摘要
围绕传统塑化剂合成工艺中存在的设备腐蚀性强、二次污染大、反应时间长等问题,分析柠檬酸酯合成过程中可能对产率影响的因素,探讨了微波辅助A型分子筛(SiO2与Al2O3的摩尔比为50)高效合成柠檬酸正丁酯的绿色工艺条件。采用控制单因素实验,研究了在不同的微波辐照功率、微波辐照时间、酸醇比(摩尔比)、A型分子筛催化剂的用量、反应温度等实验条件下,微波辅助A型分子筛催化对柠檬酸正丁酯产率的影响,并在最适宜的工艺条件下,研究了柠檬酸正丁酯的产率,同时对分子筛催化剂进行了回收实验处理。实验结果表明:最适宜合成工艺为微波辐照功率300 W,辐照时间3 min,反应温度130℃,酸醇摩尔比1:7,A型分子筛催化剂用量为4%,产率可达70.30%,分子筛催化剂经过两次回收循环使用后的产率仍达65.42%。
Aim at the problems of strong corrosion,large secondary pollution and long reaction time in the traditional synthesis process of plasticizer,the factors that may affect the yield of citrate in the process of synthesis were analyzed,and the green process synthesis conditions of tri-n-butyl citrate by microwave synergistic A molecular sieve(SiO2/Al2O3 mole ratio 50)were discussed.Under different experimental conditions,such as the power of microwave irradiation,the time of microwave irradiation,the ratio of acidic alcohol(mole ratio),the amount of A molecular sieve catalyst and the reaction temperature,the effects of microwave synergetic A molecular sieve on the yield of tri-n-butyl were studied by control single variable method.Under the most suitable conditions,the yield of tri-n-butyl citrate was studied.Meanwhile,the recovery experiment of A molecular sieve was done.The experimental results show that the most suitable synthetic process was the microwave irradiation power 300 W,the irradiation time 3 min,the microwave reaction temperature 130℃,the acid alcohol mole ratio 1:7,the dosage of A molecular sieve catalyst 4%and the yield can reach 70.30%.The yield of molecular sieve catalyst was still 65.42%after two recovery and recycling.
作者
邹训重
陈金伟
冯安生
廖延智
黎彧
Zou Xunzhong;Chen Jinwei;Feng Ansheng;Liao Yanzhi;Li Yu(Guangdong Research Center for Special Building Materials and Its Green Preparation Technology/Foshan Research Center for Special Functional Building Materials and Its Green Preparation Technology,Guangdong Industry Polytechnic,Guangzhou 510300,China)
出处
《塑料科技》
CAS
北大核心
2019年第12期152-155,共4页
Plastics Science and Technology
基金
广东省高等职业院校珠江学者岗位计划资助项目(2015,2018)
广东轻院珠江学者人才类项目(RC2015-001)
广东省自然科学基金项目(2016A030313761)
广东省高校创新团队项目(2017GKCXTD001,2017GWCXTD002)
广州市科技计划项目(201904010381)
广东省教育厅特色创新类项目(2017GKTSCX005、2017GkQNCX004)
广东轻院优秀青年基金项目(QN2018-007)
广东轻工职业技术学院2017年拔尖人才自选项目(IB040103)
广东大学生科技创新培育专项(pdjh2019b0690)
