Photochromic microspheres and preparation method thereof

A photochromic and photochromic dye technology, applied in the field of photochromic polymer microspheres, can solve the problems of poor thermal stability and mechanical properties, unfavorable large-scale production, complex double-layer coating process, etc. Good stability, excellent mechanical properties, and the effect of expanding the application field

Inactive Publication Date: 2018-04-24
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method still has the defects in the above-mentioned patent CN101225296A, that is, poor thermal stability and mechanical properties, and also requires a complicated double-layer coating process, which is not conducive to large-scale production

Method used

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  • Photochromic microspheres and preparation method thereof
  • Photochromic microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 2g polylactic acid, 0.2g spirooxazine organic photochromic dye, 0.5g dibutyl hydroxytoluene, 0.3g 2-hydroxyl-4-n-octyloxybenzophenone and 0.3g 1-hydroxyl-2-naphthoyl phenyl Dissolve in 10g of dichloromethane solvent, then add to 50g of 2wt% polyvinyl alcohol aqueous solution, add 2g of isobutanol at the same time, emulsify at a high speed of 3000rpm for 10min, after making a stable oil-in-water emulsion, the emulsion The particle size is 5-35 microns by optical microscope observation. Transfer the above-mentioned oil-in-water emulsion to a three-necked flask, heat up to 50°C while stirring and keep it warm for 120 minutes. After that, a polymer containing photochromic compound molecules uniformly dispersed can be obtained. Lactic acid microsphere suspension. The suspension was suction filtered and washed to obtain a filter cake. After the filter cake is vacuum-dried, the photochromic microsphere dry powder can be obtained.

[0025] The morphology of the microspheres p...

Embodiment 2

[0027] Swell 10g cellulose acetate with 100g chloroform, 10g 1-hydroxyethyl-3,3-dimethyl-nitroindoline spiropyran optical variable dye, 1g thiodipropionate dilaurate, 0.5g4 - Benzoyloxy-2,2,6,6-tetramethylpiperidine and 0.3 g of p-benzylbiphenyl were dissolved for 24 hours, then stirred and dissolved to obtain a homogeneous oil phase solution. Add it to 800g concentration of 4wt% alkylphenol polyoxyethylene ether formaldehyde condensate sulfate solution, emulsify at a high speed at 30000rpm for 30min, after making a stable oil-in-water emulsion, the emulsion droplet size is observed by optical microscope Measured from 0.1 to 2 microns. Transfer the above stable oil-in-water emulsion to a 2-liter three-neck flask, raise the temperature to 60°C while stirring and keep it warm for 120 minutes, then the cellulose ester microsphere suspension containing photochromic compound molecules uniformly dispersed can be prepared. The suspension was suction filtered and washed to obtain a f...

Embodiment 3

[0029] With 20kg ethyl acetate, 1kg thermoplastic polyurethane, 1kg spiropyran organic photochromic dye, 60g tert-butyl hydroquinone, 50g resorcinol monobenzoate and 30g dibenzyl oxalate are dissolved to obtain a solution, Then add it to 100kg of sodium lauryl sulfate solution, which contains 1kg of sodium lauryl sulfate, 1kg of n-octanol, 2kg of Tween 60, and emulsify at a high speed of 9000rpm for 60min to obtain a stable oil-in-water type After the emulsion, the particle size of the emulsion droplets is observed and measured by an optical microscope to be 2 to 15 microns, and the above-mentioned oil-in-water emulsion is directly spray-dried, and the spray-drying conditions are that the inlet temperature is set to 150°C, and the outlet temperature is set to 80°C, namely The dry powder of photochromic microspheres can be obtained directly. The particle size of the microspheres measured by an electron microscope is regular and spherical, and the particle size distribution is w...

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Abstract

The invention discloses photochromic microspheres with excellent thermal stability and a preparation method of the photochromic microspheres. The method comprises following steps: 1), a polymer or oligomer, a photochromic compound, an antioxidant, an ultraviolet absorbent and a sensitizer are swollen in an oil-soluble solvent with low boiling point; 2), after being heated to certain temperature and stirred and dissolved into uniform oil phase, a mixture is added to an aqueous solution containing an emulsifier and a co-emulsifier, and an oil-in-water type stable emulsion with emulsion droplet particle size range being 10 nm-1000 mu m is obtained through shearing emulsification; 3), the temperature of the emulsion system is increased and kept for a period of time, the low-boiling-point solvent in emulsion droplets is completely volatilized, polymer microspheres with uniformly dispersed photochromic molecules are obtained, and dry polymer microsphere powder with the uniformly dispersed photochromic molecules can also be directly prepared from the emulsion with a spray drying process. The microspheres prepared with the method are of a homogeneous solid structure, excellent in mechanical property and good in heat stability and have great application prospect in the fields of anti-counterfeiting, plastic products, fabric clothing, chemical printing and dyeing and the like.

Description

technical field [0001] The invention relates to a photochromic polymer microsphere with excellent thermal stability, in particular to a microsphere in which a photochromic compound is uniformly dispersed in a solid polymer substrate in a molecular state and a synthesis method thereof. Background technique [0002] In the more than 100 years since the advent of photochromic materials and technology, photochromic materials have attracted more and more attention due to their ability to produce color changes when excited by light sources, and are being applied to intelligent anti-counterfeiting, information storage, textiles, and daily necessities. , characteristic photosensitive materials and other fields. However, if photochromic materials are directly exposed to natural environments such as visible light for a long time, they are easily affected by temperature, pH value, oxygen and other environments, which will eventually lead to attenuation or instability of color changing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K9/02C09K11/02
CPCC09K9/02C09K11/025
Inventor 李伟霍晓楠郭茂莲耿晓叶边俊民
Owner TIANJIN POLYTECHNIC UNIV
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