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合成聚对苯二甲酸丙二醇酯负载型催化剂钛酸四丁酯/纳米二氧化硅的制备

叶冲1,姜敏2,张强2,刘茜1,周光远2*   

  1. (1.长春工业大学化学工程学院 长春 130022；
    2.中国科学院长春应用化学研究所， 中国科学院生态环境高分子材料重点实验室 长春130022)
  • 收稿日期:2012-02-09 修回日期:2012-04-27 出版日期:2013-01-10 发布日期:2013-01-10
  • 通讯作者: 周光远，研究员; Tel/Fax:0431-85262795; E-mail:gyzhou@ciac.jl.cn; 研究方向：可控聚合
  • 基金资助:
    国家自然科学基金委青年科学基金（51103152）资助项

Preparation of n-Butyl Titanate/Nano Silicon Oxide Synthesis of Poly(trimethylene terephthalate)

YE Chong1, JIANG Min2, ZHANG Qiang2, LIU Qian1, ZHOU Guangyuan2*   

  1. (1.College of Chemistry and Engineering,Changchun University of Technology,Changchun 130022,China；
    2.Key Laboratory of Polymer Ecomaterials,Changchun Institute of Applied Chemistry,Chinese Academy of Sciences,Changchun 130022,China)
  • Received:2012-02-09 Revised:2012-04-27 Published:2013-01-10 Online:2013-01-10

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2209

被引次数

10 | 1

摘要： 以钛酸酯偶联剂（TMC-201）为改性剂，采用超声波分散方法对亲水性纳米二氧化硅(nano-SiO2)进行了表面改性。采用浸渍法将钛酸四丁酯(Ti(OC4H9)4)负载于表面改性的nano-SiO2上，制备了纳米级Ti(OC4H9)4/nano-SiO2负载型催化剂。 考察了偶联剂用量、温度、时间对纳米SiO2表面改性的影响，研究了负载时间、负载温度和Ti(OC4H9)4用量对表面改性后纳米SiO2负载Ti(OC4H9)4的影响。 结果表明，当TMC-201质量分数为35%、反应温度为90 ℃、反应时间为3.5 h时，纳米SiO2粒子表面接枝的偶联剂量最大；在室温下，负载48 h，Ti(OC4H9)4用量为表面改性纳米SiO2量的1/2时得到的Ti(OC4H9)4/nano-SiO2负载型催化剂负载Ti(OC4H9)4量最大；运用ICP-AES、FESEM等测试技术对修饰后的纳米SiO2及Ti(OC4H9)4/nano-SiO2负载型催化剂进行了表征；将Ti(OC4H9)4/nano-SiO2负载型催化剂用于聚对苯二甲酸丙二醇酯(PTT)聚酯合成的结果表明，与均相Ti(OC4H9)4催化剂相比，Ti(OC4H9)4/nano-SiO2负载型催化剂催化合成PTT聚酯过程中酯化时间177 min，与均相催化剂催化酯化时间相近，在缩聚2 h后得到PTT的特性粘度高达1.05，证明该负载型催化剂具有高的催化活性，既可催化酯化反应又可催化缩聚反应。

关键词: 纳米二氧化硅, 钛酸四丁酯/纳米二氧化硅负载型催化剂, 浸渍法, 聚对苯二甲酸丙二醇酯

Abstract: Nano-SiO2 was modified with titanate coupling agent（TMC-201） under ultrasonic dispersion. n-Butyl titanate[Ti(OC4H9)4]/nano-SiO2 catalysts were successfully prepared by loading Ti(OC4H9)4 on the surface of modified nano-SiO2 particles via impregnation method. The impacts of titanate coupling agent， temperature and time on the surface modification of hydrophilic nano-SiO2 were studied. The impacts of Ti(OC4H9)4 content, supported temperature and supported time loading on modified nano-SiO2 particles were investigated. The results indicated that the titanate coupling agent was fully grafted on nano-SiO2 when TMC-201 content was 35% of nano-SiO2, modification temperature was 90 ℃, modification time was 3.5 h. The Ti(OC4H9)4/nano-SiO2 catalysts were the best when the using of Ti(OC4H9)4 was 50% of modified nano-SiO2, supported time was 48 h at room temperature. The modified nano-SiO2 and Ti(OC4H9)4/nano-SiO2 catalysts were characterized by ICP-AES and FESEM. Compared with the Ti(OC4H9)4 catalysts, the Ti(OC4H9)4/nano-SiO2 catalysts exhibited excellent catalytic activity. The esterification time in the synthesis of the poly(trimethylene terephthalate)(PTT) with Ti(OC4H9)4/nano-SiO2 catalysts was 177 min. The viscosity was improved to 1.05 after 2 h polycondensation.

Key words: nano silicon oxide, n-butyl titanate/nano silicon oxide , catalyst, impregnation method, poly(trimethylene terephthalate)

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