拼混活性染料染色多组分定量分析方法

doi:10.13475/j.fzxb.20221100501

纺织学报 ›› 2023, Vol. 44 ›› Issue (07): 141-150.doi: 10.13475/j.fzxb.20221100501

拼混活性染料染色多组分定量分析方法

郭玉秋¹^,², 钟毅¹^,²^,³, 徐红¹^,²^,³, 毛志平¹^,⁴^,⁵()

1.东华大学化学与化工学院, 上海 201620
2.东华大学生态纺织教育部重点实验室, 上海 201620
3.东华大学纺织科技创新中心, 上海 201620
4.国家先进印染技术创新中心, 山东泰安 271000
5.国家染整工程技术研究中心, 上海 201620

收稿日期:2022-11-03 修回日期:2023-04-24 出版日期:2023-07-15 发布日期:2023-08-10
通讯作者: 毛志平(1969-),男,研究员,博士。主要研究方向为纺织品功能性整理及绿色环保助剂。E-mail:zhpmao@dhu.edu.cn。
作者简介:郭玉秋(1997—),女,硕士生。主要研究方向为多组分活性染料拼色染色定量分析方法。
基金资助:
山东省重点研发计划项目(2022ZDPT02)

Multi-component quantitative analysis method for dyeing with reactive dyes

GUO Yuqiu¹^,², ZHONG Yi¹^,²^,³, XU Hong¹^,²^,³, MAO Zhiping¹^,⁴^,⁵()

1. College of Chemistry and Chemical Engineering, Donghua University, Shanghai 201620, China
2. Key Laboratory of Science & Technology of Eco-Textile, Ministry of Education, Donghua University, Shanghai 201620, China
3. Innovation Center for Textile Science and Technology, Donghua University, Shanghai 201620, China
4. Research Institute of Advanced Dyeing & Finishing Technology Co., Ltd., Taian, Shandong 271000, China
5. National Engineering Research Center For Dyeing and Finishing of Textiles, Shanghai 201620, China

Received:2022-11-03 Revised:2023-04-24 Published:2023-07-15 Online:2023-08-10

摘要/Abstract

摘要：

将拉曼光谱技术与化学计量法(偏最小二乘法)结合,建立了一种简便、灵敏、精确的多组分定量分析方法,可对混合液体多组分同时进行定量分析,进而有效提高织物色光稳定性和产品质量。首先根据拉曼光谱特征峰与染料质量浓度之间的线性关系测定待测组分的检测极限,确定定量成分适用的质量浓度范围;然后构建多组分混合体系定量分析模型;最后通过检测双乙烯砜活性基结构的活性染料拼混染色在吸附过程中各组分质量浓度变化和纤维上染百分率,进一步评价染料的配伍性。结果表明:模型的拟合值与标准值之间的相关系数均大于0.99,内部交互验证均方根误差和预测均方根误差值均小于0.2,通过本文方法构建的多组分定量分析模型具有较高的准确性,且拼混的染料结构和质量比会影响单一组分的上染过程。

关键词: 拉曼光谱技术, 多组分定量分析模型, 活性染料, 拼色染色, 棉织物

Abstract:

Objective Color matching dyes in the dyeing process has been attracting more attention, and more research efforts have been made to explore the principle and technology of color matching dyeing. The key to study the dyeing principle and promote the dyeing technology is to monitor the change of dye concentration in the dyeing process. At present, there is a lack of a mature and systematic online detection method and detection equipment. The difficulty lies in how to achieve fast and accurate online detection which offers strong applicability and a wide range of concentration detection.

Method A simple, sensitive and accurate multi-component quantitative analysis method was established by combining Raman spectroscopy with chemometrics method (partial least squares method), for simultaneous quantitative analysis of multi-components in mixed liquids. This detection method was adopted to construct a rapid detection and quantitative analysis model for the concentration of each component in the mixed dye solution of Reactive Violet 4 (RR4), Reactive Orange 4(RY4) and Reactive Black 5(RB5), and the process of dyeing cotton fabrics with different concentration ratios was monitored online. The detection limit of the components to be tested was determined according to the linear relationship between the characteristic peaks of Raman spectroscopy and the dye concentration, and the applicable concentration range of the quantitative components was determined.

