WO2011050523A1 - 纳米后整理纺织品耐久性能的测定方法 - Google Patents

纳米后整理纺织品耐久性能的测定方法 Download PDF

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Publication number
WO2011050523A1
WO2011050523A1 PCT/CN2009/074658 CN2009074658W WO2011050523A1 WO 2011050523 A1 WO2011050523 A1 WO 2011050523A1 CN 2009074658 W CN2009074658 W CN 2009074658W WO 2011050523 A1 WO2011050523 A1 WO 2011050523A1
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nano
particle size
textile
artificial
nanometer
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PCT/CN2009/074658
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English (en)
French (fr)
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陈军
顾娟红
郑晨
郑利
杨天宇
Original Assignee
Chen Jun
Gu Juanhong
Zheng Chen
Zheng Li
Yang Tianyu
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Application filed by Chen Jun, Gu Juanhong, Zheng Chen, Zheng Li, Yang Tianyu filed Critical Chen Jun
Priority to PCT/CN2009/074658 priority Critical patent/WO2011050523A1/zh
Publication of WO2011050523A1 publication Critical patent/WO2011050523A1/zh

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/36—Textiles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples

Definitions

  • the invention belongs to the technical field of product safety and detection, and particularly relates to a method for determining the durability of a nano-finished textile. Background technique
  • Nanomaterials generally referred to as any type of material composed of nano-sized structural units, also include single crystals or polycrystals, clusters, and nanoparticles with particle sizes less than 100 nm. Because nano-materials have the characteristics and functions unmatched by conventional materials, their application range has been involved in various fields of various industries, especially as textile finishing agents with special effects are supporting the transformation of traditional textile industry into high-tech industries. Industry technology advancement has played a huge role in promoting.
  • the nano-powder materials used in the textile industry are mainly inorganic or inorganic composite materials, and most of them are fixed or adsorbed by the dyeing or fabric dyeing of the blending method (there is also a way of synthesizing the nanoparticles in situ under study). ). Although the blending process can achieve permanent effects, it is only suitable for the production of functionalized fibers.
  • the post-processing of nano-functional finishing agents has become the most common method for producing nano-textiles due to its process flexibility and operability.
  • nanomaterials and nanotechnology in the textile industry must address the safety issues in the handling of nanofunctional textiles.
  • the toxicity study of single nanomaterials shows that free nanoparticles and nanotubes may penetrate cells and damage human health. Whether the final finished nano-textiles also have the release of nanoparticles is worthy of attention.
  • the United States and the European Union are actively considering the application of nanomaterials and nanotechnology products in consumer products.
  • the durability and safety of nanofunctional textile products Some researchers have studied nanometers.
  • the durability of the antibacterial fabric is wash resistance and solvent resistance.
  • the content of nano zinc oxide on the fabric or sweat foot water is determined by atomic absorption spectrometry, and the dissolution resistance data can be obtained according to the size.
  • the nanomaterial is attached to the fabric by post-finishing, there is bound to be a problem of nanoparticle falling off due to perspiration, washing and rubbing, and loss of related efficacy. Since the size of the nanoparticles is small, whether they are absorbed into the body during migration, and whether the nanoparticles washed or rubbed on the fabric lose their nano-properties due to aggregation, these problems cannot be effectively confirmed.
  • the content of nano-materials used in textiles is not high in the fabric, and the amount of dissolution in simulated body fluids and the particle size analysis of dissolved particles have great practical significance for the safety evaluation of nano-textiles, and will help Understand the uncertain risks that may result from the environmental exposure of nano-textile nano-materials, making it more acceptable for manufacturers and consumers to accept nano-textiles that meet safety requirements. Due to the large number of nano-materials used in textiles, it is not covered as much as possible. As a nano-finished textile nano-particles shedding and dissolution safety limit detection is still in the preliminary exploration stage. The invention thus proceeds. Summary of the invention
  • the object of the present invention is to provide a method for determining the durability of nano-finished textiles, which is capable of determining the durability of the product (ie, washing resistance and solvent resistance) by measuring the shedding and dissolution of the nano-particles on the nano-finished textile. It solves the problem of product quality safety and quality control caused by the lack of safety research and testing standards for nano-textiles, and the safety evaluation of nano-material environmental release during the nano-textile life cycle.
