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Up-conversion resin based on polydimethylsiloxane and its preparation method and application

A technology of polydimethylsiloxane and dimethylsiloxane, which is applied in the field of solid-state up-conversion two-component systems, can solve problems that cannot meet practical applications, low conversion efficiency, and the triplet state of photosensitizers and luminescent agents is easily destroyed. Oxygen quenching and other problems, to achieve the effect of improving conversion efficiency, good compatibility, and solving application bottlenecks

Active Publication Date: 2019-06-21
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a solid-state up-conversion two-component system to solve the problem that the triplet state of the photosensitizer and luminescent agent in the existing solution state is easily quenched by oxygen, and to overcome the low up-conversion efficiency of the existing solid-state system and cannot meet the actual requirements. application defect

Method used

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  • Up-conversion resin based on polydimethylsiloxane and its preparation method and application
  • Up-conversion resin based on polydimethylsiloxane and its preparation method and application
  • Up-conversion resin based on polydimethylsiloxane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 Preparation of up-conversion resin (PdTPP / DPA / PDMS) based on polydimethylsiloxane

[0041] (1) In a nitrogen atmosphere, mix phenyltributanoximinosilane (crosslinking agent) and dimethylsiloxane monomer (DMS) at a ratio of 1:20 (mass ratio), vacuumize, and keep for 30 min. Then keep it at 100 °C for 2 h, take it out and cool it naturally to form a transparent polymer body (PDMS);

[0042] (2) First prepare photosensitizer (PdTPP) mother solution (concentration is 4×10 -5 mol / L), luminescent agent (DPA) mother solution (concentration is 1×10 -2 mol / L); then a certain amount of photosensitizer (PdTPP) solution and luminescent agent (DPA) solution were mixed and degassed to obtain a two-component up-conversion solution, and the solvent was spectrally pure toluene;

[0043] (3) Mix the PDMS polymer with the upconversion solution at a ratio of 1:1, place it under nitrogen protection for 24 h, take it out and dry it to form a transparent upconversion resin based...

Embodiment 2

[0048] Example 2 The application of the 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 10 mg / L), prepare 6 copies of the same solution (A~F) for standby.

[0050] Up-conversion blue light irradiation: use 532 nm (power density 70 mW / cm 2 ) semiconductor laser, irradiate the solid up-conversion two-component system based on polysiloxane in Example 1 to produce blue up-conversion fluorescence, and use this up-conversion blue light to directly irradiate the above-mentioned coumarin solution (A~F) respectively, and irradiate The time is: Group A (0 min), Group B (20 min), Group C (40 min), Group D (60 min), Group E (80 min), Group F (100 min).

[0051] Fluorescence spectrum test of solution: such as Figure 5 , the coumarin solution is colorless, and the fluorescence peak of the solu...

Embodiment 3

[0052] Example 3 Application of up-conversion resin based on polydimethylsiloxane in photolysis of water for hydrogen production

[0053] according to Figure 6 As shown in the device, ZnCdS nanoparticles were deposited on FTO glass as photoanode, platinum wire electrode as counter electrode, Ag / AgCl (0.1 M) as reference electrode to form a standard three-electrode cell (1.0 M of H 2 SO 4 As electrolyte, the solvent is deionized water). Under the excitation of a solid-state laser (excitation wavelength of 532 nm, power density of 60 mW cm -2 ), ZnCdS photoanode (E g = 2.35 eV) to absorb the blue light generated by the polysiloxane-based solid up-conversion two-component system in Example 1. The current is detectable by the electrochemical workstation, confirming that solid-state upconversion of blue light can drive photoelectrochemical reactions, such as Figure 7 As shown, the up-conversion resin based on polydimethylsiloxane can generate a photocurrent value of 0.9 μA, ...

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Abstract

The invention discloses an up-conversion resin based on polydimethylsiloxane and its preparation method and application; in a nitrogen atmosphere, a silane crosslinking agent and a dimethylsiloxane monomer are mixed at a ratio of 1:10 to Mixed at a mass ratio of 30; then vacuum treated and kept at 100°C for 2 h; then naturally cooled to form polysiloxane; then, under a nitrogen atmosphere, polysiloxane was placed in an organic solvent containing a photosensitizer and a luminescent agent , soaked for 18 to 30 hours, taken out and dried to obtain a solid up-conversion two-component system based on polysiloxane. The present invention discloses for the first time the preparation method of a solid-state up-conversion resin using PDMS as a matrix, and uses the green-to-blue light generated by the solid-state up-conversion resin to convert the solution-state up-conversion system into a solid-state material, which has high up-conversion efficiency and can be used in photolysis It has potential application value in hydrogen production and photosynthesis.

Description

[0001] The invention belongs to the field of triplet annihilation up-conversion, and specifically relates to a solid-state up-conversion two-component system formed by using polysiloxane as a matrix, wrapping a photosensitizer and a luminescent agent, a preparation method and an application thereof. Background technique [0002] Materials based on triplet-triplet annihilation upconversion (TTA-UC) usually consist of a two-component system consisting of a photosensitizer and a luminescent agent dissolved in an organic solvent. The mechanism is: (1) Irradiated by low-energy excitation light, the photosensitizer absorbs the energy of the excitation light and changes from its ground state (S 0 ) to the singlet excited state ( 1 S*), and then transition to the triplet excited state ( 3 S*); (2) The photosensitizer transfers the energy of its triplet excited state ( 3 S*) transferred to the luminescent agent ( 3 A*); (3) When the concentration of acceptor molecules in the triplet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/06C08G77/06C25B1/04C07D311/16
CPCC09K11/06C25B1/04C07D311/16C08G77/06C09K2211/1011C09K2211/185Y02E60/36
Inventor 叶常青孙彬王筱梅朱赛江吴正伟戚守善
Owner SUZHOU UNIV OF SCI & TECH
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