CN1102647A - Nicotine and its salt prepn. - Google Patents
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- CN1102647A CN1102647A CN 94110582 CN94110582A CN1102647A CN 1102647 A CN1102647 A CN 1102647A CN 94110582 CN94110582 CN 94110582 CN 94110582 A CN94110582 A CN 94110582A CN 1102647 A CN1102647 A CN 1102647A
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Abstract
The process for preparing nicotine and its salt includes leaching with dynamic counter-flowing water, acidic adsorption of leaching liquid with ion exchange resin, alkaline eduction, eluviation adsorption with organic solid solvent and counter-eluviation of organic solid solven with acidic solution and features short leaching period, the nicotine extraction rate>95%, eluviation rate>95%, less pollution, high quality of product.
Description
The present invention relates to the alkaloid preparation field, particularly comprise crumbled tobacco, offal water extraction, the water extract is through organic solvent extraction, again with the nicotine of steps such as acids salify and the preparation method of salt thereof.
Nicotine (Nicotine) is a kind of main alkaloid in the tobacco, mainly is used as the raw material of additive, agricultural insecticide and the medicine industry of tobacco industry.
Traditional preparation method is that tobacco is flooded with diluted acid, with alkali neutralization, and vapor distillation then, and with oxalic acid treatment, row alkalization and getting again.
Though, retrieve some in recent years and improve report, but still many deficiencies are arranged, for example:
US 4,967, and 771, CN 1,032,165A, CN 1,039,025A, CN 1,064,680, CN 88 1 05700A etc., the water extraction operation is no matter be ordinary water, sour water or alkaline water all are " immersion " formulas, thereby the cycle is long, even reaching 72h, the low water extract of extraction yield often need concentrate the organic solvent extraction operation, substantially be still routine " liquid-liquid extraction " pattern, be subjected to the restriction percentage extraction of partition curve not high, below 70%, emulsification, dissolving and volatilization cause solvent loss and pollution, the many power consumptions of solvent treatment amount are big, and drawbacks such as the low-cost raising of the rate of recovery are inevitable.
US 4,506,682 earlier with organic solvent to the elementary extraction of tobacco row, boil off solvent and elementary extract is adsorbed in some carrier, the carbonic acid gas of using criticality again is to its row reextraction, not only the drawback of solvent method still exists, and the technology of the critical extraction of carbonic acid gas and equipment have improved cost again.
CN 1,050, and 540 A have proposed dry distillation, consumes the tobacco leaf that a large amount of energy remove to handle low levels, and wasting energy is its fatal weakness.
The industrializing implementation of above-mentioned technology all has certain difficulty, so limited the scale operation of natural nicotine and salt thereof.
Purpose of the present invention will overcome the deficiencies in the prior art exactly, and it is short to design a kind of process cycle, and it is few to consume solvent, and reduce and pollute, save energy, cost is low and continuous high-efficient, has the preparation method of the nicotine and the salt thereof of industrialization meaning.
The objective of the invention is to realize by following scheme:
Design a kind of crumbled tobacco, offal water extraction of mainly comprising, the water extract with the nicotine of steps such as acids salify and the preparation method of salt thereof, is characterized in that through organic solvent extraction again:
1. the water extraction step is a dynamic countercurrent subsequent leaching technology,
2. the water extract is through the acid absorption-alkaline wash-out of ion exchange resin,
3. alkaline eluant drenches the collection absorbing process through the solid phase organic solvent,
4. acidic solution is to the anti-collection salify that drenches of solid phase organic solvent.
The above-mentioned nicotine and the preparation method of salt thereof, it is characterized in that described water extraction step is a dynamic countercurrent subsequent leaching technology, be meant in leacher, water used in solvent goes downstream, crumbled tobacco, offal are sailed against the current, the solid-liquid weight ratio is 1: 2～5,20～60 ℃ of leaching temperatures, and tobacco leaf, offal are 0.5～2.5h by the leacher time.
The above-mentioned nicotine and the preparation method of salt thereof, it is characterized in that described water extract is through the acid absorption-alkaline wash-out of ion exchange resin, be meant the clean water extract of filter in PH3～6 by strong acid type vinylbenzene-second diene benzene series row cationic exchange resin adsorption, get nicotine solution with 4～15% alkaline solution wash-out again.