  • a method for determining the durability of nano-finished textiles characterized in that the method comprises the following steps:
  • the nanoparticle target in the step (1) is selected from the group consisting of nano zinc oxide and nano silver.
  • the detecting of the shedding and dissolution of the nano-finished textile nanoparticle in the step (2) comprises the following steps:
  • the filter membrane is a filter membrane having a pore size of 0.25 ⁇ m.
  • the analysis condition of the inductively coupled plasma mass spectrometry is: RF power is 1500 W, cooling gas is 15.00 L/min, auxiliary gas is lL/min, atomizing gas is lL/min, measuring point is 3, and integration time is 0.3s.
  • the detection limits of the method for zinc and silver are 0.08 u g /L and 0.06 u g / L, respectively.
  • the detecting the particle size distribution of the nano-finished textile in the step (3) in the simulated body fluid and the soaping condition comprises the following steps:
  • the analysis condition of the laser particle size analyzer is: the laser source wavelength is 5 mw ⁇ laser, the wavelength is 632.8 nm; the density of silver is 10.53 g / cm 3 , the refractive index is 1.446, and the density of zinc oxide is 5.606 g/cm 3 , the refractive index is 1.2.
  • the bath ratio of the sample to the artificial acid solution, the artificial alkali liquor and the soap liquid is 1:50, and the ultrasonic treatment conditions are: 37° C. ultrasonic power 50 W, ultrasonic intensity is about 0.072 W/cm. 2 , sonicated for 15min.
  • the technical problem to be solved by the present invention is to provide a convenient and accurate method for evaluating the safety of detachment or dissolution of nano-particles on nano-textiles, including sample pretreatment methods and corresponding target detection methods.
  • the method of the invention selects nano zinc oxide and nano silver as target compounds, establishes a method for detecting and detaching nano textile nano particles, and determines the dissolution and particle size distribution of the target compound under different conditions, so as to further study and observe
  • the safety of nano-textiles under simulated conditions is used to provide technical support for establishing an effective nano-textile safety evaluation system and reasonable textile safety thresholds.
  • Figure 1 is a standard curve of zinc obtained in an embodiment of the present invention.
  • FIG. 3 is a particle size distribution diagram of an ZnO finishing fabric extract (acidic sweat) according to an embodiment of the present invention
  • FIG. 4 is a particle size distribution diagram (acid sweat) of an Ag finishing fabric extract according to an embodiment of the present invention.
  • Branson 200ULTRASONIC Cleaner (frequency 48kHz, power 50Watt) ; Germany New Patek nanometer particle size analyzer, model nanophox; Agilent 7500cx quadrupole inductively coupled plasma mass spectrometer; Milli-Q pure water machine (Mllipore, USA); liner: cotton standard adjacent (ISO 105-F09); acidic artificial sweat (solution II): take L- histidine hydrochloride 0.5g, NaCl 5g, sodium dihydrogen phosphate dihydrate 2.2 g, 1L solution dubbed Adjust pH 5.5 with 0.01 mol/L HCl solution and 0.01 mol/L sodium hydroxide, now ready for use; Artificial saliva: Accurately weigh NaC 14.5g, KC1 0.3g, Na 2 S0 4 0.3g, NH 4 C1 0.4g, 90% lactic acid urea 0.2g, dissolved in a small amount of double distilled water, to a volume of l OOOmL, that is, a simulated
  • the analysis conditions of the laser particle size analyzer are as follows: the light source is 5m W HeNe laser, the wavelength is 632.8nm; the sample cell: 10x 10mm 2 ; the test volume is 0.3mL; the temperature control precision is 0.1 °C, the test accuracy of the particle is ⁇ 0.2%; The density of silver was 10.53 g / cm 3 , the refractive index was 1.446, the density of zinc oxide was 5.606 g/cm 3 , and the refractive index was 1.2.
  • the calibration standard series solution was prepared from the standard stock solution, which were 0, 1, 2, 5, 10, 20 g/L, respectively, and analyzed by ICP/MS to obtain a linear relationship between the concentration of the target compound and the response value.
  • the standard curve is based on the concentration of the target compound to be tested, and the measured value is the ordinate to make a standard curve.
  • the linear range is determined.
  • the compound amount of the five concentration points is used for partial least squares regression to obtain the regression equation.
