Amidoxime group-containing chitosan modified adsorbent and preparation method thereof
A chitosan modification and adsorbent technology, which is applied in the field of oilfield wastewater pretreatment and heavy metal removal, can solve the problems of long adsorption time, high price, and particle sensitivity, and achieves improved adsorption capacity, fast adsorption speed, and large adsorption capacity. Effect
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Embodiment 1
[0031] Embodiment 1 The preparation of the chitosan modified adsorbent containing amidoxime group
[0032](1) Preparation of MAc-CTS / AN copolymer: In the laboratory, natural polymer chitosan was methacrylated to obtain modified chitosan (MAc-CTS), and MAc was added to No. 1 250mL three-necked flask -CTS powder 1g, concentrated hydrochloric acid 100μL, urea 0.2g, then add 25mL deionized water and stir to dissolve; then add acrylonitrile 1425μL, stir well, adjust pH=7; 2 10min, respectively add 0.3365g sodium bisulfite and 0.738g ammonium persulfate as redox initiator, and reflux at 45°C for 12h; CTS / AN copolymer, pale yellow in color.
[0033] (2) Oximation of MAc-CTS / AN copolymer: Weigh 1g of powdered MAc-CTS / AN copolymer and place it in No. 2 250mL three-necked flask; then take 1.5134g of hydroxylamine hydrochloride, add 22mL of methanol and 28mL of water to prepare solution; the solution was slowly poured into No. 2 250mL three-necked flask, and N 2 , stirred and refluxe...
Embodiment 2
[0034] Structural characterization of embodiment 2 methacryloyl modified chitosan (MAc-CTS)
[0035] The sample prepared in Example 1 was analyzed structurally by infrared spectrogram, and the structure of methacrylylated modified chitosan (MAc-CTS) was characterized by WQF-510A Fourier Transform Infrared Spectrometer by KBr tablet method. Spectrum such as figure 1 shown. The following is the analysis and attribution of the main characteristic peaks: 3506cm -1 The moderately strong single absorption peak is the stretching vibration ν of the N-H bond of the amide NH ;1661cm -1 The C=O bond stretching vibration absorption band of the associated amide (amide I band); 1565cm -1 The place is the in-plane bending vibration absorption band of the N-H bond of the solid secondary amide (amide II band); 1315cm -1 is the in-plane bending vibration δ of the O-H bond OH ;1082cm -1 and 1026cm -1 is C-O bond stretching vibration ν CO ;896cm -1 It is a ring asymmetric stretching vib...
Embodiment 3
[0036] Embodiment 3 Structural characterization of chitosan modified adsorbent containing amidoxime group
[0037] The sample prepared in Example 1 was analyzed structurally by infrared spectrum, and the MAc-CTS / AN copolymer and the MAc-CTS / AO copolymer were characterized by the WQF-510A Fourier Transform Infrared Spectrometer by using the KBr tablet method. The infrared spectrum of figure 2 shown. The following is the analysis and attribution of the main characteristic peaks: 3175cm -1 The nearby strong and broad absorption band is the OH stretching vibration frequency ν OH and the N-H stretching frequency ν of the amide NH ;2194cm -1 It is the C≡N bond stretching vibration peak, 1652cm -1 It is the C=O bond stretching vibration absorption band of the amide. Compared with the spectrum of MAc-CTS / AO copolymer after oximation, it can be seen that the stretching vibration peak of the cyano group C≡N disappears after amidoximation (ie, MAc-CTS / AO copolymer), and by compari...
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