Preparation method of photo-responding molecularly imprinted material for selectively separating and purifying cyclodextrin and derivatives of cyclodextrin
A separation, purification and molecular imprinting technology, applied in the fields of chemistry and material and molecular separation, can solve the problems of restricting the industrial production of cyclodextrin, low industrial yield and high price, and achieve excellent light response characteristics, remarkable separation effect, and use long life effect
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[0038] Example 1
[0039] (1) Aniline (15g, 162mmol), 10mL of water and 10mL of concentrated hydrochloric acid with a concentration of 12mol / L are mixed and stirred for 10min, then NaNO dissolved in 20mL of water is added dropwise 2 (12g). After stirring for 20 minutes under ice bath conditions, a phenol solution dissolved in 40 mL of 8% NaOH was added dropwise. After the addition, keep the ice bath and continue to stir for 40 minutes. After the reaction, the filter cake was filtered with suction, and the filter cake was washed with water, and then recrystallized with a mixture of ethanol and water in a volume ratio of 1:1 to obtain 4-hydroxyazobenzene as a dark orange-red product;
[0040] (2) 0.15g N,N-dimethylaminopyridine, 2.0g triethylamine and 2.0g 4-hydroxyazobenzene are dissolved in 100.0mL acetonitrile, the mixture is placed in an ice water bath, and 2.0 is slowly added dropwise. g methacrylic acid chloride and 5.0mL acetonitrile mixture, moved to 35℃ oil bath and reacte...
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[0042] Example 2
[0043] (1) Aniline (15g, 162mmol), 80mL water and 30mL concentrated hydrochloric acid with a concentration of 11mol / L are mixed and stirred for 20 minutes, then NaNO dissolved in 30mL water is added dropwise 2 (13g). After continuing to stir for 40 minutes under ice bath conditions, a phenol solution dissolved in 90 mL of 10% NaOH was added dropwise. After the addition, keep the ice bath and continue to stir for 300 min. After the reaction, the filter cake was filtered with suction, and the filter cake was washed with water, and then recrystallized with a mixture of ethanol and water in a volume ratio of 1:1 to obtain 4-hydroxyazobenzene as a dark orange-red product;
[0044] (2) 0.75g of N,N-dimethylaminopyridine, 20.0g of triethylamine and 6.0g of 4-hydroxyazobenzene are dissolved in 150.0mL of acetonitrile, the mixture is placed in an ice water bath, and 10.0 is slowly added dropwise. g methacrylic acid chloride and 10.0mL acetonitrile mixture, moved to 50℃ ...
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[0046] Example 3
[0047] (1) Aniline (15g, 162mmol), 160mL water and 50mL concentrated hydrochloric acid with a concentration of 10mol / L are mixed and stirred for 30min, then NaNO dissolved in 40mL water is added dropwise 2 (14g). After continuing to stir for 60 min under ice bath conditions, a phenol solution dissolved in 150 mL of 12% NaOH was added dropwise. After the addition, keep the ice bath and continue to stir for 600 min. After the reaction is completed, filter with suction, wash the filter cake with water, and recrystallize with a mixture of ethanol and water in a volume ratio of 1:1 to obtain 4-hydroxyazobenzene as a dark orange-red product;
[0048] (2) 1.5g of N,N-dimethylaminopyridine, 40.0g of triethylamine and 10.0g of 4-hydroxyazobenzene were dissolved in 200.0mL of acetonitrile, the mixture was placed in an ice water bath, and 20.0 was slowly added dropwise. g methacrylic acid chloride and 20.0mL acetonitrile mixed solution, moved to 60℃ oil bath and reacted f...
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