Preparation method and application of molecularly imprinted polymer microspheres

Abstract

The invention provides a molecularly imprinted polymer microsphere, a preparation method and application thereof. The preparation method includes: (1) preparing a hollow bulb H-PS; (2) soaking the H-PS in tetrahydrofuran, and performing washing and drying; (3) adding H-PS into a sodium dodecyl sulfate solution to obtain a solution A, at the same time adding dibutyl phthalate, toluene and azodiisobutyronitrile into another sodium dodecyl sulfate solution to obtain a solution B, and mixing the two solutions; (4) mixing nicotinamide, methacrylic acid and toluene evenly, then adding ethylene glycol dimethacrylate and a polyvinyl alcohol solution, adding the H-PS bulb emulsion obtained by step (3) into the mixed solution, and carrying out reaction; (5) adding the H-PS solution obtained by step (4) into a polyvinyl alcohol solution, introducing a protective gas continuously, conducting heating and reflux condensation in the protective gas, and performing stirring and washing on the efflux liquid; and (6) removing nicotinamide from a cleaning product obtained by step (5).

Description

technical field

[0001] The invention relates to a preparation method and application of molecularly imprinted polymer microspheres, belonging to the field of chemistry. Background technique

[0002] With the continuous improvement of people's living standards and quality of life, consumers are becoming more and more aware of smoking safety and environmental protection. The incomplete combustion of tobacco in cigarette products leads to a certain amount of harmful substances in the smoke, which poses a risk to the health of smokers. Among them, tobacco-specific nitrosamines (tobacco-specific N-nitrosamines, TSNAs) are a class of special harmful substances with carcinogenicity contained in tobacco products, and are common components in tobacco leaves, especially dried tobacco leaves and cigarette smoke. TSNAs mainly include four types, N-nitrosonornicotine (NNN), N-nitrosoannicotine (NAT), N-nitroso aneunicotine (NAB) and 4-methylnitrosamino - 1-(3-pyridyl)-1-butanone (NNK)....

Examples

Embodiment 1

[0082] Weigh 2.5ml St, 0.045g AIBN, 0.045gNaSS, dissolve in 25ml methanol / water (v / v=9 / 1) solution, mix with ultrasonic wave, mechanically stir in water bath, and continue to pass nitrogen for 20min, then raise the temperature to 75 ℃, condensed and refluxed, reacted in a nitrogen atmosphere for 3 hours, slowly added 0.5ml DVB dropwise, and kept the drop rate at 2-4 drops per minute, and then continued to react for 5 hours. After the reaction was completed, it was cleaned by ultrasonic centrifugation with methanol for 3 times, and dried in a vacuum oven at 60° C. for 12 hours to obtain a dried spherical core sample.

[0083] Dissolve the dry sample in THF according to the ratio of 1g to 20ml THF, soak for 24h to dissolve the uncrosslinked part in the PS core, then wash twice with THF and once with methanol, and dry in a vacuum oven at 60°C for 12h , to get hollow bulb H-PS.

[0084] Take 0.4g of the prepared hollow bulb H-PS, add 10g of 0.2% SDS aqueous solution and sonicate ...

Embodiment 2

[0091] Weigh 2.5ml St, 0.034g AIBN, 0.04g NaSS, dissolve in 22.5ml methanol / water (v / v=9 / 1) solution, mechanically stir in a water bath after ultrasonication, and continue to blow nitrogen for 20min, then raise the temperature to 72°C , condensed and refluxed, reacted in a nitrogen atmosphere for 3.5 hours, slowly added 0.75ml DVB dropwise, controlled the dropping rate at 5-10 drops per minute, and continued to react for 6 hours. After the reaction was completed, it was cleaned by ultrasonic centrifugation with methanol three times, and dried in a vacuum oven at 55° C. for 14 hours.

[0092] Dissolve the dry sample in THF according to the ratio of 1g to 25ml THF, soak for 24h to dissolve the uncrosslinked part in the PS core, then wash twice with THF and once with methanol, and dry in a vacuum oven at 55°C for 14h , to get hollow bulb H-PS.

[0093] Take 0.4g of the prepared hollow bulb H-PS, add 12g of 0.2% SDS solution for ultrasonication, make H-PS and SDS aqueous solution...

Embodiment 3

[0100] Weigh 2.5ml St, 0.056g AIBN, 0.056g NaSS, dissolve in 30ml methanol / water (v / v=9 / 1) solution, mechanically stir in a water bath after ultrasonication, and continue argon for 30min, then heat up to 75°C , condensed and refluxed, reacted in an argon atmosphere for 3 hours, slowly added 0.6ml DVB dropwise, and kept the dropping rate at 2-4 drops per minute, and then continued to react for 5 hours. After the reaction was completed, it was cleaned by ultrasonic centrifugation with methanol for 3 times, and dried in a vacuum oven at 65° C. for 10 h.

