CN111876899A - 一种超柔软无纺布及其制备方法 - Google Patents
一种超柔软无纺布及其制备方法 Download PDFInfo
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- CN111876899A CN111876899A CN202010764116.8A CN202010764116A CN111876899A CN 111876899 A CN111876899 A CN 111876899A CN 202010764116 A CN202010764116 A CN 202010764116A CN 111876899 A CN111876899 A CN 111876899A
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- woven fabric
- parts
- polyvinyl alcohol
- polyacrylonitrile
- modified
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- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 33
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 28
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 14
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
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- NUVBSKCKDOMJSU-UHFFFAOYSA-N ethylparaben Chemical compound CCOC(=O)C1=CC=C(O)C=C1 NUVBSKCKDOMJSU-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims description 3
- IRFSXVIRXMYULF-UHFFFAOYSA-N 1,2-dihydroquinoline Chemical compound C1=CC=C2C=CCNC2=C1 IRFSXVIRXMYULF-UHFFFAOYSA-N 0.000 claims description 3
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 3
- 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 description 3
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- CYDQOEWLBCCFJZ-UHFFFAOYSA-N 4-(4-fluorophenyl)oxane-4-carboxylic acid Chemical compound C=1C=C(F)C=CC=1C1(C(=O)O)CCOCC1 CYDQOEWLBCCFJZ-UHFFFAOYSA-N 0.000 claims description 2
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
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- 239000004288 Sodium dehydroacetate Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
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- 238000007605 air drying Methods 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
