Hybrid materials and methods for their production
A hybrid material and organic hybrid technology, used in additive processing and other directions, can solve problems such as failure and invisibility
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[0103] abbreviation
[0104] DMA Dynamic Mechanical Analysis
[0105] EDS Energy Dispersive X-ray Spectroscopy
[0106] FTIR Fourier Transform Infrared Spectroscopy
[0107] ICP Inductively Coupled Plasma Elemental Analysis
[0108] Maldi-TOF matrix-assisted laser desorption ionization time-of-flight spectroscopy
[0109] NMR nuclear magnetic resonance
[0110] PBS Phosphate Buffered Saline Solution
[0111] PTFE Polytetrafluoroethylene
[0112] PTHF polytetrahydrofuran (or poly(tetramethylene ether) glycol), also known as p(THF)
[0113] SBF Simulates Body Fluids
[0114] SEM Scanning Electron Microscopy
[0115] TEM Transmission Electron Microscopy
[0116] TGA Thermogravimetric Analysis
[0117] TGA / DSC Thermogravimetric Analysis / Differential Scanning Calorimetry
[0118] μCT micro-computed tomography
[0119] XRD X-ray diffraction analysis
[0120] Material:
[0121] Glycidyl methyl ether (GME-CAS No. 930-37-0) was purchased from TCI America, US, and used as ...
example 1
[0122] Example 1: PTHF synthesis
[0123] PTHF was synthesized from tetrahydrofuran (THF) in a 1-step procedure, catalyzed by a Lewis acid, boron trifluoride etherate (BF 3 ·OEt 2 ) and glycidyl methyl ether (GME) as initiators.
[0124] In a typical procedure, GME (1 mol) was dissolved in anhydrous THF (35 mol) in a round bottom flask at room temperature with continuous stirring. The solution remained completely clear and transparent, and after 15-30 minutes, BF was added 3 ·OEt 2 (0.25mol, catalytic amount). The reaction occurred very quickly as a sudden temperature increase and occasional color change (from clear to yellow) were observed, followed by a rapid increase in viscosity due to rapid polymerization of THF.
[0125] Due to the difference in ring strain of THF (5.63 kcal / mol) and ethylene oxide (27.28 kcal / mol), it is assumed that the epoxy ring is first activated by a Lewis acid to the corresponding intermediate 1 (Step I, Scheme 1). This is then subjected t...
example 2
[0130] Example 2: From SiO 2 Synthesis of / PTHF Inorganic-Organic Hybrid Materials
[0131] Samples were prepared with GPTMS as the sole silica source and TEOS as the additional silica source. SiO 2 The synthesis of / PTHF hybrids was achieved by a 2-step procedure involving the following:
[0132] - Coupling with GPTMS to form GPTMS-PTHF gels - THF polymerization initiated by the epoxy ring of GPTMS, by combining with BF 3 ·OEt 2 interaction activation.
[0133] - Hybrid synthesis by hydrolysis and condensation (sol-gel route) - addition of TEOS (optional), deionized water and 1M HCl.
[0134] The formation of the GPTMS-PTHF gel is due to THF polymerization, the rate of which is affected by the THF:GPTMS ratio. A wide range of THF:GPTMS concentrations allows the creation of hybrid materials. Preferably, there is an excess of THF relative to the polymerized volume. When higher THF / GPTMS ratios are used, THF consumption in the polymerization reaction slows down so that...
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