;
2)取醚化液400-600ml预热至40-48℃后加入步骤1)碱化处理的海藻纤维,搅拌并加热至50-60℃反应30-50min后冷却至室温,得醚化海藻纤维;
3)将步骤2)所得醚化海藻纤维用质量分数30%的醋酸溶液洗涤,烘干,即得。
优选的,步骤2)所述的醚化液由氯乙酸钠、氢氧化钠、水和乙醇按质量比5:8:15:90组成。
优选的,步骤S2中所述的柔软剂由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成。
优选的,步骤S2中所述的抗敏剂由野菊维素和甘草酸二钾按质量比4:1组成。
优选的,步骤S3中所述的无纺布面膜与60Co中心的距离为0.9-1.2m。
优选的,步骤S3中所述的含氧气体由氧气和氮气按体积比3:1组成。
再优选的,步骤S3所述的辐照吸收剂量为2.5kGy。
海藻纤维是采用天然海藻中所提取的物质加工而成,由于原料来自天然海藻因而具有良好的生物相容性、可降解吸收性、生物相容性等特殊功能,本发明对海藻纤维进行化学改性,引入吸水性基团,使其具有吸水性和成胶性。
本发明改性壳聚糖纤维是在壳聚糖分子单元的游离氨基上接上了季铵化基团,使其带有正电荷,从而增强与细菌细胞壁表面的酸性高分子的相互作用,在细胞周围形成不具有渗透性的表层,阻止营养物质透过细胞壁使细菌不能进行新陈代谢,从而实现杀灭细菌的目的。此外壳聚糖材料没有毒性,经过季铵化改性后也没有毒性,本发明在实现季铵化改性的过程中,在壳聚糖纤维单元上的游离氨基接上季铵化基团而带上正电荷,一方面加强了材料的抗菌性能,另一方面还改善了纤维的亲水性能使纤维亲水,增加这种纤维制成的无纺布的吸湿性。
甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂性能稳定,具有优良的生物降解性,更具有抗黄变、杀菌等多项功能。
所述的甘油醚季铵盐型柔软剂的制备方法为:
(a)在250ml三口烧瓶中加入0.15ml十二醇、0.15ml十四醇、0.15mol环氧氯丙烷、0.12mol氢氧化钾、0.006mol四丁基硫酸氢铵和15ml甲苯,升温至55℃搅拌反应5h,冷却至室温抽滤,固相以15ml甲苯洗涤3次,旋转蒸馏,得烷氧基缩水甘油醚粗品;
(b)在250ml三口烧品中加入步骤(a)制备的烷氧基缩水甘油醚粗品0.15ml、三乙胺盐酸盐0.15mol和乙醇60ml,35℃搅拌反应4h,蒸出乙醇和水后用乙酸乙酯重结晶,真空干燥即得。
辐照灭菌的原理是微生物细胞间质受到高能电子射线照射后发生的电离作用和化学作用,或者是产品中的水分、有机化合物在高能射线作用下会产生自由基、氧化性物质与微生物细胞内物质发生反应,影响微生物的活动及生殖性能,进一步导致微生物死亡,目前辐照过程被认为是一种物理过程,其中任何食品、药品当其总体平均吸收剂量不超过10kGy时,不需再做毒性试验,营养学和微生物学上也是安全的。
本发明实施例1-3制备的无防腐剂无纺布面膜很好的柔软性、吸湿性和透气性;对金黄色葡萄球菌、酵母菌和黑曲霉菌具有很好的杀灭效果。与现有技术相比,本发明的技术优势在于:本发明采用聚酯纤维、改性壳聚糖纤维和改性海藻纤维作为基材配合由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成的柔软剂和由野菊维素和甘草酸二钾按质量比4:1组成的抗敏剂制备的无纺布面膜具有更好的柔软性、吸湿性、透气性和无刺激性。
具体实施方式
下面通过具体实施例对本发明做进一步详细说明,这些实施例仅用于例证的目的,绝不限制本发明的保护范围。
