CN116289172A - 改性纤维素纤维水刺非织造布、制备方法及面膜 - Google Patents
改性纤维素纤维水刺非织造布、制备方法及面膜 Download PDFInfo
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- CN116289172A CN116289172A CN202310122495.4A CN202310122495A CN116289172A CN 116289172 A CN116289172 A CN 116289172A CN 202310122495 A CN202310122495 A CN 202310122495A CN 116289172 A CN116289172 A CN 116289172A
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- nonwoven fabric
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- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 124
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910001868 water Inorganic materials 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000004744 fabric Substances 0.000 claims abstract description 28
- 239000002585 base Substances 0.000 claims abstract description 25
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910021538 borax Inorganic materials 0.000 claims abstract description 21
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 21
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 21
- TVAJJUOMNRUGQA-UHFFFAOYSA-N 2-butoxyethyl dihydrogen phosphate Chemical compound CCCCOCCOP(O)(O)=O TVAJJUOMNRUGQA-UHFFFAOYSA-N 0.000 claims abstract description 20
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 229920000297 Rayon Polymers 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 39
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005406 washing Methods 0.000 description 10
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 description 9
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- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 3
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- 238000009960 carding Methods 0.000 description 2
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
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- 229920003086 cellulose ether Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- DQYBDCGIPTYXML-UHFFFAOYSA-N ethoxyethane;hydrate Chemical compound O.CCOCC DQYBDCGIPTYXML-UHFFFAOYSA-N 0.000 description 1
- -1 ethylene glycol monobutyl ether phosphate ester Chemical class 0.000 description 1
