CN108560259A - A method of improving nano-ZnO binding strength on modified dacron fabric - Google Patents
A method of improving nano-ZnO binding strength on modified dacron fabric Download PDFInfo
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- 239000004744 fabric Substances 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229920004934 Dacron® Polymers 0.000 title abstract 7
- 239000005020 polyethylene terephthalate Substances 0.000 title abstract 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 117
- 229920000728 polyester Polymers 0.000 claims abstract description 92
- 239000011787 zinc oxide Substances 0.000 claims abstract description 76
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229920001661 Chitosan Polymers 0.000 claims abstract description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 16
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000010355 oscillation Effects 0.000 claims abstract description 9
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 37
- 238000007598 dipping method Methods 0.000 claims description 11
- 238000005096 rolling process Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000009832 plasma treatment Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 230000004048 modification Effects 0.000 abstract description 8
- 238000012986 modification Methods 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 2
- 229910021642 ultra pure water Inorganic materials 0.000 abstract 1
- 239000012498 ultrapure water Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 12
- 238000005406 washing Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 230000003373 anti-fouling effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- -1 silicon oxide anions Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
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- 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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- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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Abstract
Description
技术领域technical field
本发明属于纳米材料功能整理领域，尤其是涉及一种提高纳米ZnO在改性涤纶织物上结合牢度的方法。The invention belongs to the field of functional finishing of nanometer materials, in particular to a method for improving the bonding fastness of nanometer ZnO on modified polyester fabrics.
背景技术Background technique
纳米ZnO具有良好光催化活性、优异的稳定性和耐热性，无二次污染、无刺激性，对人体无毒及价廉等优点，成为当前最具有开发前景的绿色环保光催化材料。ZnO的禁带宽度为3.27eV，能够有效吸收紫外光，具有良好的光催化性能，通过吸收紫外光中的能量，ZnO中的电子发生跃迁，从而形成电子空穴对，可以使附着于ZnO表面的污染物发生氧化还原反应，使其转变为水和二氧化碳等小分子化合物。纳米ZnO材料除了光学，光催化性能外，还有防污、消毒抑菌，润湿等性能。其防污性能主要依赖于ZnO材料的光催化性能，在一定的光照下，ZnO材料能将水及空气中的氧转化为活性氧，从而破坏有机污物，达到自清洁的效果。因此当ZnO处理至涤纶织物上后，能显著增强织物的防污效率；抑制微生物的生长，大大提高织物的使用寿命。Nano-ZnO has the advantages of good photocatalytic activity, excellent stability and heat resistance, no secondary pollution, no irritation, non-toxic to human body and low price. It has become the most promising green photocatalytic material. The band gap of ZnO is 3.27eV, which can effectively absorb ultraviolet light and has good photocatalytic performance. By absorbing the energy in ultraviolet light, the electrons in ZnO undergo transitions, thereby forming electron-hole pairs, which can be attached to the surface of ZnO. The pollutants undergo oxidation-reduction reactions, converting them into small molecular compounds such as water and carbon dioxide. In addition to optical and photocatalytic properties, nano-ZnO materials also have antifouling, disinfection, antibacterial, and wetting properties. Its antifouling performance mainly depends on the photocatalytic performance of ZnO material. Under certain light, ZnO material can convert oxygen in water and air into active oxygen, thereby destroying organic dirt and achieving self-cleaning effect. Therefore, when ZnO is treated on polyester fabric, it can significantly enhance the antifouling efficiency of the fabric; inhibit the growth of microorganisms, and greatly improve the service life of the fabric.
