Spiropyrane photochromic optical material and preparation method thereof

A photochromic and spiropyran-based technology, which is applied in optics, microsphere preparation, optical components, etc., can solve the problems of low discoloration efficiency, reduced discoloration coating space, and discoloration space reduction, etc.

Active Publication Date: 2018-03-09
南京米兰达视光科学研究院有限公司
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  • 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 technical content. In theory, any product can be made, and the color difference of the product is small. The disadvantage is that the space of the color-changing coating is relatively reduced, and the color-changing space is reduced. Therefore, the development of lens coating technology with high photochromic efficiency is an important development direction in the future

Method used

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  • Spiropyrane photochromic optical material and preparation method thereof
  • Spiropyrane photochromic optical material and preparation method thereof
  • Spiropyrane photochromic optical material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0097] Example 1: Preparation of photochromic nanocomposite microspheres, photochromic coating liquid and photochromic lenses

[0098] (1) Preparation of photochromic nanocomposite microspheres:

[0099] (1) in 1600g ethylene glycol, add 9.7g zinc nitrate hexahydrate, after stirring, add 1.6g sublimation sulfur powder, be warming up to 150 ℃ of insulation reaction 24 hours, be cooled to 55 ℃, drip 85g mercaptoethanol and stir; Then add 6.7g of the spiropyran photochromic compound shown in formula III, stir vigorously for 30 minutes, continue to cool to room temperature, filter and wash the precipitate, and dry it in a vacuum drying oven at 65°C for 8 hours to obtain a spiropyran coating Zinc sulfide nanospheres;

[0100] (2) 8g spiropyran-coated zinc sulfide nanospheres and 8.2g diphenylmethane-4,4'-diisocyanate (MDI) were added to 1000g butyl acetate solvent, and after stirring evenly, 7g were respectively added to mix and react agent (1.2g n-butanol, 5.8g polytetrahydrofur...

Embodiment 2

[0115] (1) Preparation of photochromic nanocomposite microspheres:

[0116] (1) Add 6.5g of zinc nitrate to 1600g of ethylene glycol, after stirring, add 1.7g of sublimation sulfur powder, be warming up to 150°C and keep reacting for 24 hours, cool to 55°C, drip 70g of mercaptoethanol and stir; 3.5g of spiropyran photochromic compound (I) was vigorously stirred for 30 minutes, cooled to room temperature, filtered and washed by precipitation, and dried in a vacuum drying oven at 65° C. for 8 hours to obtain spiropyran-coated zinc sulfide nanospheres;

[0117] (2) get 5.5g spiropyran-coated zinc sulfide nanospheres, add 5g MDI into 1000g butyl acetate solvent, after stirring, add 5.5g mixed reactants (1.0g n-butanol, 4.5g polytetrahydrofuran ether in turn) Diol), 20g Tween80, the temperature was kept at 25°C, the prepolymerization reaction was carried out at 500r / min rotation speed for 50min, 6g chain extender (ethylene glycol 4.5g, ethylenediamine 1.5g), 0.1g DBTL were added, a...

Embodiment 3

[0126] (1) Preparation of photochromic nanocomposite microspheres:

[0127] (1) to 1600g of ethylene glycol, add 11g of zinc nitrate hexahydrate, after stirring evenly, add 3g of sulfur powder, be warming up to 145 ℃ of insulation reaction for 24 hours, cool to 50 ℃, drip 92g of mercaptoethanol and stir; add 8g again The spiropyran photochromic compound (I) was vigorously stirred for 35 minutes, continued to be cooled to room temperature, the precipitate was filtered and washed, and dried in a vacuum drying oven at 60° C. for 9 hours to obtain spiropyran-coated zinc sulfide nanospheres;

[0128] (2) get 10g spiropyran-coated zinc sulfide nanospheres, 10.8g iso-xylylene diisocyanate (XDI) and add to 1000g butyl acetate solvent, after stirring, add 7.4g mixed reactant (1.0 g n-butanol, 6.4g polytetrahydrofuran ether glycol), 16g Tween80, temperature kept at 25°C, prepolymerization reaction at 600r / min rotation speed for 60min, adding 8g chain extender (5.5g ethylene glycol, 2.5g...

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Abstract

The invention relates to a preparation method of a spiropyrane photochromic optical material. The surface of the optical material prepared by adopting the preparation method is coated with a photochromic coating, the coating contains a polyurethane/spiropyrane/zinc sulfide composite multilayer photochromic material, a core of the coating is zinc sulfide mesoporous nano microspheres, an intermediate layer is a photochromic layer composed of spiropyrane compounds, and a shell is polyurethane; and the outer diameter of the composite microspheres is 50-350nm, the diameter of the zinc sulfate mesoporous nano microspheres is 30-250nm, the thickness of the intermediate layer is 5-25nm, and the thickness of the shell is 5-25nm. The optical material prepared by adopting the preparation method can become colored from colorless under ultraviolet irradiation condition, can also be rapidly faded to be colorless after ultraviolet rays disappear and has the advantages of strong fatigue resistance, good stability and high color-changing speed.

Description

technical field [0001] The invention belongs to the technical field of photochromism, and in particular relates to an optical material containing spiropyran-based photochromic nanocomposite microspheres in a coating and a preparation method thereof. Background technique [0002] Photochromism refers to the change of the molecular structure of the material with the change of the absorption spectrum of certain compounds under the action of light of a certain wavelength and intensity, resulting in changes 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 field of optical material subdivision, it is of great importance in high-tech fields such as optical lenses, optical information storage, molecular switches, and anti-counterfeiting identification. Value. Humans have discovered the phenomenon of photochromism for mo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J7/04C08J7/14B01J13/18C08G18/76C08G18/48C08G18/12C08G18/66C07D491/107C07D311/94G02C7/10C08L75/04
CPCB01J13/185C07D311/94C07D491/107C08G18/12C08G18/4854C08G18/6685C08G18/7671C08J7/0427C08J7/14C08J2375/04C08J2475/08G02C7/102C08G18/3206C08G18/3228
Inventor 王明华张鹤军纪立军范为正乔振安司云凤王志飞郑永华薛晓花吴潇刘洋
Owner 南京米兰达视光科学研究院有限公司
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