纺织学报 ›› 2026, Vol. 47 ›› Issue (07): 202-208.doi: 10.13475/j.fzxb.20260203901

• 染整工程 • 上一篇    下一篇

成膜交联型弹性有机硅乳液的制备及其整理织物的性能

王建军1,2,3, 胡柳1,2,3, 陈天逸4, 沈军炎2,3, 杨雷1,2,3()   

  1. 1 浙江理工大学 纺织科学与工程学院(国际丝绸学院), 浙江 杭州 310018
    2 现代纺织技术创新中心(鉴湖实验室), 浙江 绍兴 312033
    3 浙江理工大学绍兴柯桥研究院, 浙江 绍兴 312000
    4 传化智联股份有限公司, 浙江 杭州 311200
  • 收稿日期:2026-02-28 修回日期:2026-05-11 出版日期:2026-07-15 发布日期:2026-07-29
  • 通讯作者: 杨雷(1975—),男,教授,博士。主要研究方向为功能纺织助剂设计与开发。E-mail:yanglei@zstu.edu.cn。
  • 作者简介:王建军(1997—),男,硕士生。主要研究方向为乳液及乳液聚合。
  • 基金资助:
    浙江省“尖兵领雁+X”研发攻关计划项目(ZX20251230X001);海宁市协同创新项目(20250108)

Preparation of film-forming crosslinkable elastic silicone emulsion and its fabric-finishing performance

WANG Jianjun1,2,3, HU Liu1,2,3, CHEN Tianyi4, SHEN Junyan2,3, YANG Lei1,2,3()   

  1. 1 School of Textile Science and Engineering, Zhejiang Sci-Tech University (International Institute of Silk), Hangzhou, Zhejiang 310018, China
    2 Zhejiang Modern Textile Technology Innovation Center(Jianhu Laboratory), Shaoxing, Zhejiang 312033, China
    3 Shaoxing-Keqiao Research Institute, Zhejiang Sci-Tech University, Shaoxing, Zhejiang 312000, China
    4 Chuanhua Zhilian Co., Ltd., Hangzhou, Zhejiang 311200, China
  • Received:2026-02-28 Revised:2026-05-11 Published:2026-07-15 Online:2026-07-29

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摘要：

针对纺织品弹性整理的市场需求,以及现有弹性聚氨酯改性有机硅体系存在的组分相容性差、使用性能不稳定等问题,提出一种基于乳液聚合、复配和后交联技术制备弹性有机硅乳液的新策略:首先以八甲基环四硅氧烷(D4)为单体,分别与含环氧基、氨基的硅烷偶联剂进行共聚,制备得到环氧官能化、氨基官能化2种有机硅乳液;将二者复配后应用于织物定形后整理,在织物热定形过程中,乳液中的环氧基与氨基发生跨粒子固化反应,形成三维交联网络,赋予织物良好弹性。采用红外光谱分析和差示扫描量热法,系统研究了复配比例、固化温度对交联反应的影响,优化了乳液复配组成;共聚时,将三乙氧基氨基偶联剂替换为二甲氧基结构后,有效降低了氨基硅油链的交联密度,复配乳液的交联反应峰顶温度降低30 ℃,据此构建了适配织物低温定形的弹性有机硅整理剂。结果表明,所得复配乳液在50 ℃贮存48 h及高剪切条件下仍保持优良的化学和分散稳定性;经该乳液整理后,涤纶织物的总弹性回复角较整理前提升45°。

关键词: 乳液聚合, 弹性有机硅乳液, 氨基硅油, 环氧硅油, 乳液成膜, 后交联反应, 有机硅整理剂

Abstract:

Objective In order to address the market demand for elastic textile finishing and to overcome the instability and performance limitations of polyurethane-silicone hybrid systems, a novel strategy is proposed based on emulsion polymerization, blending, and post-crosslinking to prepare elastic silicone oil emulsions, aiming to develop a stable, effective elastic silicone finishing agent that is capable of providing elasticity for textiles.

