Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of spiropyrane/titanic acid composite photochromic thin film

A technology of spiropyran and compound light, which is applied in the field of preparation of spiropyran/titanic acid composite photochromic film, which achieves the effects of simple operation, good wear resistance and high mechanical strength

Inactive Publication Date: 2017-08-29
CHENDU NEW KELI CHEM SCI CO LTD
View PDF3 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since most photochromic materials can only change color in solution, from the perspective of functional practicality, organic photochromic materials with photochromic properties in the solid state can better meet their requirements in high-density information storage and holographic anti-counterfeiting. Comprehensive application in the field

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of a spiropyran / titanic acid composite photochromic film, comprising the following steps:

[0034] A. (1) Add 2,3,3-trimethyl-4,5-benzindole and ethyl iodide to the reaction vessel at a molar ratio of 1:1.1~1.2, add absolute ethanol, 75~79 Stir and reflux at ℃ for 20-24 hours, cool to room temperature, rotary evaporate, wash, and dry to obtain a blue-purple solid, namely N-ethyl-2,3,3-trimethyl-4,5-benzindoline-N - iodized salt;

[0035] (2) N-ethyl-2,3,3-trimethyl-4,5-benzindoline-N-iodide and 5-nitrosalicylaldehyde prepared in step (1) in molar ratio 1:1 into the reaction vessel, add triethylamine and absolute ethanol, stir and reflux at 75-79°C for 14-16 hours, cool to room temperature, filter with suction, and dry to obtain dark purple powder, namely 1'-ethyl-3 ',3'-Dimethyl-6-nitrospiro[4',5'-benzoindoline-2,2'[2H-1]benzopyran] crude product;

[0036] (3) The 1'-ethyl-3',3'-dimethyl-6-nitrospiro[4',5'-benzindoline-2,2'[2H -1] Benzopyran] us...

Embodiment 2

[0041] A preparation method of a spiropyran / titanic acid composite photochromic film, comprising the following steps:

[0042] A. (1) Add 2,3,3-trimethyl-4,5-benzindole and ethyl iodide to the reaction vessel at a molar ratio of 1:1.1~1.2, add absolute ethanol, 75~79 Stir and reflux at ℃ for 20-24 hours, cool to room temperature, rotary evaporate, wash, and dry to obtain a blue-purple solid, namely N-ethyl-2,3,3-trimethyl-4,5-benzindoline-N - iodized salt;

[0043] (2) N-ethyl-2,3,3-trimethyl-4,5-benzindoline-N-iodide and 5-nitrosalicylaldehyde prepared in step (1) in molar ratio 1:1 into the reaction vessel, add triethylamine and absolute ethanol, stir and reflux at 75-79°C for 14-16 hours, cool to room temperature, filter with suction, and dry to obtain dark purple powder, namely 1'-ethyl-3 ',3'-Dimethyl-6-nitrospiro[4',5'-benzoindoline-2,2'[2H-1]benzopyran] crude product;

[0044] (3) The 1'-ethyl-3',3'-dimethyl-6-nitrospiro[4',5'-benzindoline-2,2'[2H -1] Benzopyran] us...

Embodiment 3

[0049] A preparation method of a spiropyran / titanic acid composite photochromic film, comprising the following steps:

[0050] A. (1) Add 2,3,3-trimethyl-4,5-benzindole and ethyl iodide to the reaction vessel at a molar ratio of 1:1.1~1.2, add absolute ethanol, 75~79 Stir and reflux at ℃ for 20-24 hours, cool to room temperature, rotary evaporate, wash, and dry to obtain a blue-purple solid, namely N-ethyl-2,3,3-trimethyl-4,5-benzindoline-N - iodized salt;

[0051] (2) N-ethyl-2,3,3-trimethyl-4,5-benzindoline-N-iodide and 5-nitrosalicylaldehyde prepared in step (1) in molar ratio 1:1 into the reaction vessel, add triethylamine and absolute ethanol, stir and reflux at 75-79°C for 14-16 hours, cool to room temperature, filter with suction, and dry to obtain dark purple powder, namely 1'-ethyl-3 ',3'-Dimethyl-6-nitrospiro[4',5'-benzoindoline-2,2'[2H-1]benzopyran] crude product;

[0052] (3) The 1'-ethyl-3',3'-dimethyl-6-nitrospiro[4',5'-benzindoline-2,2'[2H -1] Benzopyran] us...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of composite photochromic thin films and particularly provides a preparation method of a spiropyrane / titanic acid composite photochromic thin film. The preparation method includes the steps of: A) dissolving spiropyrane and a vinyl monomer in an organic solvent, and adding vinyltriethoxysilane to perform a copolymerization reaction in oil bath to prepare a compound copolymer; B) mixing the compound copolymer with a titanium source, treating the mixture in water bath at 50-60 DEG C, continuously dropwise adding an acid source into the mixture system with continuous stirring, and when the acid source is all added dropwise, gradually dropwise adding a mixed solution of ethanol and water to the mixture system; C) continuously stirring the mixture to form sol, pouring a suspension liquid into a glass trough and drying the suspension liquid to prepare the spiropyrane / titanic acid composite photochromic thin film. The preparation method achieves further application of a spiropyrane-type photochromic compound, under solid state, in the fields of high density optical information storage devices and nondestructive readout, and develops the applications of the materials in the field of practical devices.

Description

technical field [0001] The invention belongs to the technical field of composite photochromic films, in particular to a preparation method of spiropyran / titanic acid composite photochromic films. Background technique [0002] After Hirshberg proposed the scientific significance of photochromism for the first time, photochromism research broke away from the previous aimlessness and randomness. The specificity of photochromic materials brings broad development and application prospects to organic photochromic compounds. Compared with inorganic materials, it has the advantages of fast response, easy processing and low cost. It has been used in photochromic glasses, optical information recording materials, molecular wires and molecular switches, etc. Photochromic materials refer to a compound that absorbs external electromagnetic waves in two or at least one direction and undergoes a reversible configuration transition between two states. After the compound is excited by an el...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C09K9/02
CPCC09K9/02C09K2211/145C09K2211/1466
Inventor 陈庆司文彬王镭迪曾军堂
Owner CHENDU NEW KELI CHEM SCI CO LTD