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- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical group O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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- A—HUMAN NECESSITIES
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- A61Q19/00—Preparations for care of the skin
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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Abstract
本发明涉及纤维素纤维水刺非织造布领域,公开了改性纤维素纤维水刺非织造布、制备方法及面膜,所述方法包括:(1)在第一反应条件下将碱液与纤维素纤维水刺非织造布进行第一接触,得到碱化纤维素纤维水刺非织造布;(2)在第二反应条件下将碱化纤维素纤维水刺非织造布与醚化液进行第二接触,得到羧甲基化纤维素纤维水刺非织造布;(3)使用酸溶液对所述羧甲基化纤维素纤维水刺非织造布进行中和处理,然后将得到的产物脱除溶液并干燥,得到所述改性纤维素纤维水刺非织造布;其中,所述醚化液含有一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠和水。本发明的改性纤维素纤维水刺非织造布用于面膜基布时,具有良好的机械力学性能,透光率高,柔软、透气性良好。
Description
技术领域
本发明涉及纤维素纤维水刺非织造布领域,具体涉及一种改性纤维素纤维水刺非织造布、制备方法及面膜。
背景技术
随着美容业的发展,面膜产品异军突起,成为人们关注的焦点。市场上供应的面膜80%是以纤维成膜材料为载体(即面膜基布),辅以营养成分和药物的载体式纤维面膜,其功能差异主要取决于面膜基布,而载体式面膜基布大多以非织造布为主,非织造布的特点是高速高产、工艺变化多、可应用纤维广泛、结构性能多样化,符合“一次性使用、实用方便、安全卫生、低成本”的面膜使用要求。非织造布种类繁多,能够用于面膜基布的非织造布产品,有热轧非织造布、纺粘非织造布、水刺非织造布和熔喷非织造布等,其中以水刺非织造布应用最多,因为它手感绵软,质地可人,孔隙率高,保湿性能好,能够保证面膜携带大量的营养液,保证皮肤充分吸收,是近年来的新宠。
但是目前市场上的面膜基布普遍存在贴肤性较差、透明度差、保水率低、功能性不强等缺点,人们大多只关注面膜中精华液的营养成份,而往往忽视了面膜基布的护肤效果。
羧甲基纤维素纤维是纤维素纤维经羧甲基化后制成的一类纤维素醚,现有技术通常通过对纤维素纤维进行羧甲基化制得羧甲基纤维素纤维来提升其吸水性、保水性、柔软度、吸水后具有较高的透明度等性能。因此,对纤维素纤维水刺非织造布中的纤维素进行羧甲基化的这种改性方法经常用于制备改性纤维素纤维水刺非织造布,制得的改性纤维素纤维水刺非织造布非常适用于制作美容面膜基布。但是,现有技术中,羧甲基化改性的反应过程复杂,耗时较长,能耗较高,且难以控制羧甲基化反应程度,当醚化程度低时易造成吸水、保水性不足、透明性差,而醚化程度高时候则易导致力学性能下降严重、湿强低,手感偏硬,且透气性大幅降低,难以满足应用需求。
CN109674721A公开了一种羧甲基纤维素纤维面膜的制备方法,制备方法包括以下步骤:(1)用冷轧堆染色法将原料加入到氢氧化钠溶液中从而得到碱性织物;(2)在步骤(1)所得的碱性织物中加入一氯乙酸溶液进行浸轧,获得羧甲基纤维素纤维;(3)将步骤(2)所得的羧甲基纤维素纤维加入至水中洗涤至中性后晾干;(4)将步骤(3)晾干得到的羧甲基纤维素纤维进行静电纺丝后通过高速梳理机中梳理得面膜基布。该面膜基布在低温下通过冷轧堆染色法进行两次浸轧工艺,减少了原料在生产过程中的化学损失,且反应更稳定,制造的羧甲基纤维素纤维面膜具有良好的保水性。但是此发明方法生产时间长,过程复杂,难以批量进行面膜基布生产,且生产出来的面膜基布柔软性较差。
因此,需要研制出一种便于产业化的水刺非织造布的纤维素羧甲基化改性方法。
发明内容
本发明的目的是为了克服现有技术存在的水刺非织造布的纤维素羧甲基化改性方法复杂、耗时长、羧甲基化程度难以控制、改性后的水刺非织造布湿强低、透明性差、柔软性和吸水性能不足等的问题,提供一种改性纤维素纤维水刺非织造布、制备方法及面膜。本发明的制备方法反应时间短、工艺流程简单、反应条件温和、产品均一性好,自动化程度高,符合产业化的要求。本发明的改性纤维素纤维水刺非织造布具有较小的弯曲刚度、较高的透气性、较强的吸水率、保湿性好、透明度高,湿强度大,天然的生物相容性和可生物降解性。