The above-mentioned nicotine and the preparation method of salt thereof, it is characterized in that described alkaline eluant drenches the collection absorbing process through the solid phase organic solvent, be meant that alkaline eluant drenches collection post or thermopnore through vinylbenzene-second diene benzene series row or an Aluminosilicates polymer support particulate that is comprising organic solvent, nicotine is adsorbed by the organic solvent in the solid phase carrier particulate.
The above-mentioned nicotine and the preparation method of salt thereof is characterized in that described acidic solution to the anti-collection salify that drenches of solid phase organic solvent, are meant that the acid solution with 0.3～2N gets nicotine salt by solid phase organic solvent post or the anti-collection of drenching of thermopnore.
The above-mentioned nicotine and the preparation method of salt thereof is characterized in that described 4～15% alkaline solutions that the strongly acidic cation-exchange wash-out is used, and can be the aqueous solution of sodium hydroxide, potassium hydroxide, ammonium hydroxide, yellow soda ash or sodium bicarbonate.
The above-mentioned nicotine and the preparation method of salt thereof is characterized in that the organic solvent that comprises in the described solid phase organic solvent can be halogenated alkane, haloolefin or solvent oil.
The above-mentioned nicotine and the preparation method of salt thereof, it is characterized in that describedly to the anti-acid solution that drenches 0.3～2N of using of collection salify of solid phase organic solvent, can be organic acid or mineral acids such as sulfuric acid, nitric acid, hydrochloric acid or phosphoric acid such as oxalic acid, citric acid, tartrate, phenylformic acid, toluylic acid or picric acid.
Technology provided by the invention, be applicable to preparation nicotine and salt thereof from useless, hypo-tobacco leaf, offal, by a leacher inclination, that be with warming apparatus, helix agitator, water used in solvent goes downstream, the helical ribbon agitator that crumbled tobacco, offal are rotated at a slow speed promotes to sail against the current, and the weight ratio of tobacco leaf, offal and water is 1: 2～5, and is few more than the prior art water, 20～60 ℃ of leaching temperatures, tobacco leaf, stalk are 0.5～2.5h by the time of leacher.
Crumbled tobacco, offal after flooding are discharged by slag notch, the water extract filters, filter clean water extract in PH3～6 by the absorption of strong acid type vinylbenzene-second diene benzene series row cation exchange resin column, get nicotine solution with 4～15% sodium hydroxide, potassium hydroxide, ammonium hydroxide, yellow soda ash or sodium bicarbonate aqueous solution wash-out again.Ion exchange ratio is 100%, alkaline eluting rate 95%.
Subsequently, nicotine solution drenches collection post or thermopnore through vinylbenzene-second diene benzene series row or an Aluminosilicates polymer support particulate that is comprising halogenated alkane, haloolefin or solvent wet goods organic solvent, and nicotine is adsorbed by solid phase organic solvent particulate.Drench the collection yield more than 95%.
Mineral acid or organic acid soln with 0.3～2N gets nicotine salt solution by solid phase organic solvent post or the anti-collection of drenching of thermopnore again.The anti-collection yield of drenching also reaches more than 95%, and the nicotine salt concentration that obtains is about 5～10%, can get 〉=40% nicotine salt through vacuum-evaporation, and quality product is content 〉=40%, PH5～6, and the dark brown liquid of outward appearance meets general international standard.
Advantage of the present invention is:
1. after adopting dynamic countercurrent subsequent leaching technology, shortened the cycle of water extraction, 12～72h by prior art shortens to 0.5～2.5h, and efficient improves 24～28 times; Consume the few vat liquor concentration ratio prior art of the water yield and improve several times, the treatment capacity of vat liquor only is 20～30% of a prior art.
2. the water extract is handled through ion exchange method, the organic impurity of non-ionic type as sugar, resin, cured etc., is at first separated from the water extract, avoided drenching the emulsification of collection, the nicotine extraction yield of ion-exchange resin is up to more than 95%, and this is that prior art is incomparable.
