CN107164947B - 一种耐用超疏水织物及其制备方法 - Google Patents

一种耐用超疏水织物及其制备方法 Download PDF

Info

Publication number
CN107164947B
CN107164947B CN201710388112.2A CN201710388112A CN107164947B CN 107164947 B CN107164947 B CN 107164947B CN 201710388112 A CN201710388112 A CN 201710388112A CN 107164947 B CN107164947 B CN 107164947B
Authority
CN
China
Prior art keywords
fabric
preparation
durable
durable superhydrophobic
superhydrophobic fabric
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201710388112.2A
Other languages
English (en)
Other versions
CN107164947A (zh
Inventor
李红强
苏晓竞
曾幸荣
赖学军
张�林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
South China University of Technology SCUT
Original Assignee
South China University of Technology SCUT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by South China University of Technology SCUT filed Critical South China University of Technology SCUT
Priority to CN201710388112.2A priority Critical patent/CN107164947B/zh
Publication of CN107164947A publication Critical patent/CN107164947A/zh
Priority to US16/466,304 priority patent/US20200063336A1/en
Priority to PCT/CN2017/112634 priority patent/WO2018218891A1/zh
Application granted granted Critical
Publication of CN107164947B publication Critical patent/CN107164947B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • D06M11/77—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 silicon or compounds thereof
    • D06M11/79—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 silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/38—Polysiloxanes modified by chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/54—Silicon-containing compounds
    • C08K5/541—Silicon-containing compounds containing oxygen
    • C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • 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
    • 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
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
    • D06M2101/28—Acrylonitrile; Methacrylonitrile
    • 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides
    • 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
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/05—Lotus effect
    • 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
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10—Repellency against liquids
    • D06M2200/12—Hydrophobic properties
    • 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
    • D06M2400/00—Specific information on the treatment or the process itself not provided in D06M23/00-D06M23/18
    • D06M2400/02—Treating compositions in the form of solgel or aerogel

Abstract

本发明公开了一种耐用超疏水织物及其制备方法。该制备方法是将织物浸入正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中，取出后置于装有盐酸溶液的密闭容器中且位于盐酸溶液液面之上，在30‐60℃温度下反应0.5‐2h，制得耐用超疏水织物。本发明制备的织物表面水滴静态接触角大于150°，水滴在其表面极易滚动，同时该织物具有优异的化学稳定性和力学耐久性，且制备工艺简单，无污染。

