CN113679618A - 一种凝胶化改性纤维静电纺丝面膜的制备方法 - Google Patents
一种凝胶化改性纤维静电纺丝面膜的制备方法 Download PDFInfo
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- CN113679618A CN113679618A CN202110888598.2A CN202110888598A CN113679618A CN 113679618 A CN113679618 A CN 113679618A CN 202110888598 A CN202110888598 A CN 202110888598A CN 113679618 A CN113679618 A CN 113679618A
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- electrostatic spinning
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- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 55
- 239000000835 fiber Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
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- 229920002678 cellulose Polymers 0.000 claims abstract description 25
- 239000001913 cellulose Substances 0.000 claims abstract description 25
- 238000005516 engineering process Methods 0.000 claims abstract description 15
- 230000001815 facial effect Effects 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 4
- 230000004048 modification Effects 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 3
- 239000010410 layer Substances 0.000 claims abstract 9
- 230000003020 moisturizing effect Effects 0.000 claims abstract 6
- 239000002346 layers by function Substances 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 32
- 239000003513 alkali Substances 0.000 claims description 29
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 22
- 239000003085 diluting agent Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000002243 precursor Substances 0.000 claims description 16
- 239000008213 purified water Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 230000003472 neutralizing effect Effects 0.000 claims description 15
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- 238000009987 spinning Methods 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 230000003113 alkalizing effect Effects 0.000 claims description 13
