CN107904935A - 疏水蚕丝织物及其制备方法和应用 - Google Patents
疏水蚕丝织物及其制备方法和应用 Download PDFInfo
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- CN107904935A CN107904935A CN201711216741.3A CN201711216741A CN107904935A CN 107904935 A CN107904935 A CN 107904935A CN 201711216741 A CN201711216741 A CN 201711216741A CN 107904935 A CN107904935 A CN 107904935A
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- Prior art keywords
- silk fabric
- hydrophobic
- preparation
- water
- hydrophobic silk
- Prior art date
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- -1 alkyl Compound Chemical class 0.000 claims description 6
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- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
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- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
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- NPGIHFRTRXVWOY-UHFFFAOYSA-N Oil red O Chemical compound Cc1ccc(C)c(c1)N=Nc1cc(C)c(cc1C)N=Nc1c(O)ccc2ccccc12 NPGIHFRTRXVWOY-UHFFFAOYSA-N 0.000 description 1
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- 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
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
- D06M13/238—Tannins, e.g. gallotannic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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- 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
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- 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
- D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
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- 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
- D06M13/152—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 having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
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- 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
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- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明提供了一种疏水蚕丝织物的制备方法,包括以下步骤:将蚕丝织物浸泡于水和有机溶剂的混合溶液中,向其中加入植物多酚、酶催化剂和铜盐助催化剂,调节pH至2‑6,再加入含烷基的疏水化合物,在25‑65℃下反应0.5‑6h,得到疏水蚕丝织物。本发明还提供了一种采用上述制备方法所得到的疏水蚕丝织物。本发明还公开了上述制备方法所得到的疏水蚕丝织物在油水分离中的应用。本发明的方法简单、环保、高效,反应条件温和,所制备的疏水蚕丝织物在各种环境中具有稳定的疏水能力,且可用于油水分离领域。
Description
技术领域
本发明涉及纺织领域以及油水分离技术领域,尤其涉及一种疏水蚕丝织物及其制备方法和应用。
背景技术
在自然界中存在很多天然的疏水表面,最常见的就是荷叶和蚊子眼睛。目前,超疏水材料已经被应用于很多领域,如油水分离、减阻、自清洁和防污等。人们利用很多方法模拟超疏水表面,如气象沉积法、等离子体刻蚀、溶胶-凝胶法和浸渍法等。然而,从环境和可持续发展的角度看,现有方法存在很多缺陷:如需复杂的工艺、有机溶剂和含氟物质(一般都有毒,难降解)的使用、原材料价格贵等。因此,目前亟需一种简单、环境友好和低成本的方法制备超疏水材料。
蚕丝在中国已经有几千年的使用历史,并广泛用于纺织行业中。其性能优异,容易获得,蚕丝织物已经被用于多种改性研究中,包括抗紫外和阻燃,甚至抗拒和电化学。为了满足人们日益增长的需要,功能化蚕丝织物的制备已经被广泛研究。蚕丝织物本身具有很多反应性功能基团,可以在此基础上附加低表面能物质,制备超疏水蚕丝织物。同时,受自然界启发的现象也被广泛研究,代表性的有受贻贝邻苯二酚启发的超疏水表面制备方法。该方法一般分为三步:通过邻苯二酚的自聚,构造聚邻苯二酚表面涂层;通过自聚物的还原性制备纳米微粗糙度;通过迈克尔加成或者席夫碱反应接枝带有H2N-或HS-基团的低表面能的物质。然而,上述反应常使用多巴胺,而且制备过程非常耗时(一般为24小时)且成本高。因此探索制备廉价、环境友好、制备工艺简单的超疏水蚕丝织物具有很大意义。
近年来,油水分离的材料的研究非常广泛,但是目前的油水分离材料价格昂贵,材料本身的制备过程复杂,且分离效率还有不足,且分离过程浪费能源,因此,研究可连续高效的油水分离技术在实际应用中具有很高的应用价值。
发明内容
为解决上述技术问题,本发明的目的是提供一种疏水蚕丝织物及其制备方法和应用,本发明的方法简单、环保、高效,反应条件温和,所制备的疏水蚕丝织物在各种环境中具有稳定的疏水能力,且可用于油水分离领域。
在一方面,本发明提供了一种疏水蚕丝织物的制备方法,包括以下步骤:
将蚕丝织物浸泡于水和有机溶剂的混合溶液中,向其中加入植物多酚、酶催化剂和铜盐助催化剂,调节pH至2-6,再加入含烷基的疏水化合物,在25-65℃下反应0.5-6h,得到疏水蚕丝织物。
进一步地,蚕丝织物与混合溶液的质量比为0.1-1:50-200。
进一步地,有机溶剂为乙醇、甲醇和丙酮中的一种或几种。优选地,有机溶剂为乙醇。
进一步地,混合溶液中水和有机溶剂的体积比为1:9-9:1。
进一步地,酶催化剂为漆酶或酪氨酸酶;铜盐助催化剂为硫酸铜或氯化铜。优选地,酶催化剂为漆酶,铜盐助催化剂为硫酸铜。
进一步地,植物多酚为单宁酸、茶多酚、绿原酸、咖啡酸和阿魏酸中的一种或几种。
本发明中,植物多酚为天然多酚,天然植物多酚广泛的存在于自然界中,来源广泛,价格便宜,生物相容性好,同时还可以赋予织物天然的色彩,在超疏水整理的同时实现织物的染色。
在酶催化剂和铜盐助催化剂下,植物多酚发生氧化聚合反应,在铜离子和酶的催化下,多酚迅速聚合,且在氧气的作用下,氧化自聚合,与蚕丝表面的氨基或羧基反应。
进一步地,植物多酚、铜盐助催化剂和混合溶液的质量比为0.05-0.5:0.5-3:95-100,混合溶液中,酶催化剂的用量为0.10-5U/mL。
