Preparation method of magnetic beads of dendritic molecular imprinting polymer on surface of estrogenic nano silica gel
A nano-silica gel and molecular imprinting technology, which is applied in chemical instruments and methods, and other chemical processes, to achieve the effects of avoiding the difficulty of product separation and purification, expanding the adsorption capacity, and improving the imprinting efficiency
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Embodiment 1
[0030] Embodiment 1: prepare Fe 3 o 4 SiO 2 Nanoparticles
[0031] In a 250ml three-neck bottle, add 80ml deoxygenated deionized water, add FeCl under nitrogen protection 3 ·6H 2 O (4.72g) and FeCl 2 4H 2 O (1.98g), stirred at 800rmp / min, 15ml of concentrated ammonia water and 1ml of oleic acid were added dropwise at 85°C, reacted for 1h, and black Fe was obtained by magnetic separation. 3 o 4 Nanoparticles, washed with deionized water until neutral;
[0032] Take 0.3gFe 3 o 4 Nanoparticles, uniformly dispersed in 30ml isopropanol and 2ml deionized water, keep the stirring speed at 200rmp / min, add 2ml concentrated ammonia water and 5ml tetraethyl orthosilicate (TEOS), react at room temperature for 12h, and magnetically separate Fe 3 o 4 SiO 2 Nanoparticles, washed with deionized water until neutral, dried for later use;
Embodiment 2
[0034] a) Preparation of dendrimer-modified magnetic nanoparticles
[0035] (1): 0.3g Fe 3 o 4 SiO 2 Nanoparticles were dispersed in toluene, silane coupling agent was added, heated at 120°C for 24h under the protection of nitrogen, and subjected to conventional magnetic separation to obtain amino-terminated magnetic nanoparticles (MNPs-NH 2 ), the volume ratio of the silane coupling agent to toluene is 0.05: 1ml / ml;
[0036] (2): 0.3g MNPs-NH 2 Nanoparticles were dispersed in methanol, methyl acrylate (MA) was added, heated at 50 °C for 30 h under nitrogen protection, and subjected to conventional magnetic separation to obtain dendritic magnetic nanoparticles modified with terminal ester groups (MNPs-OCH 3 ), the mol ratio of the MA and the silane coupling agent added in (1) is 4:1;
[0037] (3): 0.3g MNPs-OCH 3 Nanoparticles are dispersed in N, N-dimethylformamide (DMF), and serinol and appropriate amount of potassium carbonate are added at the same time, heated at 45°...
Embodiment 3
[0043] a) Preparation of dendrimer-modified magnetic nanoparticles
[0044] (1): the Fe prepared according to the method of Example 1 3 o 4 SiO 2 Nanoparticles were dispersed in toluene, a silane coupling agent was added, heated at 140°C for 18h under the protection of nitrogen, and subjected to conventional magnetic separation to obtain magnetic nanoparticles modified with amino groups (Magnetic Nanoparticles-NH 2 , MNPs-NH 2 ), the volume ratio of the silane coupling agent to toluene is 0.06: 1;
[0045] (2): 0.3g MNPs-NH 2 Nanoparticles were dispersed in methanol, methyl acrylate (MA) was added, heated at 60°C for 24h under nitrogen protection, and subjected to conventional magnetic separation to obtain dendritic magnetic nanoparticles modified with terminal ester groups (Magnetic Nanoparticles-OCH 3 , MNPs-OCH 3 ), the molar ratio of the MA and the silane coupling agent added in (1) is 2:1; (3): the MNPs-OCH 3 Nanoparticles are dispersed in N, N-dimethylformamide (D...
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