涤纶纤维具有优异的物理及化学性能，在面料、床上用品、服装等纺织产业及其他工业上倍受青睐。然而其纤维表面光滑，以及大分子链上没有亲水基团，导致涤纶纤维易起静电、亲水性差、服用性差；而且纳米ZnO中也无基团可以与涤纶织物相结合，所以只能通过物理吸附的方式存在于织物表面，因此纳米ZnO在织物上没有很强力的化学键，很容易脱落，导致织物失去多种优异的性能。以上问题都限制了功能性纺织品在市场上的推广，所以急需解决ZnO在涤纶织物上耐久性差的问题。Polyester fiber has excellent physical and chemical properties, and is favored in the textile industry such as fabrics, bedding, clothing, and other industries. However, its fiber surface is smooth, and there are no hydrophilic groups on the macromolecular chain, resulting in polyester fibers prone to static electricity, poor hydrophilicity, and poor wearability; and there are no groups in nano-ZnO that can be combined with polyester fabrics, so it can only be passed through The way of physical adsorption exists on the surface of the fabric, so nano-ZnO does not have a strong chemical bond on the fabric, and it is easy to fall off, causing the fabric to lose a variety of excellent properties. The above problems have limited the promotion of functional textiles in the market, so it is urgent to solve the problem of poor durability of ZnO on polyester fabrics.
发明内容Contents of the invention
本发明的目的就是为了克服上述现有技术存在ZnO在涤纶织物上不耐水洗的缺陷而提供一种提高纳米ZnO在改性涤纶织物上结合牢度的方法，制备所得到的ZnO改性涤纶织物的表面具有大量的ZnO，且较为均匀，赋予涤纶织物光催化、抗紫外等优异性能。该制备工艺可以有效提高ZnO与改性涤纶织物的结合牢度，拓宽了功能性涤纶织物的应用范围，而且工艺简单，操作方便。The purpose of the present invention is exactly to provide a kind of method that improves the combination fastness of nano-ZnO on the modified polyester fabric in order to overcome the defect that ZnO is not washable on the polyester fabric existing in the above-mentioned prior art, prepare the obtained ZnO modified polyester fabric The surface has a large amount of ZnO, and it is relatively uniform, which endows the polyester fabric with excellent properties such as photocatalysis and UV resistance. The preparation process can effectively improve the binding fastness of ZnO and the modified polyester fabric, broaden the application range of the functional polyester fabric, and has simple process and convenient operation.
本发明的目的可以通过以下技术方案来实现：The purpose of the present invention can be achieved through the following technical solutions:
一种提高纳米ZnO在改性涤纶织物上结合牢度的方法，采用以下步骤：A method for improving the combination fastness of nanometer ZnO on modified polyester fabrics, adopting the following steps:
(1)将低分子量壳聚糖溶解在醋酸稀溶液中；(1) low molecular weight chitosan is dissolved in dilute acetic acid solution;
(2)将经过等离子体处理的涤纶织物浸入步骤(1)得到的溶液中反应，采用二浸二轧使壳聚糖能充分渗入织物中，预烘、焙烘干燥，得到改性涤纶织物；(2) Immerse the plasma-treated polyester fabric in the solution obtained in step (1) to react, adopt two dipping and two rolling to make chitosan fully penetrate into the fabric, pre-baking, baking and drying, and obtain the modified polyester fabric;
(3)采用超声震荡将氧化锌均匀分散在超纯水溶液中；(3) Ultrasonic vibration is used to uniformly disperse zinc oxide in the ultrapure aqueous solution;
(4)将氯化镁加入到步骤(3)得到的溶液中，充分搅拌；(4) magnesium chloride is added in the solution that step (3) obtains, fully stirs;
(5)在步骤(4)得到的溶液中加入硅烷偶联剂，充分搅拌；(5) add silane coupling agent in the solution that step (4) obtains, fully stir;
(6)将改性涤纶织物放入步骤(5)得到的溶液中，控温超声振荡，并对织物采用二浸二轧的方式浸轧，预烘、焙烘干燥，得到提高纳米ZnO结合牢度的功能性改性涤纶织物。(6) Put the modified polyester fabric into the solution obtained in step (5), control the temperature and ultrasonically oscillate, and pad the fabric in a two-dipping and two-rolling mode, pre-baking, baking and drying, so as to improve the binding strength of nano-ZnO High degree of functional modified polyester fabric.
步骤(1)中所述醋酸稀溶液的浓度为1-3wt％。The concentration of the dilute acetic acid solution in step (1) is 1-3 wt%.
