Ni 2+ chelated affinity type super-macroporous crystal gel medium for column chromatography and its preparation method
A technology of crystal gel medium and column chromatography, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem of low adsorption capacity, achieve high separation efficiency, convenient regeneration, and wide application fields
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Embodiment 1
[0032] Dissolve 1.5g of AAm monomer, 0.09g of cross-linking agent MBAAm and 0.09g of ethylene glycol diglycidyl ether in 15mL of deionized water, stir well, then quickly add 10mg of TEMED and 20mg of APS, and fill the resulting mixture into a 16mm , In a 200mm-long glass chromatography column, placed in a programmable temperature-controlled constant temperature cooling system, from 0 ° C to -40 ° C, and then at a constant temperature, cooling crystallization-induced pore polymerization. After 24 hours, the temperature was raised to room temperature to obtain a crystal gel medium matrix.
[0033] At 25°C, use 0.4 matrix volume of 0.05M Na 2 CO 3 solution, 0.05M IDA solution with 5 times the volume of the matrix, respectively activated the obtained matrix for 24 hours, and then used 0.5M NiSO with 2 times the volume of the matrix 4 The solution undergoes a chelation reaction to obtain Ni 2+ Chelating affinity gel medium. Its porosity is 59%, and SEM shows that its pore diame...
Embodiment 2
[0035] Dissolve 2g of DMAAm monomer, 0.6g of cross-linking agent N,N'-diacryloyl ethylenediamine and 0.5g of ligand material ethylene glycol diglycidyl ether in 50ml of deionized water, stir well, then quickly add 20mg TEMED and 50mg APS, put the resulting mixture into a chromatographic column with an inner diameter of 26mm and a length of 200mm, seal it, and perform cooling and crystallization in a programmable temperature-controlled constant temperature cooling system to form pores. The temperature change process is: (A) cooling: from 0°C to -70°C; (B) heating: heating to -10°C; (C) constant temperature: constant temperature for 5 hours; (D) cooling: cooling from -10°C again to -20°C; (E) constant temperature: constant temperature for 16 hours; (F) heating up: heating up to room temperature to obtain a crystal gel medium matrix.
[0036] The obtained matrix was activated with 15 times the matrix volume of 0.15M NaHB solution, and then the obtained matrix was circulated with 3 ...
Embodiment 3
[0038] Dissolve 0.76g of DMAEMA monomer, 0.38g of cross-linking agent MBAAm, and 0.5g of a mixture of ligand material AGE and ethylene glycol diglycidyl ether (mass ratio 1:0.5) in 12ml of deionized water, stir well, and quickly add 45mg TEMED and 50mg APS, put the resulting mixture into a glass chromatography column with an inner diameter of 10mm and a length of 200mm, and cool down to -25°C in a programmable temperature-controlled constant temperature cooling system for cooling and crystallization to cause pores. Then, the crystals were melted at room temperature to obtain a gel medium matrix.
[0039] The obtained medium matrix was reacted with 4.5 times the volume of the matrix of 1M NaOH solution at 40°C, and then reacted with 0.5M EDT solution of 3 times the volume of the matrix at 55°C for 6 hours, and finally reacted with 9 times the volume of the matrix of 5M NiCl 2 Solution chelation reaction, namely to obtain Ni 2+ Chelating affinity gel medium. Its porosity is 73...
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