Method for preparing stimuli-responsive silicon dioxide nano particle
A stimuli-responsive, silicon dioxide technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve problems that cannot meet the development requirements, and achieve the effect of stable products, good stability, and high stimuli responsiveness
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Embodiment 1
[0028] The specific steps for preparing stimuli-responsive silica nanoparticles are as follows:
[0029] 1) Synthesis of thioalkylammonia-2-thiopyridine hydrochloride
[0030] Dissolve 1.1g (5mmol) of mercaptopyrimidine disulfide in a solution composed of 10ml of methanol and 0.2ml of acetic acid, dissolve 0.25g (2.2mmol) of mercaptoethylamine hydrochloride in another 10ml of methanol, and drop the latter After adding to the former, the reaction was 48h. After the reaction, the solvent was evaporated under reduced pressure to obtain a yellow oily substance (the crude product of thioalkylammonia-2-thiopyridine hydrochloride). After washing with 50 ml of ether, the product was dissolved in 10 ml of ethanol and precipitated with 400 ml of ether to give 0.4 g of a white solid. Yield: 77%; 1 H NMR: δppm (400M, CDCl 3 ) 8.66(d, 1H), 7.75(t, 1H), 7.48(d, 1H), 7.1(t, 1H), 3.46(t, 2H) and 2.8(m, 2H).
[0031] 2) Preparation of silica nanoparticles
[0032] Mix 50ml of absolute et...
Embodiment 2
[0039] According to the steps of 1) in Example 1, thioalkylammonium-2-thiopyridine hydrochloride was prepared from mercaptopropylamine hydrochloride. 3g (13.6mmol) of mercaptopyrimidine disulfide was dissolved in a solution consisting of 40ml of methanol and 1ml of acetic acid. 4.95 g (54.4 mmol) of mercaptopropylamine hydrochloride were dissolved in another 40 ml of methanol. The latter was added dropwise to the former at room temperature and reacted for 48h. After the reaction, the solvent was evaporated under reduced pressure to obtain a crude product. After washing with 100 ml of ether, the product was dissolved in 50 ml of ethanol and precipitated with 400 ml of ether to give thioalkylammonium-2-thiopyridine hydrochloride.
[0040] According to the step 3) in Example 1, the silica nanoparticles were treated with aminopropyltrimethoxysilane. Take 0.5g of silica nanoparticles and disperse them in 100ml of toluene solution, then add 5ml of aminopropyltrimethoxysilane, sti...
Embodiment 3
[0045] According to the steps of 1) in Example 1, 0.1g (0.5mmol) mercaptopyrimidine disulfide was dissolved in a solution composed of 5ml methanol and 0.1ml acetic acid, and 0.025g (0.2mmol) mercaptoethylamine hydrochloride was dissolved in another In 5ml of methanol, the latter was added dropwise to the former at room temperature and reacted for 24 hours. After the reaction, the solvent was evaporated under reduced pressure to obtain a yellow oily substance (the crude product of thioalkylammonia-2-thiopyridine hydrochloride). After washing with 15 ml of ether, the product was dissolved in 5 ml of ethanol and precipitated with 40 ml of ether to give 0.1 g of a white solid. Yield: 67%; 1 H NMR: δppm (400M, CDCl 3 ) 8.56(d, 1H), 7.65(t, 1H), 7.42(d, 1H), 7.1(t, 1H), 3.43(t, 2H) and 2.6(m, 2H).
[0046] According to the steps of 2) in Example 1, 10ml of absolute ethanol and 1ml of tetraethyl orthosilicate were mixed evenly, and then 10ml of ammonia water with a mass fraction o...
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