3. alkaline eluant adopts the solid phase organic solvent to drench the collection absorbing process, because being solia particle, solvent contains, not volatile, the loss of solvent, avoided in the conventional liquid-liquid extraction process, dissolution with solvents and volatilization cause solvent loss and pollution, the many power consumptions of solvent treatment amount are big, drawbacks such as the low-cost raising of the rate of recovery; Micronized solid phase solvent has increased the contact area of solvent with the liquid that come together simultaneously; And the ion exchange resin elutriant removed the organic impurity in the water extract substantially, and nicotinic density is higher, by 0.5～1% of routine, brings up to 2～4%.Therefore drench collection and very easily carry out, no emulsification phenomenon is drenched the collection yield up to more than 95%.
4. in sum, technology of the present invention, the water extraction cycle shortens greatly, and overall power consumption is few, and pollution-free, product yield high quality is good.Compared with the prior art, same investment and production site, output can improve more than five times, and cost reduces by 30～40%, is an operational path with industrial value.
Facts have proved that the present invention has reached the goal of the invention of expection, economy, society and obvious environment benefit satisfactorily.
Below in conjunction with drawings and Examples the utility model is further elaborated:
Fig. 1 is a process flow diagram of the present invention;
Fig. 2 is a water leacher structural representation of the present invention.
Among the figure, (1) is the tobacco input port; (2) be flow inlet; (3) be the outlet of water extract; (4) be useless scarp relief outlet; (5) be the steam-in; (6) be the exhaust steam outlet; (7) be water leacher body; (8) be chuck; (9) be helix agitator.
[embodiment one] is the broken tobacco of water extraction, offal 1.: water=1: 5
Drop into broken tobacco, offal 500g(nicotine content 3.5%), water 2500ml, extract in 20 ℃ of continuous leachers of dynamic countercurrent, the control stirring velocity, making the tobacco cycle of operation therein is 2.5h ± 10min, carry complete, water extract filter cleaner gets brown clear liquid 2500ml, measures through the silicotungstic acid precipitator method, nicotine content 0.6755%, water are put forward rate 96.5%.
2. the acid absorption-alkaline wash-out of ion exchange resin
Water extract after the last step filter, transfer to PH3～4 with sulfuric acid, make by strong acid type vinylbenzene-second diene benzene series row cation exchange resin column absorption, resin model 001 * 4 stops when nicotine reaches 5.5g when resin absorbs, with 5%KOH liquid wash-out, get nicotine solution 200ml, the same method detection level is 2.66%, ion exchange ratio 100%, eluting rate 96.8%.
3. solid phase organic solvent post drenches collection absorption
Last step nicotine solution, the vinylbenzene through comprising trichloroethane-second diene benzene series row polymeric solid phase solvent carrier particulate drench the collection post and drench collection absorption, drench collection adsorption rate 98.5%.
4. the anti-collection salify that drenches of acidic solution
With the capable anti-collection of drenching of 0.8N oxalic acid, get the nicotine oxalate solution 85.8g of content 7.5%, the anti-collection rate 96.03% of drenching is in nicotine scale in the water extract, yield 91.56%.The little yellow liquid of outward appearance gets oxalic acid nicotinic liquid 15.61g through vacuum concentration, and the silicotungstic acid precipitator method are measured content 41.2%, outward appearance reddish dark brown liquid.
[embodiment two] broken tobacco, offal: water=1: 4
Broken tobacco, offal 500g(content are the same), water 2000ml, extract in 50 ℃ of continuous leachers of dynamic countercurrent, making the tobacco cycle of operation therein is 1.5h ± 10min, all the other get the nicotine oxalate solution 89.9g of content 7.2%, the anti-collection rate 95.7% of drenching at last all with embodiment one, in nicotine scale in the water extract, yield 92.10%.The little yellow liquid of outward appearance.
