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Photochromic polyester material and preparation method thereof

A polyester material and photochromic technology, applied in the direction of color-changing fluorescent materials, chemical instruments and methods, etc., can solve the problems of high addition of photochromic microcapsules, low spiropyran content, poor color fastness, etc.

Active Publication Date: 2021-09-07
WUHAN TEXTILE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main methods for preparing organic photochromic polyester materials are as follows: 1) Melt blending method is adopted, that is, directly blending and melting photochromic materials and polymers, or dispersing photochromic materials in energy and polymer The method of making luminescent masterbatch in the resin carrier mixed with the material, and then mixed into the high polymer for melting, but the photochromic material is easy to agglomerate in the polyester matrix, and the dispersion is poor
2) The coating method is adopted, that is, the photochromic material is dispersed in an appropriate solvent, and then mixed with a binder such as a resin liquid to make a luminescent color paste, and then coated on the surface of the polyester material, but the prepared polyester product It is easy to fall off after washing, so that the luminous performance will decline and the service life will be shortened
3) The photochromic microcapsules of the spiropyran class are blended with the low melting point polyester material, but the spiropyran content of the photochromic polyester material prepared by it is low, and the addition amount of the photochromic microcapsules is high, The color change is not bright, the color fastness is poor and other shortcomings, so its application is limited
However, the disadvantage of this method is that it is limited to the preparation of photochromic fiber products, the types of polyester products are limited, and the photochromic effect is not significantly improved.

Method used

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  • Photochromic polyester material and preparation method thereof
  • Photochromic polyester material and preparation method thereof
  • Photochromic polyester material and preparation method thereof

Examples

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preparation example Construction

[0033] see figure 1 As shown, the invention provides a kind of preparation method of photochromic polyester material, comprises the steps:

[0034] S1. Preparation of dual-active spirooxazine materials:

[0035] S11. Dissolve methyl isopropyl ketone and p-methylphenylhydrazine in ethanol according to a predetermined molar ratio to obtain a first mixed solution, and add concentrated sulfuric acid dropwise to the first mixed solution, at 75-85°C Reacting in an oil bath for 3.0 to 4.5 hours; then adding NaOH solution dropwise to the first mixed solution to make it alkaline, and performing extraction and distillation treatment to prepare indole;

[0036] S12. Change CH 3 CH 2 I and the indole prepared in step S11 were dissolved in ethanol and mixed uniformly, placed in an oil bath at 75-85°C for reflux reaction for 2-4 hours, and purified to obtain an intermediate product; the intermediate product was dissolved in ethanol, and added A predetermined amount of 1-nitroso-2,7-dihydr...

Embodiment 1

[0049] S1. Preparation of dual-active spirooxazine materials:

[0050] Slowly add 1 mol of methyl isopropyl ketone distilled under atmospheric pressure into 1 mol of p-methyl phenylhydrazine, use ethanol as a solvent, add the catalyst concentrated sulfuric acid dropwise within 30 minutes, and react in an oil bath at 80°C for 4 hours, After the reaction is complete, NaOH solution is added dropwise until alkaline, then extracted with anhydrous ether, filtered with suction, and distilled under reduced pressure to obtain indole;

[0051] CH 3 CH 2 I and the prepared indole are added into absolute ethanol in a molar mass ratio of 1::0.8 to dissolve and mix uniformly, react at reflux in an oil bath at 80°C for 3h, cool and crystallize, filter, and purify by recrystallization to obtain an intermediate product; then The intermediate product was dissolved in ethanol, 1-nitroso-2,7-dihydroxynaphthalene with the same molar mass as the intermediate product was added, refluxed in an oil ...

Embodiment 2-4

[0062] The difference from Example 1 is that the molar ratio of bishydroxyethyl terephthalate to the bisactive spirooxazine material is different, and the other steps are the same as in Example 1, and will not be repeated here.

[0063] Table 1 is the setting of the molar ratio of bishydroxyethyl terephthalate and bisactive spirooxazine materials in Examples 1-4

[0064]

[0065] Embodiment 1-4 is analyzed in conjunction with Table 1: The influence of the molar ratio change of bishydroxyethyl terephthalate and bisactive spirooxazine material on the photochromic polyester material prepared by the present invention is: The molar ratio of hydroxydiethyl ester to the dual-active spirooxazine photochromic material ranges from 1:0.5% to 20%, and different proportions of spirooxazine materials are added to prepare spirooxine with different color depths and color fastnesses. Azinoid photochromic polyester material.

[0066] The higher the ratio of the dual-active spirooxazine mate...

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Abstract

The invention provides a photochromic polyester material and a preparation method thereof. The preparation method comprises the following steps of: dissolving methyl isopropyl ketone and p-methyl phenylhydrazine in ethanol, dropwise adding concentrated sulfuric acid, and carrying out an oil bath reaction to prepare indole; dissolving CH3CH2I and the indole in ethanol, performing uniform mixing, and carrying out an oil bath reflux reaction to obtain an intermediate product; adding 1-nitroso-2, 7-dihydroxy naphthalene, and carrying out an oil bath reflux to prepare a double-activity spirooxazine material; mixing terephthalic acid and ethylene glycol, adding antimony trioxide and phenyl triphosphate, and carrying out an esterification reaction to obtain bis (2-hydroxyethyl) terephthalate; and finally, mixing the bis (2-hydroxyethyl) terephthalate with the double-active spirooxazine material, and carrying out condensation polymerization to prepare the photochromic polyester material. The spirooxazine material with dihydroxyl activity is grafted to a main chain of polyethylene glycol terephthalate macromolecules, so that the prepared photochromic polyester material is remarkable in photochromic effect and excellent in color fastness.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a photochromic polyester material and a preparation method thereof. Background technique [0002] Photochromic polyester materials have important application prospects in high-tech fields such as high-density information storage, optical computing, and information display. At present, the main methods for preparing organic photochromic polyester materials are as follows: 1) Melt blending method is adopted, that is, directly blending and melting photochromic materials and polymers, or dispersing photochromic materials in energy and polymer The method of making luminescent masterbatch in the resin carrier mixed with the material, and then mixed into the high polymer for melting, but the photochromic material is easy to agglomerate in the polyester matrix, and the dispersibility is poor. 2) The coating method is adopted, that is, the photochromic material is dispersed in an appr...

Claims

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Application Information

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IPC IPC(8): C08G63/685C08G63/86C08G63/87C09K9/02
CPCC08G63/6856C08G63/866C08G63/87C09K9/02C09K2211/1475
Inventor 王栋赵青华毛秦岑王雯雯宋银红尤海宁吴建美
Owner WUHAN TEXTILE UNIV
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