CN105768202B - A kind of method of nicotine in extraction tobacco waste - Google Patents

Abstract

The invention discloses a kind of method for extracting nicotine in tobacco waste, comprise the following steps：Atmospheric extraction is carried out during alkali ionic liquid salting liquid and tobacco waste are added into synthesis abstraction instrument, temperature is 50~70 DEG C, and extraction time is 25~35min, obtains nicotine；The alkali ionic liquid salting liquid is made up of alkali ionic liquid and potassium acetate.The method of nicotine substantially increases the extraction efficiency of nicotine in tobacco waste in extraction tobacco waste of the invention, and be conducive to the application of nicotine to produce, reconstituted tobacoo quality is improve, and alkali ionic liquid can be recycled repeatedly, and pollution is not resulted in environment.

Description

A method for extracting nicotine from tobacco waste

technical field

The invention relates to a method for extracting tobacco extract, in particular to a method for extracting nicotine from tobacco waste.

Background technique

Tobacco extract has the original aroma of tobacco, and is often used as a raw material for tobacco products. Its aroma can coordinate with the aroma of tobacco and make the aroma of tobacco rich. It is widely used in cigarette flavoring. Tobacco is a complex system from which thousands of chemical constituents have been identified. Tobacco extracts have different chemical components due to different extraction processes, and the most important and most interesting component in tobacco extracts is nicotine.

Nicotine is an important chemical component in tobacco. Nicotine, also known as nicotine, is a pyridine alkaloid that exists in tobacco crops. Nicotine is a colorless or light bronze oily liquid at room temperature. The pure product is a colorless oily liquid. It quickly turns brownish yellow when it contacts with air. High nicotine content means strong energy, strong irritation, spicy taste, high content If it is low, the energy will be small, and the smoking will be bland and tasteless. Therefore, the level of nicotine content in tobacco extract has an important impact on its added amount, and is an important parameter to measure the quality and specification of tobacco extract, and is the main index to control tobacco extract.

Nicotine has many uses, first of all it can be used as an insecticide. Nicotine sulfate obtained by reacting nicotine with sulfuric acid is an example. 40% nicotine sulfate is traded as "Blaikleaf 40" in the United States, and it is a widely used insecticide in the world. According to the research on the structure of nicotine, people have developed nicotine-like insecticides, and nicotine can also be used as raw materials for some nicotine-like insecticides. For example, in 1991, Henan University successfully synthesized the neonicotinoid insecticide "Mephidin" by using nicotine as the substrate.

In addition, nicotine has a wide range of medicinal value. The Swiss Langsha company used nicotine to oxidize to make niacin (vitamin F, anti-rough dermatosis) for a long time and mass-produced it. In foreign countries, nicotinic drugs can be used as smoking cessation drugs. Such as nicotine transdermal adhesives, which use nicotine or its organic acid salts (lactate, citrate, salicylate, etc.) to absorb nicotine through the skin with the help of a transdermal slow-release system, reducing addiction. It can also be made into an ion exchange resin containing a certain amount of nicotine, similar to chewing gum, which can be chewed in the mouth, and the nicotine released during chewing is absorbed by the oral mucosa, which can also reduce the symptoms of smoking addiction. It can also be mixed with other natural plant extracts to make snus tablets. In addition, nicotine compounds such as nicotine citrate, nicotine oxide, and quaternary ammonium salt of nicotine can be used as tobacco additives to make the aroma of tobacco leaves more pleasant. For tobacco with high nicotine content, extraction, steam distillation and other methods are often used to extract part of the nicotine, and then a part of the extracted nicotine is turned into citrate and added to the tobacco leaves to enhance the aroma of tobacco. The further development of nicotine emerges in endlessly and has a good market prospect.

Nicotine can be combined with nicotinic choline applied externally and in the central nervous system. It has a stimulating effect on the nervous system, which can improve wakefulness, attention and responsiveness, and reduce anxiety and stress reactions. Nicotine tartrate immediately and significantly lowers diastolic and systolic blood pressure in hypertensive patients. The bitartrate salt of nicotine is applied topically to treat muscle spasms and joint pain.

At present, the extraction methods of nicotine in tobacco mainly include methods such as distillation extraction, ion exchange and supercritical fluid extraction. Distillation extraction is a common extraction method that was earlier applied to industrial production, Lu Xuwang et al. 48-53) The nicotine with a purity of 40% was obtained from waste tobacco leaves by secondary extraction and distillation. However, the method has complicated operation steps and long extraction time. The ion exchange method is to extract the raw material with dilute acid, heat and reflux, make the filtrate flow through the ion exchange resin, and then exchange with alkali to obtain the aqueous solution of free nicotine. Although this method has low energy consumption, it still has the disadvantage of cumbersome pretreatment and regeneration of the ion exchange resin. Rincon et al. (Preliminary study on the supercritical carbon dioxide extraction of nicotine from tobacco wastes [J]. Separation Science and Technology, 1998, 33(3): 411-423.) used supercritical CO ₂ to extract solid smoke samples at 25MPa and 60°C The nicotine of this method obtains better extraction efficiency, but the equipment cost of this method is higher, is unfavorable for popularization and promotion.