[0101]Dissolve the dry sample in THF according to the ratio of 1g to 30ml THF, soak for 20h to dissolve the uncrosslinked part in the PS core, then wash twice with THF and once with methanol, and dry in a vacuum oven at 65°C for 10h , to get hollow bulb H-PS.

[0102] Take 0.4g of the prepared hollow bulb H-PS, add 15g of 0.3% SDS solution for ultrasonication, make H-PS and SDS aqueous solution form a uniform emulsion, and add ...

technical field

[0001] The invention relates to a preparation method and application of molecularly imprinted polymer microspheres, belonging to the field of chemistry. Background technique

[0002] With the continuous improvement of people's living standards and quality of life, consumers are becoming more and more aware of smoking safety and environmental protection. The incomplete combustion of tobacco in cigarette products leads to a certain amount of harmful substances in the smoke, which poses a risk to the health of smokers. Among them, tobacco-specific nitrosamines (tobacco-specific N-nitrosamines, TSNAs) are a class of special harmful substances with carcinogenicity contained in tobacco products, and are common components in tobacco leaves, especially dried tobacco leaves and cigarette smoke. TSNAs mainly include four types, N-nitrosonornicotine (NNN), N-nitrosoannicotine (NAT), N-nitroso aneunicotine (NAB) and 4-methylnitrosamino - 1-(3-pyridyl)-1-butanone (NNK)....

Examples

Embodiment 1

[0082] Weigh 2.5ml St, 0.045g AIBN, 0.045gNaSS, dissolve in 25ml methanol / water (v / v=9 / 1) solution, mix with ultrasonic wave, mechanically stir in water bath, and continue to pass nitrogen for 20min, then raise the temperature to 75 ℃, condensed and refluxed, reacted in a nitrogen atmosphere for 3 hours, slowly added 0.5ml DVB dropwise, and kept the drop rate at 2-4 drops per minute, and then continued to react for 5 hours. After the reaction was completed, it was cleaned by ultrasonic centrifugation with methanol for 3 times, and dried in a vacuum oven at 60° C. for 12 hours to obtain a dried spherical core sample.

[0083] Dissolve the dry sample in THF according to the ratio of 1g to 20ml THF, soak for 24h to dissolve the uncrosslinked part in the PS core, then wash twice with THF and once with methanol, and dry in a vacuum oven at 60°C for 12h , to get hollow bulb H-PS.

[0084] Take 0.4g of the prepared hollow bulb H-PS, add 10g of 0.2% SDS aqueous solution and sonicate ...

Embodiment 2

[0091] Weigh 2.5ml St, 0.034g AIBN, 0.04g NaSS, dissolve in 22.5ml methanol / water (v / v=9 / 1) solution, mechanically stir in a water bath after ultrasonication, and continue to blow nitrogen for 20min, then raise the temperature to 72°C , condensed and refluxed, reacted in a nitrogen atmosphere for 3.5 hours, slowly added 0.75ml DVB dropwise, controlled the dropping rate at 5-10 drops per minute, and continued to react for 6 hours. After the reaction was completed, it was cleaned by ultrasonic centrifugation with methanol three times, and dried in a vacuum oven at 55° C. for 14 hours.

[0092] Dissolve the dry sample in THF according to the ratio of 1g to 25ml THF, soak for 24h to dissolve the uncrosslinked part in the PS core, then wash twice with THF and once with methanol, and dry in a vacuum oven at 55°C for 14h , to get hollow bulb H-PS.

[0093] Take 0.4g of the prepared hollow bulb H-PS, add 12g of 0.2% SDS solution for ultrasonication, make H-PS and SDS aqueous solution...

Embodiment 3

[0100] Weigh 2.5ml St, 0.056g AIBN, 0.056g NaSS, dissolve in 30ml methanol / water (v / v=9 / 1) solution, mechanically stir in a water bath after ultrasonication, and continue argon for 30min, then heat up to 75°C , condensed and refluxed, reacted in an argon atmosphere for 3 hours, slowly added 0.6ml DVB dropwise, and kept the dropping rate at 2-4 drops per minute, and then continued to react for 5 hours. After the reaction was completed, it was cleaned by ultrasonic centrifugation with methanol for 3 times, and dried in a vacuum oven at 65° C. for 10 h.

[0101]Dissolve the dry sample in THF according to the ratio of 1g to 30ml THF, soak for 20h to dissolve the uncrosslinked part in the PS core, then wash twice with THF and once with methanol, and dry in a vacuum oven at 65°C for 10h , to get hollow bulb H-PS.

[0102] Take 0.4g of the prepared hollow bulb H-PS, add 15g of 0.3% SDS solution for ultrasonication, make H-PS and SDS aqueous solution form a uniform emulsion, and add ...

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