Journal of Textile Research ›› 2025, Vol. 46 ›› Issue (04): 103-108.doi: 10.13475/j.fzxb.20240602301

• Dyeing and Finishing Engineering • Previous Articles     Next Articles

Application of choline chloride deep eutectic solvent in degumming and auxiliary bleaching of silk sheets

ZHANG Hui1, YANG Haiwei1, JIN Xianhua2, YANG Chao2, WANG Zongqian1()   

  1. 1. Anhui Provincial Ecological Textile Printing and Dyeing Innovation Center, Anhui Polytechnic University,Wuhu, Anhui 241000, China
    2. Transfar Zhilian Co., Ltd., Hangzhou, Zhejiang 311215, China
  • Received:2024-06-12 Revised:2024-11-27 Online:2025-04-15 Published:2025-06-11
  • Contact: WANG Zongqian E-mail:wzqian@ahpu.edu.cn

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Abstract:

Objective Silk is an extremely important natural protein fiber, and degumming is an essential step in silk processing. The conventional degumming method has problems such as long degumming time and high pollution caused by degumming. It is hence necessary to develop a new degumming process so as to improve the degumming efficiency. In this study, the degumming mechanism of silk was analyzed based on the application of choline chloride/oxalic acid dihydrate deep eutectic solvent in the degumming and auxiliary bleaching of silk sheets.

Method Silk sheets were accurately weighed, and were immerged into choline chloride deep eutectic solvents with different concentrations, followed by magnetical stirring at 90 ℃ for 80 min and washing with deionized water and drying to a constant weight. The performance of the degummed silk was tested by the LB-48B fluorescence whiteness meter and the Datacolor 650 color matching instrument, and the best deep eutectic solvent degumming process was screened. The morphology and aggregate structure of the degummed silk were measured by the VHX-970F ultra-depth-of-field microscope system and the D8 ADVANCE X-ray diffractometer. On the other hand, the mechanical properties of sodium carbonate and deep eutectic solvent degummed silk sheets were compared. In order to improve the whiteness of degummed silk with deep eutectic solvent, a mass concentration of 5 g/L hydrogen peroxide was further used to bleach the degummed silk, and the properties of the bleached silk were analyzed.

Results The experimental results showed that the prepared choline chloride/oxalic acid dihydrate deep eutectic solvent had the best degumming effect on silk sheets, with the degumming condition of the degumming rate 24.5% at 90 ℃, 1∶50 and 80 min. Compared with choline chloride/ethylene glycol deep eutectic solvent and choline chloride/urea deep eutectic solvent, it was neutral and weakly alkaline, which was not conducive to the dissolution and removal of sericin. The apparent viscosity of choline chloride/oxalic acid deep eutectic solvent was larger, and its degumming effect was relatively poor. Compared with the urea and sodium carbonate degumming processes, urea degumming took a long time, while sodium carbonate degumming caused silk fibroin fiber damage failing to achieve the desired degumming effect. The standard deviation of the whiteness value of the degummed silk by the choline chloride/oxalic acid dihydrate deep eutectic solvent was relatively small, indicating that the choline chloride/oxalic acid dihydrate deep eutectic solvent degumming was more uniform, and the breaking strength of sodium carbonate degummed silk was decreased significantly with the increase of tensile force. Based on the swelling and dissolution of deep eutectic solvents, the sericin on the silk surface was removed, and the fiber diameter expanded 1.17 times over the original size. X-ray diffractometer and Fourier transform infrared spectrometer analyses revealed that the intensity of the β-fold structure peak of degummed silk was enhanced, the signal of the diffraction peak of silk I. structure was weakened, and the diffraction peak of silk II structure remained unchanged. Furthermore, the reflectivity and whiteness of the degummed silk after bleaching with hydrogen peroxide were improved.

Conclusion Choline chloride/oxalate dihydrate deep eutectic solvent has strong acidity, which has the best degumming effect for silk sheets, optimizes the degumming conditions, shortens the process flow and improves efficiency compared with urea degumming, and sodium carbonate degumming is easy to cause silk damage. Compared with silk sheets, the peak strength of the β-fold structure of degummed silk was enhanced, the signal of the diffraction peak of silk I. structure was weakened, and the diffraction peak of silk II structure was not changed. Due to the excellent swelling and dissolution effect of eutectic solvent, the swelling of silk fibers is promoted and the removal of sericin components is accelerated. At the same time, the effective interaction between fiber and hydrogen peroxide is enhanced, and the whiteness of degummed silk was further improved.

Key words: deep eutectic solvent, silk, degumming process, bleaching, degumming mechanism, choline chloride

CLC Number: 

  • TS143.3

Tab.1

PH value of different deep eutectic solvents and degumming rate of silk"

样品编号 pH值 脱胶率/%
DES-1 6.75 11.5
DES-2 9.31 9.5
DES-3 1.25 23.0
DES-4 1.46 24.5

Fig.1

Degumming rate, whiteness of silk under different degumming processes"

Fig.2

Strength curves of silk with different degumming processes"

Fig.3

Morphological changes of silk before and after degumming. (a) Silk sheets; (b) Degummed silk"

Fig.4

Infrared spectra of silk sheets and degummed silk"

Fig.5

X-ray diffraction curves of silk sheets and degummed silk"

Fig.6

Reflectance curves of silk treated by different processes"

Fig.7

Whiteness value of silk sheets treated by different processes"

Fig.8

Schematic diagram of the degumming mechanism of silk"

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