技术领域technical field
本发明涉及一种织物抗紫外线涂层的制备方法，特别是一种简易高效的织物抗紫外线涂层的制备方法。The invention relates to a preparation method of a fabric anti-ultraviolet coating, in particular to a simple and efficient preparation method of a fabric anti-ultraviolet coating.
背景技术Background technique
近年来随着人们生活水平的提高，人们对服装的要求也越来越高。高档、舒适、具有抗紫外线、抗菌、自清洁等功能的纺织品越来越受到消费者的青睐。In recent years, with the improvement of people's living standards, people's requirements for clothing are getting higher and higher. High-grade, comfortable textiles with anti-ultraviolet, antibacterial, self-cleaning and other functions are more and more favored by consumers.
ZnO是一种多功能的半导体材料，对紫外线具有优良屏蔽保护作用。当这些材料的颗粒尺寸与光波相当或更小时，由于小尺寸效应，导致光吸收显著增强，粒径小的微粒散射能力强，屏蔽效果好。因此氧化锌纳米粉体能够衰减紫外线，尤其是波长为280nm-320nm的紫外线；同时纳米氧化锌颗粒具有较好的可见光透过效应，与传统有机紫外线吸收剂相比，纳米氧化锌为无机成分，有效作用时间长，对光辐射屏蔽的波段长，有很高的化学稳定性和热稳定结构，无毒、无刺激性，使用安全可靠。因此借助纳米氧化锌的这些特性可以开发具有抗菌、除臭、防辐射功能的纺织产品，现已形成工业化产品的有抗菌内衣、手术服、护士服、消臭敷料、除臭绷带、厕所用纺织品及夏日防晒装、夏日帽、日光伞、运动服等。ZnO is a multifunctional semiconductor material with excellent shielding and protection against ultraviolet rays. When the particle size of these materials is equal to or smaller than that of light waves, due to the small size effect, the light absorption is significantly enhanced, and the particles with small particle sizes have strong scattering ability and good shielding effect. Therefore, zinc oxide nanopowder can attenuate ultraviolet rays, especially ultraviolet rays with a wavelength of 280nm-320nm; at the same time, nano-zinc oxide particles have better visible light transmission effect. Compared with traditional organic ultraviolet absorbers, nano-zinc oxide is an inorganic component. It has a long effective action time, a long wavelength band for optical radiation shielding, high chemical stability and thermal stability structure, non-toxic, non-irritating, safe and reliable to use. Therefore, with the help of these properties of nano-zinc oxide, textile products with antibacterial, deodorizing, and radiation-proof functions can be developed. Industrialized products include antibacterial underwear, surgical gowns, nurse uniforms, deodorant dressings, deodorant bandages, and toilet textiles. And summer sunscreen clothing, summer hats, sun umbrellas, sportswear, etc.
目前，提高芳纶耐紫外老化性能的方法主要是利用溶胶-凝胶法，如CN103898767A公开的二氧化钛改性甲基硅树脂芳纶涂层，须先对芳纶纤维活化1～2h,制备二氧化钛凝胶反应还需4～6h，改性有机硅树脂及固化还需要5～10h，该过程复杂，耗时较长。二是混合纺丝法，即在纤维纺丝液中加入紫外吸收剂，但加入的紫外吸收剂往往会影响到纤维结晶性，使得所制备纤维的本体强度降低较大。CN101012621A中制备氧化锌溶胶，通过浸渍、干燥、烘培在纤维表面沉积氧化锌纳米晶种，这个沉积过程中纳米级的氧化锌会发生团聚，使得最终的颗粒不再保持纳米级，氧化锌晶种在纤维表面分布也不均匀，而且这种方法沉积的氧化锌微粒容易脱落。三是在纤维表面离子溅射镀膜，如CN1970882A采用磁控溅射镀膜机在纤维表面镀上金属涂层，该方法处理使的纤维织物丧失了绝缘性，而且处理时需要较高的真空条件，并不利于工业化大规模生产。At present, the method for improving the UV aging resistance of aramid fiber is mainly to utilize the sol-gel method, such as the titanium dioxide modified methyl silicone resin aramid fiber coating disclosed in CN103898767A. It takes 4-6 hours for the glue reaction, and 5-10 hours for the modified silicone resin and curing. The process is complicated and time-consuming. The second is the mixed spinning method, that is, an ultraviolet absorber is added to the fiber spinning solution, but the added ultraviolet absorber often affects the crystallinity of the fiber, so that the bulk strength of the prepared fiber is greatly reduced. Zinc oxide sol is prepared in CN101012621A, and zinc oxide nano crystal seeds are deposited on the fiber surface by dipping, drying, and baking. During this deposition process, nano-scale zinc oxide will agglomerate, so that the final particles no longer maintain nano-scale, zinc oxide crystals The distribution of seeds on the fiber surface is also uneven, and the zinc oxide particles deposited by this method are easy to fall off. The 3rd, ion sputter coating on fiber surface, as CN1970882A adopts magnetron sputtering coating machine to coat metal coating on fiber surface, the fiber fabric that this method handles loses insulation, and needs higher vacuum condition during processing, It is not conducive to industrialized mass production.
