纺织学报 ›› 2025, Vol. 46 ›› Issue (12): 133-141.doi: 10.13475/j.fzxb.20250301001

• 染整工程 • 上一篇    下一篇

液态靛蓝染料的制备及其对棉织物的染色性能

宋佳怡1,2,3, 王政驿1,2, 程献伟1,2,3(), 关晋平1,2, 朱亚伟1,2,3   

  1. 1.苏州大学 纺织与服装工程学院, 江苏 苏州 215123
    2.苏州大学 纺织行业纺织材料阻燃整理重点实验室,江苏 苏州 215123
    3.苏州大学 江苏省纺织印染节能减排与清洁生产工程研究中心, 江苏 苏州 215123
  • 收稿日期:2025-03-06 修回日期:2025-09-17 出版日期:2025-12-15 发布日期:2026-02-06
  • 通讯作者: 程献伟(1992—),男,副教授,博士。主要研究方向为生物质化学品及功能性纺织品加工理论与技术。E-mail: chengxianwei@suda.edu.cn
  • 作者简介:宋佳怡(1998—),女,硕士生。主要研究方向为天然染料染色和纺织品阻燃整理。
  • 基金资助:
    苏州市产业前瞻与关键核心技术项目(SYC2022017);国家自然科学基金青年科学基金项目(22408247)

Preparation of liquid indigo dye and its dyeing performance on cotton fabrics

SONG Jiayi1,2,3, WANG Zhengyi1,2, CHENG Xianwei1,2,3(), GUAN Jinping1,2, ZHU Yawei1,2,3   

  1. 1. College of Textile and Clothing Engineering, Soochow University, Suzhou, Jiangsu 215123, China
    2. Key Laboratory of Flame Retardancy Finishing of Textile Materials (CNTAC), Soochow University, Suzhou, Jiangsu 215123, China
    3. Jiangsu Engineering Research Center of Textile Dyeing and Printing for Energy Conservation, Discharge Reduction and Cleaner Production (ERC), Soochow University, Suzhou, Jiangsu 215123, China
  • Received:2025-03-06 Revised:2025-09-17 Published:2025-12-15 Online:2026-02-06

摘要: 粉状靛蓝染料在染色过程中存在染料利用率低、使用时易产生粉尘及废水排放量大等问题,通过施加高剪切力,使染料颗粒集群破裂为尺寸更小的颗粒,并借助表面活性剂的作用实现稳定分散,制备得到液态靛蓝染料。考察了粉状和液态靛蓝染料的吸光度、液态染料的放置稳定性及其流变性能;探究了氢氧化钠和保险粉质量浓度、还原时间、浸轧次数对染色棉织物表观色深(K/S值)与耐干湿摩擦色牢度的影响,并对比了相同浓度下液态与粉态染料染色效果,评价了染色织物的抗紫外线性能和抗菌性能。结果表明:液态靛蓝染料经稀释5万倍后放置24 h,其上下层吸光度分别为0.247和0.255,放置半年后,平均粒径由543 nm增至656 nm,显示出良好的稳定性;液态靛蓝染料的表观黏度随剪切速率增加而降低,表现出假塑性流体特征;在相同用量下,液态靛蓝染料染色棉织物的K/S值高于粉态靛蓝染料染色样品,其中当质量浓度为10 g/L时,染色棉织物的K/S值较粉态染料染色提升49.3%,且耐干湿摩擦色牢度均达到3级及以上;此外,液态靛蓝染料染色棉织物还具有优异的抗紫外线性能和一定的抗菌性能。液态靛蓝染料能够显著提升靛蓝染色效率与织物功能性,展现出良好的应用前景。

关键词: 液态染料, 植物靛蓝, 棉织物, 流变性能, 染色性能, 抗紫外线性能, 抗菌性能

Abstract:

Objective Although powdered natural indigo is convenient for storage and transportation, it readily forms soft agglomerates in aqueous media due to electrostatic adsorption during dyeing. These aggregates are difficult to disperse by stirring, leading to low dye utilization, dust generation, and excessive wastewater in industrial production. Preparing liquid indigo dyes offers a promising solution by reducing particle size, enhancing reduction efficiency and dye uptake, and eliminating dust at its source.

Method A dispersion was prepared by mixing 30 g of vegetable indigo, 3 g of abrasive MF-2000A, 0.9 g of viscosity modifier Z5, and 63.1 g of water, followed by stirring at 600-700 r/min for 15 min. The mixture was transferred into a custom grinder, combined with 100-150 g of zirconium beads, and ground at 1 700-1 900 r/min. Particle size was monitored every 30 min with adjustments in grinding speed, and grinding was terminated once particle size plateaued. The resulting suspension was filtered through silk crepe de chine to achieve a 30% liquid indigo dye. The dipping process for dyeing cotton fabrics with 10 g/L liquid indigo was then optimized via single-factor experiments at a fixed dyeing temperature of 60 ℃ and subsequent steaming at 102 ℃ for 30 s. Finally, cotton fabrics dyed with 5-25 g/L liquid or powdered indigo were evaluated and compared in terms of K/S, L*, a*, b* values, rubbing and soaping fastness, as well as UV protection and antibacterial performance.