为了实现上述目的,本发明第一方面提供一种改性纤维素纤维水刺非织造布的制备方法,其特征在于,所述方法包括:
(1)在第一反应条件下将碱液与纤维素纤维水刺非织造布进行第一接触,得到碱化纤维素纤维水刺非织造布;
(2)在第二反应条件下将碱化纤维素纤维水刺非织造布与醚化液进行第二接触,得到羧甲基化纤维素纤维水刺非织造布;
(3)使用酸溶液对所述羧甲基化纤维素纤维水刺非织造布进行中和处理,然后将得到的产物脱除溶液并干燥,得到所述改性纤维素纤维水刺非织造布;
其中,所述醚化液含有一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠和水。
本发明第二方面提供一种改性纤维素纤维水刺非织造布,所述改性纤维素纤维水刺非织造布上述制备方法制得。
本发明第三方面提供一种面膜,所述面膜包括面膜基布和精华液,所述面膜基布为上述改性纤维素纤维水刺非织造布。
通过上述技术方案,本发明获得的有益效果是:
(1)本发明的制备方法反应时间短、工艺流程简单、反应条件温和、产品均一性好、自动化程度高;
(2)本发明的改性纤维素纤维水刺非织造布的克重为28-60g/m2,厚度为0.15-0.42mm,湿抗张强度≥14N/cm,吸水率为≥995%,湿态透光率≥85%,柔软度≤160mN,透气性≥2300mm/s,缩水率≤5%,单位面积质量偏差率≤7%,单位面积质量变异系数≤6%,厚度偏差≤0.04,断裂强力≥35N,幅宽偏差≤2mm。用于面膜基布时,具有良好的机械力学性能,满足面膜使用时的轻拉扯拽,不易破损;透光率高,满足面膜使用时透明性的要求;柔软、透气性良好,使用时敷于面部,可于皮肤紧密贴合,舒适性好,不影响肌肤的正常呼吸作用。
具体实施方式
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值,这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说,各个范围的端点值之间、各个范围的端点值和单独的点值之间,以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围,这些数值范围应被视为在本文中具体公开。
本发明第一方面提供一种改性纤维素纤维水刺非织造布的制备方法,所述方法包括:
(1)在第一反应条件下将碱液与纤维素纤维水刺非织造布进行第一接触,得到碱化纤维素纤维水刺非织造布;
(2)在第二反应条件下将碱化纤维素纤维水刺非织造布与醚化液进行第二接触,得到羧甲基化纤维素纤维水刺非织造布;
(3)使用酸溶液对所述羧甲基化纤维素纤维水刺非织造布进行中和处理,然后将得到的产物脱除溶液并干燥,得到所述改性纤维素纤维水刺非织造布;
其中,所述醚化液含有一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠和水。
发明人在研究中发现,醚化液含有上述组分时,各组分之间具有协同作用,能够有效地缩短制备所需的时间,大幅降低生产成本,并且能够显著提升制得的改性纤维素纤维水刺非织造布的强度(湿强度和干强度)、透明度、柔软度和透气性等性能。申请人意外发现,乙二醇单丁醚磷酸酯能够极大地增加醚化液中各组分的渗透性,能够缩短反应时间,制得的改性纤维素纤维水刺非织造布的强度、透明度等性能也有显著提升;而适量四硼酸钠的加入,可以有效减小一氯乙酸与氢氧化钠的副反应,降低氯乙酸钠的消耗量。
本发明的一些实施方式中,所述纤维素纤维水刺非织造布选自天丝纤维水刺非织造布、黏胶纤维水刺非织造布、铜氨纤维水刺非织造布中的一种。
本发明的一些实施方式中,所述碱液的浓度为3.5-4.5mol/L。
本发明的一些实施方式中,所述碱液的温度为25-35℃。所述碱液为氢氧化钠的水溶液。
本发明的一些实施方式中,所述醚化液中,一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水的质量比为:8-15:2-6:0.5-8:71-90。所述氯乙酸钠、乙二醇单丁醚磷酸酯、四硼酸钠、水的质量分数在上述范围内时,第二接触的反应过程温和,反应时间短,最终制得的改性纤维素纤维水刺非织造布透明性好、柔软、透气、强度高。
本发明的一些实施方式中,所述醚化液的温度为25-30℃。
本发明的一些实施方式中,所述第一反应的条件包括:第一浴比1:10-20,第一反应温度为25-35℃,第一反应时间为20-50min。其中,所述第一浴比指的是:纤维素纤维水刺非织造布与第一反应阶段溶液的质量比例。
本发明的一些实施方式中,所述第二反应的条件包括:第二浴比1:20-60,第二反应温度为35-45℃,第二反应时间为30-60min。其中,所述第二浴比指的是:碱化纤维素纤维水刺非织造布与第二反应阶段醚化液的质量比例。
