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林产化学与工业 ›› 2019, Vol. 39 ›› Issue (1): 53-60.doi: 10.3969/j.issn.0253-2417.2019.01.008

• 研究报告 • 上一篇    下一篇

硅烷化纳米SiO2改性酚醛泡沫的性能表征

张娜(),胡立红*(),郭亚军,周永红   

  1. 中国林业科学研究院 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局 林产化学工程重点开放性实验室;江苏省 生物质能源与材料重点实验室,江苏 南京 210042
  • 收稿日期:2018-08-30 出版日期:2019-02-25 发布日期:2019-03-14
  • 通讯作者: 胡立红 E-mail:zhangna060625@163.com;zhlh990907@sina.com
  • 作者简介:张娜(1991—),女,山东邹平人,硕士生,主要从事生物基酚醛树脂研究;E-mail:zhangna060625@163.com
  • 基金资助:
    “十三五”重点研发计划(2017YFD0601003);国家自然科学基金资助项目(31470613);中国林科院林产化学工业研究所团队建设创新工程项目(LHSXKQ11)

Characterization of Phenolic Foam Modified by Silanized Nano-SiO2

Na ZHANG(),Lihong HU*(),Yajun GUO,Yonghong ZHOU   

  1. Institute of Chemical Industry of Forest Products, CAF; National Engineering Lab. for Biomass Chemical Utilization; Key and Open Lab. of Forest Chemical Engineering, SFA; Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China
  • Received:2018-08-30 Online:2019-02-25 Published:2019-03-14
  • Contact: Lihong HU E-mail:zhangna060625@163.com;zhlh990907@sina.com
  • Supported by:
    “十三五”重点研发计划(2017YFD0601003);国家自然科学基金资助项目(31470613);中国林科院林产化学工业研究所团队建设创新工程项目(LHSXKQ11)

摘要:

采用溶胶-凝胶法制备纳米SiO2,并通过加入硅烷偶联剂1, 1, 3, 3-四甲基二硅氧烷对纳米SiO2进行硅烷化,用硅烷化后的纳米SiO2制备改性酚醛树脂(PR1~PR6),将改性酚醛树脂制成相应的酚醛泡沫(PF1~PF6)。采用FT-IR、TGA/FT-IR和TGA等方法对酚醛树脂的性能进行表征和检测。测试结果表明:改性后的酚醛树脂成功引入硅烷化的纳米SiO2,并与树脂发生了化学交联反应,形成Si—O—Si和Si—O;游离酚测试结果显示,随着纳米SiO2含量的增加游离酚含量急剧下降,正硅酸四乙酯(TEOS)含量相同而硅烷偶联剂含量不同时对游离酚含量影响不大,当硅脂为3.22 g,硅烷偶联剂为2 g时与PR4组成时其效果最好;羟甲基含量检测结果显示随着纳米SiO2含量的增加,羟甲基含量迅速增加至高值;机械性能测试显示,当硅脂质量分数为0.5%(以酚醛树脂的质量计),硅烷偶联剂为0.3%时,PF4的弯曲强度和抗压强度较PF1分别提高了73.3%和83.4%,较好地提高了泡沫的机械性能。

关键词: 酚醛树脂, 纳米SiO2, 硅烷化, 游离酚, 机械性能

Abstract:

Nano-SiO2 was prepared by sol-gel method. Then the silanization of nano-SiO2 was carried out by adding silane coupling agent 1, 1, 3, 3-tetramethyldisiloxane and obtained a silanized nano-SiO2 that was used to modify phenolic resins (PR1 -PR6). These modified phenolic resins were then converted into the corresponding phenolic foam (PF1 -PF6). FT-IR, TGA/FT-IR and TGA were applied to investigated the properties of these modified phenolic resins. The test results showed that the modified phenolic resin has successfully incorporated silanized nano-silica via the chemical crosslinking reaction that formed Si—O—Si and Si—O bonds. Free phenol test results showed that with the increase of nano-silica content, the free phenol content drastically decreased. However, the same content of tetraethoxysilane(TEOS) with the different content of silane coupling agent had little effect on the free phenol content. When the silicone grease was 3.22 g and the silane coupling agent was 2 g, PR4 composition had the best performance. It was also found that with the increase of nano-silica content, the hydroxymethyl content rapidly increased to a high value. The mechanical properties test showed that when the mass fraction of silicone grease was 0.5% (calculated by the mass of phenolic resin, the same below)and the silane coupling agent was 0.3%, the flexural strength and compressive strength of PF4 were increased by 73.3% and 83.4% respectively, while compared with those of PF1, which resulted in the improve of the mechanical properties of the foam. In view of these test results, PF4 has exhibited the best modification effect and met the initial requirements.

Key words: phenolic resin, nano-SiO2, silanization, free phenol, mechanical properties

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