- 229920002385 Sodium hyaluronate Polymers 0.000 claims description 12
- 229940010747 sodium hyaluronate Drugs 0.000 claims description 12
- 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 compound [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 description 12
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 11
- 229930003268 Vitamin C Natural products 0.000 claims description 11
- DFPAKSUCGFBDDF-ZQBYOMGUSA-N [14c]-nicotinamide Chemical compound N[14C](=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-ZQBYOMGUSA-N 0.000 claims description 11
- 229940069521 aloe extract Drugs 0.000 claims description 11
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
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- 239000007924 injection Substances 0.000 claims description 3
- 238000001523 electrospinning Methods 0.000 claims 2
- 239000004480 active ingredient Substances 0.000 claims 1
- -1 aloe extract Chemical compound 0.000 claims 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims 1
- 238000001879 gelation Methods 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 3
- 241000894006 Bacteria Species 0.000 abstract description 2
- 241000233866 Fungi Species 0.000 abstract description 2
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- 229920000663 Hydroxyethyl cellulose Polymers 0.000 abstract description 2
- 238000009395 breeding Methods 0.000 abstract description 2
- 230000001488 breeding effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 2
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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Abstract
本发明公开了一种凝胶化改性纤维静电纺丝面膜的制备方法,此面膜的功能层包括凝胶保湿层和固态精华释放层,其中所述的凝胶保湿层采用天然纤维素原位凝胶化改性技术制备而成,所制备的凝胶化改性纤维无纺布凝胶是新型的无纺布凝胶,其主要成分是羟乙基纤维素。而固态精华释放层采用静电纺丝技术,将液态精华液制备成固态精华膜,解决了细菌与真菌的腐败滋生问题,从而提高了面膜的存储时间,又解决了使用过程中造成的精华液浪费和滴液问题。通过两种技术的有机结合制备出保湿性、敷贴性、便捷性俱佳的固态面膜,提高了面膜的使用效果。
Description
技术领域
本发明属于面膜领域,具体涉及一种凝胶化改性纤维静电纺丝面膜的制备方法。
背景技术
纤维素是地球上历史最悠久、储量最丰富的天然高分子。其取之不尽用之不竭,是人类最宝贵的天然可再生资源。纤维素化学与工业始于160多年前,是高分子化学诞生及发展时期的主要研究对象。目前,基布面膜大多数都是纤维素材质,然而纤维素柔顺性很差,敷贴性也不佳。因此需要对纤维素无纺布进行改性,增加其敷贴性和无纺布的柔顺性。在纤维素无纺布改性中,大多数人都是将其改性为羧甲基纤维素。如,发明专利CN109674721A公开了一种羧甲基纤维素面膜的制备方法,其使用先碱化再浸轧一氯乙酸的方法进行羧甲基纤维素的制备,然后将羧甲基纤维素通过静电纺丝纺制成无纺布,最后再加入面膜液,虽然面膜布敷贴性有所提高,但是制备过程过于繁琐复杂。
从吉尔伯特首次发现当液滴置于摩擦过的琥珀附近时,液滴的表面会变形为锥体的这一发现,到1934~1944年间,福姆哈尔斯发明了三种静电纺丝实验设备,再到1971年,鲍姆加登将可以批量生产丙烯酸纤维的设备的研制成,再到,如今世界各地对静电纺丝纳米纤维的研究掀起来了纳米科技热,静电纺丝这项技术已经发展了400多年。目前,无论是学术领域还是工业领域都普遍认为,静电纺丝技术是21世纪纳米纤维工业化最有希望的工艺方法。静电纺丝技术的发展,使得固态精华面膜变成了可能。
因此,一种制备简单、敷贴性佳、易存储、精华少浪费的面膜成为面膜企业和大众所追求的目标。
发明内容
本发明针对上述目前面膜制备过程中存在的问题,以及人们对使用更高端的面膜产品的需求,提供一种凝胶化改性纤维静电纺丝面膜的制备方法。本发明不仅使用了原位凝胶化改性纤维技术对纤维素无纺布进行了凝胶化改性,还使用静电纺丝技术对凝胶化改性无纺布进行了固态精华纳米纤维的制备,此两种技术结合在一起而制备的面膜,将面膜推向一个全新的高度,提供了全新的概念——凝胶化改性纤维静电纺丝面膜,为面膜制备技术的迭代升级提供了全新的可行性方案。
为解决上述的技术问题,满足上述的技术要求,本发明采用如下具体技术方案:
(1)无纺布纤维碱化:将42 g/m2天然纤维素无纺布完全浸入适量质量分数为10~40 %的碱液中,在30~55 ℃下,进行碱化15~35 min后,挤压干净无纺布中多余的碱液,备用;
(2)无纺布纤维醚化:在碱化反应后的干无纺布中低温加入具有稀释剂保护的醚化剂10~30 mL,在40~70 ℃下,进行醚化35~60 min后,加入pH中和液,将pH值调节至5.5~7.0,用75 %稀释剂水溶液洗涤3~5次,每次洗涤时间为15 min,最后用高温压干机压干且平整,备用;
(3)静电纺丝前驱液配置:将聚乙烯醇加入适量乙醇水溶液中,加热至95 ℃,搅拌直至溶解均匀,降温至40 ℃,再依次加入透明质酸钠和聚乙烯基吡咯烷酮,继续搅拌直至溶解均匀,继续降温至室温,再依次加入芦荟提取液、维生素C、烟酰胺,继续搅拌直至形成均相的纺丝前驱液;
(4)无纺布静电纺丝:将上述制备的凝胶化无纺布固定在静电纺丝接收器上,使用5~20 mL的注射抽取适量上述的纺丝前驱液,将注射器放在往复平台的注射器推进器上,进行静电纺丝制备纳米纤维后,得到凝胶化改性纤维静电纺丝面膜。
优选地,所述的碱液为氢氧化钾、氢氧化钠、三乙醇胺、尿素中两种以上的混合水溶液,所述的稀释剂为丙酮、异丙醇、叔丁醇中的一种,所述的醚化剂为环氧乙烷,所述的pH中和液为85 %磷酸、冰乙酸、盐酸中的一种。
优选地,所述的天然纤维素无纺布与所用碱液的质量比为1~3:96~100。
优选地,所述静电纺丝前驱液的成分组成,透明质酸钠1~5份、聚乙烯醇15~35份、聚乙烯基吡咯烷酮0.5~1.3份、烟酰胺3~5份、维生素C 0.5~1份、芦荟提取液5~10份、无水乙醇15~45份、纯化水30~60份,其中,无水乙醇与纯化水的体积比为1~3:2~4。