进一步地,含烷基的疏水化合物为十二烷基硫醇、十二烷基胺、氨丙基异丁基倍半硅氧烷、硅烷和十八烷基胺中的一种或几种。含烷基的疏水化合物能够进一步为蚕丝织物提供疏水性能,蚕丝可以与带氨基和硫醇基的疏水性物质发生迈克尔加成反应或者席夫碱反应,使得疏水性物质成功接枝到织物上。
进一步地,含烷基的疏水化合物与混合溶液的质量比为0.1-5:95-100。
进一步地,采用磷酸缓冲液、醋酸缓冲液或Tris-HCl缓冲液调节pH至2-6。
进一步地,反应在震荡条件下进行,具体是在恒温震荡染色机中反应。
进一步地,在溶液pH=2-6的条件下反应0.5-6h后,还包括取出织物,洗涤、干燥的步骤。
进一步地,采用去离子水洗涤织物,在45-80℃干燥15-45min。
在另一方面,本发明还提供了一种采用上述制备方法所得到的疏水蚕丝织物。
采用本发明的方法所制备的疏水蚕丝织物,其对油滴的接触角几乎为零,对水滴的接触角大于145°。
在又一方面,本发明还公开了上述制备方法所得到的疏水蚕丝织物在油水分离中的应用。
应用时,在疏水蚕丝织物中包裹多孔材料,制备成超疏水吸油包,置于油水混合物或水包油乳液中,在负压条件下进行油水分离。
借由上述方案,本发明至少具有以下优点:
本发明的疏水蚕丝织物的制备方法简单,为一步法,不需要复杂繁琐的流程,不需要复杂的工艺设备,实用性强,可以通过相应调节各物质的用量来获得大小不一的超疏水蚕丝织物。
本发明在制备过程中不用到任何氟化物和有机溶剂,原材料成本低,经济环保。
采用本发明的方法制备的疏水蚕丝织物具有很强的疏水性,可耐受各种极端条件,且仍然保持良好的稳定性。
采用本发明的方法制备的疏水蚕丝织物可用于油水分离领域,包括原油泄漏、含油工业废水处理和修复领域,其分离效率高,且疏水蚕丝织物可重复利用。
本发明的整个疏水蚕丝织物的制备过程和其油水分离应用过程对环境友好,几乎无污染,符合可持续发展观,且工艺其极简单非常适合大规模生产。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1是本发明实施例1制备的超疏水蚕丝织物的扫描电镜图;
图2是本发明实施例2制备的超疏水蚕丝织物的接触角测试结果;
图3是本发明简单的油水分离装置的结构示意图;
图4是本发明油水分离装置对各种有机物的油水的分离效率实验结果;
附图标记说明:
1-油水混合物;2-吸油包;3-橡胶管;4-收集装置;5-油。
具体实施方式
下面结合附图和实施例,对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。
本发明以下实施例中,将蚕丝织物浸泡于水和有机溶剂的混合溶液中,向其中加入植物多酚、漆酶催化剂和助催化剂,调节pH至2-6,再加入含烷基的疏水化合物,在25-65℃下反应0.5-6h,取出织物,洗涤、干燥后即可得到疏水蚕丝织物。具体方法见实施例。
实施例1
将4×4cm2的蚕丝织物浸入100mL水和乙醇的混合溶液(水和乙醇的体积比为8:2)中,然后加入0.5g硫酸铜、0.2g茶多酚和1U/mL漆酶,用醋酸缓冲液调节pH值约为4,然后再加入十二烷基硫醇0.5mL,在恒温震荡染色机震荡反应,45℃下反应2h,取出处理后的蚕丝织物并洗净烘干,即得到超疏水蚕丝织物。
图1是本实施例制备的超疏水蚕丝织物的扫描电镜图,从图中可看出,蚕丝纤维表面成功附着多酚物质的低聚合体。
实施例2
将4×4cm2的蚕丝织物浸入100mL水和乙醇的混合溶液(水和乙醇的体积比为8:2)中,然后加入0.5g硫酸铜、0.2g单宁酸和2U/mL漆酶,用醋酸缓冲液调节pH值约为3,然后再加入十二烷基硫醇1mL,在恒温震荡染色机震荡反应,50℃下反应3h,取出处理后的蚕丝织物并洗净烘干,即得到超疏水蚕丝织物。
实施例3
将4×4cm2的蚕丝织物浸入100mL水和乙醇的混合溶液(水和乙醇的体积比为8:2)中,然后加入0.5g硫酸铜、0.2g咖啡酸和3U/mL漆酶,用醋酸缓冲液调节pH值约为3.5,然后再加入1g氨丙基异丁基倍半硅氧烷(POSS),在恒温震荡染色机震荡反应,45℃下反应4h,取出处理后的蚕丝织物并洗净烘干,即得到超疏水蚕丝织物。
图2是本实施例制备的超疏水蚕丝织物的接触角测试结果,结果表明,织物对水滴的静态接触角大于145°。