步骤(2)中等离子体处理的时间为3min-10min，功率为30-80W，等离子体处理时板间距控制为2.5mm-10mm，二浸二轧的轧余率为65％-85％，预烘的温度为60℃-90℃，焙烘的温度为120℃-180℃。The time of plasma treatment in step (2) is 3min-10min, the power is 30-80W, the plate spacing is controlled as 2.5mm-10mm during plasma treatment, and the pass rate of two dipping and two rolling is 65%-85%. The baking temperature is 60°C-90°C, and the baking temperature is 120°C-180°C.
步骤(3)中氧化锌的浓度为14g/L-20g/L。The concentration of zinc oxide in step (3) is 14g/L-20g/L.
步骤(4)中氧化镁的浓度为2g/L-3g/L。The concentration of magnesium oxide in step (4) is 2g/L-3g/L.
步骤(5)中所述硅烷偶联剂为N-β-(氨乙基)-γ-氨丙基甲基二甲氧基硅烷，在溶液中的浓度为1-4wt％。The silane coupling agent in step (5) is N-β-(aminoethyl)-γ-aminopropylmethyldimethoxysilane, and the concentration in the solution is 1-4wt%.
步骤(6)中超声震荡时间为0.5-2.5h，超声震荡频率40KHz，温度控制在30-60℃，二浸二轧的轧余率为65％-90％，预洪温度为70℃-90℃，焙烘温度为120℃-180℃。In step (6), the ultrasonic oscillation time is 0.5-2.5h, the ultrasonic oscillation frequency is 40KHz, the temperature is controlled at 30-60°C, the excess rate of the second dipping and second rolling is 65%-90%, and the pre-flooding temperature is 70°C-90°C. °C, the baking temperature is 120 °C-180 °C.
硅烷偶联剂与水接触时，容易与水发生水解和缩聚反应，如下所示。硅烷偶联剂发生水解时，会脱去偶联剂中的烷氧基，形成硅羟基；硅羟基在中性或者碱性环境下会与溶液中的OH-反应，形成硅氧负离子；而硅氧负离子会对攻击另一发分子的硅，形成二聚体，硅烷偶联剂通过此方法形成缩聚物，缩聚后硅烷偶联剂中含有大量硅羟基和氨基。When the silane coupling agent is in contact with water, it is easy to undergo hydrolysis and polycondensation reactions with water, as shown below. When the silane coupling agent is hydrolyzed, the alkoxy group in the coupling agent will be removed to form a silicon hydroxyl group; the silicon hydroxyl group will react with the OH in the solution in a neutral or alkaline environment to form a silicon oxide anion; Oxygen negative ions will attack another molecule of silicon to form a dimer. The silane coupling agent forms a polycondensate through this method. After polycondensation, the silane coupling agent contains a large amount of silanol and amino groups.
当体系中加入ZnO后，水解所形成的硅氧负离子会有一部分攻击ZnO，从而使硅烷偶联剂接枝于ZnO，如下所示。经过偶联剂处理后的ZnO能够以共价键的形式牢固的与偶联剂相结合。When ZnO is added to the system, some of the silicon oxide anions formed by hydrolysis will attack ZnO, so that the silane coupling agent is grafted on ZnO, as shown below. The ZnO treated with the coupling agent can be firmly combined with the coupling agent in the form of covalent bonds.
通过上述分析可知，硅烷偶联剂水解缩聚后形成大量的羟基基团，能够与改性涤纶织物中的羟基与氨基反应，形成强有力的化学键，从而提高纳米ZnO与改性涤纶织物的结合牢度。Through the above analysis, it can be seen that the silane coupling agent forms a large number of hydroxyl groups after hydrolysis and polycondensation, which can react with the hydroxyl groups and amino groups in the modified polyester fabric to form a strong chemical bond, thereby improving the combination of nano-ZnO and modified polyester fabrics. Spend.
因此，硅烷偶联剂能作为连接改性涤纶织物与纳米ZnO的“分子桥”，大大的提升纳米ZnO在改性涤纶织物上的结合牢度，提高耐水洗性能。Therefore, the silane coupling agent can be used as a "molecular bridge" connecting the modified polyester fabric and nano-ZnO, greatly improving the binding fastness of nano-ZnO on the modified polyester fabric, and improving the washing resistance.