优选地,所述的静电纺丝的相关参数,高压直流电压为14~20 kV,纺丝距离10~20cm,注射器推进速率为 0.8~1.8 mL/h,针头型号为19~22 G,往复平台转轴转速为300~550rpm,接收器转速为400~550 rpm。
本发明所具有的有益效果如下:
本发明的天然纤维素无纺布凝胶化改性大幅改善了无纺布的柔顺性,从而提高了无纺布的面部敷贴性。与此同时,还增加了天然纤维素无纺布的保湿性以及润滑舒适性。本发明所进行的凝胶化改性纤维的无纺布凝胶是新型的无纺布凝胶,其主要成分为羟乙基纤维素。其无味无毒,溶于热水或冷水,高温或煮沸不沉淀,保湿性能佳。
本发明采用静电纺丝技术将液态精华液制备成固态精华膜,既解决了细菌与真菌的腐败滋生问题,从而提高了面膜的存储时间,又解决了使用过程中造成的精华液浪费和滴液问题。本发明中通过两种技术的有机结合,使得精华液的吸收更加充分,提高了面膜的使用效果。
具体实施例方式:
下面将结合具体实施例对本发明的技术方案进行进一步的描述。需理解为以下实施例仅为简明易懂的解释本发明,而不应被理解为对本发明保护范围的限制。凡基于本发明上述内容所应用的技术原理、技术整合和创新方法,均涵盖在本发明旨在保护的范围内。
本发明若未特指,以下实施例中所用原材料和试剂均为市场正规销售产品,或者可以通过已经熟知的方法进行常规制备。
实施例1
一种凝胶化改性纤维静电纺丝面膜的制备方法,所述方法包括如下具体步骤:
(1)无纺布纤维碱化:将42 g/m2天然纤维素无纺布完全浸入适量质量分数为10 %的碱液中,在40 ℃下,进行碱化15 min后,挤压干净无纺布中多余的碱液,备用;
(2)无纺布纤维醚化:在碱化反应后的干无纺布中低温加入具有稀释剂保护的醚化剂20 mL,在55 ℃下,进行醚化40 min后,加入pH中和液,将pH值调节至5.5~7.0,用75 %稀释剂水溶液洗涤3~5次,每次洗涤时间为15 min,最后用高温压干机压干且平整,备用;
(3)静电纺丝前驱液配置:将聚乙烯醇加入适量乙醇水溶液中,加热至95 ℃,搅拌直至溶解均匀,降温至40 ℃,再依次加入透明质酸钠和聚乙烯基吡咯烷酮,继续搅拌直至溶解均匀,继续降温至室温,再依次加入芦荟提取液、维生素C、烟酰胺,继续搅拌直至形成均相的纺丝前驱液;
(4)无纺布静电纺丝:将上述制备的凝胶化无纺布固定在静电纺丝接收器上,使用5~20 mL的注射抽取适量上述的纺丝前驱液,将注射器放在往复平台的注射器推进器上,进行静电纺丝制备纳米纤维后,得到凝胶化改性纤维静电纺丝面膜。
上述步骤 (1) 中,所述的碱液为氢氧化钠和三乙醇胺的混合水溶液,所述的天然纤维素无纺布与所用碱液的质量比为1:100。
上述步骤 (2) 中,所述的稀释剂为异丙醇,所述的醚化剂为环氧乙烷,所述的pH中和液为冰乙酸。
上述步骤 (3) 中,所述静电纺丝前驱液的成分组成,透明质酸钠2份、聚乙烯醇20份、聚乙烯基吡咯烷酮1份、烟酰胺3份、维生素C 0.6份、芦荟提取液7份、无水乙醇30份、纯化水45份,其中,无水乙醇与纯化水的体积比为2:3。
上述步骤 (4) 中,所述的静电纺丝的相关参数,高压直流电压为15 kV,纺丝距离16 cm,注射器推进速率为 1.2 mL/h,针头型号为20 G,往复平台转轴转速为350 rpm,接收器转速为450 rpm。
实施例2
一种凝胶化改性纤维静电纺丝面膜的制备方法,所述方法包括如下具体步骤:
(1)无纺布纤维碱化:将42 g/m2天然纤维素无纺布完全浸入适量质量分数为10 %的碱液中,在45 ℃下,进行碱化15 min后,挤压干净无纺布中多余的碱液,备用;
(2)无纺布纤维醚化:在碱化反应后的干无纺布中低温加入具有稀释剂保护的醚化剂20 mL,在60 ℃下,进行醚化40 min后,加入pH中和液,将pH值调节至5.5~7.0,用75 %稀释剂水溶液洗涤3~5次,每次洗涤时间为15 min,最后用高温压干机压干且平整,备用;
(3)同实施例1中步骤 (3);
(4)同实施例1中步骤 (4)。
上述步骤 (1) 中,所述的碱液为氢氧化钾和尿素的混合水溶液,所述的天然纤维素无纺布与所用碱液的质量比为2:100。
上述步骤 (2) 中,所述的稀释剂为异丙醇,所述的醚化剂为环氧乙烷,所述的pH中和液为冰乙酸。
上述步骤 (3) 中,所述静电纺丝前驱液的成分组成,透明质酸钠2份、聚乙烯醇20份、聚乙烯基吡咯烷酮1份、烟酰胺4份、维生素C 0.8份、芦荟提取液8份、无水乙醇15份、纯化水45份,其中,无水乙醇与纯化水的体积比为1:3。