[embodiment three] broken tobacco, offal: water=1: 5
Wherein nicotine content is the same for broken tobacco, offal 500g(), water 2500ml, extract in 60 ℃ of continuous leachers of dynamic countercurrent, making the tobacco cycle of operation therein is 0.5h ± 5min, water extract after the last step filter, transfer to PH4～6 with sulfuric acid, make by strong acid type vinylbenzene-second diene benzene series row cation exchange resin column absorption, resin model 001 * 1 stops when nicotine reaches 5.5g when resin absorbs, with 15%KOH liquid wash-out, get nicotine solution 150ml, the same method detection level is 3.45%, ion exchange ratio 100%, eluting rate 96%.With solid support material is the trichloromethane solid phase solvent particulate pouring collection post absorption of silico-aluminate base polymer, the anti-collection of drenching of 1N oxalic acid, and all the other are all with embodiment one, get the nicotine oxalate solution 90g of content 7.3% at last, the anti-collection rate 95.8% of drenching is in nicotine scale in the water extract, yield 92.2%.Get oxalic acid nicotinic liquid 15.61g through vacuum concentration, the silicotungstic acid precipitator method are measured content 41.2%, outward appearance reddish dark brown liquid.
[embodiment four] broken tobacco, offal: water=1: 2, nicotine content is the same in the tobacco.
Broken tobacco, offal 500g, water 1000ml, extract in 60 ℃ of continuous leachers of dynamic countercurrent, making the tobacco cycle of operation therein is 2.0h ± 5min, water extract after the last step filter, transfer to PH4～6 with sulfuric acid, make by strong acid type vinylbenzene-second diene benzene series row cation exchange resin column absorption, resin model 001 * 7, with 8%NaOH liquid wash-out, with solid support material is the chlorobutane solid phase solvent particulate pouring collection post absorption of silico-aluminate base polymer, the anti-collection of drenching of 2N oxalic acid, and all the other are all with embodiment one, get the nicotine oxalate solution 85.1g of content 7.5% at last, in nicotine scale in the water extract, yield 90.82%, the little yellow liquid of outward appearance.
[embodiment five] broken tobacco, offal: water=1: 2.5, nicotine content is the same in the tobacco.
Extract in 40 ℃ of continuous leachers of dynamic countercurrent, the tobacco cycle of operation is 2.0h ± 5min, and all the other get the oxalic acid nicotine solution 88.0g of content 7.4% at last all with embodiment one, in nicotine scale in the water extract, and yield 92.66%, the little yellow liquid of outward appearance.
[embodiment six] broken tobacco, offal: water=1: 2.5,40 ℃ of dynamic countercurrents leach 2.0h ± 10min continuously, ion exchange column 5%NaOH wash-out, all the other are all with embodiment one, get the oxalic acid nicotine solution 95.5g of content 6.8% at last, in nicotine scale in the water extract, yield 92.40%, the little yellow liquid of outward appearance.
[embodiment seven] broken tobacco, offal: water=1: 5,20 ℃ of continuous leaching cycles of dynamic countercurrent are 2.5h ± 5min, water extract after the last step filter, transfer to PH4～6 with sulfuric acid, make by strong acid type vinylbenzene-second diene benzene series row cation exchange resin column absorption, resin model 002 * 7, with 5%KOH liquid wash-out, be the trieline solid phase solvent streams movable bed pouring collection absorption of vinylbenzene-second diene benzene series row polymer particles with carrier, the anti-collection of drenching of 0.8N oxalic acid, all the other are all with embodiment one, get oxalic acid nicotine solution 104.6g at last, content 6.2% is in nicotine scale in the water extract, yield 92.6%, the little yellow liquid of outward appearance.
[embodiment eight] broken tobacco, offal: water=1: 5,20 ℃ of dynamic countercurrents extract 2.5h ± 5min continuously, Zeo-karb model 001 * 4, with 5%KOH liquid wash-out, vinylidene chloride solid phase solvent particulate drenches collection absorption, the anti-collection of drenching of 0.8N oxalic acid, all the other are all with embodiment one, get nicotine oxalate solution 111g at last, content 5.8% is in nicotine scale in the water extract, yield 91.60%, the little yellow liquid of outward appearance.
[embodiment nine] broken tobacco, offal: water=1: 4,50 ℃ of dynamic countercurrents extract 1.5h ± 5min continuously, adopt tri chloropropene solid phase solvent post to drench collection, all the other get oxalic acid nicotine 116.8g at last with embodiment two, content 5.6% is in nicotine scale in the water extract, yield 93.10%.The little yellow liquid of outward appearance.