本发明中,步骤(2)所述的乙二醇单丁醚磷酸酯的使用,能够极大地增加醚化液中各组分向纤维内部的渗透性,能够缩短反应时间;所述四硼酸钠溶液能够一定程度抑制因高温导致的氯乙酸钠水解速度加快,且不影响主反应阶段的醚化速率。
本发明中,所述步骤(2)的反应条件在上述范围内时,最终制得的改性纤维素纤维水刺非织造布均一性好,透明性好、柔软、透气、强力高。
本发明中,步骤(3)中所述脱除溶液指的是脱除中和处理后的多余溶液,其方法可以为本领域常用方法,例如可以为用水洗去中和处理后多余溶液。
所述羧甲基化处理的条件在上述范围内时,最终制得的改性纤维素纤维水刺非织造布透明性好、柔软、透气、强力高。
本发明的一些实施方式中,步骤(3)中,所述中和处理使得得到的产物的pH值在7.2-9.8之间。所述pH值在上述范围内时,所述中和处理可以处理掉残留的氢氧化钠,并保持最终制得的改性纤维素纤维水刺非织造布的弱碱性,提高最终制得的改性纤维素纤维水刺非织造布的吸液速度。其中,所述pH值通过GB/T7573-2009规定的方法进行测定。
本发明的一些实施方式中,步骤(3)中,所述酸溶液选自盐酸溶液、甲酸溶液、乙酸溶液、草酸溶液、磷酸溶液中的至少一种。
本发明的一些实施方式中,为了缓冲中和处理的速度,同时避免反应过度,所述酸溶液的质量分数为5-10wt%。
本发明中,所述干燥可以为本领域常规的技术手段,例如可以为烘干,在此不再赘述。
本发明第二方面提供一种改性纤维素纤维水刺非织造布,所述改性纤维素纤维水刺非织造布由如前所述的制备方法制得。
本发明的一些实施方式中,所述改性纤维素纤维水刺非织造布的平均羧甲基取代度为0.25-0.4,克重为28-60g/m2,厚度为0.15-0.42mm,湿抗张强度≥14N/cm,湿态透光率≥85%,柔软度≤160mN,透气性≥2300mm/s,吸水率为≥995%,缩水率≤5%。
本发明中,所述改性纤维素纤维水刺非织造布的平均羧甲基取代度(DS)指的是纤维素的每个失水葡萄糖单元上的活性羟基被羧甲基化取代的比例。本发明的一些实施方式中,改性纤维素纤维水刺非织造布的平均羧甲基取代度为0.25-0.4。当所述改性纤维素纤维水刺非织造布的平均羧甲基取代度≥0.4时,吸水后凝胶化严重,导致力学性能、柔软和透气性能均大幅下降。
本发明第三方面提供一种面膜,所述面膜包括面膜基布和精华液,所述面膜基布为如前所述的改性纤维素纤维水刺非织造布。
以下将通过实施例对本发明进行详细描述。
以下实施例中,除非特殊说明,所有试剂和原料可通过商购得到。
实施例1
本实施例中醚化液由一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水组成,醚化液中一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水的质量比为8:6:1:85。
(1)将天丝纤维水刺非织造布与温度为25℃、浓度为3.5mol/L的NaOH溶液按照第一浴比为1:20的量进行第一接触,在温度恒定条件下保持30min,得到碱化纤维素纤维水刺非织造布;
(2)将碱化纤维素纤维水刺非织造布与醚化液按照第二浴比为1:20的量进行第二接触,在40℃下保温50min,得到羧甲基化纤维素纤维水刺非织造布;
(3)将质量分数为5wt%的乙酸溶液缓慢加至羧甲基化纤维素纤维水刺非织造布进行中和处理,实时监测溶液pH,控制pH值为7.2-9.8(参照GB/T7573-2009方法进行测定,以下实施例和对比例同)。将中和后的羧甲基化纤维素纤维水刺非织造布用水洗三次,洗去多余溶液,烘干得到改性纤维素纤维水刺非织造布。
实施例2
本实施例中醚化液由一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水组成,醚化液中一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水的质量比为12:2:6:80。
(1)将天丝水刺非织造布与温度为30℃、浓度为3.8mol/L的NaOH溶液按照第一浴比为1:15的量进行第一接触,在温度恒定条件下保持50min,得到碱化纤维素纤维水刺非织造布;
(2)将碱化纤维素纤维水刺非织造布与醚化液按照第二浴比为1:40的量进行第二接触,在35℃下保温60min,得到羧甲基化纤维素纤维水刺非织造布;
(3)将质量分数为5%盐酸溶液溶液缓慢加至羧甲基化纤维素纤维水刺非织造布进行中和处理,实时监测溶液pH,控制pH值为7.2-9.8。将中和后的羧甲基化纤维素纤维水刺非织造布用水洗三次,洗去多余溶液,烘干得到改性纤维素纤维水刺非织造布。
实施例3
本实施例中醚化液由一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水组成,醚化液中一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水的质量比为10:5:3:82。