聚酯纤维购自扬州天伦纤维有限公司;棉纤维购自德州方元钢棉纤维有限公司;双酯基季铵盐柔软剂购自东莞市嘉宏有机硅科技有限公司。
实施例1一种无防腐剂无纺布面膜的制备方法
所述的无防腐剂无纺布面膜的制备方法为:
S1、取聚酯纤维30份、改性壳聚糖纤维10份和改性海藻纤维20份装入40℃的高速混料机中共混10min后,通过120℃的双螺杆挤出机加热熔融30min,拉伸成丝后铺设成网并热轧成型,得网布;
S2、将由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成的柔软剂、由野菊维素和甘草酸二钾按质量比4:1组成的抗敏剂和水按质量比1:4:20配制后搅拌并加热至50℃,均匀涂在步骤S1得到的网布上,烘干得无纺布粗品;
S3、将步骤S2得到的无纺布粗品放入纸箱,在常温常压下用60Co-γ射线在由氧气和氮气按体积比3:1组成的含氧气体中进行辐照处理,无纺布面膜与60Co中心的距离为0.9m,辐照吸收剂量为2kGy;
S4、将步骤S3辐照处理后的无纺布面膜经过分切机分切包装,即得。
所述的改性壳聚糖纤维的制备方法为:
(1)取壳聚糖120g和聚乙烯醇70g,溶于400ml水中,加入氧化海藻酸钠20g搅拌均匀,真空脱泡16h后在凝固浴中30℃下纺丝,得壳聚糖纤维;
(2)将步骤(1)得到的壳聚糖纤维加入到质量浓度为3%的2,3-环氧丙基三甲基氯化铵的乙醇溶液中,于80℃下反应5h后洗涤烘干,即得。
所述的改性海藻纤维的制备方法为:
1)取海藻纤维200g加入800ml质量分数为25%的氢氧化钠溶液中,浸泡15min后取出海藻纤维并挤干,得碱化处理的海藻纤维;
2)取由氯乙酸钠、氢氧化钠、水和乙醇按质量比5:8:15:90组成的醚化液400ml预热至40℃后加入步骤1)碱化处理的海藻纤维,搅拌并加热至50℃反应30min后冷却至室温,得醚化海藻纤维;
3)将步骤2)所得醚化海藻纤维用质量分数30%的醋酸溶液洗涤,烘干,即得。
实施例2一种无防腐剂无纺布面膜的制备方法
所述的无防腐剂无纺布面膜的制备方法为:
S1、取聚酯纤维35份、改性壳聚糖纤维15份和改性海藻纤维25份装入50℃的高速混料机中共混15min后,通过180℃的双螺杆挤出机加热熔融40min,拉伸成丝后铺设成网并热轧成型,得网布;
S2、将由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成的柔软剂、由野菊维素和甘草酸二钾按质量比4:1组成的抗敏剂和水按质量比1:4:20配制后搅拌并加热至60℃,均匀涂在步骤S1得到的网布上,烘干得无纺布粗品;
S3、将步骤S2得到的无纺布粗品放入纸箱,在常温常压下用60Co-γ射线在由氧气和氮气按体积比3:1组成的含氧气体中进行辐照处理,无纺布面膜与60Co中心的距离为1.05m,辐照吸收剂量为2.5kGy;
S4、将步骤S3辐照处理后的无纺布面膜经过分切机分切包装,即得。
所述的改性壳聚糖纤维的制备方法为:
(1)取壳聚糖150g和聚乙烯醇75g,溶于450ml水中,加入氧化海藻酸钠25g搅拌均匀,真空脱泡18h后在凝固浴中35℃下纺丝,得壳聚糖纤维;
(2)将步骤(1)得到的壳聚糖纤维加入到质量浓度为4%的2,3-环氧丙基三甲基氯化铵的乙醇溶液中,于85℃下反应6h后洗涤烘干,即得。
所述的改性海藻纤维的制备方法为:
1)取海藻纤维300g加入900ml质量分数为25%的氢氧化钠溶液中,浸泡20min后取出海藻纤维并挤干,得碱化处理的海藻纤维;
2)取由氯乙酸钠、氢氧化钠、水和乙醇按质量比5:8:15:90组成的醚化液500ml预热至44℃后加入步骤1)碱化处理的海藻纤维,搅拌并加热至55℃反应40min后冷却至室温,得醚化海藻纤维;