Results After grinding, the liquid indigo dye exhibited an average particle size of 543 nm with a polydispersity index of 0.01, which only increased to 656 nm after six months of storage, indicating excellent stability. Upon 50 000-fold dilution and 24 h storage, the absorbance change was merely 3.2%. MF-2000A facilitated ultrafine dispersion by preventing particle re-aggregation, while Z5 coated suspended particles to reduce interparticle friction and inhibiting sedimentation. The viscosity of the liquid dye decreased rapidly with increasing shear rate or temperature, consistent with pseudoplastic fluid behavior. In optimized conditions (10 g/L liquid indigo, 3 g/L NaOH, 12 g/L sodium hydrosulfite, 15 min reduction, six dips), the K/S value reached 15.61. The dyed fabrics achieved rubbing fastness of more than 3, soaping fastness of more than 3, UVA transmittance of 1.07, UVB transmittance of 1.15, and an ultraviolet protection factor of 90.19. Additionally, the antibacterial activity against Escherichia coli increased to 70%. Compared with powdered indigo, liquid indigo improved K/S values of cotton fabrics by 6.6%-49.3% across 5-25 g/L dye concentrations. This improvement arises from the finer particle size and absence of agglomeration, which enhance dye reduction and fabric wettability, while powdered dyes form agglomerates through van der Waals and hydrogen bonding interactions, reducing their effective surface area and diminishing reduction efficiency.

Conclusion The prepared liquid indigo dye demonstrated excellent storage stability, pseudoplastic rheology, and superior dyeing performance compared with powdered indigo. The optimal process parameters were a dye/NaOH/sodium hydrosulfite ratio of 1∶1∶4, a 15 min pre-reduction time, and six dipping cycles. At 10 g/L, liquid indigo increased the K/S value of dyed cotton fabrics by 49.3% relative to powdered indigo, while also imparting strong UV protection and moderate antibacterial activity.

Key words: liquid dye, plant indigo, cotton fabric, rheological property, dyeing property, UV protection, antibacterial property

中图分类号: 

  • TS194.2

图1

液态靛蓝和粉态靛蓝的扫描电子显微镜照片"

图2

液态靛蓝染料放置后不同位置悬浮体的吸光度曲线"

图3

液态靛蓝染料放置不同时间的粒径分布图"

表1

液态靛蓝剪切应力的一元线性回归方程"

C1 C2 R2 F P
1.0809 0.009 0.982 1574.9 0.0001

表2

液态靛蓝黏度的Morgan-Mercer-Florin方程"

模拟曲线 C3 C4 C5 C6 R2 F P
黏度-剪切速率曲线 -35.624 1 -0.995 8 -35.282 9 0.000 5 0.990 7 918.6 0.000 1
黏度-温度曲线 6.571 1 -30.585 9 6.742 1 0.606 5 0.985 5 589.0 0.000 1

图4

液态靛蓝色素的流变性能"

图5

靛蓝浸轧染色原理及工艺"

表3

氢氧化钠质量浓度对颜色特征值与耐摩擦色牢度的影响"

氢氧化钠
质量浓度/
(g·L-1)
pH值 L* a* b* 耐摩擦色牢度/级
湿
1.0 6.4 62.01 -2.20 -24.89 4~5 4
1.5 7.5 52.67 -2.27 -26.96 4~5 4
2.0 10.9 40.30 -0.80 -26.92 4 3~4
2.5 11.7 37.79 -1.18 -26.40 4 3
3.0 11.9 30.97 0.01 -23.77 4 3
3.5 12.2 35.97 -0.39 -25.39 4 3

图6

氢氧化钠和保险粉质量浓度、预还原时间和浸轧次数对液态靛蓝上染棉织物K/S值的影响"

图7

粉态与液态靛蓝染色上染棉织物K/S值对比"

表4

不同粉态和液态靛蓝染料用量染色棉织物的颜色特征值和色牢度"

染料
种类
染料质量
浓度/
(g·L-1)
L* a* b* 耐摩擦色
牢度/级
耐皂洗
色牢度/
湿
液态
染料
5 41.79 -4.04 -22.66 4~5 4 4
10 30.97 0.01 -23.77 4 3 4
15 28.75 -0.62 -21.21 3~4 2~3 3~4
20 25.59 0.78 -19.94 3 2~3 3~4
25 24.07 1.18 -18.96 3 2~3 3~4
粉态
染料
1.5 46.29 -5.30 -21.42 4~5 4 4
3.0 38.97 -0.98 -26.52 4~5 4 4
4.5 33.94 -3.34 -21.41 4 3 3~4
6.0 29.77 -2.08 -20.78 3~4 2~3 3~4
7.5 28.18 -1.77 -20.07 3 2~3 3

图8

不同质量浓度液态和粉态靛蓝染料染色织物的耐皂洗色牢度"

表5

染色织物的抗紫外线性能及对大肠埃希菌的抑菌率"

织物 抗紫外线性能 抑菌
率/%
TUVA/% TUVB/% UPF
原棉织物 4.07 7.84 13.03
染色棉织物 1.07 1.15 90.19 70
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