与现有技术相比，本发明具有以下优点：Compared with the prior art, the present invention has the following advantages:
1、本发明针对纳米氧化锌与涤纶织物耐久性能差的问题，运用一步法将纳米氧化锌、氯化镁、硅烷偶联剂KH602、以及改性涤纶织物在40℃的超声震荡中处理1h，使纳米氧化锌均匀分布在涤纶织物表面。此法生产工艺简单，耗时短，节约能源，便于操作，易推广大规模生产。1. The present invention aims at the problem of poor durability of nano-zinc oxide and polyester fabric, and uses a one-step method to treat nano-zinc oxide, magnesium chloride, silane coupling agent KH602, and modified polyester fabric in ultrasonic vibration at 40°C for 1 hour to make nano Zinc oxide is evenly distributed on the surface of polyester fabric. The method has the advantages of simple production process, short time consumption, energy saving, convenient operation and easy popularization of large-scale production.
2、本发明所制备的纳米ZnO改性涤纶织物在经过洗涤后依旧具有良好的光催化和抗紫外性能，且在处理后对涤纶织物的物理机械性能并没有太大影响。2. The nano-ZnO modified polyester fabric prepared by the present invention still has good photocatalytic and anti-ultraviolet properties after washing, and has no great influence on the physical and mechanical properties of the polyester fabric after treatment.
附图说明Description of drawings
图1为为涤纶织物改性前后的扫描电镜图；Fig. 1 is the scanning electron microscope picture before and after being modified polyester fabric;
图2为涤纶织物改性前后的接触角图；Fig. 2 is the contact angle figure of polyester fabric before and after modification;
图3为洗涤前后纳米ZnO改性涤纶织物的抗紫外性能图；Fig. 3 is the anti-ultraviolet performance figure of nanometer ZnO modified polyester fabric before and after washing;
图4为洗涤前后纳米ZnO改性涤纶织物的光催化性能图；Fig. 4 is the photocatalytic performance figure of nano ZnO modified polyester fabric before and after washing;
图5为洗涤前后ZnO改性涤纶织物扫描电镜图。Fig. 5 is a scanning electron microscope image of ZnO modified polyester fabric before and after washing.
具体实施方式Detailed ways
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进。这些都属于本发明的保护范围。The present invention will be described in detail below in conjunction with specific embodiments. The following examples will help those skilled in the art to further understand the present invention, but do not limit the present invention in any form. It should be noted that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention. These all belong to the protection scope of the present invention.
实施例1Example 1
一种提高纳米ZnO在改性涤纶织物上结合牢度的方法，采用以下步骤：A method for improving the combination fastness of nanometer ZnO on modified polyester fabrics, adopting the following steps:
(1)将低分子量壳聚糖溶解在浓度为1wt％醋酸稀溶液中；(1) low molecular weight chitosan is dissolved in concentration and is in the dilute solution of 1wt% acetic acid;
(2)将经过等离子体处理的涤纶织物浸入步骤(1)得到的溶液中反应，等离子体处理的时间为3min，功率为80W，等离子体处理时板间距控制为2.5mm，采用二浸二轧使壳聚糖能充分渗入织物中，轧余率为65％，60℃预烘、120℃焙烘干燥，得到改性涤纶织物；(2) Immerse the plasma-treated polyester fabric in the solution obtained in step (1) to react, the plasma treatment time is 3min, the power is 80W, and the plate spacing is controlled to 2.5mm during the plasma treatment, using two dipping and two rolling Chitosan can fully penetrate into the fabric, the excess rate is 65%, pre-baked at 60°C, baked and dried at 120°C, to obtain modified polyester fabric;
(3)采用超声震荡将氧化锌均匀分散在超纯水溶液中，氧化锌的浓度为14g/L；(3) Ultrasonic vibration is used to uniformly disperse zinc oxide in the ultrapure aqueous solution, and the concentration of zinc oxide is 14g/L;
(4)将氯化镁加入到步骤(3)得到的溶液中，氧化镁的浓度为2g/L，充分搅拌；(4) magnesium chloride is added in the solution that step (3) obtains, and the concentration of magnesium oxide is 2g/L, fully stirs;
(5)在步骤(4)得到的溶液中加入硅烷偶联剂N-β-(氨乙基)-γ-氨丙基甲基二甲氧基硅烷，在溶液中的浓度为1wt％，充分搅拌；(5) add silane coupling agent N-beta-(aminoethyl)-gamma-aminopropylmethyldimethoxysilane in the solution that step (4) obtains, and the concentration in solution is 1wt%, fully stir;
(6)将改性涤纶织物放入步骤(5)得到的溶液中，控温30℃超声振荡2.5h，震荡频率40KHz，并对织物采用二浸二轧的方式浸轧，轧余率为65％，70℃预烘、120℃焙烘干燥，得到提高纳米ZnO结合牢度的功能性改性涤纶织物。(6) Put the modified polyester fabric into the solution obtained in step (5), control the temperature at 30°C for ultrasonic oscillation for 2.5 hours, and oscillate at a frequency of 40KHz, and pad the fabric with two dips and two pads, and the excess rate is 65 %, pre-baking at 70°C and baking-drying at 120°C to obtain a functional modified polyester fabric with improved binding fastness to nano-ZnO.