上述步骤 (4) 中,所述的静电纺丝的相关参数,高压直流电压为17 kV,纺丝距离16 cm,注射器推进速率为 1.4 mL/h,针头型号为20 G,往复平台转轴转速为400 rpm,接收器转速为460 rpm。
实施例3
一种凝胶化改性纤维静电纺丝面膜的制备方法,所述方法包括如下具体步骤:
(1)无纺布纤维碱化:将42 g/m2天然纤维素无纺布完全浸入适量质量分数为15 %的碱液中,在30 ℃下,进行碱化35 min后,挤压干净无纺布中多余的碱液,备用;
(2)无纺布纤维醚化:在碱化反应后的干无纺布中低温加入具有稀释剂保护的醚化剂20 mL,在60 ℃下,进行醚化50 min后,加入pH中和液,将pH值调节至5.5~7.0,用75 %稀释剂水溶液洗涤3~5次,每次洗涤时间为15 min,最后用高温压干机压干且平整,备用;
(3)同实施例1中步骤 (3);
(4)同实施例1中步骤 (4)。
上述步骤 (1) 中,所述的碱液为氢氧化钠和尿素的混合水溶液,所述的天然纤维素无纺布与所用碱液的质量比为2:100。
上述步骤 (2) 中,所述的稀释剂为异丙醇,所述的醚化剂为环氧乙烷,所述的pH中和液为盐酸。
上述步骤 (3) 中,所述静电纺丝前驱液的成分组成,透明质酸钠3份、聚乙烯醇22份、聚乙烯基吡咯烷酮0.5份、烟酰胺4份、维生素C 0.8份、芦荟提取液10份、无水乙醇30份、纯化水45份,其中,无水乙醇与纯化水的体积比为2:3。
上述步骤 (4) 中,所述的静电纺丝的相关参数,高压直流电压为18 kV,纺丝距离17 cm,注射器推进速率为 1.4 mL/h,针头型号为21 G,往复平台转轴转速为400 rpm,接收器转速为460 rpm。
实施例4
一种凝胶化改性纤维静电纺丝面膜的制备方法,所述方法包括如下具体步骤:
(1)无纺布纤维碱化:将42 g/m2天然纤维素无纺布完全浸入适量质量分数为15 %的碱液中,在40 ℃下,进行碱化35 min后,挤压干净无纺布中多余的碱液,备用;
(2)无纺布纤维醚化:在碱化反应后的干无纺布中低温加入具有稀释剂保护的醚化剂18 mL,在60 ℃下,进行醚化50 min后,加入pH中和液,将pH值调节至5.5~7.0,用75 %稀释剂水溶液洗涤3~5次,每次洗涤时间为15 min,最后用高温压干机压干且平整,备用;
(3)同实施例1中步骤 (3);
(4)同实施例1中步骤 (4)。
上述步骤 (1) 中,所述的碱液为氢氧化钠和三乙醇胺的混合水溶液,所述的天然纤维素无纺布与所用碱液的质量比为1:99。
上述步骤 (2) 中,所述的稀释剂为异丙醇,所述的醚化剂为环氧乙烷,所述的pH中和液为85 %磷酸。
上述步骤 (3) 中,所述静电纺丝前驱液的成分组成,透明质酸钠3份、聚乙烯醇20份、聚乙烯基吡咯烷酮0.8份、烟酰胺4份、维生素C 1份、芦荟提取液9份、无水乙醇15份、纯化水60份,其中,无水乙醇与纯化水的体积比为1: 4。
上述步骤 (4) 中,所述的静电纺丝的相关参数,高压直流电压为18 kV,纺丝距离18 cm,注射器推进速率为 1.2 mL/h,针头型号为22 G,往复平台转轴转速为500 rpm,接收器转速为500 rpm。
实施例5
一种凝胶化改性纤维静电纺丝面膜的制备方法,所述方法包括如下具体步骤:
(1)无纺布纤维碱化:将42 g/m2天然纤维素无纺布完全浸入适量质量分数为30 %的碱液中,在40 ℃下,进行碱化20 min后,挤压干净无纺布中多余的碱液,备用;
(2)无纺布纤维醚化:在碱化反应后的干无纺布中低温加入具有稀释剂保护的醚化剂22 mL,在60 ℃下,进行醚化50 min后,加入pH中和液,将pH值调节至5.5~7.0,用75 %稀释剂水溶液洗涤3~5次,每次洗涤时间为15 min,最后用高温压干机压干且平整,备用;
(3)同实施例1中步骤 (3);
(4)同实施例1中步骤 (4)。
上述步骤 (1) 中,所述的碱液为氢氧化钠和三乙醇胺的混合水溶液,所述的天然纤维素无纺布与所用碱液的质量比为2:100。
上述步骤 (2) 中,所述的稀释剂为异丙醇,所述的醚化剂为环氧乙烷,所述的pH中和液为85 %磷酸。