  • the amount of the target compound and the amount of recovery are calculated using the same formula.
  • the detection limits of zinc and silver were determined according to the method of determining the detection limit. The results are shown in Table 1.
  • the correlation curves of the working curves of the two elements are 0.9999, and the detection limits are 0.08ug/L and 0.06ug/L.
  • the experimental process uses method blanks to control whether there is any contamination caused by human or environmental factors throughout the experiment.
  • the matrix spiked blank (the target compound is added to the blank standard lining) near the detection limit to verify the accuracy of the experimental process.
  • a standard sample was prepared at a concentration of 5 ug/L, 20 ug/L, and 100 ug/L of the target compound standard solution, and the recovery test was carried out. The measurement results are shown in Table 2. Blank plus back The yield is 89.1 -96.2%, the RSD is 1.8-4.6%, the matrix recovery is 88.6-93.5%, and the RSD is 1.9-4.8%.
  • the extract is diluted to determine the content of the target, and the results are shown in Table 3.
  • nano-finished textiles have different degrees of shedding and dissolution in acidic sweat, artificial saliva and soap, indicating that their durability, ie, washing resistance and solvent resistance, are not stable enough.
  • the experimental data show that the nano-finished textiles have less shedding and dissolution in artificial saliva and soap, and are relatively stable.
  • the nano-zinc and nano-silver on nano-textiles were used as the target.
  • the fabric samples were extracted by artificial sweat, artificial saliva and soap, supplemented by ultrasonic assisted method and determined by inductively coupled plasma mass spectrometry (ICP-MS).
  • the amount of the target compound eluted in the sample was analyzed, and the particle size of the detached nanoparticles in the extract was analyzed by a laser particle size analyzer (LPA).
  • the detection limits of the target compounds zinc and silver were 0.08ug/L and 0.06ug/L, respectively.
