纺织学报 ›› 2025, Vol. 46 ›› Issue (01): 111-118.doi: 10.13475/j.fzxb.20240203001

• 染整工程 • 上一篇    下一篇

多元色素光敏变色微胶囊的制备及其在织物中的变色性能

鲁辉1, 蔡钦泽1, 张国庆1, 周岚1,2, 刘国金2,3, 邵敏1()   

  1. 1.浙江理工大学 先进纺织材料与制备技术教育部重点实验室, 浙江 杭州 310018
    2.浙江省现代纺织技术创新中心, 浙江 绍兴 312000
    3.浙江理工大学 浙江省纤维材料和加工技术研究重点实验室, 浙江 杭州 310018
  • 收稿日期:2024-02-26 修回日期:2024-09-18 出版日期:2025-01-15 发布日期:2025-01-15
  • 通讯作者: 邵敏(1968—),女,高级工程师,博士。主要研究方向为轻工技术与工程。E-mail:shaom@zstu.edu.cn
  • 作者简介:鲁辉(1998—),男,硕士生。主要研究方向为微胶囊技术。
  • 基金资助:
    现代纺织技术创新中心(鉴湖实验室)项目(CXZX2023020HD)

Preparation of multi-colorant photochromic microcapsules and their photochromic properties in fabrics

LU Hui1, CAI Qinze1, ZHANG Guoqing1, ZHOU Lan1,2, LIU Guojin2,3, SHAO Min1()   

  1. 1. Zhejiang Provincial Key Laboratory of Fiber Materials and Manufacturing Technology, Zhejiang Sci-Tech University,Hangzhou, Zhejiang 310018, China
    2. Zhejiang Provincial Innovation Center of Advanced Textile Technology, Shaoxing, Zhejiang 312000, China
    3. Key Laboratory of Advanced Textile Materials and Manufacturing Technology,Ministry of Education, Zhejiang Sci-Tech University, Hangzhou, Zhejiang 310018, China
  • Received:2024-02-26 Revised:2024-09-18 Published:2025-01-15 Online:2025-01-15

摘要: 为解决光敏变色染料颜色变化单一且局限于无色与有色可逆变化的问题,提出了一种拓宽光敏变色染料显色范围的方法。以光敏变色染料螺噁嗪和相变溶剂硬脂酸丁酯复配物作为初始芯材,以酸性染料作为扩展染料,以密胺树脂作为壁材,采用原位聚合法制备多元色素光敏变色微胶囊,并采用丝网印花工艺将其应用在棉织物上。借助台式扫描电子显微镜、傅里叶红外光谱仪、差示扫描量热仪、热重分析仪等表征微胶囊的表面形貌、特征官能团和热性能,研究了印花织物的光敏变色性和稳定性。结果表明:优选螺噁嗪、硬脂酸丁酯与酸性染料的质量比为0.05:50:0.1,控制芯壁比为1:1,制得的微胶囊具有圆球形外观,平均粒径约为3 μm,包覆率可达73.4%;该变色微胶囊具有出色的热稳定性,可在不同环境温度的紫外和可见光辐照下实现粉红色与蓝色的可逆颜色变化,可赋予织物良好的光敏变色性和变色稳定性。

关键词: 光敏染料, 扩展染料, 变色微胶囊, 丝网印花, 光敏变色织物

Abstract:

Objective Photochromic dye is a type of intelligent material with reversible photochromic function. Most organic photochromic dyes have single color-changing color spectra, which are difficult to meet the needs of diverse color changes. In order to solve the problem that the color-changing range of photochromic dyes is narrow and the color is limited to reversible changes from colorless to colored, a method for widening the color range of photochromic microcapsules is proposed.

Method Multi-colorant photochromic microcapsules were prepared by in-situ polymerization with the composite of photochromic dye spiroxazine and phase change solvent butyl stearate as the initial core material, acid dye as the extended dye, and melamine resin as the wall material. The surface morphology, characteristic functional groups and thermal properties of microcapsules were characterized using scanning electron microscope, infrared spectrometer, differential scanning calorimeter and thermogravimetric analyzer. The photochromic fabrics were prepared by screen printing using multi-colorant photochromic microcapsules as main components and fabrics as substrates, and the related color-changing properties were studied.