上述步骤 (3) 中,所述静电纺丝前驱液的成分组成,透明质酸钠3份、聚乙烯醇20份、聚乙烯基吡咯烷酮0.8份、烟酰胺5份、维生素C 1份、芦荟提取液9份、无水乙醇30份、纯化水45份,其中,无水乙醇与纯化水的体积比为2: 3。
上述步骤 (4) 中,所述的静电纺丝的相关参数,高压直流电压为18 kV,纺丝距离16 cm,注射器推进速率为 1.4 mL/h,针头型号为22 G,往复平台转轴转速为500 rpm,接收器转速为500 rpm。
Claims (10)
1.一种凝胶化改性纤维静电纺丝面膜的制备方法,其特征在于,此面膜的功能层包括凝胶保湿层和固态精华释放层,其中所述的凝胶保湿层采用天然纤维素原位凝胶化改性技术制备而成,而固态精华释放层采用静电纺丝技术制备成纳米纤维,通过两种技术的有效结合制备出保湿性、敷贴性、便捷性俱佳的固态面膜。
2.根据权利要求1所述的凝胶化改性纤维静电纺丝面膜,其特征在于,所述的凝胶化改性保湿层使用如下改性成分:天然纤维素无纺布、碱液、醚化剂、稀释剂、pH中和液、纯化水。
3.根据权利要求1所述的凝胶化改性纤维静电纺丝面膜,其特征在于,所述的静电纺丝纳米纤维包括如下有效成分:透明质酸钠、聚乙烯醇、聚乙烯基吡咯烷酮、烟酰胺、维生素C、芦荟提取液、无水乙醇、纯化水。
4.根据权利要求3所述的凝胶化改性纤维静电纺丝面膜,其特征在于,所述的静电纺丝纳米纤维包括以下按重量份计量的各组分:透明质酸钠1~5份、聚乙烯醇15~35份、聚乙烯基吡咯烷酮0.5~1.3份、烟酰胺3~5份、维生素C 0.5~1份、芦荟提取液5~10份、无水乙醇15~45份、纯化水30~60份。
5.根据权利要求3所述的凝胶化改性纤维静电纺丝面膜,其特征在于,所述的透明质酸钠的平均分子量为350000~620000、聚乙烯基吡咯烷酮的平均分子量为42000~60000、聚乙烯醇的平均分子量为120000~150000。
6.根据权利要求1~5任一项所述的凝胶化改性纤维静电纺丝面膜的制备方法,其特征在于,所述的制备方法包括如下步骤:
(1) 无纺布纤维碱化:将42 g/m2天然纤维素无纺布完全浸入适量质量分数为10~40 %的碱液中,在30~55 ℃下,进行碱化15~35 min后,挤压干净无纺布中多余的碱液,备用;
(2) 无纺布纤维醚化:在碱化反应后的干无纺布中低温加入具有稀释剂保护的醚化剂10~30 mL,在40~70 ℃下,进行醚化35~60 min后,加入pH中和液,将pH值调节至5.5~7.0,用75 %稀释剂水溶液洗涤3~5次,每次洗涤时间为15 min,最后用高温压干机压干且平整,备用;
(3) 静电纺丝前驱液配置:将聚乙烯醇加入适量乙醇水溶液中,加热至95 ℃,搅拌直至溶解均匀,降温至40 ℃,再依次加入透明质酸钠和聚乙烯基吡咯烷酮,继续搅拌直至溶解均匀,继续降温至室温,再依次加入芦荟提取液、维生素C、烟酰胺,继续搅拌直至形成均相的纺丝前驱液;
(4) 无纺布静电纺丝:将上述制备的凝胶化无纺布固定在静电纺丝接收器上,使用5~20 mL的注射抽取适量上述的纺丝前驱液,将注射器放在往复平台的注射器推进器上,进行静电纺丝制备纳米纤维后,得到凝胶化改性纤维静电纺丝面膜。
7.根据权利要求6所述的凝胶化改性纤维静电纺丝面膜的制备方法,其特征在于,所述的碱液为氢氧化钾、氢氧化钠、三乙醇胺、尿素中两种以上的混合水溶液,所述的稀释剂为丙酮、异丙醇、叔丁醇中的一种,所述的醚化剂为环氧乙烷,所述的pH中和液为85 %磷酸、冰乙酸、盐酸中的一种。
8.根据权利要求6所述的凝胶化改性纤维静电纺丝面膜的制备方法,其特征在于,所述的天然纤维素无纺布与所用碱液的质量比为1~3:96~100。
9.根据权利要求6所述的凝胶化改性纤维静电纺丝面膜的制备方法,其特征在于,所述的纺丝前驱液中,无水乙醇与纯化水的体积比为1~3:2~4。
10.根据权利要求6所述的凝胶化改性纤维静电纺丝面膜的制备方法,其特征在于,所述的静电纺丝的相关参数,高压直流电压为14~20 kV,纺丝距离10~20 cm,注射器推进速率为 0.8~1.8 mL/h,针头型号为19~22 G,往复平台转轴转速为300~550 rpm,接收器转速为400~550 rpm。
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