Contents of the invention

In order to overcome the above-mentioned shortcomings and deficiencies of the prior art, the object of the present invention is to provide a method for extracting nicotine from tobacco waste, which effectively improves the extraction rate of nicotine from tobacco waste.

The object of the present invention is achieved through the following technical solutions:

A method for extracting nicotine in tobacco waste, comprising the following steps:

Add the alkaline ionic liquid salt solution and tobacco waste into a synthetic extractor for atmospheric extraction at a temperature of 50-70°C and an extraction time of 25-35 minutes to obtain nicotine;

The basic ionic liquid salt solution is made of basic ionic liquid and potassium acetate.

The alkaline ionic liquid is one of [MMIM]DMP, [Bmim][HCOO], [Hmim][Ac], [Emim][Ac] bases.

Described alkaline ionic liquid salt solution is made by following method:

Add the alkaline ionic liquid into the potassium acetate salt solution, control the mass concentration of potassium acetate in the system to 3% to 12%, stir at room temperature for 20 to 24 hours and then filter, wash the filtrate with ether for 2 to 3 times, and use rotary evaporation Distill under reduced pressure for 1 to 2 hours.

The synthesis extractor is a microwave catalytic synthesis extractor, and the microwave power is 400-500W during extraction.

The tobacco waste is tobacco stems; the mass ratio of the alkaline ionic liquid salt solution to the tobacco stems is 23:1˜27:1.

The tobacco waste is tobacco dust; the mass ratio of the alkaline ionic liquid salt solution to the tobacco dust is 18:1˜22:1.

Compared with the prior art, the present invention has the following advantages and beneficial effects:

(1) The present invention adopts alkaline ionic liquid salt solution as the extraction solution of grass waste, which greatly improves the extraction efficiency of nicotine in tobacco waste. Compared with the extraction by industrial tap water, the extraction rate of nicotine in tobacco powder improves The extraction rate of nicotine in tobacco stems increased by 30%, and the extraction rate of nicotine increased by 34.2%.

(2) The alkaline ionic liquid salt solution of the present invention is used as the extract of grass waste, which solves the disadvantages of using traditional organic solvent extraction to pollute the environment and using a large amount of organic solvent, and also solves some traditional extraction methods. The disadvantages of complexity, high cost and high energy consumption.

(3) The present invention can effectively improve the extraction rate of nicotine in the raw materials, is beneficial to the applied production of nicotine, improves the quality of tobacco flakes, and the alkaline ionic liquid can be recycled for many times without causing pollution to the environment.

detailed description

The present invention will be described in further detail below in conjunction with the examples, but the embodiments of the present invention are not limited thereto.

Example 1

Configure a potassium acetate solution with a mass concentration of 10%, and add ionic liquids ([MMIM]DMP, [Bmim][HCOO]), [Hmim][Ac], [Emim][Ac] to sequentially increase the alkalinity) into In different beakers filled with potassium acetate solution, stir vigorously at room temperature for 24 hours, filter to remove the white precipitate, then wash with a small amount of ether twice, and after filtration, place the filtrate at 70°C for 1 hour to obtain colorless The viscous liquid ionic liquid salt solution is used for the extracting solution of tobacco sheet raw materials. Tobacco stalks and tobacco powder were extracted in a microwave catalytic synthesis extractor at normal pressure, in which the mass ratio of the extraction liquid to the tobacco stalks was 23:1, the extraction temperature was 50°C, the extraction time was 25 minutes, and the microwave power was 400W. The mass ratio of the extraction solution to the tobacco powder was 18:1, the extraction temperature was 50°C, and the extraction time was 35 minutes. The results are shown in Table 1.

Table 1

The results in Table 1 show that the extraction rate of nicotine is also different among different ionic liquid liquids, and the extraction rate of nicotine under a certain alkaline condition increases with the increase of the alkalinity of the ionic liquid. This is due to the existence of the pyrrole ring and the pyridine ring in the nicotine base molecule, so that the nicotine can be freed only when the alkalinity is higher, and the stronger the alkalinity, the more conducive to the dissolution of nicotine in the tobacco raw material.

Example 2

Potassium acetate solutions with different mass concentrations were prepared, basic ionic liquid [Emim][Ac] was added to it, stirred vigorously at room temperature for 20 hours, filtered to remove the white precipitate, and then washed with a small amount of ether for 3 times, after filtration, the filtrate was placed in Under reduced pressure and rotary evaporation at 70°C for 2 hours, a colorless viscous liquid alkaline ionic liquid salt solution was obtained, and the raw materials of tobacco stem and tobacco powder were extracted in a microwave catalytic synthesis extractor at normal pressure for a single time. The mass ratio is 27:1, the extraction temperature is 70°C, the extraction time is 35min, the microwave power is 500W, the mass ratio of the extraction liquid and tobacco powder is 22:1, the extraction temperature is 70°C, and the extraction time is 5min. The results are shown in Table 2 .

