CN112226865A - 一种防臭鞋内垫材料及其制备方法 - Google Patents
一种防臭鞋内垫材料及其制备方法 Download PDFInfo
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- CN112226865A CN112226865A CN202011044238.6A CN202011044238A CN112226865A CN 112226865 A CN112226865 A CN 112226865A CN 202011044238 A CN202011044238 A CN 202011044238A CN 112226865 A CN112226865 A CN 112226865A
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- particles
- antibacterial
- fiber
- raw material
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 56
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- 239000001509 sodium citrate Substances 0.000 claims abstract description 21
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 21
- -1 firstly Substances 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000009987 spinning Methods 0.000 claims abstract description 10
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- 238000003756 stirring Methods 0.000 claims description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 35
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 28
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 26
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 claims description 26
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 15
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- 230000007935 neutral effect Effects 0.000 claims description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001923 silver oxide Inorganic materials 0.000 claims description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 4
- 244000025254 Cannabis sativa Species 0.000 claims description 3
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Abstract
本发明公开了一种防臭鞋内垫材料及其制备方法,该材料由改性亲水纤维与抗菌填充纤维按照一定的重量比均匀混合后纺纱制得,在抗菌填充纤维的制备过程中,首先将活性炭颗粒加入将硝酸银水溶液中浸泡,使活性炭颗粒的孔隙结构中充分吸附有硝酸银溶液,然后通过再向硝酸银溶液中滴加柠檬酸钠去离子水溶液,以柠檬酸钠作为还原剂与包覆剂,生成纳米银颗粒,纳米银颗粒附着在活性炭颗粒的表面与孔隙结构中;然后通过将聚氨酯乳液形成乳液颗粒附着在抗菌粒子表面或聚氨酯乳液颗粒包覆在抗菌粒子表面的复合结构,由于聚氨酯乳液颗粒与将抗菌粒子均为纳米结构,能够保证抗菌吸附颗粒的孔隙结构未被堵塞,使抗菌吸附颗粒保持有良好的吸附效果。
Description
技术领域
本发明属于纺织材料技术领域,具体的,涉及一种防臭鞋内垫材料及其制备方法。
背景技术
鞋垫大量应用于制鞋业、保健、特殊功用;一般分为制鞋业应用型和市场商品型两种模式。制鞋业应用的鞋垫主要是配合鞋子大底、中底、做出相应的型体;按照楦底板或者面板制作尺码板,并制作出相应的形状。市场商品型鞋垫主要是把鞋垫直接作为一种商品出售,由开发师设计,在市场上流通的产品;
鞋垫作为长期与人的脚部长时间接触的部分,且长时间处于温度适宜且潮湿的环境中,十分有利于细菌的滋生,在长期的使用过程中,还会产生恶臭,对鞋垫与鞋的使用造成了明显的影响,因此现有技术中通过多种手段对鞋垫材料进行处理,其中常用的是采用化学整理液对鞋垫进行处理,虽然能够起到良好的抗菌效果,但是大部分化学整理液会对制备鞋垫的纺织纤维造成不利影响,导致鞋垫较硬,吸水性差,且在潮湿环境下会出现部分化学整理液所含物质对人体皮肤造成伤害,为了解决上述问题,本发明提供了以下技术方案。
发明内容
本发明的目的在于提供一种防臭鞋内垫材料及其制备方法。
本发明需要解决的技术问题为:
鞋垫作为长期与人的脚部长时间接触的部分,且长时间处于温度适宜且潮湿的环境中,十分有利于细菌的滋生,在长期的使用过程中,还会产生恶臭,对鞋垫与鞋的使用造成了明显的影响,因此现有技术中通过多种手段对鞋垫材料进行处理,其中常用的是采用化学整理液对鞋垫进行处理,虽然能够起到良好的抗菌效果,但是大部分化学整理液会对制备鞋垫的纺织纤维造成不利影响,导致鞋垫较硬,吸水性差,且在潮湿环境下会出现部分化学整理液所含物质对人体皮肤造成伤害。
本发明的目的可以通过以下技术方案实现:
一种防臭鞋内垫材料,由改性亲水纤维与抗菌填充纤维按照1:0.3-0.8的重量比均匀混合后纺纱得到;
所述改性亲水纤维的制备方法为:
步骤一、对原料纤维进行碱处理;
步骤二、将马来酸酐加入N-N二甲基甲酰胺中,混合搅拌溶解后,将步骤一中处理得到的原料纤维加入其中,在90-110℃的温度下加热反应3h;通过去离子水与丙酮分别对原料纤维进行洗涤,去除原料纤维表面的马来酸酐,最后在40-48℃的温度下烘干,得到接枝原料纤维;
其中马来酸酐与N-N二甲基甲酰胺两者的重量比为3:3.5-4;
该步骤通过加热反应使马来酸酐接枝在原料纤维上,在原料纤维的表面引入羧基;
步骤三、配制摩尔浓度为0.04-0.13mol/L的硝酸银溶液,将接枝原料纤维加入其中后搅拌分散均匀后,在60-120KHz的条件下超声处理10-15min,然后在25-40℃的温度下搅拌反应1.5-2.5h,过滤取出接枝原料纤维,用去离子水冲洗三遍后,在35-40℃的温度下烘干,得到改性亲水纤维;
该步骤中首先对原料纤维进行表面改性,使马来酸酐接枝在原料纤维表面,在原料纤维的表面引入羧基,然后再将接枝处理后的原料纤维加入硝酸银溶液中,通过金属离子与羧基接枝在原料纤维的表面引入具有抗菌作用的银离子,使得到的改性亲水纤维在保持良好的亲水性能之外,还具有优异的抗菌性能。
步骤一中所述原料纤维包括棉纤维、麻纤维中的一种或两种的混合物;
步骤一中对原料纤维进行碱处理的具体步骤为:
将原料纤维加入质量浓度为1%的NaOH水溶液中,加热至65-90℃后保温处理30-40min,然后向其中加入NaOH,调节NaOH水溶液的质量浓度为3%-4%,向其中加入双氧水,保温继续反应120-130min后,过滤取出棉纤维,去离子水洗涤至中性后,在45-60℃的温度下烘干干燥后待用,其中双氧水的添加量为8g/L;该步骤能够对棉纤维表面的果胶、半纤维素与木质素等杂质去除,从而提升棉纤维表面的粗糙度,使其具有蓬松感;
