引用本文:
叶冲, 姜敏, 张强, 刘茜, 周光远. 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[J]. 应用化学,
2013, 30(1): 32-37.
doi:
DOI:10.3724/SP.J.1095.2013.20037
Citation: YE Chong, JIANG Min, ZHANG Qiang, LIU Qian, ZHOU Guangyuan. Preparation of n-Butyl Titanate/Nano Silicon Oxide Catalyst for Synthesis of Poly(trimethylene terephthalate)[J]. Chinese Journal of Applied Chemistry, 2013, 30(1): 32-37. doi: DOI:10.3724/SP.J.1095.2013.20037
Citation: YE Chong, JIANG Min, ZHANG Qiang, LIU Qian, ZHOU Guangyuan. Preparation of n-Butyl Titanate/Nano Silicon Oxide Catalyst for Synthesis of Poly(trimethylene terephthalate)[J]. Chinese Journal of Applied Chemistry, 2013, 30(1): 32-37. doi: DOI:10.3724/SP.J.1095.2013.20037
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
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。采用浸渍法将钛酯四丁酯(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。
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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
English
Preparation of n-Butyl Titanate/Nano Silicon Oxide Catalyst for Synthesis of Poly(trimethylene terephthalate)
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.
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