CN110724126B - Purification method of nicotine and nicotine - Google Patents
Purification method of nicotine and nicotine Download PDFInfo
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Abstract
The invention relates to a nicotine purification method and nicotine, the method comprises the following steps: under the condition of introducing protective gas, carrying out normal pressure distillation on the nicotine to be treated at the temperature of 90-100 ℃ to remove low-boiling-point impurities; the nicotine after atmospheric distillation is divided into two steps for vacuum distillation, the first step of vacuum distillation is distillation at the temperature of 110-150 ℃, the distillation time is 30 min-1 h, a small amount of nicotine is obtained, and the nicotine is discarded to obtain the undistilled nicotine; the second step of vacuum distillation is to distill the undistilled nicotine again at 120-150 ℃ to obtain nicotine; and (4) carrying out reduced pressure distillation on the nicotine subjected to vacuum distillation in the second step to obtain the required nicotine. The nicotine treated by the method has high purity, transparent colorless liquid and purer smell, and does not contain chemical odor residual in common nicotine products; the related operation has less manual demand and large treatment capacity, the average daily nicotine treatment amount can reach 100L, and the method is suitable for large-scale production and use.
Description
Technical Field
The invention relates to the technical field of purification of natural products, in particular to a purification method of nicotine and nicotine.
Background
Nicotine, commonly known as nicotine, is an important chemical raw material in the pharmaceutical, pesticide and chemical industries, and researches show that nicotine has obvious curative effects on senile dementia and depression, has huge application potential in the field of treating related diseases, and has large demand, and the sale price of high-purity nicotine at home and abroad is more than 50 to 100 ten thousand per ton. At present, nicotine is mainly extracted from tobacco andor waste tobacco stems and tobacco leaves.
Nicotine is easy to dissolve in organic solvents such as alcohol, ether, chloroform, alkane and the like and water, at present, the nicotine is mainly prepared in industrial production by extracting in alkali liquor and acid liquor by using extraction tank equipment, and high-purity nicotine is obtained by rectifying after the solvent is removed. A large amount of organic solvent is used in the extraction process, solvent residue (such as petroleum ether and the like) cannot be avoided, because the existing industrial production of nicotine adopts a simple distillation or rectification process, the operation temperature is over 100 ℃, oxygen components cannot be prevented from being mixed, the property of nicotine is unstable, the cracking of the residual organic solvent and the oxidation and degradation of the nicotine can be caused under the action of high temperature and oxygen, the purity of the obtained nicotine finished product is generally 95-97%, the color is yellow, the appearance is not good, the chemical odor of the nicotine produced by the conventional industrial method is found in the application process of the electronic cigarette, and the application of the nicotine in the field of biomedicine is limited.
Disclosure of Invention
Based on this, there is a need for a method of purifying nicotine and nicotine; the final purity of the nicotine obtained by the method reaches 99.693%, the appearance color is good (transparent colorless liquid), the smell is purer, chemical odor remained in common nicotine products is not contained, the equipment requirement is simple, the recovery rate is high, the method is suitable for large-scale processing production, and the production safety is high.
A method of purifying nicotine comprising the steps of:
under the condition of introducing protective gas, carrying out normal pressure distillation on the nicotine to be treated at the temperature of 90-100 ℃ to remove low-boiling-point impurities;
the nicotine after atmospheric distillation is distilled in two steps, the first step of vacuum distillation is distillation at 110-150 ℃, the distillation lasts for 30 min-1 h, a small amount of nicotine is obtained by distillation, and the small amount of nicotine obtained by distillation is discarded to obtain the residual nicotine which is not distilled;
the second step of vacuum distillation is to distill the residual undistilled nicotine again at 120-150 ℃ to obtain nicotine;
and carrying out reduced pressure distillation on the nicotine subjected to vacuum distillation in the second step to finally obtain the purified nicotine.
In one embodiment, the atmospheric distillation reaction is carried out for 3 to 5 hours.
In one embodiment, the protective gas is continuously introduced to keep the gas circulating, and the protective gas is nitrogen or argon.
In one embodiment, the vacuum degree of the first step of vacuum distillation is 0.08MPa to 0.09 MPa; the vacuum degree of the second step of vacuum distillation is 0.09 Mpa-0.1 Mpa.
In one embodiment, the time of the second step vacuum distillation is 4-6 h.
In one embodiment, the atmospheric distillation is atmospheric distillation and the reflux ratio is set to total reflux.
In one embodiment, the vacuum distillation is vacuum distillation, and the reflux ratio of the first vacuum distillation is set to be total reflux; the reflux ratio of the second step of vacuum distillation is 1: 2-1: 4.
in one embodiment, the atmospheric distillation temperature is 90 ℃; and/or the cycle time of the protective gas is 3 h; and/or; the temperature of the first step of vacuum distillation is 110 ℃; and/or, the second step vacuum distillation temperature is 130 ℃.
Nicotine is prepared by the purification method.
