PH/zinc ion and redox quadruple stimuli responsive nanocontainer and preparation method thereof
A stimuli-responsive, nano-container technology, which can be used in pharmaceutical formulations, inactive medical preparations, inorganic inactive ingredients, etc., can solve problems such as weak coordination, and achieve the effects of low toxicity, convenient preparation, and extended service life.
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[0037] References for the preparation method of mesoporous silica nanospheres of the present invention [C D Ding; Y Liu; M DWang; T Wang; J J Fu; Superhydrophobic Coating Based on Mechanized Silica Nanoparticles for Reliable Protection of Magnesium Alloy[J].J. Am.Chem.Soc.,2016,4(21):8041-8052], the specific steps are as follows:
[0038] With 0.5g cetyltrimethylammonium bromide (CTAB), 1.75mL 2mol / L sodium hydroxide solution, 240mLH 2 O was added to a 500mL three-necked flask, heated to 80°C under vigorous stirring, and kept for 30 minutes to activate CTAB, and then 2.5mL tetraethyl orthosilicate (TEOS) was added dropwise. Under vigorous stirring, white precipitates gradually appeared in the reaction vessel. generate. React at 80°C for 2 hours, filter while hot, wash the solid with water and methanol several times, and dry it in vacuum. After drying, ultrasonically disperse the solid in a mixture of 100mL methanol and 5mL concentrated hydrochloric acid, stir the reaction so...
Embodiment 1
[0040] 1. Preparation of guest molecules
[0041] Phenol (5.00g, 53.19mmol), 1,4-dibromobutane (13.77g, 63.75mmol) and K 2 CO 3 (16g, 116mmol) the mixture in 30.0mL anhydrous acetonitrile in N 2 Reflux under atmosphere for 10h. Then the crude product was purified by a silica gel column, and the eluent was petroleum ether-dichloromethane (3:1, v / v) to obtain a white crystal product (4-bromobutoxy)benzene.
[0042] Cystamine dihydrochloride (6.75 g, 30 mmol) was dissolved in 300 ml of methanol; di-tert-butyl dicarbonate (6.54 g, 30 mmol) and triethylamine (12.60 mL, 3 equivalents) in 45 mL of methanol were dissolved, Add the above solution dropwise to the methanol solution containing cystamine dihydrochloride at a rate of 0.64 mL / min. After the addition was complete, the reaction mixture was stirred for another 90 min. The solvent was then removed by rotary evaporation and 1M NaH was added 2 PO 4 (75 mL); the aqueous solution was washed three times with ether (90 mL) to r...
Embodiment 2
[0058] 1. Preparation of guest molecules
[0059] Phenol (0.473g, 5mmol), 1,4-dibromobutane (1.32g, 6mmol) and K 2 CO 3 (1.53g, 11mmol) the mixture in 35.0mL anhydrous acetonitrile in N 2 Reflux under atmosphere for 24h. Then the crude product was purified by a silica gel column, and the eluent was petroleum ether-dichloromethane (3:1, v / v) to obtain a white crystal product (4-bromobutoxy)benzene.
[0060] Cystamine dihydrochloride (2.25 g, 10 mmol) was dissolved in 100 ml of methanol; di-tert-butyl dicarbonate (2.18 g, 10 mmol) and triethylamine (4.20 mL, 3 eq) in 15 mL of methanol were dissolved, Add the above solution dropwise to the methanol solution containing cystamine dihydrochloride at a rate of 0.64 mL / min. After the addition was complete, the reaction mixture was stirred for another 30 min. The solvent was then removed by rotary evaporation and 1M NaH was added 2 PO 4 (25 mL); the aqueous solution was washed three times with ether (30 mL) to remove the double-...
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