3)将步骤2)所得醚化海藻纤维用质量分数30%的醋酸溶液洗涤,烘干,即得。
实施例3一种无防腐剂无纺布面膜的制备方法
所述的无防腐剂无纺布面膜的制备方法为:
S1、取聚酯纤维40份、改性壳聚糖纤维20份和改性海藻纤维30份装入60℃的高速混料机中共混20min后,通过240℃的双螺杆挤出机加热熔融50min,拉伸成丝后铺设成网并热轧成型,得网布;
S2、将由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成的柔软剂、由野菊维素和甘草酸二钾按质量比4:1组成的抗敏剂和水按质量比1:4:20配制后搅拌并加热至70℃,均匀涂在步骤S1得到的网布上,烘干得无纺布粗品;
S3、将步骤S2得到的无纺布粗品放入纸箱,在常温常压下用60Co-γ射线在由氧气和氮气按体积比3:1组成的含氧气体中进行辐照处理,无纺布面膜与60Co中心的距离为1.2m,辐照吸收剂量为3kGy;
S4、将步骤S3辐照处理后的无纺布面膜经过分切机分切包装,即得。
所述的改性壳聚糖纤维的制备方法为:
(1)取壳聚糖180g和聚乙烯醇80g,溶于500ml水中,加入氧化海藻酸钠30g搅拌均匀,真空脱泡20h后在凝固浴中40℃下纺丝,得壳聚糖纤维;
(2)将步骤(1)得到的壳聚糖纤维加入到质量浓度为5%的2,3-环氧丙基三甲基氯化铵的乙醇溶液中,于90℃下反应7h后洗涤烘干,即得。
所述的改性海藻纤维的制备方法为:
1)取海藻纤维400g加入1000ml质量分数为25%的氢氧化钠溶液中,浸泡25min后取出海藻纤维并挤干,得碱化处理的海藻纤维;
2)取由氯乙酸钠、氢氧化钠、水和乙醇按质量比5:8:15:90组成的醚化液600ml预热至48℃后加入步骤1)碱化处理的海藻纤维,搅拌并加热至60℃反应50min后冷却至室温,得醚化海藻纤维;
3)将步骤2)所得醚化海藻纤维用质量分数30%的醋酸溶液洗涤,烘干,即得。
对比例1一种无防腐剂无纺布面膜的制备方法
对比例1无防腐剂无纺布面膜的制备方法和改性海藻纤维的制备方法与实施例2类似。
对比例1与实施例2的区别在于:将改性壳聚糖纤维替换为棉纤维。
对比例2一种无防腐剂无纺布面膜的制备方法
对比例2无防腐剂无纺布面膜的制备方法、改性壳聚糖纤维和改性海藻纤维的制备方法与实施例2类似。
对比例2与实施例2的区别在于:步骤S2中所述的柔软剂由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比1:1组成。
对比例3一种无防腐剂无纺布面膜的制备方法
对比例3无防腐剂无纺布面膜的制备方法、改性壳聚糖纤维和改性海藻纤维的制备方法与实施例2类似。
对比例3与实施例2的区别在于:步骤S2中所述的抗敏剂由野菊维素和甘草酸二钾按质量比1:1组成。
试验例1:拉伸性能及亲水性能测试
1.试验材料:实施例1-3和对比例1-3制备的无防腐剂无纺布面膜。
2.试验方法:分别取实施例1-3和对比例1-3制备方法的无防腐剂无纺布面膜试样各5g用水浸泡后取出称重,按下式计算吸水率:吸水率=洗水后的试样重量/试样重量×100%。
其他性能测试:强力、透气性和柔软性分别参照GB/T3923.1-1997、GB/T5453-1997和ZBW04003-87进行测试(项目为断裂强力、透气性和抗弯长度),结果如表1所示。
表1实施例和对比例面膜拉伸性能及亲水性能指标
组别 | 实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 | 对比例3 |
