Method of preparing zinc contained chelating affinity super-macro-porosity crystal gel medium for column-chromatography
A technology of crystal gel medium and column chromatography, applied in chemical instruments and methods, and other chemical processes, can solve the problem of low adsorption capacity, achieve high separation efficiency, easy large-scale production, easy elution and regeneration
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Embodiment 1
[0032] Dissolve 1.45g of AAm monomer, 0.06g of cross-linking agent MBAAm and 0.1g of AGE in 15mL of deionized water. After stirring evenly, quickly add 9mg of TEMED and 23mg of APS. In the column, after being sealed, in a programmable temperature-controlled constant temperature cooling system, the temperature is lowered from 0°C to -40°C, and then the temperature is kept constant to carry out cooling crystallization and porogenous polymerization. After 39 hours, the temperature was raised to room temperature to obtain a super-large-pore continuous bed crystal gel medium matrix.
[0033] At 20°C, use 0.2 matrix volume of 0.06M Na 2 CO 3 solution, 0.01M IDA solution with 5 times the volume of the matrix, respectively activated the obtained matrix for 24 hours, and then used 0.5M ZnSO with 2 times the volume of the matrix 4 The solution undergoes a chelation reaction to obtain Zn 2+ Chelating affinity gel medium. Its porosity is 56%, and SEM shows that its pore diameter range...
Embodiment 2
[0035] Dissolve 1.95g of DMAAm monomer, 0.5g of crosslinking agent N,N'-diacryloylethylenediamine and 0.6g of AGE and ethylene glycol diglycidyl ether (mass ratio 1:1) mixture ligand material in 50ml After stirring evenly in deionized water, quickly add 29mg TEMED and 53mg APS, put the resulting mixture into a chromatographic column with an inner diameter of 26mm and a length of 200mm, seal it, and carry out cooling and crystallization in a programmable temperature-controlled constant temperature cooling system Hole-causing. The temperature change process is: (A) cooling: from 0°C to -65°C; (B) heating: heating to -7°C; (C) constant temperature: constant temperature for 5 hours; (D) cooling: cooling from -7°C again to -20°C; (E) constant temperature: constant temperature for 16 hours; (F) temperature rise: heat up to room temperature to obtain a super-large-pore continuous bed crystal gel medium matrix.
[0036] The obtained matrix was activated with 12 times the matrix volum...
Embodiment 3
[0038] Dissolve 0.8g of DMAEMA monomer, 0.41g of cross-linking agent MBAAm and 0.4g of ligand material ethylene glycol diglycidyl ether in 11ml of deionized water. After stirring evenly, quickly add 49mg of TEMED and 45mg of APS, and put the resulting mixture into In a glass chromatography column with an inner diameter of 10mm and a length of 200mm, after sealing, the temperature is lowered to -19°C in a programmable temperature-controlled constant temperature cooling system for cooling and crystallization to form pores. Then, the crystals were melted at room temperature to obtain a super-macroporous continuous bed crystal gel medium matrix.
[0039] The obtained medium matrix was reacted with 1M NaOH solution 4 times the volume of the matrix at 50°C, then reacted with 0.8M EDT solution 3 times the volume of the matrix at 50°C for 10 h, and finally reacted with 5M ZnCl 10 times the volume of the matrix 2 Solution chelation reaction to get Zn 2+ Chelating affinity gel medium. ...
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