Preparation method of up-conversion resin by taking polydimethylsiloxane as matrix

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, triplet states of photosensitizers and luminescent agents that are easily quenched by oxygen, and inability to Meet practical application and other issues, achieve good compatibility and improve conversion efficiency

Active Publication Date: 2019-06-14
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] 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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  • Preparation method of up-conversion resin by taking polydimethylsiloxane as matrix
  • Preparation method of up-conversion resin by taking polydimethylsiloxane as matrix
  • Preparation method of up-conversion resin by taking polydimethylsiloxane as matrix

Examples

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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 Image 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, w...

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Abstract

The invention discloses a preparation method of up-conversion resin by taking polydimethylsiloxane as a matrix. The preparation method comprises the following steps: in a nitrogen atmosphere, mixing asilane cross-linking agent and a dimethyl siloxane monomer according to a mass ratio of 1:(10-30); performing vacuum treatment, and performing heat preservation at 100 DEG C for 2 hours; and then conducting natural cooling to form polysiloxane; and then, in a nitrogen atmosphere, putting the polysiloxane into an organic solvent containing a photosensitizer and a luminous agent, conducting soakingfor 18-30 hours, and conducting fetching and drying to obtain a polysiloxane-based solid upconversion two-component system. The invention discloses the preparation method of the solid upconversion resin by taking PDMS as the matrix for the first time and green-to-blue light generated by using the solid upconversion resin, a solution-state upconversion system is converted into a solid material, and the solid upconversion resin has high upconversion efficiency and has potential application value in the aspects of hydrogen production by photolysis of water and photosynthesis.

Description

[0001] The present invention belongs to the divisional application of the invention titled up-conversion resin with polydimethylsiloxane as the matrix and its preparation method and application, the application date is February 5, 2016, and the application number is 201610082546.5, belonging to the product Preparation methods section. technical field [0002] The invention belongs to the field of triplet annihilation up-conversion, and in particular relates to a solid-state up-conversion two-component system formed by using polysiloxane as a matrix to wrap a photosensitizer and a luminescent agent, a preparation method and application thereof. Background technique [0003] Materials based on triplet-triplet annihilation upconversion (TTA-UC) usually consist of a two-component system consisting of photosensitizers and luminescent agents dissolved in organic solvents. The mechanism is: (1) When irradiated with low-energy excitation light, the photosensitizer absorbs the energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C08G77/04
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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