将改性前后的涤纶织物制成样品，采用捷克FEI Quanta-250型扫描电子显微镜观察改性前后的涤纶织物的表面形貌，结果如图1所示，其中a、b、c为不同分辨率的照片。The polyester fabric before and after modification was made into a sample, and the surface morphology of the polyester fabric before and after modification was observed with a Czech FEI Quanta-250 scanning electron microscope. The results are shown in Figure 1, where a, b, and c are different resolutions Photo.
由图1知，经过等离子体处理的涤纶织物表面出现大量的凹坑；经过低分子量壳聚糖处理改性的涤纶织物表面具有许多低分子量壳聚糖，能大大提高涤纶织物的亲水性能。It can be known from Figure 1 that a large number of pits appear on the surface of the polyester fabric treated with plasma; the surface of the polyester fabric modified by low molecular weight chitosan has many low molecular weight chitosan, which can greatly improve the hydrophilic property of the polyester fabric.
实施例2Example 2
一种提高纳米ZnO在改性涤纶织物上结合牢度的方法，采用以下步骤：A method for improving the combination fastness of nanometer ZnO on modified polyester fabrics, adopting the following steps:
(1)将低分子量壳聚糖溶解在浓度为2wt％醋酸稀溶液中；(1) low molecular weight chitosan is dissolved in concentration and is in the dilute solution of 2wt% acetic acid;
(2)将经过等离子体处理的涤纶织物浸入步骤(1)得到的溶液中反应，等离子体处理的时间为5min，功率为40W，等离子体处理时板间距控制为5mm，采用二浸二轧使壳聚糖能充分渗入织物中，轧余率为70％，80℃预烘、150℃焙烘干燥，得到改性涤纶织物；(2) The polyester fabric treated by plasma is immersed in the solution obtained in step (1) to react, the time of plasma treatment is 5min, and the power is 40W. Chitosan can fully penetrate into the fabric, the excess rate is 70%, pre-baked at 80°C, baked and dried at 150°C to obtain modified polyester fabric;
(3)采用超声震荡将氧化锌均匀分散在超纯水溶液中，氧化锌的浓度为16g/L；(3) Ultrasonic vibration is used to uniformly disperse zinc oxide in the ultrapure aqueous solution, and the concentration of zinc oxide is 16g/L;
(4)将氯化镁加入到步骤(3)得到的溶液中，氧化镁的浓度为2g/L，充分搅拌；(4) magnesium chloride is added in the solution that step (3) obtains, and the concentration of magnesium oxide is 2g/L, fully stirs;
(5)在步骤(4)得到的溶液中加入硅烷偶联剂N-β-(氨乙基)-γ-氨丙基甲基二甲氧基硅烷，在溶液中的浓度为2wt％，充分搅拌；(5) add silane coupling agent N-beta-(aminoethyl)-gamma-aminopropylmethyldimethoxysilane in the solution that step (4) obtains, and the concentration in solution is 2wt%, fully stir;
(6)将改性涤纶织物放入步骤(5)得到的溶液中，控温40℃超声振荡2h，震荡频率40KHz，并对织物采用二浸二轧的方式浸轧，轧余率为70％，80℃预烘、150℃焙烘干燥，得到提高纳米ZnO结合牢度的功能性改性涤纶织物。(6) Put the modified polyester fabric into the solution obtained in step (5), control the temperature at 40°C for ultrasonic oscillation for 2 hours, and oscillate at a frequency of 40KHz, and pad the fabric with two dipping and two rolling methods, and the excess rate is 70%. , pre-baking at 80°C and baking-drying at 150°C to obtain a functional modified polyester fabric with improved binding fastness to nano-ZnO.
