CN112592332A - Preparation process of high-purity nicotine - Google Patents

Preparation process of high-purity nicotine Download PDF

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Publication number
CN112592332A
CN112592332A CN202110027368.7A CN202110027368A CN112592332A CN 112592332 A CN112592332 A CN 112592332A CN 202110027368 A CN202110027368 A CN 202110027368A CN 112592332 A CN112592332 A CN 112592332A
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China
Prior art keywords
nicotine
purity
crude
layering
sulfate
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CN202110027368.7A
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Chinese (zh)
Inventor
王晨
宋一鸣
管玉雷
王洋洋
秦浩
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Northwestern University
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Northwestern University
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Priority to CN202110027368.7A priority Critical patent/CN112592332A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D401/00Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
    • C07D401/02Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
    • C07D401/04Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a new process for preparing high-purity nicotine from nicotine sulfate, which comprises the following steps: neutralizing 35-55% nicotine sulfate water solution with 25-35% sodium hydroxide water solution, cooling the system after neutralization to maintain the temperature of the solution at 5-10 ℃, and standing; filtering after the sodium sulfate decahydrate is completely precipitated out; heating the filtrate to 75-85 ℃, standing for layering, collecting the upper layer nicotine after layering, drying to remove water, filtering to obtain crude nicotine, and rectifying the crude nicotine to obtain high-purity nicotine. The invention can greatly reduce the dosage of the extracting agent and the energy consumption of evaporation and concentration of the extract liquor, save energy, reduce emission and shorten the process time.

Description

Preparation process of high-purity nicotine
Technical Field
The invention relates to a novel process for preparing high-purity nicotine from nicotine sulfate, belonging to the technical field of industrial waste recycling treatment.
Background
As a big country for tobacco production and processing in China, the interest and tax created by the tobacco industry every year is over one trillion yuan RMB from 2014. The tobacco leaf production in 2017 is more than 239 ten thousand tons. In China, nearly 10 ten thousand tons of waste tobacco powder, tobacco stems and the like are produced in the tobacco processing process every year, one part of the waste is treated by preparing biological fertilizers through fermentation, and the other part of the waste is used for producing nicotine sulfate and is used as a raw material for preparing high-purity nicotine or biological pesticides. The high-purity nicotine is an important raw material of electronic cigarettes and medical intermediates, has extremely high added value and large market gap.
At present, high-purity nicotine at home and abroad is generally prepared by alkalizing 40% nicotine sulfate, dissociating the nicotine, extracting the nicotine by using an organic solvent, recovering the solvent by using an evaporator, and rectifying the concentrated nicotine in a rectifying tower to obtain the pure nicotine. In the process, extraction and concentration are key sections which restrict the production benefit. In the extraction process, when the extraction efficiency is over 95 percent, the dosage of the organic extractant is about 6 to 8 times of the volume of the water phase, and if the extraction is carried out intermittently, 6 to 8 times is needed, which is very time-consuming. In addition, the solvent is severely lost by evaporation during the concentration of the extract under reduced pressure. According to data in actual production, the loss amount of the solvent in each reduced pressure evaporation is about 8-10%. Therefore, aiming at long extraction and concentration process time, large solvent loss and high energy consumption, the process needs to be improved to reduce energy consumption and improve efficiency.
Disclosure of Invention
The invention aims to provide a novel efficient and energy-saving process for preparing high-purity nicotine by using 35-55% nicotine sulfate, so that the load of an extraction section is greatly reduced, the loss and concentration of an extracting agent are reduced, and energy conservation and emission reduction are realized.
The invention is realized as follows, and the percentage is mass percentage.
A preparation process of high-purity nicotine comprises the following steps:
(1) neutralizing 35-55% nicotine sulfate water solution with 25-35% sodium hydroxide water solution, cooling the system after neutralization to maintain the temperature of the solution at 5-10 ℃, and standing;
(2) filtering after the sodium sulfate decahydrate is completely precipitated out;
(3) heating the filtrate to 75-85 ℃, standing for layering, collecting the upper layer nicotine after layering, drying to remove water, and filtering to obtain crude nicotine;
(4) rectifying the crude nicotine to obtain high-purity nicotine.
And (3) after the layering, extracting the lower water phase by using No. 6 solvent oil, and extracting and concentrating to obtain the crude nicotine.
In the step (3), anhydrous sodium sulfate is added to nicotine to dry and remove water.
Since nicotine-water is a two-liquid system with the highest and lowest dissolving temperatures and has a completely closed dissolving curve, the nicotine and the water phase can be separated by controlling the appropriate temperature at a certain nicotine concentration in step (3). The nicotine on the upper layer is separated, and the aqueous phase on the lower layer is extracted, so that the dosage of an extracting agent is reduced, the load of an extraction section is reduced, the energy is saved, the efficiency is improved, and the economic benefit is improved.
The invention has the advantages that: (1) the consumption of the extracting agent and the energy consumption of the evaporation and concentration of the extraction liquid can be greatly reduced, and the invention is about 50 percent of the solvent used in the traditional direct extraction process; (2) the anhydrous sodium sulfate used for dehydrating and drying the crude nicotine at the upper layer can be prepared and obtained from the process without additional purchase; (3) the process conforms to the policy of energy conservation and emission reduction, greatly reduces the extraction and concentration amount in the process, shortens the time of the whole process, and indirectly improves the economic benefit.
Drawings
FIG. 1 is a flow diagram of the process for preparing high purity nicotine from nicotine sulfate according to the present invention.
Detailed Description
The synthesis of the present invention is illustrated below by means of specific examples, which are intended to better understand the content of the present invention and not to limit the scope of protection of the present invention.
The production process for preparing high-purity nicotine comprises the following steps: neutralizing 40% nicotine sulfate water solution with 32% sodium hydroxide water solution, cooling the system after neutralization to maintain the solution temperature at 5-10 deg.C, and standing; after the precipitated sodium sulfate decahydrate is completely precipitated, carrying out centrifugal filtration, wherein the solid can be used for preparing anhydrous sodium sulfate, slowly stirring the filtrate, heating to 80 ℃, standing and waiting for layering; collecting upper layer nicotine after layering, adding anhydrous sodium sulfate, drying to remove water, and filtering to obtain crude nicotine; extracting the lower water phase by using No. 6 solvent oil, and obtaining crude nicotine after extraction and concentration; and merging the crude nicotine, and rectifying in a rectifying still to obtain high-purity nicotine.
Example 1
500L of 40% nicotine sulfate is added into a 1000L jacketed reaction kettle, then 175L of 32% NaOH is added, the mixture is stirred for 15 minutes at normal temperature, and then water is circularly cooled until the system is maintained at 9 ℃, and the mixture is kept stand for 2.5 hours. During which time slight stirring may be applied to promote precipitation of crystals. After the precipitation is completed, centrifugal filtration is carried out, and crude sodium sulfate decahydrate obtained by filtration can be used for preparing anhydrous sodium sulfate. The filtrate was heated to 80 ℃ with slow stirring in a heating kettle, then the temperature was maintained and stirring was stopped, and left to stand for 20 minutes to wait for significant stratification. The upper organic layer (about 280L) was separated and dried over 20kg of anhydrous sodium sulfate. Extracting the lower water phase (about 390L) with 1200L No. 6 solvent oil (centrifugal extraction or disc extraction), concentrating the extractive solution under reduced pressure, recovering solvent, and mixing the concentrated crude nicotine with the above crude nicotine for rectification. The final high-purity nicotine is about 227 kg (the nicotine content is more than 99%), and the total recovery rate is 96.5% (calculated by the pure nicotine contained in 40% nicotine sulfate).
Example 2
Adding 400L of 45% nicotine sulfate into a 1000L jacketed reaction kettle, then adding 140L of 35% NaOH, stirring for 15 minutes at normal temperature, circularly cooling water until the system is maintained at 7 ℃, and standing for 2.5 hours; after the precipitation is completed, centrifugal filtration is carried out, and crude sodium sulfate decahydrate obtained by filtration is used for preparing anhydrous sodium sulfate; the filtrate was heated to 82 ℃ with slow stirring in a heating kettle, then the temperature was maintained and stirring was stopped, and left to stand for 20 minutes to wait for significant stratification. The upper organic layer was separated by about 220L and dried over 20kg of anhydrous sodium sulfate. Extracting the lower water phase (about 320L) with 1000L No. 6 solvent oil (centrifugal extraction or disc extraction), concentrating the extractive solution under reduced pressure, recovering solvent, and mixing the concentrated crude nicotine with the above crude nicotine for rectification. The final high-purity nicotine is about 207 kg (the nicotine content is more than 99 percent), and the total recovery rate is 97 percent (calculated by the pure nicotine contained in 45 percent of nicotine sulfate).