吸水率(%) | 169.8 | 175.8 | 165.9 | 145.9 | 151.2 | 150.6 |
强力(N) | 51.24 | 54.25 | 52.12 | 48.23 | 47.96 | 48.12 |
透湿性(g/24h) | 3.32 | 3.41 | 3.34 | 3.12 | 3.09 | 3.11 |
透气性(L/m<sup>2</sup>/s) | 3341 | 3468 | 3328 | 3125 | 3205 | 3245 |
从表1可以看出,本发明实施例1-3制备的无防腐剂无纺布面膜较对比例1-3具有更高的吸水率、更大的抗拉力和更好的透湿性和透气性,说明本发明采用聚酯纤维、改性壳聚糖纤维和改性海藻纤维为基材配合柔软剂、抗敏剂制备的无纺布面膜具有高吸湿性、高保湿性和透气性,且实施例2制得的无防腐剂无纺布面膜的吸水率最高,且强力、透湿性和透气性较实施例1和实施例3更高,说明实施例2所采用的无防腐剂无纺布面膜的制备过程以及改性壳聚糖纤维和改性海藻纤维的制备方法中所采用的的参数为本发明的优选参数,实施例2为本发明的优选实施例。
试验例2:杀菌效果测试
1.试验材料:实施例1-3和对比例1制备的无防腐剂无纺布面膜。
2.试验对象:金黄色葡萄球菌、酵母菌和黑曲霉菌。
3.试验方法:将按照GB4789-2010方法进行微生物检测,经实施例1-3与对比例1制备的无防腐剂无纺布面膜进行微生物检测,计算杀菌率,结果如表2所示。
表2实施例和对比例面膜杀菌效果
组别 | 实施例1 | 实施例2 | 实施例3 | 对比例1 |
金黄色葡萄球菌 | 98.3% | 99.2% | 98.7% | 90.2% |
酵母菌 | 97.9% | 99.4% | 98.9% | 88.9% |
黑曲霉菌 | 96.9% | 98.8% | 97.8% | 87.5% |
从表2可以看出,本发明实施例1-3制备的无防腐剂无纺布面膜较对比例1制备的无纺布面膜对金黄色葡萄球菌、酵母菌和黑曲霉菌具有更高的杀菌率,说明本发明采用聚酯纤维、改性壳聚糖纤维和改性海藻纤维为基材配合在适宜的温度、压力和氧含量的条件下对无纺布面膜进行的辐照灭菌,对金黄色葡萄球菌、酵母菌和黑曲霉菌具有很好的杀灭效果。
试验例3:产品使用性能评价
1.试验材料:实施例1-3和对比例1-3制备的无防腐剂无纺布面膜。
2.试验对象:120名志愿者。
3.试验方法:将120名志愿者平均分为6组,分别使用本发明实施例1-3和对比例1-3制备的无防腐剂无纺布面膜,分别对面膜的柔软性、吸湿性、透气性、贴肤性和刺激性等性能进行感官评价(评分范围0-10,评分越高表示所用无纺布面膜的柔软性、吸湿性、透气性和贴肤性越好,刺激性越小),结果如表3所示。
表3实施例和对比例无防腐剂无纺布面膜性能评分
组别 | 实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 | 对比例3 |
柔软性 | 9.1 | 9.6 | 9.3 | 8.6 | 7.4 | 8.5 |
吸湿性 | 9.3 | 9.8 | 9.2 | 8.1 | 8.6 | 8.2 |
透气性 | 9.1 | 9.7 | 9.3 | 8.2 | 8.5 | 8.4 |
贴肤性 | 9.1 | 9.6 | 9.2 | 8.5 | 8.2 | 8.6 |
刺激性 | 9.0 | 9.6 | 9.1 | 8.2 | 8.4 | 7.6 |