采用YG871型毛细管效应测定仪测试涤纶织物的毛细效应，结果表1所示。以高锰酸钾为测试液，将织物垂直置于毛细管效应测定仪30min。The capillary effect of the polyester fabric was tested by a YG871 capillary effect tester, and the results are shown in Table 1. Using potassium permanganate as the test solution, place the fabric vertically in the capillary effect tester for 30 minutes.
表1涤纶织物改性前后的毛效Table 1 Gross effect of polyester fabric before and after modification
由表1可知，经过等离子处理的涤纶织物的毛效有3.4cm/30min，经过低分子量壳聚糖处理改性的涤纶织物的毛效有6.3cm/30min，比未处理涤纶织物的毛效2.8cm/30min有了很大的提升，提高了的涤纶织物的亲水性能。It can be seen from Table 1 that the capillary effect of the polyester fabric treated with plasma is 3.4cm/30min, and the capillary effect of the modified polyester fabric treated with low molecular weight chitosan is 6.3cm/30min, which is 2.8 cm higher than that of the untreated polyester fabric. cm/30min has been greatly improved, improving the hydrophilic performance of polyester fabrics.
实施例3Example 3
一种提高纳米ZnO在改性涤纶织物上结合牢度的方法，采用以下步骤：A method for improving the combination fastness of nanometer ZnO on modified polyester fabrics, adopting the following steps:
(1)将低分子量壳聚糖溶解在浓度为3wt％醋酸稀溶液中；(1) low molecular weight chitosan is dissolved in concentration and is in 3wt% dilute solution of acetic acid;
(2)将经过等离子体处理的涤纶织物浸入步骤(1)得到的溶液中反应，等离子体处理的时间为10min，功率为30W，等离子体处理时板间距控制为10mm，采用二浸二轧使壳聚糖能充分渗入织物中，轧余率为85％，90℃预烘、180℃焙烘干燥，得到改性涤纶织物；(2) Immerse the plasma-treated polyester fabric in the solution obtained in step (1) to react, the time of plasma treatment is 10min, and the power is 30W. During plasma treatment, the plate spacing is controlled to be 10mm. Chitosan can fully penetrate into the fabric, the excess rate is 85%, pre-baked at 90°C, baked and dried at 180°C to obtain modified polyester fabric;
(3)采用超声震荡将氧化锌均匀分散在超纯水溶液中，氧化锌的浓度为20g/L；(3) Ultrasonic vibration is used to uniformly disperse zinc oxide in the ultrapure aqueous solution, and the concentration of zinc oxide is 20g/L;
(4)将氯化镁加入到步骤(3)得到的溶液中，氧化镁的浓度为3g/L，充分搅拌；(4) magnesium chloride is added in the solution that step (3) obtains, and the concentration of magnesium oxide is 3g/L, fully stirs;
(5)在步骤(4)得到的溶液中加入硅烷偶联剂N-β-(氨乙基)-γ-氨丙基甲基二甲氧基硅烷，在溶液中的浓度为4wt％，充分搅拌；(5) add silane coupling agent N-beta-(aminoethyl)-gamma-aminopropylmethyldimethoxysilane in the solution that step (4) obtains, and the concentration in solution is 4wt%, fully stir;
(6)将改性涤纶织物放入步骤(5)得到的溶液中，控温60℃超声振荡0.5h，震荡频率40KHz，并对织物采用二浸二轧的方式浸轧，轧余率为90％，90℃预烘、180℃焙烘干燥，得到提高纳米ZnO结合牢度的功能性改性涤纶织物。(6) Put the modified polyester fabric into the solution obtained in step (5), control the temperature at 60°C for ultrasonic oscillation for 0.5h, and the oscillation frequency is 40KHz, and pad the fabric by two dipping and two rolling, and the excess rate is 90 %, pre-baking at 90°C and baking-drying at 180°C to obtain a functional modified polyester fabric with improved binding fastness to nano-ZnO.
