Abstract

The Mn2+ and Mo6+ based metal-mercaptoacetate (metal-MA) hybrids were prepared by a simple acid–base titration method. The prepared metal-MA hybrids were analysed by FT-IR spectroscopy, UV–visible spectroscopy, SEM, particle size analyser (PSA), XRD and EDX. The prepared metal-MA hybrids were investigated to assess their catalytic activity for ring-opening polymerization (ROP) of ε-caprolactone (CL) in the absence of an initiator at 160 °C in N2 atmosphere by varying the catalyst concentration and temperature. The catalytic activity of the metal-MA hybrid towards the ROP of CL was evidenced by the FTIR-RI method. The % yield, degradation temperature (Td), melting temperature (Tm) and molecular weight (Mw) of poly(ε-caprolactone) (PCL) were also investigated. The structure of PCL was comprehended by analysing its NMR spectrum. The activation energy (Ea) for the ROP of CL was determined as 10,363 kcal/mol. A linear increase in Mw of PCL with the increasing [M0/I0] ratio was also noticed.Graphical abstract

Highlights

  • Poly(ε-caprolactone) (PCL) is the bio-medically important polymers owing to its biodegradability and biocompatibility

  • This section has been divided into two parts namely, (i) Characterizations of Metal-MA hybrid and (ii) Characterizations of Metal-MA end-capped PCL

  • The above synthesized Metal-MA catalyst is analyzed by using various analytical tools like FT-IR, UVvisible spectroscopy, reflectance study, SEM, XRD, EDX and particle size analyser (PSA)

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Summary

Introduction

Poly(ε-caprolactone) (PCL) is the bio-medically important polymers owing to its biodegradability and biocompatibility. PCL is used in tissue engineering [1], drug release [2], low temperature splinting action [3], scaffold [4] and fluorescent probe carrier material [5] Such a high potential candidate of PCL can be synthesized by using the various catalyst and initiator systems. The removal of catalyst or initiator from the polymer backbone after the ROP is unavoidable For this purpose, the metal complexes are widely employed as a catalyst in the absence or presence of an initiator system. Metal salts and their complexes are employed as an initiator cum catalyst for the ROP of cyclic esters. Mo has various possible oxidation states due to the half-filled 4d and 5s orbital It is a bio-metal and used as a mineral. It is not necessary to remove the catalyst even after the polymerization reaction from the polymer backbone because of its biocompatibility

Experimental
Preparation of Metal-MA end-capped PCL
Characterization
Determination of band gap value
FT-IR study
Reflectance study
EDX study
XRD report
SEM analysis
UV-visible analysis
3.1.11. XRD analysis
Yield study
Effect of temperature on the FTIR-RI of PCL
NMR spectral study
GPC analysis
Thermal properties of Metal-MA end-capped PCL system
UV-visible and bandgap studies
Conclusion
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