Description

一种耐用超疏水织物及其制备方法
技术领域
本发明涉及一种超疏水材料，具体涉及一种耐用超疏水织物及其制备方法。
背景技术
受自然界中荷叶表面、蝴蝶翅膀、动物羽毛等的启发，人们设计并发明了超疏水织物，其静态液滴接触角大于150°，且水滴在其表面极易发生滚动。超疏水织物在自清洁、防覆冰、防污染、阻燃、油水分离等方面具有重要的应用价值，已引起了人们的广泛关注。
目前关于超疏水织物的制备方法已有较多报道，如化学刻蚀法、溶胶凝胶法、气相沉积法、紫外光固化法等，但仍存在如下问题：制备工艺繁琐，反应条件苛刻，需要用到特殊的昂贵仪器，只能局限于实验室研究；采用含氟的低表面能物质修饰织物以期构造超疏水表面，但长链含氟单体容易在自然环境中氧化分解，对人体健康和生态环境会造成严重的危害；制备过程中四氢呋喃、甲苯、丙酮等有毒溶剂的使用也违背了“绿色化学”的宗旨；构造出的微纳粗糙结构由于与织物、低表面能物质间微弱的结合力容易遭到破坏，导致织物抵抗外界破坏能力差，在洗涤或摩擦后易丧失超疏水性，耐用性较差。因此，发展一种制备方法简便、经济高效、绿色环保和耐用性强的超疏水织物显得尤为重要。
发明内容
本发明针对目前超疏水织物制备工艺繁琐、反应条件苛刻和耐久性较差等现有技术存在的问题，提供一种工艺简单、成本低廉和环境友好的超疏水织物及其制备方法，所得织物具有优异的化学稳定性和力学耐久性，能长期保持超疏水性。
本发明采用一步气‐液溶胶凝胶法，首先将普通织物浸入含正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中，取出后置于充满挥发性盐酸气体的密闭容器中；将该密闭容器在恒定温度下保持一定时间，正硅酸乙酯通过水解和缩聚在织物表面原位生成二氧化硅，进而二氧化硅上的硅羟基与聚二甲基硅氧烷上的端羟基之间发生交联反应，制得表面呈微纳粗糙结构的超疏水织物。本发明在盐酸气体的催化下，利用正硅酸乙酯水解和缩聚在织物上原位生成二氧化硅，进而二氧化硅上的硅羟基与聚二甲基硅氧烷的端羟基之间发生缩聚反应，形成具有交联结构的呈微纳粗糙结构的耐用超疏水织物。本发明方法具有成本低廉、绿色环保、操作简便等优点，且制备的超疏水织物具有优异的化学稳定性和力学耐久性，即使在严苛的环境下也能长期保持超疏水性。该耐用超疏水织物在制备过程中的发生的反应如下式所示：
本发明目的通过如下技术方案实现：
一种耐用超疏水织物的制备方法，包括以下步骤：将织物浸入正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中，取出后置于装有盐酸溶液的密闭容器中且位于盐酸溶液液面之上，在30‐60℃温度下反应0.5‐2h，制得耐用超疏水织物。
为进一步实现本发明目的，优选地，所述含端羟基的聚二甲基硅氧烷的分子量为400‐8000。
优选地，所述正硅酸乙酯和含端羟基的聚二甲基硅氧烷的质量比为2:1‐5:1。
优选地，所述盐酸溶液的质量百分比为10‐20wt％。
优选地，所述30‐60℃温度下反应0.5‐2h是该密闭容器放入烘箱中，控制温度为30‐60℃。
优选地，所述织物为聚酯、棉、羊毛、腈纶、聚氨酯和尼龙中的任意一种为原料的织物。
一种耐用超疏水织物，由上述的制备方法制得。
优选地，该耐用超疏水织物接触角达到150‐165°，在经过168h以上的有机溶剂浸泡、112次的洗涤(AATCC测试方法61‐2006的2A条件)或600次的耐磨测试后仍可保持超疏水性质。
本发明所述的耐用超疏水涂层的制备方法，与现有技术相比，具有如下优点：
(1)通过一步气‐液溶胶凝胶法制备出超疏水织物，具有操作简单、条件温和、无需使用含氟物质和有毒溶剂、无需特定的仪器设备等优点，可应用于大规模的工业生产。
(2)本发明制备的超疏水织物中二氧化硅堆积形成微纳粗糙结构，与聚二甲基硅氧烷通过羟基缩水脱合形成化学键链接的交联结构，在不同溶剂中长时间浸泡也能保持较高的疏水性能，且织物经多次洗涤和磨损后，其疏水性也基本不变，具有优异的化学稳定性和力学耐久性。
附图说明
图1为实施例1制备的耐磨超疏水织物的扫描电镜图(图像放大倍数为1000倍，右上角插图放大倍数为5000倍，右下角插图为水接触角照片)。
图2为实施例1中纯织物和浸泡正硅酸乙酯和聚二甲基硅氧烷混合物后45℃反应不同时间得到的织物的红外谱图。
图3为各实施例中制备的耐磨超疏水织物用于磨损测试的示意图。
具体实施方式
为更好地理解本发明，下面结合实施例对本发明作进一步说明，但是本发明的实施方式不限于此。
实施例1
将聚酯织物浸入正硅酸乙酯和分子量为400的聚二甲基硅氧烷的质量比为3:1的混合溶液中，取出后置于装有盐酸溶液(质量分数为20wt％)的密闭容器中且位于盐酸溶液液面之上，将该密闭容器放入烘箱于45℃下反应1h，即可制得耐用超疏水织物。
图1是如何得到的要有一个简要的说明，包括放大倍数。图1为本实施例耐用超疏水织物放大1000倍的扫描电镜图，其中右上角的插图为放大5000倍的扫描电镜图，右下角为水接触角的照片。从图1可以看出，在超疏水织物表面形成二氧化硅堆积的微纳粗糙结构，水接触角为160°，具有超疏水性能。
图2为本实施例中纯织物和浸泡正硅酸乙酯和聚二甲基硅氧烷混合物后45℃反应不同时间得到的织物的红外谱图。从图2可以看出，与纯织物相比，浸泡了正硅酸乙酯和聚二甲基硅氧烷混合物后的织物在3330cm‐1的羟基振动峰和1719cm‐1的羰基振动峰强度减弱，而在2972cm‐1的CH3振动峰和2896cm‐1的CH2振动峰强度增强，并且在1068cm‐1和787cm‐1出现了Si‐O‐Si和Si‐C的新峰。随反应的进行，3200‐3400cm‐1的羟基吸收峰先出现后消失，CH3峰峰强略微降低，而CH2峰峰强大幅度下降，但后期均保持不变。并且Si‐O‐Si峰位向高波数位置移动，900‐1100cm‐1处的峰宽也逐渐变大。这说明反应前期正硅酸乙酯发生水解缩合反应，生成的二氧化硅后期与两端带羟基的聚二甲基硅氧烷发生交联反应。