采用德国公司DSA30S液滴形状接触角测量仪测试不同改性涤纶织物的接触角大小，测试织物的亲水效果，结果如图2所示。adopt germany The company's DSA30S droplet shape contact angle measuring instrument tested the contact angle of different modified polyester fabrics and tested the hydrophilic effect of the fabrics. The results are shown in Figure 2.
由图2可知，a为未处理涤纶织物，其接触角为83.7°，b为经过低分子量壳聚糖处理改性的涤纶织物，其接触角下降为34.2°，证明经过低分子量壳聚糖处理改性能有效地提高涤纶织物的亲水性能。It can be seen from Figure 2 that a is an untreated polyester fabric with a contact angle of 83.7°, b is a polyester fabric modified with low molecular weight chitosan, and its contact angle is reduced to 34.2°, which proves that after low molecular weight chitosan treatment Modification can effectively improve the hydrophilic properties of polyester fabrics.
实施例4Example 4
在洗涤前，将制备的将纳米ZnO改性涤纶织物安置在UV-2000S型的紫外线透过率分析仪上，选取国标为测试标准，多次测试；在十次洗涤之后，采用相同方式对其进行测试，结果如图3所示。Before washing, the prepared nano-ZnO modified polyester fabric was placed on the UV-2000S ultraviolet transmittance analyzer, and the national standard was selected as the test standard, and tested many times; after ten times of washing, it was tested in the same way The test was carried out, and the result is shown in Figure 3.
由图3中曲线可知，采用一步法制备的纳米ZnO改性涤纶织物具有良好的抗紫外性能，紫外穿透率低于8％，且在洗涤前后，织物的抗紫外性能几乎没有发生变化。It can be seen from the curve in Figure 3 that the nano-ZnO modified polyester fabric prepared by the one-step method has good anti-ultraviolet performance, and the ultraviolet penetration rate is lower than 8%, and the anti-ultraviolet performance of the fabric hardly changes before and after washing.
实施例5Example 5
通过上海比朗仪器制造有限公司的BL-GHX-V型光化学反应仪测定纳米ZnO改性涤纶织物的光催化性能，分别以汞灯和氙灯为测试灯，以亚甲基蓝溶液的降解率来评估织物的光催化性能。结果如图4的a和b所示。The photocatalytic performance of the nano-ZnO modified polyester fabric was measured by the BL-GHX-V photochemical reaction instrument of Shanghai Bilang Instrument Manufacturing Co., Ltd., and the degradation rate of the methylene blue solution was used to evaluate the photocatalytic performance of the fabric with mercury lamp and xenon lamp respectively. Photocatalytic performance. The results are shown in a and b of Figure 4.
图4中所示，不管是在汞灯照射下还是在氙灯照射下，纳米ZnO改性涤纶织物具有优异的光催化性能，在汞灯照射180min后，亚甲基蓝溶液降解率达到了75％以上，且在氙灯照射8h后，亚甲基蓝溶液降解率也达到了60％，且经过洗涤后，降解率几乎未发生变化。As shown in Figure 4, no matter under the irradiation of mercury lamp or xenon lamp, the nano-ZnO modified polyester fabric has excellent photocatalytic performance. After 180 min of mercury lamp irradiation, the degradation rate of methylene blue solution reached more than 75%, and After 8 hours of xenon lamp irradiation, the degradation rate of methylene blue solution also reached 60%, and after washing, the degradation rate hardly changed.
实施例6Example 6
将纳米ZnO改性涤纶织物制成样品，采用日立公司S-4800型扫描电子显微镜观察纳米ZnO改性涤纶织物的形貌，结果如图5所示。The nano-ZnO modified polyester fabric was made into a sample, and the morphology of the nano-ZnO modified polyester fabric was observed with a Hitachi S-4800 scanning electron microscope. The results are shown in Figure 5.