Claims (3)

1. A preparation process of high-purity nicotine is characterized by comprising the following steps:
(1) neutralizing 35-55% nicotine sulfate water solution with 25-35% sodium hydroxide water solution, cooling the system after neutralization to maintain the temperature of the solution at 5-10 ℃, and standing;
(2) filtering after the sodium sulfate decahydrate is completely precipitated out;
(3) heating the filtrate to 75-85 ℃, standing for layering, collecting the upper layer nicotine after layering, drying to remove water, and filtering to obtain crude nicotine;
(4) rectifying the crude nicotine to obtain high-purity nicotine.
2. The process for preparing high purity nicotine according to claim 1, wherein: and (3) extracting the lower aqueous phase after layering, and extracting and concentrating to obtain the crude nicotine.
3. The process for preparing high purity nicotine according to claim 1, wherein: in the step (3), anhydrous sodium sulfate is added to nicotine to dry and remove water.
CN202110027368.7A 2021-01-09 2021-01-09 Preparation process of high-purity nicotine Pending CN112592332A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115181089A (en) * 2022-06-20 2022-10-14 托拔克生物科技(衡阳)有限公司 Natural nicotine purification process

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1110507A (en) * 1994-04-18 1995-10-25 中国农业科学院植物保护研究所 Nicotine cream and preparation method
CN105566288A (en) * 2014-10-14 2016-05-11 北京本草通汇科技中心 High purity nicotine industrial preparation method
WO2019239356A1 (en) * 2018-06-15 2019-12-19 R. J. Reynolds Tobacco Company Purification of nicotine

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1110507A (en) * 1994-04-18 1995-10-25 中国农业科学院植物保护研究所 Nicotine cream and preparation method
CN105566288A (en) * 2014-10-14 2016-05-11 北京本草通汇科技中心 High purity nicotine industrial preparation method
WO2019239356A1 (en) * 2018-06-15 2019-12-19 R. J. Reynolds Tobacco Company Purification of nicotine
CN112384504A (en) * 2018-06-15 2021-02-19 R.J.雷诺兹烟草公司 Purification of nicotine

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115181089A (en) * 2022-06-20 2022-10-14 托拔克生物科技(衡阳)有限公司 Natural nicotine purification process
CN115181089B (en) * 2022-06-20 2024-03-26 湖北托拔克生物科技有限公司 Natural nicotine purifying process

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