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Preparation method of porphyrin coupled silicon dioxide organic-inorganic nonlinear optical material

A technology of nonlinear optics and silicon dioxide, applied in nonlinear optics, optics, instruments, etc., can solve problems such as concentration quenching and achieve the effect of increasing doping concentration

Inactive Publication Date: 2011-12-14
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, many studies have found that when porphyrin is doped into inorganic gels using this technology, it is very easy to polymerize due to the shrinkage of the gel structure and the volatilization of the solvent, resulting in a serious concentration quenching effect.

Method used

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  • Preparation method of porphyrin coupled silicon dioxide organic-inorganic nonlinear optical material
  • Preparation method of porphyrin coupled silicon dioxide organic-inorganic nonlinear optical material
  • Preparation method of porphyrin coupled silicon dioxide organic-inorganic nonlinear optical material

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Put Cu(II)-TCPP and KH550 in a molar ratio of 1.955×10 -5 / 1, added to the chemical reaction bottle equipped with a condensing device, and nitrogen gas was introduced into the air port of the reflux device to prevent the hydrolysis and polymerization of the KH550 alkoxide from moisture absorption, and the mixture was heated and stirred at 160°C for 15 hours to obtain a transparent Crimson liquid.

[0035] (2) Take the above reaction product and compound it with KH560 metal alkoxide. The molar ratio of Cu(II)-TCPP to KH560 in the reaction product is 3.724×10 -6 / 1, the mixed solution was placed in a beaker and stirred for 1h, and anhydrous C was added to the beaker at the same time 2 h 5 OH, and the molar ratio of alkoxide KH560 is 1.53 / 1.

[0036] (3) will (H 2 O) / (C 2 h 5 OH) with a volume ratio of 1 / 2 is added dropwise to a beaker for hydrolysis and polymerization, and the added H 2 The total molar weight of O is 0.83 / 1 of the total molar weight of all meta...

Embodiment 2

[0039] (1) Put Cu(II)-TCPP and KH550 at a certain molar ratio of 2.645×10 -5 / 1, added to a chemical reaction bottle equipped with a condensing device, and nitrogen gas was introduced into the air port of the reflux device to prevent hydrolysis and polymerization of the KH550 alkoxide from moisture absorption, and the mixture was heated and stirred at 200°C for 30 hours to obtain a transparent Crimson liquid.

[0040] (2) Take the above reaction product and compound it with KH560 metal alkoxide. The molar ratio of Cu(II)-TCPP to KH560 in the reaction product is 5.039×10 -6 / 1, the mixed solution was placed in a beaker and stirred for 1.5h, and anhydrous C was added to the beaker at the same time 2 h 5 OH, and the molar ratio of alkoxide KH560 is 3.05 / 1.

[0041] (3) will (H 2 O) / (C 2 h 5 OH) with a volume ratio of 1 / 2 is added dropwise to a beaker for hydrolysis and polymerization, and the added H 2 The total molar weight of O is 1.25 / 1 of the total molar weight of all ...

Embodiment 3

[0044] (1) Put Cu(II)-TCPP and KH550 at a certain molar ratio of 1.830×10 -4 / 1, added to the chemical reaction bottle equipped with a condensing device, and nitrogen gas was introduced into the air interface of the reflux device to prevent the KH550 alkoxide from absorbing moisture and causing hydrolysis and polymerization reactions. Reaction to obtain a transparent dark red liquid.

[0045] (2) Take the above reaction product and compound it with KH560 metal alkoxide. The molar ratio of KH560 to Cu(II)-TCPP in the reaction product is 3.487×10 -5 / 1, the mixed solution was placed in a beaker and stirred for 2 hours, and anhydrous C was added to the mixed solution at the same time 2 h 5 OH, and the molar ratio of alkoxide KH560 is 3.82 / 1.

[0046] (3) will (H 2 O) / (C 2 h 5 OH) with a volume ratio of 1 / 2 is added dropwise to a beaker for hydrolysis and polymerization, and the added H 2 The total molar weight of O is 1.66 / 1 of the total molar weight of all metal alkoxides...

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Abstract

The invention discloses a preparation method of a porphyrin coupled silicon dioxide organic-inorganic nonlinear optical material, which comprises the following steps: 1. heating and reflowing a mixed solution of Msco-tetra-(4-carbomethoxyphenyl) porphyrin copper and gamma-aminopropyltriethoxysilane at the temperature of 160 to 250 DEG C for 10 to 60 hours to obtain a transparent deep red liquid; 2. dissolving a reaction product of step 1 and metal alkoxide into anhydrous ethanol, and stirring at room temperature for 1 to 2 hours; 3. dropwise adding a (H2O) / (C2H5OH) mixed liquid into the reaction product of step 2 at the room temperature for hydrolysis and polymerization reaction for 1 to 5 hours; and 4. pouring the obtained transparent sol into a glass or plastic utensil, sealing with a thin film, ageing at the room temperature for 35 to 45 days, and pricking a hole on the thin film every day to finally prepare compound dried gel. The invention has the advantages that the monomer doping concentration of porphyrin molecules in a gel solid medium can be greatly improved, and the molecular energy level structure and the spectral characteristic of the porphyrin molecules in the gel medium are kept.

Description

technical field [0001] The invention relates to a method for preparing an organic-inorganic photoelectric functional material, in particular to a method for preparing a porphyrin-coupled silicon dioxide organic-inorganic nonlinear optical material. Background technique [0002] Organic-inorganic composite materials are a new frontier research field that has developed rapidly since the mid-1980s. This material has the characteristics of both organic and inorganic substances, and overcomes the limitations of a single organic or inorganic material. It is the result of the penetration of inorganic chemistry, organic chemistry, mesoscopic physics and material science. It has been used in high-tech It will become the most promising important composite material in the 21st century. [1-2] . [0003] The solution-gel (sol-gel) technology is to obtain the required materials through gradual hydrolysis and polymerization of precursor raw materials such as metal alkoxides or inorganic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G02F1/355
Inventor 夏海平张晓荷王冬杰张约品
Owner NINGBO UNIV
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