所述抗菌填充纤维的制备方法为:
第一步,制备改性聚醚酯纤维;
第二步,制备抗菌吸附颗粒,具体包括如下步骤:
将活性炭颗粒加入去离子水与乙醇的混合溶液中,在80-160KHz,50-70℃的温度下超声处理10-20min后,过滤,在60-70℃温度下烘干,得到清洗后的活性炭颗粒待用,该活性炭颗粒的粒径为5-15μm;
配制浓度为4-20g/L的硝酸银溶液,将上一步骤处理过的活性炭颗粒加入其中,在频率40-80KHz,温度15-30℃的条件下浸泡6-10min,然后加热至沸腾,并向其中滴加浓度为1-4g/100mL的柠檬酸钠去离子水溶液,滴加过程中保持超声处理,待柠檬酸钠去离子水溶液完全滴加后,继续煮沸与超声处理3-6min后,自然冷却至室温,得到抗菌吸附颗粒前体,柠檬酸钠去离子水溶液在10min内完全滴加;
在该步骤中,首先将活性炭颗粒加入将硝酸银水溶液中浸泡,使活性炭颗粒的孔隙结构中充分吸附有硝酸银溶液,然后再通过在高温环境下向硝酸银溶液中滴加柠檬酸钠去离子水溶液,以柠檬酸钠作为还原剂与包覆剂,生成纳米银颗粒,纳米银颗粒附着在活性炭颗粒的表面与孔隙结构中;
配制固含量为20%-27%的聚氨酯乳液,聚氨酯乳液的颗粒直径为1-25nm,再配制浓度为0.8-21g/L的抗菌粒子的去离子水分散液,对抗菌粒子的去离子水分散液进行搅拌,并在搅拌过程中向其中加入聚氨酯乳液,然后提升转速至1600-3000r/min,搅拌20-35min,得到处理液待用,其中聚氨酯乳液与抗菌粒子的去离子水分散液的体积比为1:0.4-1.4;
所述抗菌粒子包括纳米氧化锌、纳米氧化银与纳米二氧化钛中的一种或至少两种的任意比混合物;
将抗菌吸附颗粒前体加入上一步骤制备得到的处理液中,在转速为400-600r/min的条件下搅拌处理15-19min后,将抗菌吸附颗粒前体过滤分离后在65-75℃温度下烘干干燥,得到抗菌吸附颗粒;
在该步骤中,首先通过将聚氨酯乳液与抗菌粒子的分散液高速混合,形成聚氨酯乳液颗粒附着在抗菌粒子表面或聚氨酯乳液颗粒包覆在抗菌粒子表面的复合结构,然后再通过将制备得到的处理液与抗菌吸附颗粒前体混合,由于聚氨酯乳液颗粒与将抗菌粒子均属于纳米结构,能够进入抗菌吸附颗粒前体的孔隙结构中,对抗菌吸附颗粒前体表面与孔隙结构中原有的纳米银颗粒进行固定,同时将大量的抗菌粒子固定在抗菌吸附颗粒前体的表面或孔隙结构中,从而保证抗菌吸附颗粒的孔隙结构未被堵塞,使抗菌吸附颗粒保持有良好的吸附效果;
第三步,配制固含量为12%-20%的水性环氧树脂乳液,然后将上一步骤制备的抗菌吸附颗粒加入其中,在转速400-600r/min的条件下搅拌处理10-17min,然后在频率40-60KHz的条件下超声处理5-9min,然后将改性聚醚酯纤维加入其中静置浸泡7-15min后,将改性聚醚酯纤维过滤分离后在65℃温度下烘干干燥,得到抗菌填充纤维;
其中抗菌吸附颗粒与水性环氧树脂乳液的重量比为1:11-16;
在该步骤中,通过将成型的抗菌吸附颗粒加入水性环氧树脂乳液中超声与搅拌处理,使水性环氧树脂颗粒附着在抗菌吸附颗粒的表面,然后再以附着的环氧树脂颗粒作为胶粘剂,将抗菌吸附颗粒固定在聚醚酯纤维的表面。
所述改性聚醚酯纤维的制备方法为:
S31、按比例将对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑加入聚合反应釜中,搅拌混合均匀后,向其中加入丙三醇与填充颗粒,其中丙三醇为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的0.5%-1.5%,填充颗粒为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的0.5%-1.5%;
所述填充颗粒为纳米氧化锌、纳米氧化银与纳米二氧化钛中的一种或至少两种的任意比混合物;