[embodiment ten] broken tobacco, offal: water=1: 2.5,40 ℃ of dynamic countercurrents extract 2.0h ± 10min continuously, and ion exchange column 5%NaOH wash-out adopts 200
#Solvent oil solid phase organic solvent particulate drenches collection, and all the other get nicotine oxalate solution 110.1g at last all with embodiment one, and content 5.9% is in nicotine scale in the water extract, yield 92.40%.
[embodiment 11] broken tobacco, offal: water=1: 5,20 ℃ of dynamic countercurrents extract 2.5h ± 5min continuously, resin model 002 * 7,5%KOH liquid wash-out, 140
#Solvent oil solid phase organic solvent particulate drenches collection, the anti-collection of drenching of 0.8N oxalic acid, and all the other get nicotine oxalate solution 105g at last all with embodiment one, and content 6.1% is in nicotine scale in the water extract, yield 91.1%.
[embodiment 12] tobacco: water=1: 5,20 ℃ of dynamic countercurrent continuous extraction 2.5h ± 5min, resin model 001 * 1 is with 5%KOH liquid wash-out, 120
#Solvent oil solid phase organic solvent drenches collection absorption, the anti-collection of drenching of 1N oxalic acid, and all the other get nicotine oxalate solution 106g, in nicotine scale in the water extract, yield 92.0% at last all with embodiment one.
[embodiment 13] broken tobacco, offal: water=1: 5,20 ℃ of dynamic countercurrent continuous extraction 2.5h ± 5min, 001 * 4 ion exchange column, 4% yellow soda ash wash-out, tri chloropropene solid phase solvent post drenches collection, 0.8N the anti-collection of drenching of tartrate, all the other get nicotine tartrate 121.5g, content 6.1% at last all with embodiment one, in nicotine scale in the water extract, yield 92.10%.
[embodiment 14] broken tobacco, offal: water=1: 4,50 ℃ of dynamic countercurrent continuous extraction 1.5h ± 10min, resin model 003 * 7,8%NH
4The OH wash-out, the anti-collection of drenching of 1N tartrate, all the other get nicotine tartrate 117g at last all with embodiment two, and content 6.5% is in nicotine scale in the water extract, yield 94.50%.
[embodiment 15] broken tobacco, offal: water=1: 5,60 ℃ of dynamic countercurrent continuous extraction 0.5h ± 5min, resin model 001 * 1,15%KOH liquid wash-out, trichloromethane solid phase solvent post drench collection absorption, 1.5N the anti-collection of drenching of tartrate, all the other get nicotine tartrate 117g, content 6.5% at last all with embodiment three, in nicotine scale in the water extract, yield 94.5%.
[embodiment 16] tobacco: water=1: 2,60 ℃ of dynamic countercurrent continuous extraction 2h ± 5min, resin model D61 uses 5%Na
2CO
3Liquid wash-out, chlorobutane solid phase solvent drench collection absorption, the anti-collection of drenching of 2N tartrate, and all the other get nicotine tartrate solution 122g at last all with embodiment four, and content 6.1% is in nicotine scale in the water extract, yield 92.50%.
[embodiment 17] tobacco: water=1: 5,20 ℃ of dynamic countercurrent continuous extraction 2.5h ± 5min, resin model 001 * 1, adopt trichloroethane solid phase solvent post to drench collection, the anti-collection of drenching of 1N citric acid, all the other are with embodiment one, get nicotine citric acid solution 104g at last, content 7.0% is in nicotine scale in the water extract, yield 94.88%.
[embodiment 18] tobacco: water=1: 5,20 ℃ of dynamic countercurrent continuous extraction 2.5h ± 5min, ion exchange column 5%KOH wash-out, 0.5N the anti-collection of drenching of citric acid, all the other get nicotine citrate solution 118g, content 6.1% at last all with embodiment eight, in nicotine scale in the water extract, yield 93.80%.
[embodiment 19] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 0.8N sulfuric acid, all the other dosages, processing condition, process get 6.8% nicotine sulfate 105.1g, yield 95.4% with embodiment six.
[embodiment 20] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 1N sulfuric acid, all the other dosages, processing condition, process get 6.8% nicotine sulfate 98.1g, yield 93.12% with embodiment seven.