  • the recoveries of blank addition were 89.1-96.2%, the RSD was 1.8-4.6%, and the matrix recovery was 88.6.
  • LPA method can achieve particle size distribution (width %) between 1 nm and 10 microns in high concentration solution and turbid system, and can be used to determine the range of time The stability of the eluted particles.
  • the method can perform safety limit detection and product safety evaluation on the elution amount of nanoparticles in the nano-textile and the particle size of the fallen particles.

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Description

纳米后整理紡织品耐久性能的测定方法
技术领域
本发明属于产品安全与检测技术领域，具体涉及一种纳米后整理紡织品 耐久性能的测定方法。 背景技术
纳米材料， 泛指由纳米尺寸的结构单元构成的任何类型的材料， 也包括 粒子尺寸小于 l OOnm 的单晶体或多晶体、 团族以及纳米微粒。 由于纳米材 料具有常规材料所无法比拟的特点和功能， 其应用范围已涉及到各个行业各 个领域， 尤其是作为具特殊功效的紡织整理剂正支撑着传统的紡织行业向高 科技产业转化， 对紡织行业科技进步起到巨大的推动作用。 目前紡织业所用 纳米粉体材料主要以无机或无机复合材料为主， 大多通过掺和方式聚合紡丝 或织物染色整理使织物固着或吸附纳米颗粒（也有正在研究中的原位合成纳 米颗粒物的方式）。 掺和型工艺虽然能得到永久性的效果， 但仅适合功能化 纤的生产， 纳米功能整理剂的后加工则以其工艺灵活性和可操作性已成为最 为常见的生产纳米紡织品的方法。
纳米材料和纳米技术在紡织行业的应用必须解决纳米功能紡织品服用 过程中的安全性问题， 单一纳米材料的毒性研究显示： 游离的纳米颗粒和纳 米管可能会穿透细胞有损人体健康， 作为最终成品的纳米紡织品是否同样存 在纳米颗粒物的释放值得关注。 有资料显示， 美国和欧盟正在积极考虑规范 纳米材料和纳米科技产品在消费品中的应用， 但关于纳米功能紡织品的产品 耐久性和安全性的专业文献报道极少， 曾有研究者研究了纳米抗菌织物的耐 久性即耐洗涤性能和耐溶剂性能， 通过采用人工汗液来模拟真实汗液， 采用 原子吸收光谱测定织物上或汗液脚水中纳米氧化锌的含量， 根据其大小既可 获得耐溶出性数据， 同时作为评价纳米抗菌织物安全性的依据， 但并未对安 全性做出评价。 事实上， 当纳米材料经后整理加工方式附着到织物上后， 必 然存在因汗渍、 洗涤和摩擦引起的纳米颗粒物脱落问题以及相关功效的丧 失。 由于纳米微粒的尺寸很小， 在迁移过程中是否会被吸收而进入体内， 以 及织物上洗涤或摩擦下来的纳米粒子是否因聚集而失去纳米属性， 这些问题 均无法得到有效确认。 截止目前， 尚未见针对纳米紡织品的安全性研究， 也 缺乏相关的安全性评价体系及检测标准。 欧洲环境局 （EEB ) 2009年 8月甚 至公开呼吁禁止在消费者产品中使用纳米材料， 包括目前市场化程度甚高的 纳米二氧化钛、 氧化锌及制品等， 其理由亦是基于单一纳米材料高暴露显示 的生物毒性。
实际上紡织品所用纳米材料在织物内的含量并不高，其在模拟体液中的 溶出量以及溶出颗粒的粒径分析作为对纳米紡织品安全评价具有极大的现 实意义， 并将有助于了解纳米紡织品生命周期纳米材料环境暴露可能导致的 不确定风险， 使得业者与消费者更能接受合乎安全要求的纳米紡织品。 因应 用于紡织品的纳米材料很多， 无法尽数涵盖其中， 作为纳米后整理紡织品纳 米颗粒物脱落和溶出安全限量检测还处于初步探索阶段。 本发明由此而来。 发明内容
本发明目的在于提供一种纳米后整理紡织品耐久性能的测定方法，该方 法通过对纳米后整理紡织品上纳米颗粒物的脱落和溶出测定实现产品耐久 性能（即耐洗涤性能和耐溶剂性能）测定， 解决了缺乏纳米紡织品的安全性研 究及检测标准带来的产品质量安全和质量控制、纳米紡织品生命周期内纳米 材料环境释放的安全性评价问题。
为了解决现有技术中的这些问题， 本发明提供的技术方案是： 一种纳米后整理紡织品耐久性能的测定方法，其特征在于所述方法包括 以下步骤：