S32、将上述混合物在100℃温度下抽真空脱水后,提升反应温度至200℃,当甲醇馏出量达到理论馏出量的90%时,提升反应温度至250℃,在真空条件下,保温缩聚反应3-4h后,得到聚醚酯原料;
S33、将步骤S32中得到聚醚酯原料首先在80℃下保温干燥10h,然后在105℃下保温干燥48h后,通过熔融纺丝法,将聚醚酯原料纺丝制成改性聚醚酯纤维;
在该步骤中,丙三醇能够提升相邻分子之间的相互作用力,降低大分子之间的相互滑移,纤维具有良好的可逆弹性形变,而填充颗粒的纳米结构导致其表面具有较高表面表面能,对聚合物的大分子链具有较强的吸附作用,从而形成空间网状结构,同样提升了分子间的相互作用力,降低了大分子之间的相互滑移,使纤维具有良好的可逆弹性形变,同时,均匀分散在聚醚酯纤维中的填充颗粒暴露在聚醚酯纤维表面的部分具有良好的抗菌抑菌效果。
本发明的有益效果:
本发明所述一种防臭鞋内垫材料由改性亲水纤维与抗菌填充纤维按照一定的重量比均匀混合后纺纱制得,在改性亲水纤维的制备过程中,首先通过加热反应使马来酸酐接枝在原料纤维上,在原料纤维的表面引入羧基,然后再将接枝处理后的原料纤维加入硝酸银溶液中,通过金属离子与羧基接枝在原料纤维的表面引入具有抗菌作用的银离子,使得到的改性亲水纤维在保持良好的亲水性能之外,还具有优异的抗菌性能;而在抗菌填充纤维的制备过程中,首先将活性炭颗粒加入将硝酸银水溶液中浸泡,使活性炭颗粒的孔隙结构中充分吸附有硝酸银溶液,然后再通过在高温环境下向硝酸银溶液中滴加柠檬酸钠去离子水溶液,以柠檬酸钠作为还原剂与包覆剂,生成纳米银颗粒,纳米银颗粒附着在活性炭颗粒的表面与孔隙结构中;然后通过将聚氨酯乳液与抗菌粒子的分散液高速混合,形成聚氨酯乳液颗粒附着在抗菌粒子表面或聚氨酯乳液颗粒包覆在抗菌粒子表面的复合结构,然后再通过将制备得到的处理液与抗菌吸附颗粒前体混合,由于聚氨酯乳液颗粒与将抗菌粒子均属于纳米结构,能够进入抗菌吸附颗粒前体的孔隙结构中,对抗菌吸附颗粒前体表面与孔隙结构中原有的纳米银颗粒进行固定,同时将大量的抗菌粒子固定在抗菌吸附颗粒前体的表面或孔隙结构中,从而保证抗菌吸附颗粒的孔隙结构未被堵塞,使抗菌吸附颗粒保持有良好的吸附效果;再然后通过将成型的抗菌吸附颗粒加入水性环氧树脂乳液中超声与搅拌处理,使水性环氧树脂颗粒附着在抗菌吸附颗粒的表面,然后再以附着的环氧树脂颗粒作为胶粘剂,将抗菌吸附颗粒固定在聚醚酯纤维的表面;在聚氨酯纤维的制备过程中,丙三醇能够提升相邻分子之间的相互作用力,降低大分子之间的相互滑移,纤维具有良好的可逆弹性形变,而填充颗粒的纳米结构导致其表面具有较高表面表面能,对聚合物的大分子链具有较强的吸附作用,从而形成空间网状结构,同样提升了分子间的相互作用力,降低了大分子之间的相互滑移,使纤维具有良好的可逆弹性形变,同时,均匀分散在聚醚酯纤维中的填充颗粒暴露在聚醚酯纤维表面的部分具有良好的抗菌抑菌效果。
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作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
一种防臭鞋内垫材料,由改性亲水纤维与抗菌填充纤维按照1:0.4的重量比均匀混合后纺纱得到;
所述改性亲水纤维的制备方法为:
步骤一、对原料纤维进行碱处理;
步骤二、将马来酸酐加入N-N二甲基甲酰胺中,混合搅拌溶解后,将步骤一中处理得到的原料纤维加入其中,在98℃的温度下加热反应3h;通过去离子水与丙酮分别对原料纤维进行洗涤,去除原料纤维表面的马来酸酐,最后在45℃的温度下烘干,得到接枝原料纤维;
其中马来酸酐与N-N二甲基甲酰胺两者的重量比为3:4;
步骤三、配制摩尔浓度为0.09mol/L的硝酸银溶液,将接枝原料纤维加入其中后搅拌分散均匀后,在80KHz的条件下超声处理12min,然后在30℃的温度下搅拌反应2h,过滤取出接枝原料纤维,用去离子水冲洗三遍后,在40℃的温度下烘干,得到改性亲水纤维;
步骤一中所述原料纤维为棉纤维;