[embodiment 21] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 1N phosphoric acid, all the other dosages, processing condition, process get 6.8% phosphoric acid nicotine 93.6g, yield 96.3% with embodiment eight.
[embodiment 22] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 0.3N nitric acid, all the other dosages, processing condition, process get 4.1% nitric acid nicotine 165.6g, yield 88.9% with embodiment nine.
[embodiment 23] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 0.5N hydrochloric acid, all the other dosages, processing condition, process get 5.1% nicotine hydrochloride 118g, yield 89.3% with embodiment ten.
[embodiment 24] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 1N hydrochloric acid, all the other dosages, processing condition, process get 6.3% nicotine hydrochloride 100.9g, yield 94.3% with embodiment 11.
[embodiment 25] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 2N picric acid, all the other dosages, processing condition, process get 7.1% nicotine picrate 163.8g, yield 87.6% with embodiment 12.
[embodiment 26] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 1N phenylformic acid, all the other dosages, processing condition, process get 5.5% phenylformic acid nicotine 151.6g, yield 86.5% with embodiment 17.
[embodiment 27] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 1N toluylic acid, all the other dosages, processing condition, process get 4.1% toluylic acid nicotine 211g, yield 85.5% with embodiment eight.
[embodiment 28] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 2N sulfuric acid, all the other dosages, processing condition, process get 8.1% nicotine sulfate 81.5g, yield 92.2% with embodiment 14.
[embodiment 29] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 1.5N sulfuric acid, all the other dosages, processing condition, process get 7.5% nicotine sulfate 87g, yield 91.1% with embodiment 13.
[embodiment 30] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 1N sulfuric acid, all the other dosages, processing condition, process get 6.8% nicotine sulfate 94.1g, yield 89.3% with embodiment seven.
[embodiment hentriaconta-] water is carried 60 ℃ of 30min, the D61 ion exchange column, and the pouring collection adopts drenches the collection post, and with the anti-collection of drenching of 1N sulfuric acid, all the other dosages, processing condition, process get 5.4% nicotine sulfate 119.5g, yield 90.1% with embodiment one.
[embodiment 32] are drenched collection and are adopted thermopnore, and with the anti-collection of drenching of 2N phosphoric acid, all the other dosages, processing condition, process get 8.1% nicotine sulfate 79.6g, yield 90.0% with embodiment ten.
Claims (8)
1, a kind of alkaloid preparation field that belongs to mainly comprises crumbled tobacco, offal water extraction, and the water extract with the nicotine of steps such as acids salify and the preparation method of salt thereof, is characterized in that through organic solvent extraction again:
1.1 the water extraction step is a dynamic countercurrent subsequent leaching technology,
1.2 the water extract is through the acid absorption-alkaline wash-out of ion exchange resin,
1.3 alkaline eluant drenches the collection absorbing process through the solid phase organic solvent,
1.4 acidic solution is to the anti-collection salify that drenches of solid phase organic solvent.
2, the preparation method of nicotine according to claim 1 and salt thereof, it is characterized in that described water extraction step is a dynamic countercurrent subsequent leaching technology, be meant in leacher, water used in solvent goes downstream, crumbled tobacco, offal are sailed against the current, the solid-liquid weight ratio is 1: 2～5,20～60 ℃ of leaching temperatures, and tobacco leaf, offal are 0.5～2.5h by the leacher time.
3, the preparation method of nicotine according to claim 1 and salt thereof, it is characterized in that described water extract is through the acid absorption-alkaline wash-out of ion exchange resin, be meant the clean water extract of filter in PH3～6 by strong acid type vinylbenzene-second diene benzene series row cationic exchange resin adsorption, get nicotine solution with 4～15% alkaline solution wash-out again.
4, the preparation method of nicotine according to claim 1 and salt thereof, it is characterized in that described alkaline eluant drenches the collection absorbing process through the solid phase organic solvent, be meant that alkaline eluant drenches collection post or thermopnore through vinylbenzene-second diene benzene series row or an Aluminosilicates polymer support particulate that is comprising organic solvent, nicotine is by organic solvent absorption in the solid phase carrier particulate.