Method Within the emulsion system, octamethylcyclotetrasiloxane (D4) is copolymerized with coupling agents containing epoxy and amino groups, respectively, yielding two types of organosilicon emulsions functionalized with epoxy and amino groups. These two emulsions are then blended and applied to fabric finishing. During the curing stage, the epoxy and amino groups in the emulsion undergo interparticle crosslinking reactions, forming a three-dimensional network that imparts the fabric with elastic handling. The influences of blending ratio and curing temperature on the post-crosslinking reaction were systematically investigated using infrared spectroscopy and differential scanning calorimetry, intending to optimize the emulsion blend composition.

Results When the triethoxy groups of the amino coupling agent were replaced with dimethoxy groups during emulsion copolymerization, the polysiloxane chains transformed from a crosslinked structure to a linear structure, reducing the crosslinking temperature peak of the blended emulsion by 30 ℃. This enabled the development of a low-temperature crosslinking solution. Fourier transform infrared spectroscopy (FT-IR) analysis confirmed the successful ring-opening reaction between amino and epoxy groups of the emulsion blends during the high-temperature film formation process. Differential scanning calorimetry (DSC) results showed that the maximum crosslinking enthalpy was 25.3 J/g at the mass ratio of E3 to A3 of 1∶1, corresponding to an equimolar functional group ratio of amino and epoxy groups. The crosslinking reaction was sensitive to the curing temperature as well as chain structure. The increase of curing temperature from 120 ℃ to 180 ℃ led to the extent of reaction growing from 24.3% to 93.5%, as a result of enhanced polymer chain diffusion among particles at high temperature. The replacement of crosslinked chain structure amino silicone with linear one resulted in a 30 ℃ decrease in the reaction peak temperature, which benefits the finishing of heat-sensitive fabrics like nylon. The amino-epoxy blended emulsion also showed excellent chemical and disperse stability. The blend emulsion with a 1∶1 mixing was applied to finish polyester fabric, endowing a 45°increment of the elastic recovery angle to the finished fabric.

Conclusion Amino and epoxy functionalized silicone emulsion were successfully prepared by emulsion copolymerization of D4 with amino and epoxy coupling agents. The high efficiency curing reaction between amino and epoxy functionalities occurred during the film formation process of the blend latex at an increased temperature of 180 ℃. The reactivity of the blend emulsion was successfully maneuvered by blending ratio as well as chain structure of amino silicon emulsion. The measurement of reaction enthalpy indicated that the maximum value was achieved at 1∶1 blending ratio. Compared to the blend emulsion engaging amino silicon with crosslinked chain structure, the one blended with a linear chain structured amino silicon exhibited a significant decrease in the curing reaction temperature. The blend emulsion had excellent chemical and shear stability. All the above findings indicated the blend emulsion was applicable for fabric elastic finishing, which was further confirmed by the significant improvement in polyester fabric elastic recovery angle. In conclusion, a new and stable platform was demonstrated for developing high-performance silicone-based finishing agents showing elastic handling.

Key words: emulsion polymerization, elastic silicone emulsion, amino silicone oil, epoxy silicone oil, latex film formation, post-crosslinking reaction, silicone finishing agent

中图分类号: 

  • TS195.2

图1

E3、A3和E3-A3复配乳液烘干样的FT-IR谱图"

图2

E3-A3复配乳胶膜内交联网络示意图"

图3

E3-A3复配乳液膜及膜拉伸和应力释放后的照片"

图4

E3与A3质量比对复配乳液反应焓的影响"

图5

Tmax为120 ℃时的E3-A3(1∶1)三阶段固化反应热升温曲线"

图6

阶段Ι的Tmax对三阶段升温过程焓变及环氧基与氨基反应程度的影响"

图7

氨基硅油链结构对复配乳液反应的影响"

图8

温度对E3-A3复配乳液反应活性的影响"

图9

E3-A3(1∶1)复配乳液剪切前后的粒径分布图"

图10

涤纶织物表面形貌"

表1

乳液组成对整理织物弹性回复角的影响"

整理工作
液组成		 回复角/(°)
急弹 缓弹 总回复
未整理 115 139 254
E3 127 141 268
A3 120 137 257
E3-A3(1∶1) 143 156 299
E3-A3(1∶2) 137 152 289
E3-A3(1∶3) 130 147 277
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