Azobenzol liquid crystal holography storage material and preparation method thereof
A storage material and optical holography technology, applied in liquid crystal materials, information storage, recorded information storage, etc., can solve the problems of limited application, easy loss of stored information, refractive index modulation, etc., and achieves simple preparation method, good optical properties, increased The effect of information storage capacity
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Embodiment 1
[0031] ①Synthesis of azobenzene unit
[0032] Add p-butoxyaniline (7.8g, 0.05mol) to a solution of 17ml (0.2mol) of concentrated hydrochloric acid and 10ml of water, stir and mix well. Heat with an oil bath to make the solution clear, then quickly put it into an ice-salt bath and stir to obtain good crystals. Keeping the temperature at 0-5°C, sodium nitrite (3.5 g, 0.05 mol) and 20 ml of water were added dropwise with stirring. After 30 min, an equal amount of urea was added to neutralize the remaining sodium nitrite, and the reaction progress was monitored by starch-potassium iodide test paper to obtain a diazonium salt solution. Phenol (4.9 g, 0.05 mol) was dissolved in 10% aqueous sodium hydroxide (4 g, 0.05 mol), and the mixture was cooled to below 10° C. in an ice bath, and then 20 g of ice was added. The above-mentioned diazonium salt solution was slowly added dropwise and stirred rapidly for 1 h, and then a saturated sodium acetate solution was added to adjust the pH ...
Embodiment 2
[0046] ①Synthesis of compounds containing azobenzene and liquid crystal groups
[0047] To 100 ml of dichloromethane were added 4-cyano-4'-carboxybiphenyl (8.3 g, 0.037 mmol), 4,4'-dihydroxyazobenzene (2.6 g, 0.012 mmol) and 4-dimethylaminopyridine (4.5g, 0.037mmol), mix well, pass nitrogen as a protective gas, and then add 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC·HCl). After the mixture was stirred at room temperature for 12 h, dichloromethane was added to dilute, and then saturated NH 4 Cl aqueous solution and saturated sodium chloride aqueous solution were washed. The organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated to dryness, and purified by silica gel chromatography to obtain compound 4.
[0048] ② Preparation of optical holographic materials
[0049] Add 2.8 ml of water to γ-glycidyloxypropyltrimethoxysilane (9.4 g, 0.04 mol) and ethyl orthosilicate (2 g, 0.01 mol), and adjust the pH to about 3 with hydrochloric ...
Embodiment 3
[0054] ①Synthesis of azobenzene unit
[0055] p-Methoxyaniline (6.2 g, 0.05 mmol) was added to a solution of 17 ml of concentrated hydrochloric acid (0.2 mol) and 10 ml of water, and stirred to mix well. Heat it with an oil bath to make the solution clear, then quickly put it into an ice-salt bath and stir to get good crystals. Keeping the temperature at 0-5°C, sodium nitrite (3.5 g, 0.05 mol) and 20 mol of water were added dropwise and stirred. After 30 minutes, an equal amount of urea was added to neutralize the remaining sodium nitrite, and the reaction progress was monitored by starch-potassium iodide test paper to obtain a diazonium salt solution. Phenol (4.9 g, 0.05 mol) was dissolved in 10% aqueous sodium hydroxide (4 g, 0.05 mol), and the mixture was cooled to below 10° C. with an ice bath, and then 20 g of ice was added. The above diazonium salt solution was slowly added dropwise, stirred rapidly for 1 h, and then a saturated sodium acetate solution was added to adj...
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