聚硅氧烷改性环氧衣康酸酯水性UV固化树脂的制备及性能

doi:10.3969/j.issn.0253-2417.2022.04.002

林产化学与工业 ›› 2022, Vol. 42 ›› Issue (4): 9-15.doi: 10.3969/j.issn.0253-2417.2022.04.002

聚硅氧烷改性环氧衣康酸酯水性UV固化树脂的制备及性能

边均娜¹^,², 陈健¹^,², 杨兆哲¹^,², 吴国民¹^,²^,*(), 孔振武¹^,²

1. 中国林业科学研究院林产化学工业研究所；江苏省生物质能源与材料重点实验室；国家林业和草原局林产化学工程重点实验室；林木生物质低碳高效利用国家工程研究中心，江苏南京 210042
2. 南京林业大学江苏省林业资源高效加工利用协同创新中心，江苏南京 210037

收稿日期:2021-05-15 出版日期:2022-08-28 发布日期:2022-09-01
通讯作者: 吴国民 E-mail:wooguomin@163.com
作者简介:吴国民，副研究员，博士，硕士生导师，主要从事天然资源化学与利用研究；E-mail: wooguomin@163.com
边均娜(1995—)，女，山东潍坊人，硕士生，从事生物基水性光固化树脂研究
基金资助:
中国林科院中央级公益性科研院所基本科研业务费专项资金重点项目(CAFYBB2020GA001)

Preparation and Properties of Waterborne UV Curable Epoxy Itaconate Resin Modified by Polysiloxane

Junna BIAN¹^,², Jian CHEN¹^,², Zhaozhe YANG¹^,², Guomin WU¹^,²^,*(), Zhenwu KONG¹^,²

1. Institute of Chemical Industry of Forest Products, CAF; Key Lab.of Biomass Energy and Material, Jiangsu Province; Key Lab. of Chemical Engineering of Forest Products, National Forestry and Grassland Administration; National Engineering Research Center of Low-Carbon Processing and Utilization of Forest Biomass, Nanjing 210042, China
2. Jiangsu Co-Innovation Center of Efficient Processing and Utilization of Forest Resources, Nanjing Forestry University, Nanjing 210037, China

Received:2021-05-15 Online:2022-08-28 Published:2022-09-01
Contact: Guomin WU E-mail:wooguomin@163.com

摘要/Abstract

摘要：

利用端氢聚硅氧烷改性环氧衣康酸酯(IE)树脂，将所得聚硅氧烷改性环氧衣康酸树脂(SiIE)与半封端异氰酸酯中间体接枝共聚，制得聚硅氧烷改性半封端异氰酸酯环氧衣康酸酯树脂(IPDIHSiIE)。采用红外光谱(FT-IR)、核磁氢谱(¹H NMR)表征了IPDIHSiIE的化学结构，考察了聚硅氧烷用量对改性树脂及漆膜理化性质的影响。实验结果表明：聚硅氧烷与IE树脂在90 ℃下8 h可反应完全，通过硅氢加成可成功制备目标产物。随着聚硅氧烷用量的增加，改性树脂水分散体的粒径逐渐增大，贮存稳定性变差，凝胶率先上升后下降，当聚硅氧烷用量为5%时，水分散体的Z均粒径为129.8 nm，水分散体呈半透明，贮存一个月无明显变化，凝胶率达到最大，为93.1%。漆膜的疏水性能随聚硅氧烷用量的增加而提高，改性漆膜具有良好的热稳定性能；随着聚硅氧烷用量的增加，漆膜的铅笔硬度和柔韧性得到提高，附着力略有下降，玻璃化转变温度逐渐下降。

关键词: 衣康酸, 环氧树脂, 水性, UV固化, 聚硅氧烷

Abstract:

Semi-terminated isocyanate epoxy itaconate resin modified by silicone(IPDIHSiIE) was synthesized by graft copolymerization of polysiloxane modified epoxy itaconate resin(SiIE) that was prepared from the reaction between hydroterminated polysiloxane modified epoxy itaconic acid ester resin and half-terminated isocyanate. The chemical structure of IPDIHSiIE was characterized by FT-IR and ¹H NMR. Effects of the amount of polysiloxane on the physical and chemical properties of the modified resin and the film were investigated. The results showed that the reaction between polysiloxane and epoxy itaconate resin was completed at 90 ℃ for 8 h, indicating that the target product could be successfully prepared by silicohydride addition. With the increase of the amount of polysiloxane, the particle size of the modified resin dispersion gradually increased, the storage stability became worse, and the gel first risen and then fell. When the content of polysiloxane was 5%, the Z-mean particle size of aqueous dispersion was 129.8 nm, the aqueous dispersion was translucent and had no obvious change after storage for one month. Meanwhile, the gel rate reached the maximum of 93.1%. The hydrophobic property of the modified film was improved with the increase of polysiloxane content, and the film had good thermal stability. With the increase of polysiloxane content, the pencil hardness and flexibility of the film were improved, the adhesion decreased slightly and the glass transition temperature decreased gradually.

Key words: itaconic acid, epoxy resin, waterborne, UV curable, polysiloxane

中图分类号:

TQ35

边均娜, 陈健, 杨兆哲, 吴国民, 孔振武. 聚硅氧烷改性环氧衣康酸酯水性UV固化树脂的制备及性能[J]. 林产化学与工业, 2022, 42(4): 9-15.

Junna BIAN, Jian CHEN, Zhaozhe YANG, Guomin WU, Zhenwu KONG. Preparation and Properties of Waterborne UV Curable Epoxy Itaconate Resin Modified by Polysiloxane[J]. Chemistry and Industry of Forest Products, 2022, 42(4): 9-15.

图/表 7

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用量/% dosage	Z均粒径/nm Z-average size	外观 appearance	贮存时间/d storage time
1	62.3	半透明translucence	≥30
3	65.1	半透明translucence	≥30
5	129.8	半透明translucence	≈30
7	142.6	乳白色milk-white	＜7
9	186.5	乳白色milk-white	＜7

用量/% dosage	铅笔硬度 pencil hardness	附着力/级 adhesion/grade	柔韧性/mm flexibility	抗冲击性/(kg·cm) impact strength
1	2H	1	5	35
3	2H	1	3	30
5	2H	1	1	30
7	2H	2	1	30
9	3H	2	2	30

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聚硅氧烷改性环氧衣康酸酯水性UV固化树脂的制备及性能

Preparation and Properties of Waterborne UV Curable Epoxy Itaconate Resin Modified by Polysiloxane

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