Table 2

The results in Table 2 show that in the extraction process, adding potassium acetate is obviously beneficial to improve the extraction rate of nicotine in tobacco stems and tobacco powder. This is because under the heating condition of ionic liquid medium, the polarity of inorganic salt potassium acetate can destroy The hydrogen bond connection and network structure between fibers in the substance promote the dissolution of nicotine. The addition concentration of potassium acetate in the leaching process is advisable with 3%-12%, when the addition concentration is higher than 12%, the extraction rate drops slightly, is unfavorable for follow-up treatment, so the present invention selects 3%-12% potassium acetate The solution is added to the leach solution as an extraction solution system.

Example 3

Prepare a potassium acetate solution with a mass concentration of 10%, add the basic ionic liquid [Emim][Ac] made in the laboratory or commercially available, stir vigorously at room temperature for 24 hours, filter to remove the white precipitate, and then wash with a small amount of ether , after filtration, put the filtrate under reduced pressure and rotary evaporation at 70°C for 1 hour to obtain a colorless viscous liquid alkaline ionic liquid salt solution, and extract tobacco stems and Tobacco powder raw material, wherein the mass ratio of extract liquid to tobacco stem is 25:1, the extraction temperature is 60°C, the extraction time is 30min, the mass ratio of extract liquid to tobacco powder is 20:1, the extraction temperature is 50-70°C, The extraction time is 35-45 minutes, and the results are shown in Table 3.

table 3

The results in Table 3 show that under microwave catalysis conditions, the extraction rate of nicotine in the raw material is remarkable, all above 85%, which is significantly higher than the extraction process without microwave catalysis under the same conditions, because the movement of biomass macromolecules under microwave conditions It is more intense and produces a greater thermal effect, and microwaves can also have certain effects on hydrogen bonds, hydrophobic bonds and van der Waals forces in biomacromolecules, making microwave dissolution promote the dissolution and extraction of nicotine in raw materials.

Example 4

Prepare a potassium acetate solution with a mass concentration of 10%, add ionic liquid ([MMIM]DMP) to it, stir vigorously at room temperature for 20 hours, filter to remove the white precipitate, then wash with a small amount of ether, and place the filtrate at 70°C after filtration Under reduced pressure and rotary evaporation for 2 hours, a colorless viscous liquid alkaline ionic liquid salt solution was obtained, and the raw materials of tobacco stem and tobacco powder were extracted in a microwave catalytic synthesis extractor at normal pressure, wherein the extraction liquid and the tobacco stem were in a mass ratio of 27 :1, the extraction temperature is 70°C, the extraction time is 35min, the mass ratio of the extract and tobacco powder is 22:1, the extraction temperature is 70°C, and the extraction time is 5min, the results are shown in Table 4.

Table 4

The results in Table 4 show that compared with industrial tap water and [MMIM] DMP ionic liquid extraction, the extraction solution of the present invention is very effective in extracting nicotine in tobacco waste, effectively improving the nicotine in tobacco waste The extraction rate can effectively improve the quality and smoking effect of tobacco flakes.

The above-mentioned embodiment is a preferred embodiment of the present invention, but the embodiment of the present invention is not limited by the embodiment, and any other changes, modifications, substitutions and combinations made without departing from the spirit and principle of the present invention , simplification, all should be equivalent replacement methods, and are all included in the protection scope of the present invention.

Claims (6)

1. it is a kind of extract tobacco waste in nicotine method, it is characterised in that comprise the following steps：

Atmospheric extraction is carried out during alkali ionic liquid salting liquid and tobacco waste are added into synthesis abstraction instrument, temperature is 50~70 DEG C, extraction time is 25~35min, obtains nicotine；

The alkali ionic liquid salting liquid is made up of alkali ionic liquid and potassium acetate.

2. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the alkali ion liquid Body is the one kind in [MMIM] DMP, [Bmim] [HCOO], [Hmim] [Ac], [Emim] [Ac] alkali.

3. it is according to claim 2 extract tobacco waste in nicotine method, it is characterised in that the alkali ion liquid Body salting liquid is made up of following methods：

By in alkali ionic liquid addition potassium salt solution, it is 3%~12% to control mass concentration of the potassium acetate in system, Filtered after stirring 20~24 hours at room temperature, filtrate washed with diethylether 2~3 times is small using Rotary Evaporators vacuum distillation 1~2 When.

4. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the synthesis abstraction instrument For microwave catalysis synthesize abstraction instrument, microwave power is 400~500W during extraction.

5. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the tobacco waste It is offal；The offal is 23 with the mass ratio of alkali ionic liquid salting liquid:1~27:1.

6. it is according to claim 1 extract tobacco waste in nicotine method, it is characterised in that the tobacco waste It is offal；The offal is 18 with the mass ratio of alkali ionic liquid salting liquid:1~22:1.