Preparation of water-soluble crosslinked chitosan and application thereof
A cross-linked chitosan, water-soluble technology, applied in other chemical processes, flocculation/sedimentation water/sewage treatment, anti-toxic agents, etc., can solve the problems of chitosan's easy dissolution and loss, unfavorable recovery of heavy metal ions, etc.
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Embodiment 1
[0032] The preparation of embodiment 1 copper ion template glyoxal cross-linked chitosan resin
[0033] Weigh 10 g of chitosan and suspend in 75 ml of 10% CuSO 4 Stir in the middle for 2h, soak overnight, filter to remove the solution, wash with water until NaS 2 method (5gNaS 2 Dissolved in 20ml distilled water) No Cu can be detected 2+ After pressing dry, suspend it in 60ml of water, add 3.75ml of 50% glyoxal, stir at room temperature for 3h to make it cross-linked, filter off the liquid, and wash the solid with ethanol and ether once respectively. Then use 0.1mol / l hydrochloric acid solution to dissolve Cu 2+ Elution, then washed with water to neutral, eluent with NaS 2 Can not detect Cu 2+ After that, wash with ethanol and ether once respectively.
[0034] The synthesis of embodiment 2 glutaraldehyde cross-linked chitosan
[0035] Synthetic process is the same as embodiment 1, replaces glyoxal and CuSO with glutaraldehyde 4 The complexed chitosan was reacted to obt...
Embodiment 3
[0036] The hydrogenation of embodiment 3 cross-linked chitosan
[0037]Take 10g of cross-linked chitosan and add 150ml of 1% acetic acid solution, adjust the pH to 4 with 0.1mol / l NaOH solution, weigh 5g of NaBH 4 Dissolve in 50ml of water, slowly add to the acetic acid solution of cross-linked chitosan, bubbling, react for 3 hours after adding, adjust the pH to 10 with 0.1mol / l NaOH solution, filter and dry in the air.
Embodiment 4
[0038] Synthesis of embodiment 4 water-soluble cross-linked chitosan
[0039] Get 12g crosslinked chitosan and pack in 1L three-neck flask, add 200ml w(H 2 o 2 ) = 6% aqueous hydrogen peroxide solution, stirred and reacted in a water bath at 60°C for 1 h, filtered under reduced pressure while heating, added 3 times the volume of 95% ethanol to the filtrate, stood for 12 h and suction filtered to obtain a light yellow solid, washed with 20 ml of absolute ethanol, and dried 4.6 g of the product was obtained, and the molecular weight measured by the viscosity method was 1500-2500.
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