Preparation method of spiropyrane type photochromic nano-composite microsphere

A nano-composite and photochromic technology, applied in the field of photochromism, can solve the problems of reduced color changing space, reduced color changing coating space, and low color changing efficiency

Active Publication Date: 2018-02-23
JIANGSU SHIKEXINCAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The spin coating method is to add the prepared discoloration solution into the tank of the spin coater after the substrate is made, and after fully mixing, fix the substrate on the spin coater for centrifugal rotation and solidify it to form a discoloration effect. Compared with the substrate method, the spin-coating method has the advantage of high technic...

Method used

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  • Preparation method of spiropyrane type photochromic nano-composite microsphere
  • Preparation method of spiropyrane type photochromic nano-composite microsphere
  • Preparation method of spiropyrane type photochromic nano-composite microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Embodiment 1: Preparation of photochromic nanocomposite microspheres, photochromic coating liquid and photochromic lens

[0073] (1) Preparation of photochromic nanocomposite microspheres:

[0074] (1) Add 9.7g of zinc nitrate hexahydrate to 1600g of ethylene glycol, stir evenly, add 1.6g of sublimated sulfur powder, heat up to 150°C for 24 hours, cool to 55°C, add 85g of mercaptoethanol dropwise and stir; Then add 6.7 g of the spiropyran photochromic compound represented by formula III, stir vigorously for 30 minutes, continue to cool to room temperature, filter and wash the precipitate, and dry it in a vacuum oven at 65°C for 8 hours to obtain spiropyran coating Zinc sulfide nanospheres;

[0075] (2) Add 8g of spiropyran-coated zinc sulfide nanospheres and 8.2g of diphenylmethane-4,4'-diisocyanate (MDI) to 1000g of butyl acetate solvent, stir well, and then add 7g to mix the reaction agent (1.2g n-butanol, 5.8g polytetrahydrofuran ether glycol), 18g Tween80, the tem...

Embodiment 2

[0090] (1) Preparation of photochromic nanocomposite microspheres:

[0091](1) Add 6.5g of zinc nitrate to 1600g of ethylene glycol, stir evenly, add 1.7g of sublimated sulfur powder, heat up to 150°C for 24 hours, cool to 55°C, add 70g of mercaptoethanol dropwise and stir; then add 3.5 g of spiropyran photochromic compound (I), vigorously stirred for 30 minutes, cooled to room temperature, filtered and washed the precipitate, and dried in a vacuum oven at 65° C. for 8 hours to obtain spiropyran-coated zinc sulfide nanospheres;

[0092] (2) Get 5.5g spiropyran-coated zinc sulfide nanospheres, 5g MDI is added in 1000g butyl acetate solvent, after stirring evenly, add 5.5g mixed reactants (1.0g n-butanol, 4.5g polytetrahydrofuran ether) Diol), 20g Tween80, keep the temperature at 25°C, prepolymerize at 500r / min for 50min, add 6g chain extender (4.5g ethylene glycol, 1.5g ethylenediamine), 0.1g DBTL, heat to 65°C Polymerization chain extension reaction was carried out for 15 min...

Embodiment 3

[0101] (1) Preparation of photochromic nanocomposite microspheres:

[0102] (1) Add 11g of zinc nitrate hexahydrate to 1600g of ethylene glycol, stir evenly, add 3g of sulfur powder, heat up to 145°C for 24 hours, cool to 50°C, add 92g of mercaptoethanol dropwise and stir; then add 8g The spiropyran photochromic compound (I), vigorously stirred for 35 minutes, continued to cool to room temperature, filtered and washed the precipitate, and dried in a vacuum oven at 60°C for 9 hours to obtain spiropyran-coated zinc sulfide nanospheres;

[0103] (2) Get 10g spiropyran-coated zinc sulfide nanospheres, 10.8g m-xylylene diisocyanate (XDI) and join in 1000g butyl acetate solvent, after stirring evenly, add 7.4g mixed reaction agent (1.0 g n-butanol, 6.4g polytetrahydrofuran ether glycol), 16g Tween80, keep the temperature at 25°C, prepolymerize at 600r / min for 60min, add 8g chain extender (5.5g ethylene glycol, 2.5g ethylenediamine) , 0.2g DBTL, heated to 60°C for polymerization cha...

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Abstract

The invention relates to a preparation method of a spiropyrane type photochromic nano-composite microsphere. The prepared material prepared by the method is of a three-layer compound core-shell structure, wherein an inner core is a zinc sulfide mesoporous nano microsphere, an intermediate layer is a photochromic layer composed of spiropyrane type compounds, and a shell is polyurethane; the outer diameter of the composite microsphere is 50-350nm, the diameter of the zinc sulfide mesoporous nano microsphere is 30-250nm, the thickness of the intermediate layer is 5-25nm, and the thickness of theshell is 5-25nm. The prepared photochromic composite microsphere can be added into a photochromic coating or resin optical material as a photochromic material. The prepared material can become coloredfrom colorless under ultraviolet irradiation condition, also can be rapidly faded to be colorless after ultraviolet rays disappear and has the advantages of strong fatigue resistance, good stability,high discoloring speed and the like.

Description

technical field [0001] The invention belongs to the technical field of photochromism, and in particular relates to a preparation method of photochromic nanocomposite microspheres containing spiropyran compounds. Background technique [0002] Photochromism refers to certain compounds under the action of light of a certain wavelength and intensity, as the absorption spectrum changes, the molecular structure of the material changes, resulting in a change in the absorbance and color of the material, and this change is generally reversible , a functional material that can automatically return to its original state when the light is stopped, as a new material in the subdivision of optical materials, it has important roles in high-tech fields such as optical lenses, optical information storage, molecular switches, and anti-counterfeiting identification. Value. It has been more than 100 years since human beings discovered the phenomenon of photochromism. The first successful comme...

Claims

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Application Information

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IPC IPC(8): C07D491/107C07D311/94C09K9/02C09K11/02C09K11/88B82Y30/00B01J13/14
CPCB01J13/14B82Y30/00C07D311/94C07D491/107C09K9/02C09K11/025C09K11/883
Inventor 王明华乔振安张鹤军纪立军范为正司云凤王志飞郑永华薛晓花吴潇刘洋
Owner JIANGSU SHIKEXINCAI CO LTD
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