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- 235000010331 calcium propionate Nutrition 0.000 claims description 2
- REZZEXDLIUJMMS-UHFFFAOYSA-M dimethyldioctadecylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC REZZEXDLIUJMMS-UHFFFAOYSA-M 0.000 claims description 2
- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 claims description 2
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- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 claims description 2
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
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Classifications
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- 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
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- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/08—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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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
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
- D04H3/147—Composite yarns or filaments
-
- 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
- D06M11/01—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 hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof
- D06M11/05—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 hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof with water, e.g. steam; with heavy water
-
- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
-
- D—TEXTILES; PAPER
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Abstract
本发明涉及纺织技术领域,具体涉及一种超柔软无纺布及其制备方法,其由以下原料制备而成:聚丙烯腈、改性聚乙烯醇母液和改性助剂;所述改性助剂包括:二甲基硅油、微晶纤维素、抗氧化剂、防腐剂、纳米氧化锌、石蜡、柔软剂、紫外线吸收剂和膨润土。本发明提供的高柔软度无纺布,通过添加改性聚乙烯醇母液,改善了粘合面的粘合性能、抗菌性能、可降解性能,大幅度降低施胶量,提升无纺布产品的轻薄感,从而不仅提高无纺布产品的品质,还达到了降低生产成本的效果。
Description
技术领域
本发明涉及无纺布技术领域,具体涉及一种超柔软无纺布及其制备方法。
背景技术
目前应用于卫生产品的薄型柔软类纺粘无纺布的大部分产品其上下两面的摩擦系数基本相同。在这类产品中一般会含有爽滑添加剂,而这类添加剂会影响热熔胶与无纺布的粘结效果,如果添加量没有控制好,一旦添加过多,则会导致柔软无纺布与其他材料粘结不好甚至发生无法粘合的情况。
