新型亲和双水相成相剂Triton X-100-IDA-Cu(Ⅱ)的制备

Preparation of a novel phase-forming component Triton X-100-IDA-Cu( Ⅱ) for affinity aqueous two-phase system

以小分子表面活性剂Triton X-100为载体,采用环氧氯丙烷(ECH)活化法偶联亚氨基二乙酸(IDA),通过配位反应螯合Cu(Ⅱ),合成了一种新型亲和双水相成相剂Triton X-100-IDA-Cu(Ⅱ),并对其合成条件进行了优化.结果表明:最佳活化工艺为n(ECH)∶n(Triton X-100)=2∶1,n(BF_3)∶n(Triton X-100)=1∶25,冰浴反应22 h,按n(NaOH)∶n(Triton X-100)=1∶1加入Na OH,环氧化反应3 h,环氧产物得率达到72.4%;最佳偶联工艺为pH 13条件下,加入等摩尔的IDA,55℃反应21 h,IDA的偶联率为76.3%;最佳螯合工艺为在0.05 mol/L醋酸钠溶液中,n(CuSO+4)∶n(Triton X-100-IDA)=1∶1,室温反应6 h,Cu(Ⅱ)的螯合率可达80.5%.通过测定Triton X-100-IDA-Cu(Ⅱ)与阳离子型疏水改性聚氧乙烯(HM-EO)所构成的双水相系统的相图,知两者可形成带亲和配基的稳定双水相系统.

A novel phase-forming component for affinity aqueous two-phase system , Triton X-100-IDA-Cu(Ⅱ) was prepared.The nonionic surfactant (Triton X-100) was used as the matrix, which was activated by epichlorohydrin ( ECH) and coupled with iminodiacetic acid ( IDA) , and finally chelated with Cu (Ⅱ). The synthesis conditions on Triton X-100-IDA-Cu (Ⅱ) was optimized systematacially.The result indicated that the yield of Triton X-100-epoxide above 72.4% was achieved in the ice-water bath consisting of n( ECH):n( Triton X-100) =2:1, n( BF3 ):n( Triton X-100) =1:25 for 22 hours and then as the mo-lar ratio of NaOH to Triton X-100 was 1:1 for 3 hours.After reacting under the optimal linkaging conditions as n(IDA):n(Triton X-100) =1:1, pH 13, 55 ℃, 21 hours, the maximum yield of Triton X-100-IDA was 76.3%.In the solution composed of n(CuSO4):n(Triton X-100-IDA) =1:1 at room temperature for 6 hours, the chelating yield of Cu (Ⅱ) reached 80.5%.Phase diagram determination showed that Triton X-100-IDA-Cu(Ⅱ) and HM-EO could compose stable affinity aqueous two-phase system ( ATPS).