无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2019, Vol. 51 ›› Issue (10): 22-27.doi: 10.11962/1006-4990.2018-0615

• 无机盐工业 • 上一篇    下一篇

[N2,2,2,2]BF4的合成及其对双水相 体系成相行为的影响

余 垒,朱新儒,曾 颖,李 雄,张海德   

  1. 海南大学食品学院,海南海口 570228
  • 出版日期:2019-10-10 发布日期:2020-03-06
  • 作者简介:余垒(1992— ),女,硕士研究生,研究方向为天然产物分离提取研究;E-mail:429267803@qq.com。 通讯作者:张海德(1970— ),男,教授,博士,研究方向为生物活性物质分离方法;E-mail:zhanghaide@163.com。

Synthesis of [N2,2,2,2]BF4 and its effect on phase formation behavior of aqueous twophase system

Yu Lei,Zhu Xinru,Zeng Ying,Li Xiong,Zhang Haide   

  1. College of Food Science and Engineering,Hainan University,Haikou 570228,China
  • Online:2019-10-10 Published:2020-03-06

摘要: 为研究添加[N2,2,2,2]BF4对PEG-NaH2PO4·2H2O双水相系统成相行为的影响,首先,采用正交优化法合成了[N2,2,2,2]BF4并对其进行1H NMR表征和纯度验证;其次,25 ℃条件下通过浊点法分别绘制PEG-NaH2PO4·2H2O和PEG-NaH2PO4·2H2O-4%[N2,2,2,2]BF4双水相体系的相图;最后,研究添加4%(质量分数)的[N2,2,2,2]BF4对PEG-NaH2PO4·2H2O双水相系统成相行为的影响。结果表明,通过单因素实验和L9(34)正交优化实验得出合成反应的优化条件为:n([N2,2,2,2]Br)∶n(NaBF4)为1.0∶1.1、乙腈用量为100 mL、反应时间为8 h、温度为80 ℃,[N2,2,2,2]BF4的产率达90.7%;通过Merchuk方程对两种体系的相图数据进行关联,拟合度都在0.997以上。随着PEG相对分子质量的增加,添加4%的[N2,2,2,2]BF4能替代部分PEG,使得双水相区域的面积逐渐增加,增大了成相剂的选择范围,有利于双水相体系的选择,为后续双水相分离生物分子奠定基础。

关键词: [N2,2,2,2]BF4;合成;双水相系统;PEG-NaH2PO4·2H2O

Abstract: In order to study the effect of the addition of [N2,2,2,2]BF4 on the phase formation behavior of PEG-NaH2PO4· 2H2O aqueous two phase system,firstly,[N2,2,2,2]BF4 was synthesized by orthogonal optimization method and character ized by 1H NMR and its purity was verified.Secondly,under the condition of 25 ℃,the phase diagrams of PEG-NaH2PO4· 2H2O and PEG-salt-4%[N2,2,2,2]BF4 aqueous two phase systems were plotted by cloud point method respectively.Finally, the effect of[N2,2,2,2]BF4 with 4%(mass fraction) addition on the phase formation behavior of PEG-NaH2PO4·2H2O aque ous two phase system was studied.The results showed that,through single factor experiment and L9(34) orthogonal optimiza tion experiment,the optimum conditions of the synthetic reaction were obtained as follows:the amount of substance ratio of[N2,2,2,2]Br to NaBF4 was 1.0∶1.1,the amount of ACN was 100 mL,the reaction time was 8 h,the temperature was 80 ℃ and the yield of [N2,2,2,2]BF4 was up to 90.7%.The Merchuk equation was used to correlate the phase diagram data of the two systems,the fitting degree of them were more than 0.997.With the increase of the relative molecular mass of PEG,the area of the aqueous two phase region increased gradually by the addition of 4%[N2,2,2,2]BF4 instead of PEG partly,which enlarged the selection range of the phase forming agent and is beneficial to the selection of the aqueous two phase systems and laid a foundation for the subsequent separation of biomolecules in aqueous two phase system.

Key words: [N2,2,2,2]BF4;synthesis;aqueous two phase system;PEG-NaH2PO4·2H2O

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