海岛纤维是采用复合纺丝技术将两种成纤聚合物分别作为“海”组分和“岛”组分,按不同的配比进行纺丝得到。通过利用“海”组分和“岛”组分在某种化学试剂中的不同溶解度,使得“海”组分溶去,留下“岛”组分,得到的这种纤维,也称为复合超细纤维。目前未见采用海岛纤维制备超柔软无纺布的例子。
目前,已有公开采用PVA作为海的海岛纤维,但是由于PVA熔点与分解温度十分接近,不能采用熔喷工艺制备无纺布,因此必须要对其进行改性。
发明内容
本发明的目的在于提出一种超柔软无纺布及其制备方法,采用复合纺丝+水解剥离方法,采用复合纺丝法纺制成以聚丙烯腈为岛,以改性聚乙烯醇为海的“海-岛”型复合纤维,将这种复合纤维用水、碱液、酸液等溶剂处理,则可溶解掉海组分,得到表面凹凸不平的0.1-0.5dtex左右的超细纤维,采用超细纤维制备无纺布,其手感、覆盖性和蓬松性等有明显提高,具有极柔软的手感。
本发明的技术方案是这样实现的:
本发明提供一种超柔软无纺布,主要由以下原料制备而成:聚丙烯腈、改性聚乙烯醇母液和改性助剂;所述改性助剂包括:二甲基硅油、微晶纤维素、抗氧化剂、防腐剂、纳米氧化锌、石蜡、柔软剂、紫外线吸收剂和膨润土。
作为本发明的进一步改进,由以下原料按重量份制备而成:聚丙烯腈100-200份、改性聚乙烯醇母液30-50份和改性助剂10-15份;所述改性助剂由以下原料按重量份制备而成:二甲基硅油5-10份、微晶纤维素2-5份、抗氧化剂1-3份、防腐剂1-2份、纳米氧化锌5-10份、石蜡3-7份、柔软剂1-3份、紫外线吸收剂0.5-1份和膨润土10-20份。
作为本发明的进一步改进,由以下原料按重量份制备而成:聚丙烯腈150份、改性聚乙烯醇母液40份、改性助剂12份;所述改性助剂由以下原料按重量份制备而成:二甲基硅油7份、微晶纤维素3份、抗氧化剂2份、防腐剂1.5份、纳米氧化锌7份、石蜡5份、柔软剂3份、紫外线吸收剂0.7份和膨润土15。
作为本发明的进一步改进,所述改性聚乙烯醇母液由以下方法制备而成:用去离子水淘洗聚乙烯醇颗粒,在恒温鼓风干燥箱中于50-60℃干燥5-10h,将干燥的聚乙烯醇颗粒加入去离子水中,在50-70℃下恒温搅拌溶胀1-2h后加入甘油,混合均匀后,加入聚乳酸和氧化石墨烯,在90-100℃下搅拌2-4h,冷却,真空抽气0.5-1h,除去溶液里的气泡,得到改性聚乙烯醇母液。
作为本发明的进一步改进,所述聚乙烯醇颗粒、甘油、聚乳酸和氧化石墨烯的质量比为100:(5-10):(10-20):(3-7)。
作为本发明的进一步改进,所述柔软剂选自聚乙烯蜡、端羟基聚硅氧烷乳液、亲水性有机硅柔软剂、氨基聚硅氧烷乳液、氨基聚硅氧烷微乳和双十八烷基二甲基氯化铵中的一种或几种混合;所述抗氧化剂选自二苯胺、对苯二胺、二氢喹啉、2,6-三级丁基-4-甲基苯酚、双(3,5-三级丁基-4-羟基苯基)硫醚、四〔β-(3,5-三级丁基-4-羟基苯基)丙酸〕季戊四醇酯、双十二碳醇酯、双十四碳醇酯和双十八碳醇酯、硫代二丙酸双酯、三辛酯、三癸酯、三(十二碳醇)酯和三(十六碳醇)酯中的一种或几种混合;所述防腐剂选自苯甲酸钠、山梨酸钾、脱氢乙酸、脱氢乙酸钠、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、双乙酸钠、丙酸钙和乳酸钠中的一种或几种混合;所述紫外线吸收剂选自水杨酸酯类紫外线吸收剂、二苯甲酮类紫外线吸收剂、苯并三唑类紫外线吸收剂、取代丙烯腈类紫外线吸收剂和三嗪类阿紫外线吸收剂中的一种或几种混合。
本发明进一步保护一种上述超柔软无纺布的制备方法,包括以下步骤:
S1.聚丙烯腈/聚乙烯醇复合超细纤维的制备:将聚丙烯腈与四氢呋喃加入N,N-二甲基甲酰胺中,加入改性聚乙烯醇母液,搅拌混合均匀,在50-80℃恒温条件下搅拌至完全溶解,加入改性助剂,搅拌至充分均匀,静置消泡后得到复合料液,静电纺丝,得到聚丙烯腈/聚乙烯醇复合超细纤维;
S2.无纺布单体的制备:将喷出的纤维经牵伸气流牵引,吹向接收板,并收集到平板上,依靠自身的热黏合成为无纺布单体;
S3.无纺布的制备:将多个无纺布单体进行熔喷后得到无纺布;
S4.超柔软无纺布的制备:将无纺布浸入去离子水中,然后将所得无纺布先后转移至水、乙醇中,分别在4℃,25℃下浸泡15-30min,继续将无纺布浸泡在碱液中0.5-2h,取出,洗至中性后继续浸泡在酸液中0.5-2h,取出,洗至中性,随后在30℃下真空干燥,得到超柔软无纺布。