发明内容Contents of the invention
本发明的目的在于，提供一种简易高效的织物抗紫外线涂层的制备方法，以弥补现有技术的不足或缺陷，满足生产和生活的需要。本发明具有制备简单，耗时短，纤维表面氧化锌保持纳米尺寸，分布均匀，纳米氧化锌与纤维结合紧密，不易脱落，以溶液体系在纤维表面原位生成氧化锌晶种，反应后的溶液可回收重复利用的特点。The object of the present invention is to provide a simple and efficient method for preparing an anti-ultraviolet coating for fabrics, so as to make up for the deficiencies or defects of the prior art and meet the needs of production and life. The invention has the advantages of simple preparation, short time consumption, zinc oxide on the surface of the fiber maintains a nanometer size, uniform distribution, and the nano-zinc oxide is closely combined with the fiber, and is not easy to fall off. Recyclable and reusable features.
本发明的技术方案：一种简易高效的织物抗紫外线涂层的制备方法，包括如下步骤：Technical scheme of the present invention: a kind of simple and efficient preparation method of fabric anti-ultraviolet coating comprises the following steps:
(1)将织物浸入氯化锌乙醇溶液，超声处理，然后取出织物，用水清洗至除去残余的氯化锌，然后烘干；(1) Immerse the fabric in zinc chloride ethanol solution, ultrasonically treat it, then take out the fabric, wash it with water to remove residual zinc chloride, and then dry it;
(2)将含锌盐溶液与氢氧化钠溶液混合，然后将烘干的织物放入混合液中，在反应釜中保温；(2) Mix the zinc-containing salt solution with the sodium hydroxide solution, then put the dried fabric into the mixed solution, and keep it warm in the reactor;
(3)将反应釜中的织物取出，用水清洗干净，然后烘干即可。(3) Take out the fabric in the reactor, wash it with water, and then dry it.
前述的简易高效的织物抗紫外线涂层的制备方法，包括如下步骤：The preparation method of aforementioned simple and efficient fabric anti-ultraviolet coating comprises the steps:
(1)将织物浸入质量分数为5％～50％的氯化锌乙醇溶液，超声处理至少3分钟，取出织物，用水清洗至除去残余的氯化锌，然后在40-60℃下烘干；(1) Immerse the fabric in a zinc chloride ethanol solution with a mass fraction of 5% to 50%, ultrasonically treat it for at least 3 minutes, take out the fabric, wash it with water until the residual zinc chloride is removed, and then dry it at 40-60°C;
(2)将锌盐与氢氧化钠按摩尔比1:0.5～1.5配成混合溶液，然后将烘干的织物放入混合液中，在反应釜中保温至少1小时，温度70-90℃；(2) Make a mixed solution of zinc salt and sodium hydroxide in a molar ratio of 1:0.5 to 1.5, then put the dried fabric into the mixed solution, and keep it warm in the reaction kettle for at least 1 hour at a temperature of 70-90°C;
(3)将反应釜中的织物取出，用水清洗干净，然后烘干即可。(3) Take out the fabric in the reactor, wash it with water, and then dry it.
前述的简易高效的织物抗紫外线涂层的制备方法，所述锌盐与氢氧化钠的摩尔比为1:1。In the aforementioned simple and efficient method for preparing an anti-ultraviolet coating for fabrics, the molar ratio of the zinc salt to sodium hydroxide is 1:1.
前述的简易高效的织物抗紫外线涂层的制备方法，所述织物为芳纶或锦纶。In the aforementioned simple and efficient method for preparing an anti-ultraviolet coating for fabrics, the fabric is aramid or nylon.
前述的简易高效的织物抗紫外线涂层的制备方法，所述锌盐为葡萄糖酸锌、硝酸锌、氯化锌或醋酸锌。In the aforementioned simple and efficient method for preparing an anti-ultraviolet coating for fabrics, the zinc salt is zinc gluconate, zinc nitrate, zinc chloride or zinc acetate.
前述的简易高效的织物抗紫外线涂层的制备方法，所述步骤(1)中，超声处理时间为3分钟，超声功率600W，烘干温度50℃。In the aforementioned simple and efficient method for preparing an anti-ultraviolet coating for fabrics, in the step (1), the ultrasonic treatment time is 3 minutes, the ultrasonic power is 600W, and the drying temperature is 50°C.
