Synthesis method of silicon-based photochromic elastomer containing naphthol pyran with cross-linked structure

A photochromic and naphthol pyran technology, applied in the direction of color-changing fluorescent materials, chemical instruments and methods, etc., can solve the problems such as no silicon-based photochromic elastomers, and achieve rich varieties, excellent performance and simple operation. easy effect

Inactive Publication Date: 2014-10-01
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report about this kind of silicon-based photochromic elastomer containing naphthol pyran group with cross-linked structure.

Method used

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  • Synthesis method of silicon-based photochromic elastomer containing naphthol pyran with cross-linked structure
  • Synthesis method of silicon-based photochromic elastomer containing naphthol pyran with cross-linked structure
  • Synthesis method of silicon-based photochromic elastomer containing naphthol pyran with cross-linked structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: In a 100ml three-necked flask equipped with a reflux condenser and a dropping funnel, add 1.5g of hydrogen-containing silicone oil, 25ml of toluene and 0.004g of chloroplatinic acid in water, and heat it after feeding argon for 15 minutes. When the temperature rises to 65 o At C, add 0.3g monomer dropwise 1 and 0.1g monomer 4 15ml of the toluene mixed solution was dropped within 2 hours, and then continued to be heated to reflux, and the reaction was stopped after 2 hours. Distill under reduced pressure to remove the remaining toluene, and dissolve the residue in a small amount of tetrahydrofuran solvent, remove the catalyst through an aluminum oxide column, and settle in cold methanol for 3 times to obtain a photochromic elastomer. The product is a solid substance with very low hardness , 1.64g, yield 86.3%. The structural formula of the product is as follows:

[0041]

[0042] After the product is pressed into a film by a flat vulcanizer, the film ...

Embodiment 2

[0044] In a 100ml three-necked flask equipped with a reflux condenser and a dropping funnel, add 1.0g of hydrogen-containing silicone oil, 18ml of toluene and 0.003g of chloroplatinic acid aqueous solution, and heat it after feeding argon for 15 minutes. When the temperature rises to 80 o At C, add 0.2g monomer dropwise 2 and 0.08g monomer 4 10ml of the toluene mixed solution was dropped within 1.5 hours, and then continued to be heated to reflux, and the reaction was stopped after 3 hours. Distill under reduced pressure to remove the remaining toluene, and dissolve the residue in a small amount of tetrahydrofuran solvent, remove the catalyst through an aluminum oxide column, and settle in cold methanol for 3 times to obtain a photochromic elastomer. The product is a solid substance with very low hardness , 0.98g, yield 76.5%. The structural formula of the product is as follows:

[0045]

Embodiment 3

[0047] In a 100ml three-necked flask equipped with a reflux condenser and a dropping funnel, add 1.2g of hydrogen-containing silicone oil, 25ml of toluene and an aqueous solution of 0.003g of chloroplatinic acid, and heat it after feeding argon for 15 minutes. 45 o At C, add 0.25g monomer dropwise 3 and 0.1g monomer 4 The toluene mixed solution of 15ml is dripped within 2.5 hours, then continues to be heated to reflux, stops reaction after 3 hours. Distill under reduced pressure to remove the remaining toluene, and dissolve the residue in a small amount of tetrahydrofuran solvent, remove the catalyst through an aluminum oxide column, and settle in cold methanol for 3 times to obtain a photochromic elastomer. The product is a solid substance with very low hardness , 1.28g, yield 82.6%. The structural formula of the product is as follows:

[0048]

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Abstract

The invention belongs to the synthesis method of organic / polymer materials, in particular to the synthesis method of a silicon-based photochromic elastomer containing naphthol pyran and having a cross-linked structure, using hydrogen-containing silicone oil as a soft segment, and containing a polymerization unit The naphthol pyran polymerized monomer is a photochromic functional group, and the naphthol pyran polymerized monomer containing two polymerized units is used as a crosslinking agent. At a certain temperature, chloroplatinic acid is used as a catalyst to prepare a crosslinked Structured silicon-based photochromic elastomers. During the preparation process, the conditional reaction material ratio is used to make the content of the photochromic monomer between 20-50%, so as to ensure that the finally prepared block polymer has the property of the elastomer. At present, there is no report about this silicon-based photochromic elastomer with a cross-linked structure and a naphthol-pyranyl group. The elastomer with this structure not only has the characteristics of an elastomer, but also has photochromic properties, which can be used in the preparation of flexible optical devices.

Description

technical field [0001] The invention belongs to a method for synthesizing organic / polymer materials, in particular to a method for synthesizing a silicon-based photochromic elastomer with a cross-linked structure and containing a naphthol pyran group. Background technique [0002] Photochromism refers to the reversible change of a compound molecule between two molecular states with different spectral properties under the radiation of different wavelengths, and these two molecules with different structures have different Spectral properties, such as color changes or different absorption spectra. This phenomenon that the molecular structure of the compound can undergo reversible changes under the action of light or heat is called photochromism. [1] . Photochromic compounds and their polymers are new functional materials that can be widely used in frontier fields such as optical switches, optical storage, and nonlinear optics [2-3] , Among them, another well-known applicat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08L83/05C08K5/1545C09K9/02
Inventor 王广刘龙波徐小涵
Owner NORTHEAST NORMAL UNIVERSITY
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