步骤一中对原料纤维进行碱处理的具体步骤为:
将原料纤维加入质量浓度为1%的NaOH水溶液中,加热至80℃后保温处理35min,然后向其中加入NaOH,调节NaOH水溶液的质量浓度为4%,向其中加入双氧水,保温继续反应120min后,过滤取出棉纤维,去离子水洗涤至中性后,在55℃的温度下烘干干燥后待用,其中双氧水的添加量为8g/L;
所述抗菌填充纤维的制备方法为:
第一步,制备改性聚醚酯纤维;
第二步,制备抗菌吸附颗粒,具体包括如下步骤:
将活性炭颗粒加入去离子水与乙醇的混合溶液中,在120KHz,60℃的温度下超声处理15min后,过滤,在65℃温度下烘干,得到清洗后的活性炭颗粒待用,该活性炭颗粒的粒径为10μm;
配制浓度为12g/L的硝酸银溶液,将上一步骤处理过的活性炭颗粒加入其中,在频率60KHz,温度20℃的条件下浸泡8min,然后加热至沸腾,并向其中滴加浓度为2.4g/100mL的柠檬酸钠去离子水溶液,滴加过程中保持超声处理,待柠檬酸钠去离子水溶液完全滴加后,继续煮沸与超声处理4.5min后,自然冷却至室温,得到抗菌吸附颗粒前体,柠檬酸钠去离子水溶液在10min内完全滴加;
配制固含量为23%的聚氨酯乳液,聚氨酯乳液的颗粒直径为1-10nm,再配制浓度为11g/L的抗菌粒子的去离子水分散液,对抗菌粒子的去离子水分散液进行搅拌,并在搅拌过程中向其中加入聚氨酯乳液,然后提升转速至2600r/min,搅拌30min,得到处理液待用,其中聚氨酯乳液与抗菌粒子的去离子水分散液的体积比为1:1.1;
所述抗菌粒子为纳米氧化锌;
将抗菌吸附颗粒前体加入上一步骤制备得到的处理液中,在转速为480r/min的条件下搅拌处理16min后,将抗菌吸附颗粒前体过滤分离后在70℃温度下烘干干燥,得到抗菌吸附颗粒;
第三步,配制固含量为16%的水性环氧树脂乳液,然后将上一步骤制备的抗菌吸附颗粒加入其中,在转速480r/min的条件下搅拌处理13min,然后在频率50KHz的条件下超声处理7min,然后将改性聚醚酯纤维加入其中静置浸泡12min后,将改性聚醚酯纤维过滤分离后在65℃温度下烘干干燥,得到抗菌填充纤维;
其中抗菌吸附颗粒与水性环氧树脂乳液的重量比为1:13;
所述改性聚醚酯纤维的制备方法为:
S31、按比例将对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑加入聚合反应釜中,搅拌混合均匀后,向其中加入丙三醇与填充颗粒,其中丙三醇为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的0.9%,填充颗粒为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的0.7%;
所述填充颗粒为纳米氧化锌;
S32、将上述混合物在100℃温度下抽真空脱水后,提升反应温度至200℃,当甲醇馏出量达到理论馏出量的90%时,提升反应温度至250℃,在真空条件下,保温缩聚反应3.5h后,得到聚醚酯原料;
S33、将步骤S32中得到聚醚酯原料首先在80℃下保温干燥10h,然后在105℃下保温干燥48h后,通过熔融纺丝法,将聚醚酯原料纺丝制成改性聚醚酯纤维。
实施例2
一种防臭鞋内垫材料,由改性亲水纤维与抗菌填充纤维按照1:0.3-0.8的重量比均匀混合后纺纱得到;
所述改性亲水纤维的制备方法为:
步骤一、对原料纤维进行碱处理;
步骤二、将马来酸酐加入N-N二甲基甲酰胺中,混合搅拌溶解后,将步骤一中处理得到的原料纤维加入其中,在105℃的温度下加热反应3h;通过去离子水与丙酮分别对原料纤维进行洗涤,去除原料纤维表面的马来酸酐,最后在40-48℃的温度下烘干,得到接枝原料纤维;
其中马来酸酐与N-N二甲基甲酰胺两者的重量比为3:4;
步骤三、配制摩尔浓度为0.10mol/L的硝酸银溶液,将接枝原料纤维加入其中后搅拌分散均匀后,在80KHz的条件下超声处理12min,然后在35℃的温度下搅拌反应2h,过滤取出接枝原料纤维,用去离子水冲洗三遍后,在40℃的温度下烘干,得到改性亲水纤维;
