A kind of chiral polyamide membrane and its preparation method and application
A polyamide membrane and chiral technology, applied in the field of chiral separation, can solve the problems of high energy consumption, large pollution, and low efficiency of the resolution method, and achieve wide tolerance to pH, simple preparation process, and wide range of resolution objects Effect
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Embodiment 1
[0036] First, an ethylenediamine-β-cyclodextrin chiral polyamide membrane was prepared by the following steps, and then the concentration ratio of the two configurations in the filtrate filtered by the chiral membrane and the The concentration ratio of the two configurations in the stock solution was used to evaluate the resolution performance.
[0037] Synthesis of ethylenediamine-β-cyclodextrin:
[0038]The recrystallized β-cyclodextrin (100 g, 88 mmol) was weighed into a 1000 mL beaker containing 833 mL of purified water. NaOH (10.95g, 0.27mol) was dissolved in 33mL of water, and added dropwise to the above suspension within 10min under magnetic stirring conditions. After the dropwise addition was completed, the suspension became a uniform and slightly yellow solution. Weigh p-toluenesulfonyl chloride (p-TsCl, 16.82 g, 0.09 mol) and dissolve it in 50 mL of acetonitrile, and add the solution dropwise to the light yellow reaction solution containing β-cyclodextrin. A large ...
Embodiment 2
[0053] A preparation method of ethylenediamine-β-cyclodextrin, comprising the following steps:
[0054] (1) Weigh recrystallized β-cyclodextrin (90 g, 79 mmol) and add it to a 1000 mL beaker containing 800 mL of purified water, dissolve NaOH (10 g, 0.25 mol) in 30 mL of water, under magnetic stirring conditions, in be added dropwise to the above-mentioned suspension within 8min;
[0055] (2) After the β-cyclodextrin suspension becomes a clear pale yellow solution, weigh p-toluenesulfonyl chloride (p-TsCl, 16 g, 0.086 mol) and dissolve it in 45 mL of acetonitrile, and add the solution dropwise to the above-mentioned solution containing In the light yellow reaction solution of β-cyclodextrin, after 70 minutes, all the dropwise additions were completed, and a large amount of white precipitates were formed;
[0056] (3) The above reaction system was vigorously stirred at room temperature for 2h, and then used 2mol·L -1 The hydrochloric acid was adjusted to near neutral, and plac...
Embodiment 3
[0068] A preparation method of ethylenediamine-β-cyclodextrin, comprising the following steps:
[0069] (1) Weigh recrystallized β-cyclodextrin (110g, 96.8mmol) into a 1000mL beaker containing 850mL of purified water, dissolve NaOH (12g, 0.3mol) in 40mL of water, and under magnetic stirring conditions, Add dropwise to the above suspension within 11min;
[0070] (2) After the β-cyclodextrin suspension becomes a clear pale yellow solution, weigh p-toluenesulfonyl chloride (p-TsCl, 18 g, 0.096 mol) and dissolve it in 50 mL of acetonitrile, and add the solution dropwise to the above-mentioned solution containing In the light yellow reaction solution of β-cyclodextrin, after 80 minutes, it was completely added dropwise, and a large amount of white precipitates were formed;
[0071] (3) The above reaction system was vigorously stirred at room temperature for 3h, and then used 2mol·L -1 The hydrochloric acid was adjusted to near neutral, and placed in a refrigerator at 4°C overnigh...
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