前述的简易高效的织物抗紫外线涂层的制备方法，所述步骤(2)中，保温时间为1小时，保温温度80℃。In the aforementioned simple and efficient method for preparing an anti-ultraviolet coating for fabrics, in the step (2), the holding time is 1 hour, and the holding temperature is 80°C.
本发明的有益效果：Beneficial effects of the present invention:
1、本发明反应时为溶液体系，相较于现有的溶胶体系，制备配置简单，可回收重复利用，节约原料，降低生产成本。1. The reaction of the present invention is a solution system. Compared with the existing sol system, the preparation and configuration are simple, recyclable and reusable, saving raw materials and reducing production costs.
2、本发明利用锌离子仅与纤维表面的羰基、氨基发生作用，在超声波热效应下在纤维表面原位生成纳米氧化锌晶种，超声波处理所需时间短，由于锌离子的定向性，生成的晶种在纤维表面分布均匀。纳米氧化锌晶种是在超声波剧烈振动环境中生成的，与纤维结合非常紧密，难以脱落。2. The present invention utilizes zinc ions to only interact with carbonyl groups and amino groups on the fiber surface, and generates nano zinc oxide crystal seeds in situ on the fiber surface under the ultrasonic thermal effect. The time required for ultrasonic treatment is short, and due to the orientation of zinc ions, the generated The seeds are evenly distributed on the fiber surface. The nano-zinc oxide crystal seeds are generated in the environment of violent ultrasonic vibration, and are very tightly combined with the fibers, making it difficult to fall off.
3、本发明利用低温水热沉积扩大晶种生长，纳米氧化锌在纤维表面定向生长，结晶度好，抗紫外性佳。3. The present invention utilizes low-temperature hydrothermal deposition to expand seed crystal growth, and nano zinc oxide grows directional on the fiber surface, with good crystallinity and good ultraviolet resistance.
实验例：Experimental example:
分别取20组原始纤维和20组经本发明制备得到的纤维，将其中5组原始纤维和5组经本发明制备得到的纤维先进行原始强度测试，将另外5组进行紫外辐照6小时后测试其强度，将另外5组进行紫外辐照12小时后测试其强度，将另外5组进行紫外辐照24小时后测试其强度，并将测试的结果取平均值，结果如表1所示，从表1可以看出：与原始纤维相比，本发明制备得到的纤维在初始时的强度相差不大，而当受到紫外辐照之后，原始纤维和经本发明制得的纤维的强度均有所降低，但是，原始纤维的强度随着紫外辐照时间的增加，强度下降幅度较大，而经本发明制得的纤维的强度下降较为缓慢，说明本发明制备得到的纤维的抗紫外能力得到了明显的提高。Take 20 groups of raw fibers and 20 groups of fibers prepared by the present invention respectively, and test the original strength of 5 groups of raw fibers and 5 groups of fibers prepared by the present invention first, and then irradiate the other 5 groups with ultraviolet radiation for 6 hours. Test its intensity, test its intensity after another 5 groups are subjected to ultraviolet irradiation for 12 hours, and test its intensity after another 5 groups are subjected to ultraviolet irradiation for 24 hours, and the results of the test are averaged, the results are shown in Table 1, As can be seen from Table 1: compared with the original fiber, the strength of the fiber prepared by the present invention is not much different at the initial stage, and after being subjected to ultraviolet radiation, the strength of the original fiber and the fiber prepared by the present invention are similar However, the intensity of the original fiber decreases greatly with the increase of the ultraviolet irradiation time, while the intensity of the fiber prepared by the present invention decreases slowly, indicating that the anti-ultraviolet ability of the fiber prepared by the present invention is improved. significantly improved.
表1原始纤维和经本发明制备得到的纤维的强度对比The intensity contrast of table 1 original fiber and the fiber prepared by the present invention
附图说明Description of drawings
附图1为经本发明制备得到的芳纶表面的原子力显微镜图。Accompanying drawing 1 is the atomic force microscope picture of the surface of the aramid fiber prepared by the present invention.
从附图1可看出：纳米氧化锌均匀的分布在芳纶纤维的表面，且纳米氧化锌的尺寸小于100nm。It can be seen from accompanying drawing 1 that nano zinc oxide is evenly distributed on the surface of the aramid fiber, and the size of nano zinc oxide is less than 100nm.
具体实施方式detailed description
下面结合附图和实施例对本发明作进一步的说明，但并不作为对本发明限制的依据。The present invention will be further described below in conjunction with the accompanying drawings and embodiments, but not as a basis for limiting the present invention.
本发明的实施例：Embodiments of the invention:
实施例1：一种简易高效的织物抗紫外线涂层的制备方法，包括如下步骤：Embodiment 1: a kind of preparation method of simple and efficient fabric anti-ultraviolet coating comprises the steps:
(1)将芳纶或锦纶浸入质量分数为30％的氯化锌乙醇溶液，超声功率600W下超声处理3分钟，取出芳纶，用水清洗至除去残余的氯化锌，然后在50℃下烘干；(1) Immerse the aramid fiber or nylon fiber in a zinc chloride ethanol solution with a mass fraction of 30%, ultrasonically treat it for 3 minutes at an ultrasonic power of 600W, take out the aramid fiber, wash it with water until the residual zinc chloride is removed, and then bake it at 50°C Dry;
(2)将硝酸锌与氢氧化钠按摩尔比1:1配成混合溶液，然后将烘干的芳纶放入混合液中，在反应釜中保温1小时，温度80℃；(2) Make a mixed solution of zinc nitrate and sodium hydroxide in a molar ratio of 1:1, then put the dried aramid fiber into the mixed solution, and keep it in the reaction kettle for 1 hour at a temperature of 80°C;
(3)将反应釜中的芳纶取出，用水清洗干净，然后烘干即可。(3) Take out the aramid fiber in the reaction kettle, wash it with water, and then dry it.
实施例2：一种简易高效的织物抗紫外线涂层的制备方法，包括如下步骤：Embodiment 2: a kind of preparation method of simple and efficient fabric anti-ultraviolet coating comprises the steps:
(1)将锦纶浸入质量分数为5％的氯化锌乙醇溶液，超声功率600W下超声处理10分钟，取出锦纶，用水清洗至除去残余的氯化锌，然后在40℃下烘干；(1) Immerse the nylon fiber in a zinc chloride ethanol solution with a mass fraction of 5%, ultrasonically treat it for 10 minutes at an ultrasonic power of 600W, take out the nylon fiber, wash it with water until the residual zinc chloride is removed, and then dry it at 40°C;
(2)将葡萄糖酸锌与氢氧化钠按摩尔比1:0.5配成混合溶液，然后将烘干的锦纶放入混合液中，在反应釜中保温2小时，温度70℃；(2) Zinc gluconate and sodium hydroxide are formulated into a mixed solution at a molar ratio of 1:0.5, then the dried nylon is put into the mixed solution, and kept in the reaction kettle for 2 hours at a temperature of 70°C;
(3)将反应釜中的锦纶取出，用水清洗干净，然后烘干即可。(3) Take out the nylon in the reactor, wash it with water, and then dry it.
实施例3：一种简易高效的织物抗紫外线涂层的制备方法，包括如下步骤：Embodiment 3: a kind of preparation method of simple and efficient fabric anti-ultraviolet coating comprises the following steps:
(1)将芳纶浸入质量分数为50％的氯化锌乙醇溶液，超声功率600W下超声处理30分钟，取出芳纶，用水清洗至除去残余的氯化锌，然后在60℃下烘干；(1) Immerse the aramid fiber in a zinc chloride ethanol solution with a mass fraction of 50%, ultrasonically treat it for 30 minutes at an ultrasonic power of 600W, take out the aramid fiber, wash it with water until the residual zinc chloride is removed, and then dry it at 60°C;
(2)将醋酸锌与氢氧化钠按摩尔比1:1.5配成混合溶液，然后将烘干的芳纶放入混合液中，在反应釜中保温5小时，温度90℃；(2) Make a mixed solution of zinc acetate and sodium hydroxide in a molar ratio of 1:1.5, then put the dried aramid fiber into the mixed solution, and keep it in the reaction kettle for 5 hours at a temperature of 90°C;
(3)将反应釜中的芳纶取出，用水清洗干净，然后烘干即可。(3) Take out the aramid fiber in the reaction kettle, wash it with water, and then dry it.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610613827.9ACN106243786B (en) | 2016-07-29 | 2016-07-29 | A kind of preparation method of the fabric ultraviolet resistant of simple and efficient |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610613827.9ACN106243786B (en) | 2016-07-29 | 2016-07-29 | A kind of preparation method of the fabric ultraviolet resistant of simple and efficient |
| Publication Number | Publication Date |
|---|---|
| CN106243786Atrue CN106243786A (en) | 2016-12-21 |
| CN106243786B CN106243786B (en) | 2018-05-11 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610613827.9AExpired - Fee RelatedCN106243786B (en) | 2016-07-29 | 2016-07-29 | A kind of preparation method of the fabric ultraviolet resistant of simple and efficient |
| Country | Link |
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| CN (1) | CN106243786B (en) |
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| CN106243786B (en) | 2018-05-11 |
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