步骤一中所述原料纤维包括棉纤维、麻纤维中的一种或两种的混合物;
步骤一中对原料纤维进行碱处理的具体步骤为:
将原料纤维加入质量浓度为1%的NaOH水溶液中,加热至80℃后保温处理35min,然后向其中加入NaOH,调节NaOH水溶液的质量浓度为3.5%,向其中加入双氧水,保温继续反应125min后,过滤取出棉纤维,去离子水洗涤至中性后,在50℃的温度下烘干干燥后待用,其中双氧水的添加量为8g/L;
所述抗菌填充纤维的制备方法为:
第一步,制备改性聚醚酯纤维;
第二步,制备抗菌吸附颗粒,具体包括如下步骤:
将活性炭颗粒加入去离子水与乙醇的混合溶液中,在140KHz,65℃的温度下超声处理16min后,过滤,在65℃温度下烘干,得到清洗后的活性炭颗粒待用,该活性炭颗粒的粒径为5-8μm;
配制浓度为13g/L的硝酸银溶液,将上一步骤处理过的活性炭颗粒加入其中,在频率65KHz,温度25℃的条件下浸泡8min,然后加热至沸腾,并向其中滴加浓度为2.5g/100mL的柠檬酸钠去离子水溶液,滴加过程中保持超声处理,待柠檬酸钠去离子水溶液完全滴加后,继续煮沸与超声处理4.5min后,自然冷却至室温,得到抗菌吸附颗粒前体,柠檬酸钠去离子水溶液在10min内完全滴加;
配制固含量为24%的聚氨酯乳液,聚氨酯乳液的颗粒直径为1-7nm,再配制浓度为13g/L的抗菌粒子的去离子水分散液,对抗菌粒子的去离子水分散液进行搅拌,并在搅拌过程中向其中加入聚氨酯乳液,然后提升转速至2600r/min,搅拌30min,得到处理液待用,其中聚氨酯乳液与抗菌粒子的去离子水分散液的体积比为1:0.7;
所述抗菌粒子为纳米氧化锌;
将抗菌吸附颗粒前体加入上一步骤制备得到的处理液中,在转速为600r/min的条件下搅拌处理15min后,将抗菌吸附颗粒前体过滤分离后在70℃温度下烘干干燥,得到抗菌吸附颗粒;
第三步,配制固含量为18%的水性环氧树脂乳液,然后将上一步骤制备的抗菌吸附颗粒加入其中,在转速580r/min的条件下搅拌处理14min,然后在频率50KHz的条件下超声处理7min,然后将改性聚醚酯纤维加入其中静置浸泡14min后,将改性聚醚酯纤维过滤分离后在65℃温度下烘干干燥,得到抗菌填充纤维;
其中抗菌吸附颗粒与水性环氧树脂乳液的重量比为1:14;
所述改性聚醚酯纤维的制备方法为:
S31、按比例将对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑加入聚合反应釜中,搅拌混合均匀后,向其中加入丙三醇与填充颗粒,其中丙三醇为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的1.2%,填充颗粒为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的1.2%;
所述填充颗粒为纳米氧化锌;
S32、将上述混合物在100℃温度下抽真空脱水后,提升反应温度至200℃,当甲醇馏出量达到理论馏出量的90%时,提升反应温度至250℃,在真空条件下,保温缩聚反应4h后,得到聚醚酯原料;
S33、将步骤S32中得到聚醚酯原料首先在80℃下保温干燥10h,然后在105℃下保温干燥48h后,通过熔融纺丝法,将聚醚酯原料纺丝制成改性聚醚酯纤维。
对比例1
所述抗菌填充纤维的制备方法为:
第一步,制备改性聚醚酯纤维;
第二步,制备抗菌吸附颗粒,具体包括如下步骤:
配制浓度为12g/L的硝酸银溶液,然后加热至沸腾,并向其中滴加浓度为2.4g/100mL的柠檬酸钠去离子水溶液,滴加过程中保持超声处理,待柠檬酸钠去离子水溶液完全滴加后,继续煮沸与超声处理4.5min后,自然冷却至室温,得到抗菌吸附颗粒前体,柠檬酸钠去离子水溶液在10min内完全滴加;