(1)将黏胶纤维水刺非织造布与温度为32℃、浓度为4.2mol/L的NaOH溶液按照第一浴比为1:12的量进行第一接触,在温度恒定条件下保持40min,得到碱化纤维素纤维水刺非织造布;
(2)将碱化纤维素纤维水刺非织造布与醚化液按照第二浴比为1:30的量进行第二接触,在45℃下保温30min,得到羧甲基化纤维素纤维水刺非织造布;
(3)将质量分数为10wt%的草酸溶液缓慢加至羧甲基化纤维素纤维水刺非织造布进行中和处理,实时监测溶液pH,控制pH值为7.2-9.8。将中和后的羧甲基化纤维素纤维水刺非织造布用水洗三次,洗去多余溶液,烘干得到改性纤维素纤维水刺非织造布。
实施例4
本实施例中醚化液由一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水组成,醚化液中一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水的质量比为15:4:7:74。
(1)将铜氨纤维水刺非织造布与温度为35℃、浓度为4.5mol/L的NaOH溶液按照第一浴比为1:10的量进行第一接触,在温度恒定条件下保持30min,得到碱化纤维素纤维水刺非织造布;
(2)将碱化纤维素纤维水刺非织造布与醚化液按照第二浴比为1:60的量进行第二接触,在40℃下保温45min,得到羧甲基化纤维素纤维水刺非织造布;
(3)将质量分数为10wt%的柠檬酸溶液缓慢加至羧甲基化纤维素纤维水刺非织造布进行中和处理,实时监测溶液pH,控制pH值为7.2-9.8。将中和后的羧甲基化纤维素纤维水刺非织造布用水洗三次,洗去多余溶液,烘干得到改性纤维素纤维水刺非织造布。
对比例1
按照实施例1的方法制备改性纤维素纤维水刺非织造布,不同之处在于:步骤(2)中的醚化液中的组成为一氯乙酸和水,质量比为15:85,反应时间为200min。
对比例2
按照实施例2的方法制备改性纤维素纤维水刺非织造布,不同之处在于:步骤(2)中的醚化液中的组成为一氯乙酸、乙二醇单丁醚磷酸酯、水的质量比为14:6:80。
对比例3
按照实施例3的方法制备改性纤维素纤维水刺非织造布,不同之处在于:步骤(2)中的醚化液中的组成为一氯乙酸、四硼酸钠、水的质量比为8:4:88。
测试例
本实验例对实施例和对比例所得的改性纤维素纤维水刺非织造布的性能进行检测,结果如表1所示。其中,
湿强度通过用湿抗张强度表征。湿抗张强度的测量方法是:在20℃、65%的相对湿度下,将试样(即改性纤维素纤维水刺非织造布)在去离子水中浸泡15min后,取出试样,垂直悬挂至无连续水珠滴落,按照GB/T 465.2测定测试湿抗张强度;
吸湿性是通过吸水率表征。吸水率的测量方法是:在20℃、65%的相对湿度下,将试样(即改性纤维素纤维水刺非织造布)称重后,在去离子水中浸泡5min,取出试样后垂直悬挂,至无连续水珠滴落后,获得浸湿的试样,称量浸湿的试样重量,按以下公式计算吸水率:吸水率=(浸湿的试样质量-干燥的试样质量)/干燥的试样质量×100%;
柔软度通过用弯曲刚度表征,弯曲刚度越小,柔软性越好。测量方法是:按照标准GB/T 18318.1-2009测定,用斜面法对试样的弯曲性能进行测定;
透气性是影响面膜舒适性的重要因素,透气性参照GB/T5453-2007测试,压力为100Pa,测试面积为20cm2;
改性纤维素纤维水刺非织造布的羧甲基化程度取代度(DS)来描述。取代度(DS)通过GB 1886.232-2016中附录A中规定的取代度的测定方法测定。
湿态透光率通过将改性纤维素纤维水刺非织造布浸渍于足量水中1min,取出沾去表面水份,然后采用紫外/可见/近红外分光光度计测试的透光率,参照GB/T2410-2008测得;
表1
实施例1 | 实施例2 | 实施例3 | 实施例4 | |
厚度(mm) | 0.19 | 0.20 | 0.22 | 0.35 |
克重(g/m2) | 37.49 | 39.20 | 39.87 | 43.31 |
湿抗张强度(N/cm) | 4.1 | 4.58 | 4.32 | 2.05 |
湿态透光率(%) | 83 | 89 | 97 | 89 |
弯曲刚度(gf·cm2/cm) | 0.0432 | 0.0392 | 0.0413 | 0.059 |
吸水率(%) | 997 | 1025 | 1011 | 1988 |
缩水率(%) | 7.2% | 8.8% | 8.1% | 9.2% |
透气性(mm/s) | 2304 | 2357 | 2372 | 1572 |
平均羧甲基取代度(DS) | 0.21 | 0.25 | 0.27 | 0.39 |
表1(续)
对比例1 | 对比例2 | 对比例3 | |
厚度(mm) | 0.35 | 0.42 | 0.36 |
克重(g/m2) | 43.31 | 56.31 | 44.56 |
湿抗张强度(N/cm) | 3.05 | 0.95 | 2.98 |
湿态透光率(%) | 49 | 95 | 52 |