由图5(a)可看出，经过一步法制备的纳米ZnO改性涤纶织物表面能够完全被纳米ZnO覆盖，但表面颗粒较大，直径都在1μm以上；由图5(b)可看出，经过水洗10次后，纳米ZnO改性涤纶织物表面附着的大颗粒已经几乎完全清洗去除，但在织物表面接枝着大量细小而致密的纳米ZnO。It can be seen from Figure 5(a) that the surface of the nano-ZnO modified polyester fabric prepared by one-step method can be completely covered by nano-ZnO, but the surface particles are relatively large, with a diameter of more than 1 μm; it can be seen from Figure 5(b) , after washing 10 times, the large particles attached to the surface of the nano-ZnO modified polyester fabric were almost completely removed, but a large amount of fine and dense nano-ZnO was grafted on the surface of the fabric.
实施例7Example 7
参照GB/T8424.2-2001方法，采用温州大荣纺织仪器有限公司WSB-3A数字白度仪测试，对洗涤前后纳米ZnO改性涤纶织物进行测试，评价整理前后织物的白度变化；采用大荣纺织仪器有限公司YG(B)026D-250型电子织物强力机对纳米ZnO改性涤纶织物进行强力测试，参照GBT3923.1-1997方法，以原涤纶织物为空白对照。结果如表2所示。Referring to GB/T8424.2-2001 method, Wenzhou Darong Textile Instrument Co., Ltd. WSB-3A digital whiteness meter is used to test the nano-ZnO modified polyester fabric before and after washing, and evaluate the whiteness change of the fabric before and after finishing; Rong Textile Instrument Co., Ltd. YG(B)026D-250 electronic fabric strength tester is used to test the strength of nano-ZnO modified polyester fabric, referring to the method of GBT3923.1-1997, and using the original polyester fabric as a blank control. The results are shown in Table 2.
表2整理前后涤纶织物的白度和断裂强力的变化Table 2 Changes in whiteness and breaking strength of polyester fabrics before and after finishing
由表2可知，涤纶织物的白度为69.3％，而经过一步法处理的纳米ZnO改性涤纶织物的白度达到了76.6％，处理之后的涤纶织物白度有所提升，对后期使用没有影响；经过整理后，涤纶织物的断裂强力比较相近，都为3870N左右，这是因为涤纶本身具有高强度、耐热、耐腐蚀等性能，即使在高温等处理下依旧能够保持原有的性能。It can be seen from Table 2 that the whiteness of the polyester fabric is 69.3%, while the whiteness of the nano-ZnO modified polyester fabric after one-step treatment reaches 76.6%. ; After finishing, the breaking strength of polyester fabrics is relatively similar, all about 3870N. This is because polyester itself has high strength, heat resistance, corrosion resistance and other properties, and it can still maintain the original properties even under high temperature treatment.
以上对本发明的具体实施例进行了描述。需要理解的是，本发明并不局限于上述特定实施方式，本领域技术人员可以在权利要求的范围内做出各种变形或修改，这并不影响本发明的实质内容。Specific embodiments of the present invention have been described above. It should be understood that the present invention is not limited to the specific embodiments described above, and those skilled in the art may make various changes or modifications within the scope of the claims, which do not affect the essence of the present invention.
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| CN111733591A (en) * | 2020-06-24 | 2020-10-02 | 上海工程技术大学 | A method for controlling the growth of spherical zinc oxide on modified polyester fabric |
| CN112301742A (en) * | 2020-11-09 | 2021-02-02 | 广东国色婚纱礼服有限公司 | Durable polyester fabric antistatic finishing method |
| CN114318860A (en) * | 2021-11-17 | 2022-04-12 | 武汉纺织大学 | Warm-keeping polyester fabric based on tourmaline powder and preparation method thereof |
| CN114381955A (en) * | 2022-01-12 | 2022-04-22 | 武汉纺织大学 | Inorganic pigment dyeing method for polyester textiles |
| CN114381955B (en) * | 2022-01-12 | 2024-06-21 | 武汉纺织大学 | Inorganic pigment dyeing method for polyester textile |
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