为了评价超疏水织物的化学稳定性，将其分别浸泡在装有30mL丙酮、乙醇、甲苯、己烷的50mL烧杯中，并用保鲜膜密封，在室温下浸泡168h后取出用乙醇洗涤，并在50℃的鼓风干燥箱中干燥1h，对其接触角进行测试。表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后，取出后干燥所测得的接触角。从表1可以看出，本实施例所制备的耐用超疏水织物在不同溶剂中长时间浸泡后，其水接触角变化不大，表明其具有优异的化学稳定性。
为了评价超疏水织物的耐洗涤性，照AATCC测试方法61‐2006的2A条件对其进行洗涤，具体方法为：调节水洗色牢度仪(SW‐12A，温州方圆仪器有限公司)水温达到49℃，向大小为90×200mm的钢杯中加入150mL的去离子水，0.015g的洗涤剂和50颗直径6mm、质量1g的钢球。预热钢杯两分钟后，将尺寸为50×150mm的织物放入钢杯，再启动仪器，以40±2rpm的转速运转45min。最后取出试样用乙醇清洗三次，在60℃烘箱中干燥。表2列出了本实施例耐用超疏水织物按照AATCC测试方法61‐2006的2A条件洗涤112次所测得的接触角。
为了评价超疏水织物的耐磨性，采用了如图3所示的装置对其进行测试，耐磨测试装置由280目的砂纸和200g的砝码组成，将砂纸放在平整的桌子上并固定，再将织物试样放在砂纸上面，并用200g的砝码压在织物试样上面，以4cm/s的速度将织物试样拉动20cm，视为1次摩擦，经过600次摩擦后，测试织物试样的接触角。
表2列出了织物磨损600次后的水接触角。从表2可以看出，本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损，其水接触角均可保持在150°以上，表明其具有优良的耐洗涤和耐磨损性能。
结合图1、图2、表1和表2，本实施例制备的耐用超疏水织物接触角大于150°，这主要归因于正硅酸乙酯水解生成的二氧化硅在聚二甲基硅氧烷链段的作用下堆积形成微纳粗糙结构以及聚二甲基硅氧烷链段的疏水性；而超疏水织物优良的化学稳定性和力学耐久性主要是由于二氧化硅上的羟基进一步与聚二甲基硅氧烷上的羟基缩合形成了化学交联结构。
实施例2
将棉织物浸入正硅酸乙酯和分子量为8000的聚二甲基硅氧烷的质量比为2:1的混合溶液中，取出后置于装有盐酸溶液(质量分数为10wt％)的密闭容器中且位于盐酸溶液液面之上，将该密闭容器放入烘箱于30℃下反应2h，即可制得耐用超疏水织物。
表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后，取出洗涤干燥所测得的接触角，表2列出了本实施例耐用超疏水织物分别按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照3示意图磨损600次后(垂直压强为2.5kPa，拉伸速度为4cm/s，拉伸距离为20cm，砂纸为280目)的水接触角。从表1可以看出，本实施例所制备的耐用超疏水织物在不同溶剂中浸泡168h，其水接触角均保持在150°以上，表明其具有优良的化学稳定性。从表2可以看出，本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损，其水接触角均可保持在150°以上，表明其具有优良的耐洗涤和耐磨损性能。
实施例3
将尼龙织物浸入正硅酸乙酯和分子量为2000的聚二甲基硅氧烷的质量比为5:1的混合溶液中，取出后置于装有盐酸溶液(质量分数为15wt％)的密闭容器中且位于盐酸溶液液面之上，将该密闭容器放入烘箱于45℃下反应1.5h，即可制得耐用超疏水织物。
表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后，取出洗涤干燥所测得的接触角，表2列出了本实施例耐用超疏水织物分别按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照图3示意图磨损600次后(垂直压强为2.5kPa，拉伸速度为4cm/s，拉伸距离为20cm，砂纸为280目)的水接触角。从表1可以看出，本实施例所制备的耐用超疏水织物在不同溶剂中浸泡168h，其水接触角均保持在150°以上，表明其具有优良的化学稳定性。从表2可以看出，本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损，其水接触角均可保持在150°以上，表明其具有优良的耐洗涤和耐磨损性能。
实施例4
将腈纶织物浸入正硅酸乙酯和分子量为5000的聚二甲基硅氧烷的质量比为4:1的混合溶液中，取出后置于装有盐酸溶液(质量分数为20wt％)的密闭容器中且位于盐酸溶液液面之上，将该密闭容器放入烘箱于60℃下反应0.5h，即可制得耐用超疏水织物。
表1为本发明实施例耐用超疏水织物在不同溶剂中浸泡168h后的水接触角。表1列出了本实施例耐用超疏水织物分别浸泡在丙酮、乙醇、甲苯、己烷中168h后，取出洗涤干燥所测得的接触角，表2列出了本实施例耐用超疏水织物分别按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照图3示意图磨损600次后(垂直压强为2.5kPa，拉伸速度为4cm/s，拉伸距离为20cm，砂纸为280目)的水接触角。从表1可以看出，本实施例所制备的耐用超疏水织物在不同溶剂中浸泡168h，其水接触角均保持在150°以上，表明其具有优良的化学稳定性。从表2可以看出，本实施例所制备的耐用超疏水织物即使经过112次洗涤和600次磨损，其水接触角均可保持在150°以上，表明其具有优良的耐洗涤和耐磨损性能。
表1
注：采用德国KRUSS公司的DSA100接触角测试仪进行测试，每个样品取5个点计算平均值。
表2为本发明实施例耐用超疏水织物按照AATCC测试方法61‐2006的2A条件洗涤112次后、按照图3示意图磨损600次后(垂直压强为2.5kPa，拉伸速度为4cm/s，拉伸距离为20cm，砂纸为280目)的水接触角。
表2
注：耐洗测试按照AATCC测试方法61‐2006的2A条件进行，耐磨测试按照图3示意图(垂直压强为2.5kPa，拉伸速度为4cm/s，拉伸距离为20cm，砂纸为280目)进行。水接触角采用德国KRUSS公司的DSA100接触角测试仪进行，每个样品取5个点计算平均值。