实施例4
将4×4cm2的蚕丝织物浸入100mL水和乙醇的混合溶液(水和乙醇的体积比为2:8)中,然后加入0.5g硫酸铜、0.2g绿原酸和1U/mL漆酶,用醋酸缓冲液调节pH值约为3.5,然后再加入2g氨丙基异丁基倍半硅氧烷(POSS),在恒温震荡染色机震荡反应,50℃下反应3h,取出处理后的蚕丝织物并洗净烘干,即得到超疏水蚕丝织物。
实施例5
将4×4cm2的蚕丝织物浸入100mL水和乙醇的混合溶液(水和乙醇的体积比为3:7)中,然后加入0.5g硫酸铜、0.25g阿魏酸和1U/mL漆酶,用醋酸缓冲液调节pH值约为4,然后再加入十八烷基胺0.6g,在恒温震荡染色机震荡反应,55℃下反应4h,取出处理后的蚕丝织物并洗净烘干,即得到超疏水蚕丝织物。
实施例6
将4×4cm2的蚕丝织物浸入100mL水和甲醇的混合溶液(水和甲醇的体积比为8:2)中,然后加入0.4g氯化铜、0.24g茶多酚和1U/mL漆酶,用醋酸缓冲液调节pH值约为5,然后再加入十二烷基胺0.8mL,在恒温震荡染色机震荡反应,45℃下反应3h,取出处理后的蚕丝织物并洗净烘干,即得到超疏水蚕丝织物。
实施例7
将4×4cm2的蚕丝织物浸入100mL水和甲醇的混合溶液(水和甲醇的体积比为8:2)中,然后加入0.4g氯化铜、0.24g茶多酚和1U/mL酪氨酸酶,用醋酸缓冲液调节pH值约为5,然后再加入十二烷基胺0.8mL,在恒温震荡染色机震荡反应,25℃下反应0.5h,取出处理后的蚕丝织物并洗净烘干,即得到超疏水蚕丝织物。
实施例8
用海绵填充于上述实施例制备的超疏水蚕丝织物中,制作吸油包2,制作简单的油水分离装置,如图2所示(图2未图示真空泵)。
将50毫升有机物(用油红O染色)与100毫升水在烧杯中混合,其中有机物包括甲苯、庚烷、四氯甲烷、植物油、甲基硅油、氯仿和石油醚。将吸油包2置于上述油水混合物1中,吸油包2的一端与橡胶管3的一端连接,橡胶管3的另一端连接密封的收集装置4,收集装置4与真空泵连通。由于吸油包2表面疏水亲油,油(即各种有机物)会浸入吸油包2内,在真空泵提供的负压下,海绵吸附的油5经橡胶管3被吸到收集装置4中。在实验过程中可明显看到,混合物表面的油很快被吸附,而水相几乎无变化,计算得其对各种有机物的分离效率均在98%以上(图4)。
以上所述仅是本发明的优选实施方式,并不用于限制本发明,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本发明的保护范围。
Claims (10)
1.一种疏水蚕丝织物的制备方法,其特征在于,包括以下步骤:
将蚕丝织物浸泡于水和有机溶剂的混合溶液中,向其中加入植物多酚、酶催化剂和铜盐助催化剂,调节pH至2-6,再加入含烷基的疏水化合物,在25-65℃下进行反应,得到所述疏水蚕丝织物。
2.根据权利要求1所述的疏水蚕丝织物的制备方法,其特征在于:所述蚕丝织物与混合溶液的质量比为0.1-1:50-200。
3.根据权利要求1所述的疏水蚕丝织物的制备方法,其特征在于:所述有机溶剂为乙醇、甲醇和丙酮中的一种或几种。
4.根据权利要求1所述的疏水蚕丝织物的制备方法,其特征在于:所述酶催化剂为漆酶或酪氨酸酶;所述铜盐助催化剂为硫酸铜或氯化铜。
5.根据权利要求1所述的疏水蚕丝织物的制备方法,其特征在于:所述植物多酚为单宁酸、茶多酚、绿原酸、咖啡酸和阿魏酸中的一种或几种。
6.根据权利要求1所述的疏水蚕丝织物的制备方法,其特征在于:所述植物多酚、铜盐助催化剂和混合溶液的质量比为0.05-0.5:0.5-3:95-100,所述混合溶液中,酶催化剂的用量为0.10-5U/mL。
7.根据权利要求1所述的疏水蚕丝织物的制备方法,其特征在于:所述含烷基的疏水化合物为十二烷基硫醇、十二烷基胺、氨丙基异丁基倍半硅氧烷、硅烷和十八烷基胺中的一种或几种。
8.根据权利要求1所述的疏水蚕丝织物的制备方法,其特征在于:所述含烷基的疏水化合物与所述混合溶液的质量比为0.1-5:95-100。
9.一种根据权利要求1-8中任一项所述的制备方法所得到的疏水蚕丝织物。
10.根据权利要求1-8中任一项所述的制备方法所得到的疏水蚕丝织物在油水分离中的应用。
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