作为本发明的进一步改进,步骤S1中所述静电纺丝的方法为:将复合料液注入到注射器中,注射器针头与高电压相连,调节电压为10-15kV,复合料液的流量由注射泵控制为0.1-0.2mL/h,接收板接地。
作为本发明的进一步改进,步骤S1中所述聚丙烯腈、四氢呋喃、N,N-二甲基甲酰胺的质量比为100:(20-40):(150-300)。
作为本发明的进一步改进,步骤S4中所述碱液为(0.5-2)mol/L的碱液,所述碱选自NaOH、KOH、Ba(OH)2、Na2CO3和NaHCO3中的一种或几种混合。
作为本发明的进一步改进,步骤S4中所述碱液为(0.5-2)mol/L的酸液,所述酸选自HCl、H2SO4、HNO3、H3PO4和乙酸中的一种或几种混合。
本发明具有如下有益效果:
(1)本发明采用复合纺丝+水解剥离方法,采用复合纺丝法纺制成以聚丙烯腈为“岛”组分,以改性聚乙烯醇为“海组分”的“海-岛”型复合纤维。通过该工艺制备得到的复合纤维的平均线密度在2-2.5dtex,将这种复合纤维用水、碱液、酸液等溶剂处理,则可溶解掉海组分,得到表面凹凸不平的0.1-0.5dtex左右的超细纤维,采用超细纤维制备无纺布,其手感、覆盖性和蓬松性等有明显提高,具有极柔软的手感;
(2)本发明的高柔软度无纺布,通过采用甘油、聚乳酸和氧化石墨烯对聚乙烯醇进行改性,使其可以应用于熔喷工艺中,且发现,加入经特殊改性的聚乙烯醇母液进一步提高了无纺布的柔软度、轻薄感及吸水性能。
(3)通过添加抗氧化剂与紫外线吸收剂,不仅保证了生产的稳定性,而且增加无纺布的耐老化性能,有效地延长了无纺布的使用寿命。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1超柔软无纺布
原料组成(重量份):聚丙烯腈100份、改性聚乙烯醇母液30份、改性助剂10份;改性助剂由以下原料按重量份制备而成:二甲基硅油5份、微晶纤维素2份、对苯二胺1份、山梨酸钾1份、纳米氧化锌5份、石蜡3份、氨基聚硅氧烷微乳1份、苯并三唑类紫外线吸收剂0.5份和膨润土10份。
改性聚乙烯醇母液由以下方法制备而成:用去离子水淘洗100g聚乙烯醇颗粒,在恒温鼓风干燥箱中于50℃干燥5h,将干燥的聚乙烯醇颗粒加入去离子水中,在50℃下恒温搅拌溶胀1h后加入5g甘油,混合均匀后,加入10g聚乳酸和3g氧化石墨烯,在90℃下搅拌2h,冷却,真空抽气0.5h,除去溶液里的气泡,得到改性聚乙烯醇母液。
超柔软无纺布的制备方法,包括以下步骤:
S1.聚丙烯腈/聚乙烯醇复合超细纤维的制备:将100g聚丙烯腈与20g四氢呋喃加入150gN,N-二甲基甲酰胺中,加入改性聚乙烯醇母液,搅拌混合均匀,在50℃恒温条件下搅拌至完全溶解,加入改性助剂,搅拌至充分均匀,静置消泡后得到复合料液,静电纺丝,静电纺丝的方法为:将复合料液注入到注射器中,注射器针头与高电压相连,调节电压为10kV,复合料液的流量由注射泵控制为0.1mL/h,接收板接地,得到聚丙烯腈/聚乙烯醇复合超细纤维;
S2.无纺布单体的制备:将喷出的纤维经牵伸气流牵引,吹向接收板,并收集到平板上,依靠自身的热黏合成为无纺布单体;
S3.无纺布的制备:将多个无纺布单体进行熔喷后得到无纺布;
S4.超柔软无纺布的制备:将无纺布浸入去离子水中,然后将所得无纺布先后转移至水、乙醇中,分别在4℃,25℃下浸泡15min,继续将无纺布浸泡在0.5mol/L碱液中0.5h,取出,洗至中性后继续浸泡在0.5mol/L酸液中0.5h,取出,洗至中性,随后在30℃下真空干燥,得到超柔软无纺布。
实施例2超柔软无纺布
原料组成(重量份):聚丙烯腈200份、改性聚乙烯醇母液50份和改性助剂15份;改性助剂由以下原料按重量份制备而成:二甲基硅油10份、微晶纤维素5份、三(十二碳醇)酯3份、苯甲酸钠2份、纳米氧化锌10份、石蜡7份、端羟基聚硅氧烷乳液3份、三嗪类紫外线吸收剂1份和膨润土20份。
改性聚乙烯醇母液由以下方法制备而成:用去离子水淘洗100g聚乙烯醇颗粒,在恒温鼓风干燥箱中于60℃干燥10h,将干燥的聚乙烯醇颗粒加入去离子水中,在70℃下恒温搅拌溶胀2h后加入10g甘油,混合均匀后,加入20g聚乳酸和7g氧化石墨烯,在100℃下搅拌4h,冷却,真空抽气1h,除去溶液里的气泡,得到改性聚乙烯醇母液。