从表3可以看出,本发明实施例1-3较对比例1-3产品柔软性、吸湿性、透气性、贴肤性和刺激性评分更高,说明本发明实施例1-3制备的无纺布面膜柔软性、吸湿性、透气性和贴肤性好、刺激性小,另外可以看出对比例2制备的无纺布面膜的柔软性评分明显低于实施例1-3,对比例3制备的无纺布面膜的刺激性评分也明显低于实施例1-3,说明本发明采用聚酯纤维、改性壳聚糖纤维和改性海藻纤维作为无纺布面膜基材配合由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成柔软剂和由野菊维素和甘草酸二钾按质量比4:1组成抗敏剂制备的无纺布面膜具有更好的柔软性、吸湿性、透气性、贴肤性和无刺激性。
以上仅是本发明的优选实施方式,应当指出的是上述优选实施方式不应视为对本发明的限制,本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说,在不脱离本发明的精神和范围内,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (8)
1.一种无防腐剂无纺布面膜的制备方法,其特征在于,包括以下步骤:
S1、取聚酯纤维30-40份、改性壳聚糖纤维10-20份和改性海藻纤维20-30份装入40-60℃的高速混料机中共混10-20min后,通过120-240℃的双螺杆挤出机加热熔融30-50min,拉伸成丝后铺设成网并热轧成型,得网布;
S2、将柔软剂、抗敏剂和水按质量比1:4:20配制后搅拌并加热至50-70℃,均匀涂在步骤S1得到的网布上,烘干得无纺布粗品;
S3、将步骤S2得到的无纺布粗品放入纸箱,在常温常压下用60Co-γ射线在含氧气体中进行辐照处理,辐照吸收剂量为2-3kGy;
S4、将步骤S3辐照处理后的无纺布面膜经过分切机分切包装,即得。
2.根据权利要求1所述的无防腐剂无纺布面膜的制备方法,其特征在于,步骤S1所述的改性壳聚糖纤维的制备方法为:
(1)取壳聚糖120-180g和聚乙烯醇70-80g,溶于400-500ml水中,加入氧化海藻酸钠20-30g搅拌均匀,真空脱泡16-20h后在凝固浴中30-40℃下纺丝,得壳聚糖纤维;
(2)将步骤(1)得到的壳聚糖纤维加入到质量浓度为3-5%的2,3-环氧丙基三甲基氯化铵的乙醇溶液中,于80-90℃下反应5-7h后洗涤烘干,即得。
3.根据权利要求1所述的无防腐剂无纺布面膜的制备方法,其特征在于,步骤S1所述的改性海藻纤维的制备方法为:
1)取海藻纤维200-400g加入800-1000ml质量分数为25%的氢氧化钠溶液中,浸泡15-25min后取出海藻纤维并挤干,得碱化处理的海藻纤维;
2)取醚化液400-600ml预热至40-48℃后加入步骤1)碱化处理的海藻纤维,搅拌并加热至50-60℃反应30-50min后冷却至室温,得醚化海藻纤维;
3)将步骤2)所得醚化海藻纤维用质量分数30%的醋酸溶液洗涤,烘干,即得。
4.根据权利要求3所述的无防腐剂无纺布面膜的制备方法,其特征在于,步骤2)所述的醚化液由氯乙酸钠、氢氧化钠、水和乙醇按质量比5:8:15:90组成。
5.根据权利要求1所述的无防腐剂无纺布面膜的制备方法,其特征在于,步骤S2中所述的柔软剂由甘油醚季铵盐型柔软剂和双酯基季铵盐柔软剂按质量比2:3组成。
6.根据权利要求1所述的无防腐剂无纺布面膜的制备方法,其特征在于,步骤S2中所述的抗敏剂由野菊维素和甘草酸二钾按质量比4:1组成。
7.根据权利要求1所述的无防腐剂无纺布面膜的制备方法,其特征在于,步骤S3中所述的含氧气体由氧气和氮气按体积比3:1组成。
8.根据权利要求1所述的无防腐剂无纺布面膜的制备方法,其特征在于,步骤S3所述的辐照吸收剂量为2.5kGy。
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