第三步,配制固含量为16%的水性环氧树脂乳液,然后将上一步骤制备的抗菌吸附颗粒前体加入其中,在转速480r/min的条件下搅拌处理13min,然后在频率50KHz的条件下超声处理7min,然后将改性聚醚酯纤维加入其中静置浸泡12min后,将改性聚醚酯纤维过滤分离后在65℃温度下烘干干燥,得到抗菌填充纤维;
其中抗菌吸附颗粒前体与水性环氧树脂乳液的重量比为1:13。
对比例2
所述改性聚醚酯纤维的制备方法为:
S31、按比例将对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑加入聚合反应釜中,搅拌混合均匀后;
S32、将上述混合物在100℃温度下抽真空脱水后,提升反应温度至200℃,当甲醇馏出量达到理论馏出量的90%时,提升反应温度至250℃,在真空条件下,保温缩聚反应3.5h后,得到聚醚酯原料;
S33、将步骤S32中得到聚醚酯原料首先在80℃下保温干燥10h,然后在105℃下保温干燥48h后,通过熔融纺丝法,将聚醚酯原料纺丝制成改性聚醚酯纤维。
对实施例1-2以及对比例1-2中的纱线的抗菌性(GB/T20944.3-2008)、断裂强力、吸附性(将材料放置在30℃,湿度为80%的阴暗环境中静置一周后,观察其状态与味道)以及手感进行测试,具体结果见表1;
表1
大肠杆菌抑菌率/% | 断裂强力/cN | 手感 | 吸附性 | |
实施例1 | >99.9% | 197.3 | 柔软有弹性 | 无异味 |
实施例2 | >99.9% | 201.7 | 柔软有弹性 | 无异味 |
对比例1 | >99.9% | 198.6 | 柔软有弹性 | 有明显异味 |
对比例2 | >99.9% | 176.1 | 柔软,弹性较差 | 无异味 |
由上述结果可知,本发明具有良好的抗菌性与吸附性能,能够及时的对气味分子进行吸附破坏,还能够对细菌进行吸附与灭杀,不会对人体皮肤造成伤害。
以上内容仅仅是对本发明结构所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的结构或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (10)
1.一种防臭鞋内垫材料的制备方法,其特征在于,将改性亲水纤维与抗菌填充纤维按照1:0.3-0.8的重量比均匀混合后纺纱,得到防臭鞋内垫材料;
所述改性亲水纤维的制备方法为:
步骤一、对原料纤维进行碱处理;
步骤二、将马来酸酐加入N-N二甲基甲酰胺中,混合搅拌溶解后,将步骤一中处理得到的原料纤维加入其中,在90-110℃的温度下加热反应3h;通过去离子水与丙酮分别对原料纤维进行洗涤,去除原料纤维表面的马来酸酐,最后在40-48℃的温度下烘干,得到接枝原料纤维;
步骤三、配制摩尔浓度为0.04-0.13mol/L的硝酸银溶液,将接枝原料纤维加入其中后搅拌分散均匀,在60-120KHz的条件下超声处理10-15min,然后在25-40℃的温度下搅拌反应1.5-2.5h,过滤取出接枝原料纤维,用去离子水冲洗三遍后,在35-40℃的温度下烘干,得到改性亲水纤维。
2.根据权利要求1所述的一种防臭鞋内垫材料的制备方法,其特征在于,步骤二中马来酸酐与N-N二甲基甲酰胺两者的重量比为3:3.5-4。
3.根据权利要求1所述的一种防臭鞋内垫材料的制备方法,其特征在于,步骤一中所述原料纤维包括棉纤维、麻纤维中的一种或两种的混合物。
4.根据权利要求1所述的一种防臭鞋内垫材料的制备方法,其特征在于,步骤一中对原料纤维进行碱处理的具体步骤为:
将原料纤维加入质量浓度为1%的NaOH水溶液中,加热至65-90℃后保温处理30-40min,然后向其中加入NaOH,调节NaOH水溶液的质量浓度为3%-4%,向其中加入双氧水,保温继续反应120-130min后,过滤取出棉纤维,去离子水洗涤至中性后,在45-60℃的温度下烘干干燥后待用,其中双氧水的添加量为8g/L。
5.根据权利要求1所述的一种防臭鞋内垫材料的制备方法,其特征在于,所述抗菌填充纤维的制备方法为:
第一步,制备改性聚醚酯纤维;
第二步,制备抗菌吸附颗粒,具体包括如下步骤:
将活性炭颗粒加入去离子水与乙醇的混合溶液中,在80-160KHz,50-70℃的温度下超声处理10-20min后,过滤,在60-70℃温度下烘干,得到清洗后的活性炭颗粒待用,该活性炭颗粒的粒径为5-15μm;
配制浓度为4-20g/L的硝酸银溶液,将上一步骤处理过的活性炭颗粒加入其中,在频率40-80KHz,温度15-30℃的条件下浸泡6-10min,然后加热至沸腾,并向其中滴加浓度为1-4g/100mL的柠檬酸钠去离子水溶液,滴加过程中保持超声处理,待柠檬酸钠去离子水溶液完全滴加后,继续煮沸与超声处理3-6min后,自然冷却至室温,得到抗菌吸附颗粒前体,柠檬酸钠去离子水溶液在10min内完全滴加;
配制固含量为20%-27%的聚氨酯乳液,聚氨酯乳液的颗粒直径为1-25nm,再配制浓度为0.8-21g/L的抗菌粒子的去离子水分散液,对抗菌粒子的去离子水分散液进行搅拌,并在搅拌过程中向其中加入聚氨酯乳液,然后提升转速至1600-3000r/min,搅拌20-35min,得到处理液待用,其中聚氨酯乳液与抗菌粒子的去离子水分散液的体积比为1:0.4-1.4;
将抗菌吸附颗粒前体加入上一步骤制备得到的处理液中,在转速为400-600r/min的条件下搅拌处理15-19min后,将抗菌吸附颗粒前体过滤分离后在65-75℃温度下烘干干燥,得到抗菌吸附颗粒;
第三步,配制固含量为12%-20%的水性环氧树脂乳液,然后将上一步骤制备的抗菌吸附颗粒加入其中,在转速400-600r/min的条件下搅拌处理10-17min,然后在频率40-60KHz的条件下超声处理5-9min,然后将改性聚醚酯纤维加入其中静置浸泡7-15min后,将改性聚醚酯纤维过滤分离后在65℃温度下烘干干燥,得到抗菌填充纤维。
6.根据权利要求5所述的一种防臭鞋内垫材料的制备方法,其特征在于,第二步中所述抗菌粒子包括纳米氧化锌、纳米氧化银与纳米二氧化钛中的一种或至少两种的任意比混合物。
7.根据权利要求5所述的一种防臭鞋内垫材料的制备方法,其特征在于,第三步中抗菌吸附颗粒与水性环氧树脂乳液的重量比为1:11-16。
8.根据权利要求5所述的一种防臭鞋内垫材料的制备方法,其特征在于,所述改性聚醚酯纤维的制备方法为:
S31、按比例将对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑加入聚合反应釜中,搅拌混合均匀后,向其中加入丙三醇与填充颗粒,其中丙三醇为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的0.5%-1.5%,填充颗粒为对苯二甲酸二甲酯、1,4-丁二醇与聚氧丁撑总重的0.5%-1.5%;
S32、将上述混合物在100℃温度下抽真空脱水后,提升反应温度至200℃,当甲醇馏出量达到理论馏出量的90%时,提升反应温度至250℃,在真空条件下,保温缩聚反应3-4h后,得到聚醚酯原料;
S33、将步骤S32中得到聚醚酯原料首先在80℃下保温干燥10h,然后在105℃下保温干燥48h后,通过熔融纺丝法,将聚醚酯原料纺丝制成改性聚醚酯纤维。
9.根据权利要求8所述的一种防臭鞋内垫材料的制备方法,其特征在于,所述填充颗粒为纳米氧化锌、纳米氧化银与纳米二氧化钛中的一种或至少两种的任意比混合物。
10.一种防臭鞋内垫材料,其特征在于,根据权利要求1至9任一所述的制备方法制备而成。
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CN114775095B (zh) * | 2022-05-13 | 2022-12-09 | 芯安健康科技(广东)有限公司 | 一种抗菌防霉除醛消臭多功能软体芯片及其制备方法 |
CN114905806A (zh) * | 2022-05-24 | 2022-08-16 | 瑞安市大虎鞋业有限公司 | 一种基于抗菌纤维的除臭鞋垫及其制备方法 |
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