超柔软无纺布的制备方法,包括以下步骤:
S1.聚丙烯腈/聚乙烯醇复合超细纤维的制备:将100g聚丙烯腈与40g四氢呋喃加入300gN,N-二甲基甲酰胺中,加入改性聚乙烯醇母液,搅拌混合均匀,在80℃恒温条件下搅拌至完全溶解,加入改性助剂,搅拌至充分均匀,静置消泡后得到复合料液,静电纺丝,静电纺丝的方法为:将复合料液注入到注射器中,注射器针头与高电压相连,调节电压为15kV,复合料液的流量由注射泵控制为0.2mL/h,接收板接地,得到聚丙烯腈/聚乙烯醇复合超细纤维;
S2.无纺布单体的制备:将喷出的纤维经牵伸气流牵引,吹向接收板,并收集到平板上,依靠自身的热黏合成为无纺布单体;
S3.无纺布的制备:将多个无纺布单体进行熔喷后得到无纺布;
S4.超柔软无纺布的制备:将无纺布浸入去离子水中,然后将所得无纺布先后转移至水、乙醇中,分别在4℃,25℃下浸泡30min,继续将无纺布浸泡在2mol/L碱液中2h,取出,洗至中性后继续浸泡在2mol/L酸液中2h,取出,洗至中性,随后在30℃下真空干燥,得到超柔软无纺布。
实施例3超柔软无纺布
原料组成(重量份):聚丙烯腈150份、改性聚乙烯醇母液40份和改性助剂12份;改性助剂由以下原料按重量份制备而成:二甲基硅油7份、微晶纤维素3份、二氢喹啉2份、脱氢乙酸1.5份、纳米氧化锌7份、石蜡5份、氨基聚硅氧烷乳液3份、水杨酸酯类紫外线吸收剂0.7份、膨润土15份。
改性聚乙烯醇母液由以下方法制备而成:用去离子水淘洗100g聚乙烯醇颗粒,在恒温鼓风干燥箱中于55℃干燥7h,将干燥的聚乙烯醇颗粒加入去离子水中,在60℃下恒温搅拌溶胀1.5h后加入7g甘油,混合均匀后,加入15g聚乳酸和5g氧化石墨烯,在95℃下搅拌3h,冷却,真空抽气1h,除去溶液里的气泡,得到改性聚乙烯醇母液。
超柔软无纺布的制备方法,包括以下步骤:
S1.聚丙烯腈/聚乙烯醇复合超细纤维的制备:将100g聚丙烯腈与30g四氢呋喃加入220gN,N-二甲基甲酰胺中,加入改性聚乙烯醇母液,搅拌混合均匀,在75℃恒温条件下搅拌至完全溶解,加入改性助剂,搅拌至充分均匀,静置消泡后得到复合料液,静电纺丝,静电纺丝的方法为:将复合料液注入到注射器中,注射器针头与高电压相连,调节电压为12kV,复合料液的流量由注射泵控制为0.15mL/h,接收板接地,得到聚丙烯腈/聚乙烯醇复合超细纤维;
S2.无纺布单体的制备:将喷出的纤维经牵伸气流牵引,吹向接收板,并收集到平板上,依靠自身的热黏合成为无纺布单体;
S3.无纺布的制备:将多个无纺布单体进行熔喷后得到无纺布;
S4.超柔软无纺布的制备:将无纺布浸入去离子水中,然后将所得无纺布先后转移至水、乙醇中,分别在4℃,25℃下浸泡20min,继续将无纺布浸泡在1.2mol/L碱液中1h,取出,洗至中性后继续浸泡在1.2mol/L酸液中1h,取出,洗至中性,随后在30℃下真空干燥,得到超柔软无纺布。
对比例1
与实施例3相比,采用聚乙烯醇母液替代改性聚乙烯醇母液,其他条件均不改变。
对比例2、
与实施例3相比,改性聚乙烯醇母液制备过程中,不加入聚乳酸进行改性,其他条件均不改变。
改性聚乙烯醇母液由以下方法制备而成:用去离子水淘洗100g聚乙烯醇颗粒,在恒温鼓风干燥箱中于55℃干燥7h,将干燥的聚乙烯醇颗粒加入去离子水中,在60℃下恒温搅拌溶胀1.5h后加入7g甘油,混合均匀后,加入5g氧化石墨烯,在95℃下搅拌3h,冷却,真空抽气1h,除去溶液里的气泡,得到改性聚乙烯醇母液。
对比例3
与实施例3相比,改性聚乙烯醇母液制备过程中,采用聚乙二醇替换甘油,其他条件均不改变。
对比例4
与实施例3相比,未添加膨润土,其他条件均不改变。
对比例5
与实施例3相比,未添加纳米氧化锌,其他条件均不改变。
测试例1柔软度测试
依据GB/T8942-2016标准,采用市售微电脑纸张/织物柔软度测定仪(型号XD-SOFTNESS01,购自阿斯特朗电子科技有限公司)对实施例1-3和对比例1-5以及市售无纺布产品的纵向柔软度和横向柔软度进行检测,检测结果如下表1。
组别 | 纵向柔软度(mN) | 横向柔软度(mN) |
实施例1 | 27 | 30 |
实施例2 | 24 | 29 |
实施例3 | 22 | 27 |
对比例1 | 75 | 96 |
对比例2 | 80 | 105 |
对比例3 | 62 | 87 |
对比例4 | 59 | 77 |