Claims (8)

1.一种耐用超疏水织物的制备方法，其特征在于包括以下步骤：将织物浸入正硅酸乙酯和含端羟基的聚二甲基硅氧烷的混合溶液中，取出后置于装有盐酸溶液的密闭容器中且位于盐酸溶液液面之上，在30‐60℃温度下反应0.5‐2h，制得耐用超疏水织物。
2.根据权利要求1所述的耐用超疏水织物的制备方法，其特征在于：所述含端羟基的聚二甲基硅氧烷的分子量为400‐8000。
3.根据权利要求1所述的耐用超疏水织物的制备方法，其特征在于：所述正硅酸乙酯和含端羟基的聚二甲基硅氧烷的质量比为2:1‐5:1。
4.根据权利要求1所述的耐用超疏水织物的制备方法，其特征在于：所述盐酸溶液的质量百分比为10‐20wt％。
5.根据权利要求1所述的耐用超疏水织物的制备方法，其特征在于：所述30‐60℃温度下反应0.5‐2h是该密闭容器放入烘箱中，控制温度为30‐60℃。
6.根据权利要求1所述的耐用超疏水织物的制备方法，其特征在于：所述织物为聚酯、棉、羊毛、腈纶、聚氨酯和尼龙中的任意一种为原料的织物。
7.一种耐用超疏水织物，其特征在于由权利要求1‐6任一项所述的制备方法制得。
8.根据权利要求7所述的耐用超疏水织物，其特征在于，该织物接触角达到150‐165°，在经过168h以上的有机溶剂浸泡、112次的洗涤或600次的耐磨测试后仍保持超疏水性质。
CN201710388112.2A 2017-05-27 2017-05-27 一种耐用超疏水织物及其制备方法 Active CN107164947B (zh)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201710388112.2A CN107164947B (zh) 2017-05-27 2017-05-27 一种耐用超疏水织物及其制备方法
US16/466,304 US20200063336A1 (en) 2017-05-27 2017-11-23 Durable super-hydrophobic fabric and preparation method thereof
PCT/CN2017/112634 WO2018218891A1 (zh) 2017-05-27 2017-11-23 一种耐用超疏水织物及其制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710388112.2A CN107164947B (zh) 2017-05-27 2017-05-27 一种耐用超疏水织物及其制备方法