5, the preparation method of nicotine according to claim 1 and salt thereof is characterized in that described acidic solution to the anti-collection salify that drenches of solid phase organic solvent, is meant that the acid solution with 0.3～2N gets nicotine salt by solid phase organic solvent post or the anti-collection of drenching of thermopnore.
6, the preparation method of nicotine according to claim 3 and salt thereof, it is characterized in that described 4～15% alkaline solutions that the strongly acidic cation-exchange wash-out is used, can be the aqueous solution of sodium hydroxide, potassium hydroxide, ammonium hydroxide, yellow soda ash or sodium bicarbonate.
7, the preparation method of nicotine according to claim 4 and salt thereof is characterized in that the organic solvent that comprises in the described solid phase organic solvent carrier particles can be halogenated alkane, haloolefin or solvent oil.
8, the preparation method of nicotine according to claim 5 and salt thereof, it is characterized in that describedly to the anti-acid solution that drenches 0.3～2N of using of collection salify of solid phase organic solvent, can be organic acid or mineral acids such as sulfuric acid, nitric acid, hydrochloric acid or phosphoric acid such as oxalic acid, citric acid, tartrate, phenylformic acid, toluylic acid or picric acid.
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| CN 94110582 CN1102647A (en) | 1994-05-13 | 1994-05-13 | Nicotine and its salt prepn. |
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| CN 94110582 CN1102647A (en) | 1994-05-13 | 1994-05-13 | Nicotine and its salt prepn. |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045960C (en) * | 1995-05-19 | 1999-10-27 | 林芝毅 | Preparing method for 40% nicotine benzene series solution and pure nicotine and equipment |
| CN1093540C (en) * | 1997-05-29 | 2002-10-30 | 中国科学院西北高原生物研究所 | Comprehensive utilizing of nicotine in low-quality tobacco leafs, and technology for preparing its by-product melim |
| CN103524484A (en) * | 2013-06-21 | 2014-01-22 | 马震 | Production method of solid nicotine |
| CN102196736B (en) * | 2008-10-22 | 2014-11-26 | 英美烟草（德国）有限公司 | Extractive tobacco material extrusion |
| CN107536099A (en) * | 2017-09-14 | 2018-01-05 | 昌宁德康生物科技（深圳）有限公司 | A kind of nicotine salt and preparation method thereof |
| CN108451002A (en) * | 2014-11-07 | 2018-08-28 | 尼科创业控股有限公司 | The solution of nicotine containing non-protonated form and protonated form |
| CN111072629A (en) * | 2019-11-22 | 2020-04-28 | 云南中烟工业有限责任公司 | Nicotine-oxalate compound crystal and application thereof |
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1994
- 1994-05-13 CN CN 94110582 patent/CN1102647A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045960C (en) * | 1995-05-19 | 1999-10-27 | 林芝毅 | Preparing method for 40% nicotine benzene series solution and pure nicotine and equipment |
| CN1093540C (en) * | 1997-05-29 | 2002-10-30 | 中国科学院西北高原生物研究所 | Comprehensive utilizing of nicotine in low-quality tobacco leafs, and technology for preparing its by-product melim |
| CN102196736B (en) * | 2008-10-22 | 2014-11-26 | 英美烟草（德国）有限公司 | Extractive tobacco material extrusion |
| CN103524484A (en) * | 2013-06-21 | 2014-01-22 | 马震 | Production method of solid nicotine |
| CN103524484B (en) * | 2013-06-21 | 2015-04-01 | 马震 | Production method of solid nicotine |
| CN108451002A (en) * | 2014-11-07 | 2018-08-28 | 尼科创业控股有限公司 | The solution of nicotine containing non-protonated form and protonated form |
| US11044937B2 (en) | 2014-11-07 | 2021-06-29 | Nicoventures Trading Limited | Solution comprising nicotine in unprotonated form and protonated form |
| CN107536099A (en) * | 2017-09-14 | 2018-01-05 | 昌宁德康生物科技（深圳）有限公司 | A kind of nicotine salt and preparation method thereof |
| CN111072629A (en) * | 2019-11-22 | 2020-04-28 | 云南中烟工业有限责任公司 | Nicotine-oxalate compound crystal and application thereof |
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