Upconversion resin with polydimethylsiloxane as matrix and preparation method and application thereof
A polydimethylsiloxane and dimethylsiloxane technology, which is applied in the field of solid-state up-conversion two-component systems, can solve the problem of low conversion efficiency, inability to meet practical applications, and the triplet state of photosensitizers and luminescent agents being easily destroyed. Oxygen quenching and other problems, to achieve the effect of improving conversion efficiency, good compatibility, and solving application bottlenecks
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[0040] Example one Preparation of up-conversion resin (PdTPP / DPA / PDMS) based on polydimethylsiloxane
[0041] (1) In a nitrogen atmosphere, mix the phenyl tributyl ketoxime silane (crosslinking agent) and dimethyl siloxane monomer (DMS) at a ratio of 1:20 (mass ratio), vacuum, keep for 30 minutes, then Keep it at 100°C for 2h, take it out and cool it naturally to form a transparent polymer body (PDMS);
[0042] (2) First, prepare the photosensitizer (PdTPP) mother liquor (concentration of 4×10 -5 mol / L), luminescent agent (DPA) mother liquor (concentration is 1×10 -2 mol / L); then a certain amount of photosensitizer (PdTPP) solution and luminescent agent (DPA) solution are mixed and degassed to obtain a two-component up-conversion solution. The solvent is spectrally pure toluene;
[0043] (3) The PDMS polymer and the upconversion solution are mixed 1:1, placed for 24h under the protection of nitrogen, and taken out and dried to form a transparent upconversion resin with polydimethyls...
Example Embodiment
[0048] Example two Application of up-conversion resin based on polydimethylsiloxane in the synthesis of 7-hydroxycoumarin from coumarin
[0049] Coumarin solution configuration: in deionized water, add coumarin (concentration 2×10 -5 mol / L) and Pt / WO 3 Catalyst (concentration 10mg / L), configure 6 parts of the same solution (A~F) for use.
[0050] Up-conversion blue light irradiation: use 532nm (power density 70mW / cm 2 ) The semiconductor laser irradiates the polysiloxane-based solid up-conversion two-component system of Example 1 to produce blue up-conversion fluorescence. The up-conversion blue light is used to directly irradiate the coumarin solution (A~F) above, respectively. The time is respectively: A group (0min), B group (20min), C group (40min), D group (60min), E group (80min), F group (100min).
[0051] Fluorescence spectrum test of solution: such as Figure 5 , The coumarin solution is colorless, and the fluorescence peak of the solution is at 350nm. After the upconversio...
Example Embodiment
[0052] Example three Application of up-conversion resin based on polydimethylsiloxane in photolysis of water to produce hydrogen
[0053] according to Image 6 In the device shown, ZnCdS nanoparticles are deposited on FTO glass as the photoanode, platinum wire electrode is used as the counter electrode, and silver / silver chloride (0.1M) is used as the reference electrode to form a standard three-electrode battery (1.0M H 2 SO 4 As an electrolyte, the solvent is deionized water). Under the excitation of solid-state laser (excitation wavelength is 532nm, power density is 60mW·cm -2 ), ZnCdS photoanode (E g =2.35eV) Absorb the blue light generated by the solid upconversion two-component system based on polysiloxane in Example 1. The current can be detected by the electrochemical workstation, confirming that the solid-state upconversion blue light can drive the photoelectrochemical reaction, such as Figure 7 As shown, the photocurrent value that can be generated by the up-conversion...
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