弯曲刚度(gf·cm2/cm) | 0.1259 | 0.0981 | 0.1198 |
吸水率(%) | 988 | 2021 | 1021 |
缩水率(%) | 6.2% | 13.2% | 6.9% |
透气性(mm/s) | 2920 | 862 | 2857 |
平均羧甲基取代度(DS) | 0.21 | 0.71 | 0.26 |
从表1可以看出,实施例1-4所得改性纤维素纤维水刺非织造布在克重在36-40g/m2、厚度在0.19-0.22mm的区间内,湿抗张强度超过3N/cm,说明改性纤维素纤维水刺非织造布具有良好的机械力学性能,作为面膜基布时能够满足面膜使用时的轻拉扯拽,不易破损。实施例1-4所得改性纤维素纤维水刺非织造布的吸水率将近1100%;该改性纤维素纤维水刺非织造布的透气率不低于2300mm/s,说明其透气性良好,作为面膜基布制备的面膜使用时敷于面部,不影响肌肤的正常呼吸作用,柔软舒适。
通过对比例1可以看出,仅使用一氯乙酸溶液进行醚化,醚化液中不含有乙二醇单丁醚磷酸酯和四硼酸钠,反应进程慢,反应需要的时间长,远超过实验1的反应时间,而且制得的改性纤维素纤维水刺非织造布的平均羧甲基取代度和吸水率均较低,导致改性纤维素纤维水刺非织造布的透光性、吸水性和弯曲刚度等性能均较差。
通过对比例2可以看出,当醚化液组成为一氯乙酸、乙二醇单丁醚磷酸酯和水,不含有四硼酸钠时,由于一氯乙酸在碱性环境下易于发生副反应,需要添加更多量的一氯乙酸,且制备的改性纤维素纤维水刺非织造布的平均羧甲基取代度不宜控制,改性纤维素纤维水刺非织造布的抗湿张强度、吸水率、透气性等性能均较差。
通过对比例3可以看出,当醚化液组成为一氯乙酸、四硼酸钠、水,不含有乙二醇单丁醚磷酸酯时,由于反应剂的渗透性差,制备的改性纤维素纤维水刺非织造布的平均羧甲基取代度较低,改性纤维素纤维水刺非织造布的抗湿张强度、弯曲刚度等性能均较差。
以上详细描述了本发明的优选实施方式,但是,本发明并不限于此。在本发明的技术构思范围内,可以对本发明的技术方案进行多种简单变型,包括各个技术特征以任何其它的合适方式进行组合,这些简单变型和组合同样应当视为本发明所公开的内容,均属于本发明的保护范围。
Claims (11)
1.一种改性纤维素纤维水刺非织造布的制备方法,其特征在于,所述方法包括:
(1)在第一反应条件下将碱液与纤维素纤维水刺非织造布进行第一接触,得到碱化纤维素纤维水刺非织造布;
(2)在第二反应条件下将碱化纤维素纤维水刺非织造布与醚化液进行第二接触,得到羧甲基化纤维素纤维水刺非织造布;
(3)使用酸溶液对所述羧甲基化纤维素纤维水刺非织造布进行中和处理,然后将得到的产物脱除溶液并干燥,得到所述改性纤维素纤维水刺非织造布;
其中,所述醚化液含有一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠和水。
2.根据权利要求1所述的制备方法,其特征在于,所述纤维素纤维水刺非织造布选自天丝纤维水刺非织造布、黏胶纤维水刺非织造布、铜氨纤维水刺非织造布中的一种。
3.根据权利要求1或2所述的制备方法,其特征在于,所述碱液的浓度为3.5-4.5mol/L,所述碱液的温度为25-35℃。
4.根据权利要求1-3中任意一项所述的制备方法,其特征在于,所述醚化液中,一氯乙酸、乙二醇单丁醚磷酸酯、四硼酸钠、水的质量比为:8-15:2-6:0.5-8:71-90。
5.根据权利要求1-4中任意一项所述的方法,其特征在于,所述第一反应的条件包括:第一浴比为1:10-20,第一反应温度为25-35℃,第一反应时间为20-50min。
6.根据权利要求1-5中任意一项所述的方法,其特征在于,所述第二反应的条件包括:第二浴比为1:20-60,第二反应温度为35-45℃,第二反应时间为30-60min。
7.根据权利要求1-6中任意一项所述的制备方法,其特征在于,步骤(3)中,所述中和处理使得得到的产物的pH值在7.2-9.8之间。
8.根据权利要求1-7中任意一项所述的制备方法,其特征在于,步骤(3)中,所述酸溶液选自盐酸溶液、甲酸溶液、乙酸溶液、草酸溶液、磷酸溶液、柠檬酸溶液中的至少一种;
和/或,所述酸溶液的质量分数为5-10wt%。
9.一种改性纤维素纤维水刺非织造布,其特征在于,所述改性纤维素纤维水刺非织造布由权利要求1-8中任意一项所述的制备方法制得。
10.根据权利要求9所述的改性纤维素纤维水刺非织造布,其特征在于,所述改性纤维素纤维水刺非织造布的平均羧甲基取代度为0.25-0.4,克重为28-60g/m2,厚度为0.15-0.42mm,湿抗张强度≥14N/cm,湿态透光率≥85%,柔软度≤160mN,透气性≥2300mm/s,吸水率为≥995%,缩水率≤5%。
11.一种面膜,所述面膜包括面膜基布和精华液,其特征在于,所述面膜基布为权利要求9或10所述的改性纤维素纤维水刺非织造布。
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