Results The photochromic microcapsules prepared by in-situ polymerization were spherical and had good encapsulation integrity. A small number of irregular particles on the surface was self-polymerized melamine resin, and no obvious agglomeration occered between the microcapsules. The microcapsule particle size was relatively uniform, with an average particle size of about 3 μm. The core material with the mass ratio of spioxazine to butyl stearate to acid dye of 0.05:50:0.1 was selected, and the mass ratio of the core to wall material was adjusted. When the core to wall ratio is 1:1, the encapsulation rate of photochromic microcapsules reached 73.4%. Through the infrared spectrum analysis of the photochromic microcapsule and its components, it could be inferred that there is no chemical reaction between the core material, the extended dye and the wall material. The photochromic microcapsule contained only the initial core material, C.I. Acid Red 337 and the wall material of melamine resin. The thermogravimetric analysis showed that the thermal degradation temperature of the core material was about 190 ℃, while the thermal degradation temperature of the photochromic microcapsule under the coating of melamine resin arrived at about 370 ℃, indicating that the thermal stability of the core material was improved by the microencapsulation. The photochromic microcapsules achieved reversible color change between pink and blue when irradiated by UV and D65 light source at 0 ℃. At the same ambient temperature, dark and D65 light sources showed little effect on the color recovery time of the photochromic microcapsules. Even without visible light irradiation, the photochromic microcapsules still demonstrated good color recovery. The printed patterns on fabrics achieved reversible color change under the irradiation UV and D65 light sources. No significant difference existed in the re-color state of cotton fabrics under different temperatures and color-changing cycles.

Conclusion This paper introduced a method to broaden the photochromic microcapsule chromatography. Multi-colorant photochromic microcapsules were prepared by in-situ polymerization with the compound of photochromic dye spiroxazine, phase change solvent butyl stearate and extended dye C.I. Acid Red 337 as the initial core material, and melamine resin as the wall material. The controlled mass ratio of spiroxazine to butyl stearate to extended dye C.I. Acid Red 337 is 0.05:50:0.1. When the core to wall ratio is 1:1, the prepared microcapsules have a spherical appearance with an average particle size of about 3 μm, and then capsulation rate can reach 73.4%. The photochromic microcapsules have excellent thermal stability and color-changing sensitivity. By adding acid dyes as extended colorants with different color shades and mass ratios, the photochromic microcapsules can achieve color changes between different colors, which significantly expands the color-change range of photochromic microcapsules. The microcapsules can be applied to cotton, polyester and other fabrics through screen printing process, which can give fabrics good color sensitivity and stability.

Key words: photochromic dye, extended dye, color-changing microcapsule, screen printing, photochromic fabric

中图分类号: 

  • TS194.5

图1

不同光敏染料和硬脂酸丁酯质量比下初始芯材在0 ℃时紫外光辐照前后的颜色变化"

图2

不同光敏染料、硬脂酸丁酯和酸性染料质量比的芯材在0 ℃时紫外光辐照前后的颜色变化"

图3

不同色相的酸性染料制备的光敏微胶囊在0 ℃时紫外光辐照前后的颜色变化 A—0.1 g C.I.酸性黄79; B—0.1 g C.I.酸性艳绿81; C—0.07 g C.I.酸性艳绿81和0.03 g C.I.酸性红337;D—0.03 g C.I.酸性艳绿81和0.07 g C.I.酸性红337;E—0.01 g C.I.酸性红337。"

图4

不同芯壁比下光敏微胶囊的DSC曲线"

图5

光敏微胶囊的扫描电镜照片及粒径分布图"

图6

光敏微胶囊及其各组分的红外光谱图"

图7

光敏微胶囊及各组分的热重曲线图"

图8

0 ℃条件下光敏微胶囊在紫外光和D65光源照射下的颜色变化"

图9

不同环境温度下光敏微胶囊在黑暗和D65光源下的变色灵敏性"

图10

螺噁嗪染料光致变色过程"

图11

不同环境温度下光敏微胶囊印制棉织物分别在变色循环1、30、60次后的变色灵敏性"

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