对比例5 | 52 | 68 |
市售 | 120 | 143 |
注:试样本身的抗弯曲力和试样与缝隙处摩擦力的最大矢量之和,称之为试样的柔软度,仪器示值越小说明试样越柔软。
由上表可知,本发明制得的超柔软无纺布具有更低的纵向柔软度和横向柔软度,柔软性极佳,明显优于对比例1-5以及市售同类产品。
测试例2卫生性能及力学性能检测
实验对象:对实施例1-3和对比例1-5以及市售无纺布产品。
实验方法:采用静态透湿皿法测定透水汽性,分别按照GB/T1038-2000测定透气性,QB/T1670-92测定抗张强度,FZ/T60005-1991测定断裂伸长率,GB/T12829-2006测定撕裂强度。结果见表2。
表2
由上表可知,本发明实施例制得的超柔软无纺布透气性更好、力学性能更优,明显优于对比例1-5以及市售同类产品。
测试例3抗菌性能测试
按照CB/T20944.1-2007《纺织品抗菌性能的评价》中的琼脂平皿扩散法测定试样的抗菌性,试验菌种采用金黄色葡萄球菌ATCC25923和大肠杆菌ATCC25922,对实施例1-3和对比例1-5中抗菌效果进行测定,结果见表3。
表3试验结果
由上表可知,本发明实施例制得的超柔软无纺布还具有极好的抗菌性能,明显优于比例1-5以及市售同类产品。
测试例4吸水性能测试
实验对象:对实施例1-3和对比例1-5以及市售无纺布产品。
实验方法:参考GB/T1034-2008,将试样裁剪成5.0cm×5.0cm,置于恒温鼓风干燥箱50℃烘干至恒重,然后置于500mL的蒸馏水中,在室温24℃,浸泡24h后取出样品,用滤纸迅速吸干表面水分,然后称重(精确到0.0001g)。吸水率按式(1)计算:
η=(m1-m0)/m0×100%, (1)
式中:
η———吸水率,%;
m0———吸水前膜的质量,g;
m1———复合膜吸水后的质量,g。
结果见表4。
表4
由上表可知,本发明实施例制得的超柔软无纺布还具有极好的吸水性能,明显优于比例1-5以及市售同类产品。
综合分析,对比例1中与实施例3相比,采用普通聚乙烯醇替代改性聚乙烯醇母液,其制得的纤维平均线密度显著提高,为5.4dtex,且柔软性、抗菌性、力学性能、吸水性能等均明显下降,可见,改性聚乙烯醇采用聚乳酸对聚乙烯醇进行改性,使其更具有良好的抗菌性和力学性能,同时吸水性能也明显提高;
对比例2与实施例3相比,制备改性聚乙烯醇母液时未添加聚乳酸,其制得的纤维平均线密度显著提高,为1.3dtex,且吸水性、抗菌性、柔软性等性能显著下降,可见,聚乳酸对聚乙烯醇改性后作为纤维的“海”,溶解后能制得超细纤维,且能对纤维的吸水性、抗菌性等具有很好的提升。
对比例3与实施例3相比,采用聚乙二醇替代甘油,甘油在制备改性聚乙烯醇母液中的作用为增塑剂,能促进聚乙烯醇的改性效果,以聚乙二醇替代甘油后,改性效果下降,从而一定程度上影响了制得的无纺布的各项性能。
对比例4和对比例5中与实施例3相比,分别未添加膨润土或纳米氧化锌,得到的无纺布柔软性、吸水性显著下降,抗菌性能影响不大,可见,纳米氧化锌、膨润土的添加在提高无纺布柔软性及吸水性方面具有协同增效的作用;
与现有技术相比,本发明采用复合纺丝+水解剥离方法,采用复合纺丝法纺制成以聚丙烯腈为岛,以聚乙烯醇为海的“海-岛”型复合纤维。此法所得复合纤维的平均线密度在2-2.5dtex,将这种复合纤维用水、碱液、酸液等溶剂处理,则可溶解掉海组分,得到表面凹凸不平的0.1-0.5dtex左右的超细纤维,采用超细纤维制备无纺布,其手感、覆盖性和蓬松性等有明显提高,具有极柔软的手感;
本发明通过添加二甲基硅油、膨润土和纳米氧化锌,纺丝生产过程中迁移到纤维的表面,有效降低纤维表面的摩擦系数,进一步增加无纺布的柔软性。通过添加抗氧化剂与紫外线吸收剂,不仅保证了生产的稳定性,而且增加无纺布的耐老化性能,有效地延长了无纺布的使用寿命。本发明的高柔软度无纺布,通过添加改性聚乙烯醇母液,改善了粘合面的粘合性能、抗菌性能、可降解性能,大幅度降低施胶量,提升无纺布产品的轻薄感,从而不仅提高无纺布产品的品质,还达到了降低生产成本的效果。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种超柔软无纺布,其特征在于,主要由以下原料制备而成:聚丙烯腈、改性聚乙烯醇母液和改性助剂;所述改性助剂包括:二甲基硅油、微晶纤维素、抗氧化剂、防腐剂、纳米氧化锌、石蜡、柔软剂、紫外线吸收剂和膨润土。