Results The detection ranges of RR4, RY4 and RB5 were 0.08-15 g/L, 0.08-20 g/L and 0.05-20 g/L, respectively (Fig. 1 and 2). The quantitative analysis model of multi-component mixed system was constructed. The results showed that the correlation coefficient (R²) between the fitting value of the model and the standard value was greater than 0.99, and the values of root mean square error(RMSECV) and root mean square error of prediction (RMSEP) were smaller than 0.2. The multi-component quantitative analysis model constructed by this method offered high accuracy. Finally, the compatibility of dyes was further evaluated by detecting the concentration change of each component and the dyeing efficiency of fibers during the adsorption process of reactive dyes with divinylsulfone active group structure. Under the condition of dye dosage of 1% (o. w. f), in the RR4/RY4 mixed system, the dyeing percentage curve and S value of the two dyes were significantly different from those of the single component dyeing, but the dyeing consistency of the two dyes was stable under the experimental concentration ratio. The dyeing behaviors of RY4/RB5 and RR4/RB5 were consistent, and the difference was not significant compared with that of the single component dyeing. Therefore, it was generally believed that the three dyes selected showed good compatibility in the process of color matching and dyeing at lower dye dosage. In the mixed system of RR4/RY4, RR4 and RY4 still showed a competitive relationship when the dye dosage was 2% (o. w. f), but the dyeing synchronicity was not much different and the compatibility was still good. In the mixed system of RY4/RB5 and RR4/RB5, the dyeing percentage of single component fluctuated greatly and the compatibility became worse.

Conclusion The concentration range of Raman spectroscopy is found limited. When the dye concentration is too low, the sample content is low and the spectral signal is weak. When the dye concentration is too high, the fluorescence characteristics of the dye itself will affect the intensity and accuracy of the Raman spectral signal, and even fluorescence quenching occurs, making the Raman spectral signal annihilate, and limiting the detectable concentration range. Then, the study on the compatibility of reactive dyes with divinylsulfone active group structure shows that the structure and mass ratio of the mixed dyes will affect the dyeing process of a single component. Therefore, the compatibility can be evaluated according to the actual dyeing process of each component dye, so as to further guide the dye formulation design.

Key words: Raman spectroscopy, multi-component quantitative analysis model, reactive dye, matching dyeing, cotton fabric

中图分类号:

O657.37

郭玉秋, 钟毅, 徐红, 毛志平. 拼混活性染料染色多组分定量分析方法[J]. 纺织学报, 2023, 44(07): 141-150.

GUO Yuqiu, ZHONG Yi, XU Hong, MAO Zhiping. Multi-component quantitative analysis method for dyeing with reactive dyes[J]. Journal of Textile Research, 2023, 44(07): 141-150.

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预处理方法	混合组分		校正集参数			预测集参数
预处理方法	混合组分		PCs	RMSECV	R²	RMSEP	R²
一阶导数预处理	RR4/RY4	RR4	3	0.132 0	0.997 0	0.125	0.996 2
		RY4	4	0.112 0	0.997 2	0.127	0.996 8
	RY4/RB5	RY4	6	0.096 2	0.998 3	0.170	0.993 9
		RB5	5	0.083 4	0.997 9	0.175	0.994 8
	RB5/RR4	RB5	3	0.145 0	0.996 5	0.156	0.993 6
		RR4	5	0.128 0	0.997 5	0.128	0.992 8
一阶导数加光谱平滑预处理	RR4/RY4	RR4	3	0.135 0	0.996 8	0.125	0.996 0
		RY4	4	0.115 0	0.997 0	0.131	0.996 2
	RY4/RB5	RY4	7	0.084 6	0.998 7	0.154	0.994 4
		RB5	5	0.083 4	0.997 8	0.173	0.994 9
	RB5/RR4	RB5	3	0.144 0	0.996 4	0.152	0.993 9
		RR4	5	0.125 0	0.997 5	0.124	0.993 1

拼混活性染料染色多组分定量分析方法

Multi-component quantitative analysis method for dyeing with reactive dyes

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