Publications (2)

Publication Number Publication Date
CN107164947A CN107164947A (zh) 2017-09-15
CN107164947B true CN107164947B (zh) 2019-01-15

Family

ID=59822329

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710388112.2A Active CN107164947B (zh) 2017-05-27 2017-05-27 一种耐用超疏水织物及其制备方法

Country Status (3)

Country Link
US (1) US20200063336A1 (zh)
CN (1) CN107164947B (zh)
WO (1) WO2018218891A1 (zh)

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107164947B (zh) * 2017-05-27 2019-01-15 华南理工大学 一种耐用超疏水织物及其制备方法
CN109137467B (zh) * 2018-06-27 2020-04-28 华南理工大学 一锅法制备超疏水阻燃纺织物的方法
CN108867064B (zh) * 2018-07-20 2019-11-26 西安科技大学 一种以氧化镁为原料制备廉价稳定超疏水织物的方法
CN109322144A (zh) * 2018-10-11 2019-02-12 杭州纳微生物化学有限公司 一种耐久性超疏水纺织品整理剂及其整理方法
CN109610179B (zh) * 2018-12-07 2020-03-06 江南大学 一种耐磨超疏水织物及其制备方法
CN109930386A (zh) * 2019-03-15 2019-06-25 疏博（上海）纳米科技有限公司 一种耐压耐洗超疏水织物的制备方法
KR102029415B1 (ko) * 2019-05-14 2019-10-07 (주)로시코리아 친환경 나염원단
CN110644240B (zh) * 2019-07-26 2021-11-23 南通大学 一种多功能耐久性和自修复超疏水织物表面的制备方法
CN112663173A (zh) * 2019-10-16 2021-04-16 天津理工大学 超疏水氧化物纳米线及其制备方法和应用
CN110670344B (zh) * 2019-10-16 2020-07-17 西北大学 一种具有光催化和油水分离性能的超疏水柔性织物及其制备方法和应用
CN111206413B (zh) * 2020-03-13 2022-05-03 李宁（中国）体育用品有限公司 一种棉织物的辐照接枝改性方法
CN111501352B (zh) * 2020-04-24 2022-05-17 山东鑫纳超疏新材料有限公司 一种水性无氟稳定超疏水织物的制备方法
CN114504844B (zh) * 2020-10-28 2023-08-08 中国石油化工股份有限公司 一种聚结材料及其制备方法和除油方法
CN112813678B (zh) * 2020-12-31 2022-05-24 陕西科技大学 一种兼具耐磨和自修复功能的自清洁水滑石/纤维织物复合材料及其制备方法
CN112853750B (zh) * 2021-03-11 2022-03-11 苏州大学 基于多巴胺辅助的巯基-烯点击化学法制备超疏水纺织品
CN112962311B (zh) * 2021-03-11 2022-03-11 苏州大学 基于poss的巯基-烯点击化学法制备超疏水纺织品
CN113123129B (zh) * 2021-04-25 2022-04-01 苏州大学 基于巯基-烯点击反应制备超疏水涤纶织物的方法
CN113215813B (zh) * 2021-05-10 2022-03-04 苏州大学 TiO2辅助的巯基-烯点击化学法制备超疏水纺织品的方法
CN113308888B (zh) * 2021-06-08 2023-02-21 上海化工研究院有限公司 一种浸泡法制备疏水阻燃纺织品的方法
CN113249972B (zh) * 2021-06-11 2022-02-01 中国科学院兰州化学物理研究所 一种高耐压易清洁超疏水织物的制备方法
CN114394601A (zh) * 2021-12-09 2022-04-26 盐城工学院 一种“山莓”结构二氧化硅的制备方法及应用
CN114657789B (zh) * 2022-04-26 2023-07-07 暨南大学 一种有机硅超疏水涂料及基于其的超疏水涂层与应用
CN114875663B (zh) * 2022-07-11 2022-10-04 江苏恒力化纤股份有限公司 一种超疏水锦纶织物的制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101601940A (zh) * 2009-07-09 2009-12-16 华南理工大学 用于油液过滤脱水的疏水与亲油微纳米涂层及制备方法
CN103088629A (zh) * 2012-12-18 2013-05-08 华南理工大学 一种对pet织物表面进行超疏水改性的方法
CN103421423A (zh) * 2013-08-01 2013-12-04 华南理工大学 一种耐高温的超疏水涂层的原位制备方法
CN105536296A (zh) * 2016-01-25 2016-05-04 华南理工大学 用于油水分离的超疏水/超亲油铜网及其制备方法与应用

