Amidoxime group-containing modified silica gel adsorbent and preparation method thereof
A silica gel adsorption and modification technology, applied in chemical instruments and methods, adsorbed water/sewage treatment, other chemical processes, etc., can solve problems such as difficult separation, insufficient specific surface area, secondary pollution, etc. The effect of good regeneration performance and improved adsorption performance
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[0030] combine figure 1 , a kind of preparation method containing the modified silica gel adsorbent of amidoxime group that the present invention proposes, it is characterized in that comprising the following steps:
[0031] Step 1, activation: put 30g of 100-200 mesh column chromatography silica gel in 150mL of 5% methanesulfonic acid solution, reflux at 90°C and keep stirring for 4 hours. After the reaction is completed, rinse with distilled water repeatedly Until the washing liquid is neutral, dry it under vacuum at 50°C for 24 hours;
[0032] Step 2, impregnation: add 10g of the activated silica gel obtained in step 1 to 400mL of KH580 in toluene solution, where the volume concentration of KH580 is 2%, condense and reflux at 90°C and keep stirring for 24 hours, filter to get coarse particles, and then use Extract with toluene in a Soxhlet extractor for 24 hours to remove unreacted KH580 on the surface of silica gel to obtain impregnated particles;
[0033] Step 3, dryin...
Embodiment 1
[0038] Step 1, activation: put 30g of 100-200 mesh column chromatography silica gel in 150mL of 5% methanesulfonic acid solution, reflux at 90°C and keep stirring for 4 hours. After the reaction is completed, rinse with distilled water repeatedly Until the washing liquid is neutral, dry it under vacuum at 50°C for 24 hours;
[0039]Step 2, impregnation: Add 10g of the activated silica gel obtained in Step 1 to 400mL of toluene solution with a volume concentration of 2% KH580, condense and reflux at 90°C and continue stirring for 24 hours, filter to obtain coarse particles, and then use toluene as an extract The agent was extracted in a Soxhlet extractor for 24 hours to remove unreacted KH580 on the surface of the silica gel to obtain impregnated particles;
[0040] Step 3, drying: vacuum-dry the impregnated granules obtained in Step 2 at 50° C. for 24 hours to obtain dry granules;
[0041] Step four, modification:
[0042] (1) Add 5 g of the dried granules obtained in Step 3...
Embodiment 2
[0045] Repeat steps one to three in Example 1
[0046] Step four, modification:
[0047] (1) Add 5g of the dried granules obtained in step 3 into 100mL of acrylonitrile in N,N-dimethylformamide solution, where the volume concentration of acrylonitrile is 15%, and then blow nitrogen into it to remove the air in the bottle, Then add 0.1g initiator azobisisobutyronitrile, condense and reflux at 75°C and continue to stir for 5 hours. After the reaction, filter to obtain primary modified particles. Use N,N-dimethylformamide as extractant in Soxhlet Extract in the extractor for 24 hours to remove unreacted acrylonitrile on the surface of the silica gel to obtain impregnated primary modified particles, and vacuum dry at 50°C for 24 hours to obtain dried primary modified particles;
[0048] (2) Mix 20mL of hydroxylamine hydrochloride solution with a concentration of 1mol / L and 20mL of sodium carbonate solution with a concentration of 1mol / L, then add 1g of the modified particles obta...
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