Journal of Textile Research ›› 2024, Vol. 45 ›› Issue (11): 128-135.doi: 10.13475/j.fzxb.20231203101

• Original article • Previous Articles     Next Articles

Synthesis of polyethylene glycol citrate ester smoothing agent and performance of compound formulation design for spinning oil agents

CHEN Shichang1,2(), YANG Dongdong1,2, CHEN Wenxing1   

  1. 1. College of Materials Science and Engineering, Zhejiang Sci-Tech University, Hangzhou, Zhejiang 310018, China
    2. Modern Textile Technology Innovation Center, Shaoxing, Zhejiang 312000, China
  • Received:2023-12-19 Revised:2024-05-16 Online:2024-11-15 Published:2024-12-30

Abstract:

Objective Chemical fibers need to undergo high-temperature thermal drawing and treating during post-processing, which can easily cause scattering and breakage. Oil agents can adjust friction characteristics and give fibers high-temperature smoothness during spinning processing to run smoothly and steadily for the fiber production. However, with domestically produced oil agents used at high temperatures, abnormal phenomenon such as serious coking of hot rollers and tangled (remnant) fibers would still occur. As a result, the spinning oil agents for PET industrial fibers in domestic large-scale production are independent of imports.

Method In view of the problems of poor heat resistance and poor high-temperature smoothness of domestic chemical fiber oils, compound design of oil components was carried out on the basis of successful synthesis of excellent smoothing agents, which was prepared from polyethylene glycol and citric acid as monomers. The smoothing agent synthesis conditions was optimized, then a heat-resistant spinning oil could be achieved with the presence of self-prepared smoothing agent, selected polyether emulsifiers and other components. The chemical structure, thermal properties and viscosity of the smoothing agent, and the smoothness, interface properties, antistatic properties and thermal stability of the oil agent were also characterized and compared with the current products.

Results The optimized conditions for the synthesis of polyethylene glycol citrate as smoothing agent are considered as: the acid-to-alcohol molar ratio of 1∶2, 0.02% of catalyst, the temperature of 170 ℃ with reaction time of 1.5 h in N2 atmosphere, and the esterification rate reaches 97%. The acid value, hydroxyl value and saponification value of the synthetic smoothing agent are 0.62 mgKOH/g, 8 mgKOH/g and 182 mgKOH/g, respectively. The high temperature viscosity and heat resistance are higher than that of common smoothing agents. The vital performance parameters of the well-designed oil agent are excellent, as the surface tension is 31.05 mN/m, the wear scar diameter is 0.538 mm, the friction coefficient is 0.043, the specific resistance is 1.63 MΩ/cm, and the conductivity reaches 6.13 μS/cm, and the friction and antistatic properties exceed the imported oils. Even more importantly, the oil smokes well and has excellent thermal stability. The respective volatilization loss rate in 2 h at 140 ℃ and 250 ℃ are only 1.4% and 12%.

Conclusion The excellent physical and chemical properties of polyethylene glycol citrate were synthesized as a smoothing agent, whose viscosity and interfacial properties were equivalent to those of imported oils. With a careful selection of emulsifier, antistatic agent and other components, the formulation of the oil agent was configured to meet the high requirements of PET industrial fiber, the friction and antistatic properties exceed the imported oil. In terms of thermal properties, the three self-prepared oil agents could be completely comparable to the same type imported oil.

Key words: polyethylene glycol citrate ester, spinning oil agent, smoothing agent, heat resistance, polyester industrial filament, chemical fiber industry

CLC Number: 

  • TQ340.47

Fig.1

Influence of synthesis conditions of fatty acid ester smoothing agent on esterification rate. (a) Influence of temperature; (b) Influence of reaction time; (c)Influence of acid-to-alcohol molar ratio; (d) Influence of catalyst content"

Tab.1

Comparison of basic properties of smoothing agents"

类别 酸值/
(mgKOH·g-1)
羟值/
(mgKOH·g-1)
皂化值/
(mgKOH·g-1)
PETO 0.5 13 187
TMPTO 1 10 185
聚乙二醇柠檬酸酯 0.62 8 182

Fig.2

Comparison of viscosities of smoothing agents"

Fig.3

Comparison of heat resistance properties of smoothing agents and raw materials"

Fig.4

Structural characterization of citric acid, polyethylene glycol and polyethylene glycol citrate esters. (a) Infrared spectra;(b) 1H-NMR spectra"

Tab.2

Comparison of physical and chemical properties of oils"

油剂类别 外观(25 ℃) pH值 水分含量/%
进口油剂 黄色液体 8.18 1.38
1# 黄色液体 8.05 1.00
2# 黄色液体 7.67 1.64
3# 黄色液体 7.89 1.57

Fig.5

Comparison of viscosities of oils"

Tab.3

Interfacial properties of oils"

油剂类别 表面张力/
(mN·m-1)
润湿
时间/s
接触角/
(°)
进口油剂 34.36 4.5 12.9
1# 31.05 5.1 11.2
2# 33.37 4.3 13.4
3# 33.25 4.3 14.5

Fig.6

Comparison of antistatic properties between self-prepared oil and imported oil"

Fig.7

Comparison of friction properties between self-prepared oil and imported oil. (a) Oil friction; (b) Wear spot diameter and friction coefficient"

Tab.4

Comparison of oil smoke conditions"

油剂类别 高温冒烟 油剂热稳定性
进口油剂 少量蓝烟 无析出物
1# 少量蓝烟 无析出物
2# 少量蓝烟 无析出物
3# 少量蓝烟 无析出物

Fig.8

Comparison of volatilization loss rates of oils"

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