( 1 ) 遴选纳米后整理紡织品中的纳米颗粒目标物；
( 2 ) 检测纳米后整理紡织品在模拟体液和皂洗条件下纳米颗粒物的脱 落和溶出量；
( 3 ) 检测纳米后整理紡织品在模拟体液和皂洗条件下脱落的颗粒物的 粒径分布情况。
优选的， 所述步骤 （1 ) 中纳米颗粒目标物选自纳米氧化锌和纳米银。 优选的， 所述步骤 （2 ) 中纳米后整理紡织品纳米颗粒物的脱落和溶出 量的检测包括以下步骤：
在准确称量的纳米后整理紡织品中加入适量的浴比人工酸汗、人工唾液 和皂液， 进行超声处理， 超声后使用滤膜过滤， 用电感耦合等离子质谱分析 滤液中纳米颗粒物的溶出量。 必要时对滤液加以稀释。
优选的， 所述滤膜为 0.25um孔径的滤膜。
优选的， 所述电感耦合等离子质谱的分析条件为： RF功率为 1500W , 冷却气为 15.00L/min， 辅助气为 lL/min，雾化气为 lL/min， 测量点为 3， 积 分时间为 0.3s。
优选的， 所述方法对锌和银的方法检测限分别为 0.08ug/L和 0.06ug/L。 优选的， 所述步骤 （3 ) 中纳米后整理紡织品在模拟体液和皂洗条件下 脱落的颗粒物的粒径分布检测包括以下步骤：
在准确称取的样品中按适量的浴比分别加入人工酸液、 人工碱液和皂 液， 超声处理后， 送入激光粒度仪分析萃取液中脱落的纳米颗粒物的粒径分 布情况。
优选的， 所述的激光粒度仪的分析条件为： 激光光源波长是 5mw氦氖 激光， 波长 632.8nm ; 银的密度 10.53g/cm3， 折光率为 1.446， 氧化锌的密 度 5.606g/cm3， 折光率为 1.2。
优选的， 所述方法中样品与人工酸液、 人工碱液和皂液的浴比为 1 : 50， 所述超声处理的条件为： 37°C超声功率 50W, 超声强度约为 0.072W/cm2， 超声处理 15min。
本发明所要解决的技术问题是提供一种方便准确的纳米紡织品上纳米 颗粒物的脱落或溶出的安全性评价方法， 包括样品的预处理方法和相应的目 标物检测方法。 本发明的方法选取以纳米氧化锌和纳米银为目标化合物， 建 立纳米紡织品纳米颗粒物的脱落和溶出检测方法， 确定不同条件下目标化合 物的溶出迁移量和粒径分布情况， 以进一步研究观察在模拟服用条件下纳米 紡织品的安全性， 从而为建立有效的纳米紡织品安全评价体系及合理的紡织 品安全阈值提供技术支撑。
相对于现有技术中的方案， 本发明的优点是：
建立了纳米紡织品在模拟体液及皂液中超声辅助萃取的实验程序，藉由 电感耦合等离子质谱仪对目标物的脱落或溶出进行定型 /定量分析， 激光粒 度仪对脱落的目标物进行粒度分析， 可适用于纳米紡织品中纳米颗粒物的脱 落和溶出情况分析， 且目标物不限于所确定的两种元素。 该发明可通过样品 中纳米材料总量与溶出量的差异以及对脱落颗粒物的粒度分析， 可实现纳米 紡织品的耐久性和安全性评价， 从而更为有效地建立纳米紡织品安全性评估 体系， 完善和规范纳米紡织品检测标准。 附图说明
下面结合附图及实施例对本发明作进一步描述：
图 1为本发明实施例得到的锌的标准曲线；
图 2为本发明实施例得到的银的标准曲线；
图 3为本发明实施例 ZnO整理织物萃取液粒度分布图 （酸性汗液）; 图 4为本发明实施例 Ag整理织物萃取液粒度分布图 （酸性汗液）。 具体实施方式
以下结合具体实施例对上述方案做进一步说明。 应理解， 这些实施例是 用于说明本发明而不限于限制本发明的范围。实施例中采用的实施条件可以 根据具体厂家的条件做进一步调整， 未注明的实施条件通常为常规实验中的 条件。
实施例： 纳米紡织品中纳米颗粒物的脱落和溶出。
1 仪器与试剂：
Branson 200ULTRASONIC Cleaner (频率 48kHz , 功率 50Watt) ; 德国 新帕泰克公司纳米粒度仪， 型号为 nanophox ; Agilent 7500cx四极杆电感耦 合等离子体质谱仪； Milli-Q纯水机（美国 Mllipore公司）； 标准贴衬： 棉标准 贴衬 （ISO 105-F09) ; 人造酸性汗液（Solution II) : 取 L-组氨酸盐酸盐 0.5g， 氯化钠 5g， 水合磷酸二氢钠 2.2g， 配成 1L溶液， 用 0.01mol/L的 HC1溶液和 0.01mol/L氢氧化钠调 pH5.5， 现配现用； 人造唾液： 准确称取 NaC14.5g， KC1 0.3g , Na2S04 0.3g , NH4C1 0.4g , 90%乳酸尿素 0.2g , 用少量二次蒸馏水溶 解， 定容至 l OOOmL , 即得 pH值为 3.04的模拟唾液； 皂液： 每升水（注： 此 为去离子水）中含： 5g肥皂（符合 GB/T 3921-2008 要求）； 混合 ICP标准溶液 200ug/L(Mg、 Cr、 Mn、 Fe、 Co、 Ni、 Cu、 Zn、 As、 Se、 Ag、 Cd、 Sb、 Pb)。