2.根据权利要求1所述一种超柔软无纺布,其特征在于,由以下原料按重量份制备而成:聚丙烯腈100-200份、改性聚乙烯醇母液30-50份和改性助剂10-15份;所述改性助剂由以下原料按重量份制备而成:二甲基硅油5-10份、微晶纤维素2-5份、抗氧化剂1-3份、防腐剂1-2份、纳米氧化锌5-10份、石蜡3-7份、柔软剂1-3份、紫外线吸收剂0.5-1份和膨润土10-20份。
3.根据权利要求2所述的超柔软无纺布,其特征在于,由以下原料按重量份制备而成:聚丙烯腈150份、改性聚乙烯醇母液40份和改性助剂12份;所述改性助剂由以下原料按重量份制备而成:二甲基硅油7份、微晶纤维素3份、抗氧化剂2份、防腐剂1.5份、纳米氧化锌7份、石蜡5份、柔软剂3份、紫外线吸收剂0.7份和膨润土15份。
4.根据权利要求1~3任一所述的超柔软无纺布,其特征在于,所述改性聚乙烯醇母液由以下方法制备而成:用去离子水淘洗聚乙烯醇颗粒,在恒温鼓风干燥箱中于50-60℃干燥5-10h,将干燥的聚乙烯醇颗粒加入去离子水中,在50-70℃下恒温搅拌溶胀1-2h后加入甘油,混合均匀后,加入聚乳酸和氧化石墨烯,在90-100℃下搅拌2-4h,冷却,真空抽气0.5-1h,除去溶液里的气泡,得到改性聚乙烯醇母液。
5.根据权利要求4所述一种超柔软无纺布,其特征在于,所述聚乙烯醇颗粒、甘油、聚乳酸和氧化石墨烯的质量比为100:(5-10):(10-20):(3-7)。
6.根据权利要求1~3任一所述的超柔软无纺布,其特征在于,所述柔软剂选自聚乙烯蜡、端羟基聚硅氧烷乳液、亲水性有机硅柔软剂、氨基聚硅氧烷乳液、氨基聚硅氧烷微乳和双十八烷基二甲基氯化铵中的一种或几种混合;所述抗氧化剂选自二苯胺、对苯二胺、二氢喹啉、2,6-三级丁基-4-甲基苯酚、双(3,5-三级丁基-4-羟基苯基)硫醚、四〔β-(3,5-三级丁基-4-羟基苯基)丙酸〕季戊四醇酯、双十二碳醇酯、双十四碳醇酯和双十八碳醇酯、硫代二丙酸双酯、三辛酯、三癸酯、三(十二碳醇)酯和三(十六碳醇)酯中的一种或几种混合;所述防腐剂选自苯甲酸钠、山梨酸钾、脱氢乙酸、脱氢乙酸钠、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、双乙酸钠、丙酸钙和乳酸钠中的一种或几种混合;所述紫外线吸收剂选自水杨酸酯类紫外线吸收剂、二苯甲酮类紫外线吸收剂、苯并三唑类紫外线吸收剂、取代丙烯腈类紫外线吸收剂和三嗪类阿紫外线吸收剂中的一种或几种混合。
7.一种如权利要求1-6任一项权利要求所述超柔软无纺布的制备方法,其特征在于,包括以下步骤:
S1.聚丙烯腈/聚乙烯醇复合超细纤维的制备:将聚丙烯腈与四氢呋喃加入N,N-二甲基甲酰胺中,加入改性聚乙烯醇母液,搅拌混合均匀,在50-80℃恒温条件下搅拌至完全溶解,加入改性助剂,搅拌至充分均匀,静置消泡后得到复合料液,静电纺丝,得到聚丙烯腈/聚乙烯醇复合超细纤维;
S2.无纺布单体的制备:将喷出的纤维经牵伸气流牵引,吹向接收板,并收集到平板上,依靠自身的热黏合成为无纺布单体;
S3.无纺布的制备:将多个无纺布单体进行熔喷后得到无纺布;
S4.超柔软无纺布的制备:将无纺布浸入去离子水中,然后将所得无纺布先后转移至水、乙醇中,分别在4℃,25℃下浸泡15-30min;继续将无纺布浸泡在碱液中0.5-2h,取出,洗至中性后继续浸泡在酸液中0.5-2h,取出,洗至中性,随后在30℃下真空干燥,得到超柔软无纺布。
8.根据权利要求7所述的制备方法,其特征在于,步骤S1中所述静电纺丝的方法为:将复合料液注入到注射器中,注射器针头与高电压相连,调节电压为10-15kV,复合料液的流量由注射泵控制为0.1-0.2mL/h,接收板接地。
9.根据权利要求7所述的制备方法,其特征在于,步骤S1中所述聚丙烯腈、四氢呋喃、N,N-二甲基甲酰胺的质量比为100:(20-40):(150-300)。
10.根据权利要求7所述的制备方法,其特征在于,步骤S4中所述碱液为(0.5-2)mol/L的碱液,所述碱选自NaOH、KOH、Ba(OH)2、Na2CO3和NaHCO3中的一种或几种混合;所述酸液为(0.5-2)mol/L的酸液,所述酸选自HCl、H2SO4、HNO3、H3PO4和乙酸中的一种或几种混合。
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