Polyphenol modified chitosan adsorbent, preparation method thereof and application of polyphenol modified chitosan adsorbent to germanium recovery
A chitosan and adsorbent technology is applied to a polyphenol-modified chitosan adsorbent, a preparation method thereof, and an application field in germanium recovery, and achieves the effects of simple and fast synthesis process, safe synthesis process and low price
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Embodiment 1
[0033] The preparation of embodiment 1 polyphenol modified chitosan adsorbent
[0034] (1) Preparation of 2,3,4-trihydroxybenzaldehyde modified chitosan adsorbent THB-CS
[0035] 1. Preparation of chitin: After cleaning and drying the crab shell, weigh 5g, add 75mL of 2%-6% hydrochloric acid solution to soak, and keep stirring to dissolve the inorganic salt in the shell and soften it. After soaking for 10-15 hours , to remove inorganic salts. Then wash the crab shells until neutral, add 75mL of 8% to 10% sodium hydroxide solution, and heat to 90°C for 4h. Wash the crab shells after alkali treatment to neutrality, add 50mL of 1% KMnO 4 and NaHSO 3 The solution was rinsed separately, washed and dried to obtain a white solid, chitin.
[0036] 2. Preparation of chitosan: Take 5 g of dry chitin, add 50 mL of 40% to 50% sodium hydroxide solution, and react at 100° C. for 7 h. Finally, a white chitosan solid was obtained, abbreviated as CS.
[0037] 3. Weigh 0.25g 2,3,4-trihydr...
Embodiment 2
[0049] The adsorption effect of embodiment 2 polyphenol modified chitosan to germanium under different acidity
[0050] Get 10mg of polyphenol modified chitosan THB-CS, HBD-CS, PTD-CS prepared in Example 1 and add pH 1~6, 20mg L -1 germanium solution, and then put it into a shaking box with a rotating speed of 180r / min and a temperature of 303K for 24h, filter, take the filtrate and stock solution to measure its concentration, and calculate the adsorption rate. The result is as Figure 4 shown.
[0051] Depend on Figure 4 It can be seen that the adsorption performance of chitosan adsorbent THB-CS modified by 2,3,4 trihydroxybenzaldehyde is significantly higher than that modified by 3,4-dihydroxybenzaldehyde and 4-hydroxybenzaldehyde. The adsorbents HBD-CS and PTD-CS, because the number of phenolic hydroxyl groups in THB-CS is relatively large, and the structure is in the ortho position, so it is easier to form complexes with Ge(IV), although the ortho-diphenol structure T...
Embodiment 3
[0054] Example 3 Polyphenol-modified chitosan adsorbent to the separation effect of germanium in the presence of other rare earth ions
[0055] Weigh 10mg 2,3,4-trihydroxybenzaldehyde modified chitosan adsorbent THB-CS, add 10mL concentration to 20mg L -1 Ge(IV), Mn(II), Zn(II), Ni(II), Pb(II), As(III), Co(II), Fe(III) solution, the pH of the solution is 0~9, in Shake in a shaking box at 30°C and 180r / min for 24h.
[0056] The result is as Figure 6 , in the presence of other impurity ions, the adsorption rate of THB-CS adsorbent to Ge(IV) in the range of pH = 1-3 is above 80%. It can be seen that the pH is in the range of 0-2, and As(III ), Ni(II), Zn(II), and Mn(II) have very low adsorption rates, and in the range of pH 1 to 9, the adsorption rates for arsenic are very low, which shows that THB-CS adsorbent can work in many In the presence of such ions, it can selectively adsorb germanium ions.
[0057] In order to verify the practical applicability of THB-CS. Select th...
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