2 仪器条件
设定电感耦合等离子质谱仪仪器分析条件： RF功率为 1500W, 冷却气 为 15.00L/min， 辅助气为 lL/min，雾化气为 lL/min， 测量点为 3， 积分时间 为 0.3s。
设定激光粒度仪 （LPA ) 的分析条件为： 光源为 5mW HeNe激光， 波长 632.8nm ; 样品池： 10x 10mm2 ; 测试体积 0.3mL ; 控温精度 0.1 °C颗粒的测 试精度 ^ 0.2 % ; 银的密度 10.53g/cm3， 折光率为 1.446， 氧化锌的密度 5.606g/cm3 , 折光率为 1.2。
3 纳米整理紡织品中纳米颗粒物的脱落和溶出
准确称取 0.5g样品， 按 1 : 50 的浴比分别加入人工酸汗、 人工唾液和 皂液， 37°C下超声半小时， 0.25um滤膜过滤净化， 得萃取液。
纳米整理紡织品中纳米颗粒物的溶出量测定
( 1 ) 校准曲线的绘制
校准曲线的绘制： 由标准储备液配制校正标准系列溶液， 分别为 0， 1， 2， 5， 10， 20 g/L， 进行 ICP/MS分析， 得到目标化合物的浓度对响应值的 线性关系。
标准曲线以待测目标化合物的浓度为横坐标，测定值为纵坐标制作标准 曲线， 确定线性范围， 取五个浓度点的化合物量进行偏最小二乘回归， 获得 回归方程。 目标化合物的量和回收率的量采用相同公式计算。 根据测定检出 限的方法， 分别测定锌和银的检出限。 结果见表 1。 两种元素工作曲线的相 关系数为 0.9999， 检出限为 0.08ug/L和 0.06ug/L。
方法的线性范围、 相关系数与检出限
Figure imgf000007_0001
空白加标和基质（棉标准贴衬）加标回收率测定
实验过程以方法空白来控制整个实验过程中是否有人为或环境因素带 来的污染， 在检测限附近采用基质加标空白（在空白标准帖衬中加入目标化 合物）来验证实验过程的准确性。 以浓度 5ug/L、 20ug/L、 100ug/L的目标化 合物标准溶液制备标准小样， 进行回收率试验，测定结果见表 2。 空白加标回 收率在 89.1 -96.2% , RSD为 1.8-4.6% , 基质加标回收率在 88.6-93.5% , RSD 为 1.9-4.8%
空白加标和基质（棉标准贴衬）加标回收率测定结果
Figure imgf000008_0001
按仪器分析条件， 萃取液经稀释后测定其中目标物的含量， 所得结果见 表 3.
表 3 纳米整理紡织品在不同萃取剂中纳米颗粒物脱落溶出量
Figure imgf000008_0002
可见， 纳米整理紡织品在酸性汗液、 人工唾液和皂液中均有不同程度的 脱落和溶出， 说明其耐久性即耐洗涤性能和耐溶剂性能不够稳定。 实验数据 表明，纳米整理紡织品在人工唾液和皂液中的脱落和溶出量较少，比较稳定。
( 2 ) 纳米整理紡织品中脱落的纳米颗粒物的粒径分析
对超声萃取净化后的萃取液进行激光粒度分析， 结果见表 4。
表 4 样品脱落的纳米颗粒物粒径分析 人工酸液 人工唾液 皂液 氧化锌 （ZnO ) 1202.86 nm 415.21 nm 581.33 nm 银 （Ag ) 1375.62 nm 130.79 nm 163.96 nm 可见， 纳米颗粒物从织物表面脱落后均发生不同程度的团聚， 但仍有粒 子接近纳米范围内， 其中有 10%的部分粒径小于 100纳米， 那么该部分纳米 颗粒物仍具有纳米属性， 可能会对消费者健康构成某些负面影响。
为验证测定方法的实用性， 对 3种纳米紡织品 （抗菌袜子、 防紫外线织 物） 进行了纳米颗粒物溶出量和脱落颗粒物粒径分析水平检测。 结果表明均 有相应的目标物脱落和溶出， 但洗脱液中的颗粒物粒径均为微米级。
以纳米紡织品上的纳米氧化锌和纳米银为目标物， 织物样品经人工汗液、 人工唾液及皂液浸提， 辅以超声辅助方法， 用电感耦合等离子体质谱法 ( ICP-MS ) 测定了样品中目标化合物的溶出量， 用激光粒度仪 （LPA ) 分 析了萃取液中脱落的纳米颗粒物的粒径。 ICP-MS方法对目标化合物锌和银 的检测限分别为 0.08ug/L和 0.06ug/L，空白加标回收率在 89.1-96.2% , RSD 为 1.8-4.6%， 基质加标回收率在 88.6-93.5%， RSD为 1.9-4.8%， LPA方法 可实现高浓度溶液和混浊体系中 1 纳米到 10 微米之间颗粒粒度的分布（宽 度士％)， 并能以此判定较长一段时间范围内洗脱颗粒物的的稳定性。 该方 法可针对纳米紡织品中纳米颗粒的溶出量及脱落的颗粒物粒径实施安全限 量检测与产品安全评价。 上述实例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技 术的人是能够了解本发明的内容并据以实施， 并不能以此限制本发明的保护 范围。 凡根据本发明精神实质所做的等效变换或修饰， 都应涵盖在本发明的 保护范围之内。