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8182864B2 (en) * 2007-08-14 2012-05-22 Postech Academy-Industry Foundaction Modification method of microchannels of PDMS microchip using sol-gel solution
CN107164947B (zh) * 2017-05-27 2019-01-15 华南理工大学 一种耐用超疏水织物及其制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101601940A (zh) * 2009-07-09 2009-12-16 华南理工大学 用于油液过滤脱水的疏水与亲油微纳米涂层及制备方法
CN103088629A (zh) * 2012-12-18 2013-05-08 华南理工大学 一种对pet织物表面进行超疏水改性的方法
CN103421423A (zh) * 2013-08-01 2013-12-04 华南理工大学 一种耐高温的超疏水涂层的原位制备方法
CN105536296A (zh) * 2016-01-25 2016-05-04 华南理工大学 用于油水分离的超疏水/超亲油铜网及其制备方法与应用

Also Published As

Publication number Publication date
WO2018218891A1 (zh) 2018-12-06
US20200063336A1 (en) 2020-02-27
CN107164947A (zh) 2017-09-15

Similar Documents

Publication Publication Date Title
CN107164947B (zh) 一种耐用超疏水织物及其制备方法
Xiong et al. Diblock-copolymer-coated water-and oil-repellent cotton fabrics
CN105542221B (zh) 一种耐磨超疏水超亲油聚氨酯海绵、制备方法及其在油水连续分离中的应用
CN107858825B (zh) 一种石墨烯基超疏水织物及其制备方法
Khan et al. Superhydrophobicity, UV protection and oil/water separation properties of fly ash/Trimethoxy (octadecyl) silane coated cotton fabrics
JP2014513174A (ja) 両疎媒性ブロックコポリマーおよびその用途
CN104262639B (zh) 超疏水型交联聚硅氧烷-聚倍半硅氧烷纳米球杂化材料的制备方法
Zeng et al. Facile fabrication of durable superhydrophobic and oleophobic surface on cellulose substrate via thiol-ene click modification
CN103074768A (zh) 一种超耐用超疏水纺织品及其制备方法
WO2016077532A1 (en) Soil-resistant, stain-resistant coatings and methods of applying on textile or other flexible materials
Luo et al. Anti-smudge and self-cleaning characteristics of waterborne polyurethane coating and its construction
Shen et al. Superamphiphobic and chemical repellent aramid fabrics for applications in protective clothing
Sui et al. Preparation and properties of polysiloxane modified fluorine-containing waterborne polyurethane emulsion
CN110512428B (zh) 一种耐用无氟超疏水织物整理液及其整理织物的方法
CN111421920B (zh) 防水遮光复合面料
CN113969433A (zh) 一种超疏水抗菌面料及其制备方法
CN111910439B (zh) 一种无机纳米SiO2杂化有机硅无氟防水剂及其制备方法
CN108410077A (zh) 聚苯乙烯/硅改性聚氨酯/二氧化硅微纳米纤维膜的制备
CN111764159A (zh) 一种棉织物无氟防水整理方法
WO2016044880A1 (en) Liquid repellent article and process for the preparation of the article
CN105544187B (zh) 一种超疏水织物及其制备方法
CN115434044B (zh) 一种无溶剂双组分纺丝油剂及其制备方法和应用
Sun et al. Fabrication of durable self-repairing superhydrophobic fabrics via a fluorinate-free waterborne biomimetic silicification strategy
CN110184826B (zh) 织物用自清洁自修复涂层材料及制备织物用自清洁自修复涂层的方法
Jiang et al. Fabrication of fluoride-free water repellency cotton fabrics with water-borne polyurethane/acrylate dispersion

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant