1-Methyl-2(3-pyridyl)pyridine
Nicotine is a highly toxic substance. A few milligrams of nicotine can cause severe poisoning such as headache, vomiting, and confusion. Phenomenon, 40mg can be fatal if taken orally or inhaled.
2. Extraction
2.1 Extraction methods can be mainly divided into: solvent extraction method, steam distillation method
This experiment mainly adopts solvent extraction method, based on alkali extraction method The principle of acid precipitation extracts nicotine from tobacco. Various extraction agents were used in the experiment: diethyl ether, carbon tetrachloride and chloroform.
2.2 Process flow of nicotine extraction
2.2.1 Materials
Tobacco leaves (Alpinia nicotine, nicotine content 1.4mg)
2.2.2 Instruments and some medicines
2.2.2.1 Instruments:
Electric constant temperature water bath (37~100℃, water temperature fluctuation 1℃, power 1000w, voltage 220v, Shanghai Medical Equipment Factory 5) TN-1008 pallet torque balance (MAX=100g, e=d=10mg, Shanghai Second Balance Instrument Factory)
Electronic balance (MAX=210, d=0.1mg, BS210S), beaker , filter device, separatory funnel (60ml, 4 pieces), gauze
2.2.2.2 Drugs:
Sodium hydroxide (chemically pure) (Danyang Chemical Reagent Factory)
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Chloroform (Yilin Chemical)
Ether (Shanghai Yanchen Chemical Industry Co., Ltd.)
Carbon tetrachloride (Yixing Second Chemical Reagent Factory)
Acetic acid (Shanghai Zhenxing Chemical Factory No. 1)
Methanol (Shanghai Zhenxing Chemical Factory No. 1)
Ethanol (Yixing No. 2 Chemical Reagent Factory)
2.2.3 Nicotine extraction and separation flow chart
20g cut tobacco
Stir 250ml 5NaOH solution for 15 minutes, filter under reduced pressure, drain the cut tobacco
Add 70ml water, Stir, filter, and combine the filtrate.
Solution
Extract 3 times
Water layer Extraction layer
Extraction agent residue
Add 3 ml of water to dissolve , add 9 ml of methanol, mix, filter
Insoluble matter in the filtrate
Add 25 ml of saturated acetic acid solution, filter
Precipitate mother liquor
Pump out Dry
Crude nicotine salt
Dissolve 50 (v/v) ethanol (saturated state), place, crystallize, filter
Mother liquor refined nicotine salt
2.2.4 Operation process
2.2.4.1 Leaching
Take 20g of broken tobacco leaves, add 250ml of 5 sodium hydroxide aqueous solution, stir and soak for 15 to 30 minutes. Filter the liquid. Place the filter cake in 70ml of water, mix evenly, and filter the clear liquid.
2.2.4.2 Extraction
Move the liquid into the separatory funnel, add the extraction flux at a ratio of 1:0.5 (v/v), stir and extract, set the layers carefully, and collect the organic solvent. phase solution, repeat the extraction three times, and combine the extracts into one place.
During the extraction process, use diethyl ether to extract, collect the upper extraction layer, and perform repeated extractions. Collect the lower layer when extracting with chloroform and carbon tetrachloride.
2.2.4.3 Distillation
Heat and distill in a 100°C water bath, and use a condensing device to recover the extractant to obtain the residue.
2.2.4.4 Crude
Evaporate the residue to dryness in a water bath, add 3 ml of water solvent, then add 9 ml of methanol, mix, stir and filter.
Collect the filtrate, add 25 ml of saturated acetic acid solution, filter the precipitate, and air-dry to obtain crude nicotine salt.
2.2.4.5 Refining
Dissolve the crude product in 20ml 50 (v/v) ethanol aqueous solution, heat to boiling and make the crude product just dissolved, cool naturally, leave to crystallize, and filter Crystals are the best.
2.2.5 Screening of extraction agents
First of all, after repeated experiments and comparative screening, it was found that during the extraction process, the emulsification phenomenon of diethyl ether is very serious, and the separation of the two phases is difficult. , while the emulsification phenomenon of chloroform and carbon tetrachloride is relatively small, so they are suitable as nicotine extraction agents. Secondly, during the extraction process, when diethyl ether is used as the extraction agent, the extraction layer becomes turbid and requires multiple extractions before it can be extracted cleanly. However, the extraction layer of chloroform and carbon tetrachloride is clearer, and three extractions with diethyl ether are more effective than three extractions with diethyl ether. Finally, judging from the nicotine extraction results, using chloroform as the extraction agent has the best effect. Through the screening of extraction agents, the nicotine extraction process can have high production efficiency and produce better economic benefits.
2.2.6 Extraction results
Extracting agent: diethyl ether, chloroform, carbon tetrachloride
After extraction, residue (g) 0.2682 0.2932 0.3363 0.3670 0.1898 0.2052
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The precipitate obtained after adding acetic acid (g) 0.0534 0.0593 0.0693 0.0742 0.0398 0.0423
Nicotine salt (g) 0.0008 0.0008 0.0009 0.0010 0.0006 0.0007
Yield ( ) 57.14 57.14 64.29 71.43 42.86 50
3. Conclusion
The extraction results show that different extraction agents have different effects on extracting nicotine. The yield of ether as the extraction agent is 57.14, chloroform is around 71.43, and carbon tetrachloride is 50.