Claims

权 利 要 求 书
1、 一种纳米后整理纺织品耐久性能的测定方法， 其特征在于所述方法 包括以下步骤：
( 1 ) 遴选纳米后整理纺织品中的纳米颗粒目标物；
( 2 ) 检测纳米后整理纺织品在模拟体液和皂洗条件下纳米颗粒物的脱 落和溶出量；
( 3 ) 检测纳米后整理纺织品在模拟体液和皂洗条件下脱落的颗粒物的 粒径分布情况。
2、 根据权利要求 1所述的方法， 其特征在于所述步骤 （1 ) 中纳米颗粒 目标物选自纳米氧化锌和纳米银。
3、 根据权利要求 1所述的方法， 其特征在于所述步骤 （2 ) 中纳米后整 理纺织品纳米颗粒物的脱落和溶出量的检测包括以下步骤：
在准确称量的纳米后整理紡织品中加入适量的浴比人工酸汗、人工唾液 和皂液， 进行超声处理， 超声后使用滤膜过滤， 用电感耦合等离子质谱分析 滤液中纳米颗粒物的溶出量。
4、根据权利要求 3所述的方法， 其特征在于所述滤膜为 0.25um孔径的 滤膜。
5、 根据权利要求 3所述的方法， 其特征在于所述电感耦合等离子质谱 的分析条件为： RF功率为 1500W, 冷却气为 15.00L/min， 辅助气为 lL/min， 雾化气为 lL/min , 测量点为 3 , 积分时间为 0.3s。
6、 根据权利要求 5所述的方法， 其特征在于所述方法对锌和银的方法 检测限分别为 0.08ug/L和 0.06ug/L。
7、 根据权利要求 1所述的方法， 其特征在于所述步骤 （3 ) 中纳米后整 理紡织品在模拟体液和皂洗条件下脱落的颗粒物的粒径分布检测包括以下 步骤：
在准确称取的样品中按适量的浴比分别加入人工酸液、 人工碱液和皂 液， 超声处理后， 送入激光粒度仪分析萃取液中脱落的纳米颗粒物的粒径分 布情况。
8、 根据权利要求 7所述的方法， 其特征在于所述的激光粒度仪的分析 条件为： 激光光源波长是 5mw 氦氖激光， 波长 632.8nm ; 银的密度 10.53g/cm3， 折光率为 1.446， 氧化锌的密度 5.606g/cm3， 折光率为 1.2。
9、 根据权利要求 2或 7所述的方法， 其特征在于所述方法中样品与人 工酸液、 人工碱液和皂液的浴比为 1: 50， 所述超声处理的条件为： 37°C超 声功率 50W, 超声强度约为 0.072W/cm2， 超声处理 15min。
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050229328A1 (en) * 2004-04-06 2005-10-20 Availableip.Com Nano-particles on fabric or textile
CN101710037A (zh) * 2009-10-16 2010-05-19 陈军 纳米后整理纺织品耐久性能的测定方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050229328A1 (en) * 2004-04-06 2005-10-20 Availableip.Com Nano-particles on fabric or textile
CN101710037A (zh) * 2009-10-16 2010-05-19 陈军 纳米后整理纺织品耐久性能的测定方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
"Textiles-Determination of Heavy Metals", part 2 February 2007, article "Inductively coupled Plasmaatomic Emission Spectrometry (GB/T 17593)", pages: 1 - 4 *
LI, QUN ET AL.: "STUDY ON THE TEST METHOD FOR PERSPIRATION DISSOLUTION OF NANO ZINC OXIDE FROM FINISHED FABRICS", TEXTILE AUXILIARIES, vol. 25, no. 2, February 2008 (2008-02-01), pages 40 - 42 *
ZHENG, MIN ET AL.: "DEVELOPMENT OF NANO-FUNCTIONAL TEXTILES AND STATUS OF STUDY ON THEIR SECURITY", TEXTILE AUXILIARIES, vol. 2, no. 4, April 2009 (2009-04-01), pages 5 - 9 *

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