According to the method, the nicotine to be treated is distilled at the normal pressure at the temperature of 90-100 ℃, the distillation can ensure that the nicotine does not boil and is not heated to volatilize, but low-boiling-point impurities such as organic solvents and the like remained in the nicotine are continuously heated to volatilize at the temperature of 90-100 ℃, so that the low-boiling-point impurities are distilled out, and the low-boiling-point impurities are removed. The method can avoid the problems that the existing method has overhigh temperature, leads to nicotine volatilization, and can cause the cracking of residual organic solvent and the oxidation and degradation of nicotine due to the action of high temperature and oxygen, and simultaneously carries out two-step vacuum distillation on the nicotine after atmospheric distillation, wherein the temperature of the first-step vacuum distillation is controlled to be 110-150 ℃, so that the residual organic solvent (petroleum ether and the like) after atmospheric distillation can be thoroughly removed, and then the second-step distillation is carried out, the temperature is controlled to be 120-150 ℃, and the temperature range is the boiling point of the nicotine, therefore, the temperature in the range is selected for the second-step vacuum distillation, so that the nicotine can be distilled and collected. Finally, reduced pressure distillation and collection are carried out, and the nicotine obtained by the method is almost colorless and transparent, has pure smell and high purity of 99.693%; the related operation has less manual demand and large treatment capacity, the average daily nicotine treatment amount can reach 100L, and the method is suitable for large-scale production and use.
Drawings
FIG. 1 is a GC-MS spectrum of nicotine prepared in example 1;
FIG. 2 is a GC-MS profile of untreated nicotine;
FIG. 3 is a GC-MS spectrum obtained in comparative example 1.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The purification method of nicotine according to an embodiment can produce nicotine with high purity, almost colorless transparency, pure smell, and purity of 99.693%. Specifically, the method comprises the following steps:
step S1: under the condition of introducing protective gas, carrying out normal pressure distillation on the nicotine to be treated at the temperature of 90-100 ℃ to remove low-boiling-point impurities;
specifically, the nicotine to be treated is obtained by extracting in alkali liquor and acid liquor by using extraction tank equipment at present, and because a large amount of organic solvent is used in the extraction process, solvent residues (such as petroleum ether and the like) cannot be avoided, the nicotine needs to be further treated; the nicotine is produced by Yuxi mangrove biotechnology limited.
Specifically, the nicotine to be treated is distilled under normal pressure at 90-100 ℃, and the distillation temperature can be 90 ℃, 95 ℃ and 100 ℃. By selecting the temperature range, nicotine can not be boiled and volatilized by heating, but low-boiling-point impurities such as organic solvents remained in nicotine are continuously heated and volatilized at 90-100 ℃, so that the impurities are distilled out, and the low-boiling-point impurities are removed.
Further, nicotine is in the atmospheric distillation process, through constantly letting in protective gas to inside formation circulation, can be constantly along with protective gas outflow with the volatile low boiling point impurity that is heated this moment.
In one embodiment, the protective gas is nitrogen or argon.
In one embodiment, under the condition of continuously introducing protective gas, the nicotine is distilled for 3-5 hours under normal pressure. Distillation reaction time is too short, the low boiling point impurity can not be heated completely and volatilize, lead to impurity to remain, distillation reaction time overlength, distillation time overlength, although there is the inert gas protection, high temperature heating time overlength, the final color and luster of product can not keep for a long time, can become yellowish in the storage process, consequently, distillation time sets up 3 ~ 5h most suitable, consequently, select this scope time, can be with the low boiling point impurity such as the organic solvent that remains in nicotine constantly heated and volatilizes, the nicotine purity that obtains is higher, and the smell is purer, colorless transparent.
In one embodiment, the reflux ratio of the atmospheric distillation is set to total reflux; further, this distillation adopts the mode of rectification to handle, has some low boiling point impurity and organic solvent to remain in the unprocessed sample, through setting for the total outflow, guarantees that impurity doubly distills out when being less than nicotine's boiling point temperature, separates with nicotine, can not get back to reation kettle once more, guarantees first step distillation process's separation effect.
Step S2: the nicotine after atmospheric distillation is distilled in two steps for vacuum distillation, wherein the vacuum distillation in the first step is distillation for 30 min-1 h at the temperature of 110-150 ℃, a small amount of nicotine is obtained by distillation, and the small amount of nicotine obtained by distillation is discarded to obtain the residual nicotine which is not distilled;
specifically, distilling for 30min to 1h at the temperature of 110 ℃ to 150 ℃, wherein no obvious oily substance is left on the tube wall; distilling to obtain a small amount of nicotine, and discarding the small amount of nicotine obtained by distillation; wherein, the temperature of the first step of vacuum distillation can be 110 ℃, 120 ℃, 130 ℃, 140 ℃ or 150 ℃. Wherein the temperature of the first step of vacuum distillation is higher than the temperature of atmospheric distillation; when the range is selected for the first distillation, the organic solvent (petroleum ether, etc.) remaining in the pipeline after the atmospheric distillation can be completely removed, and a small amount of nicotine is distilled off, and the nicotine is mixed with the remaining organic solvent impurities, and therefore, the nicotine needs to be discarded.
In one embodiment, the vacuum degree of the first step of vacuum distillation is 0.08MPa to 0.09 MPa. The vacuum degree is higher than the range, so that a large amount of nicotine is distilled off in the distillation process, and the waste and the loss of the nicotine are caused; when the degree of vacuum is less than this range, the efficiency of the distillation is reduced, the distillation time is prolonged, and the energy consumption is increased.
In one embodiment, the reflux ratio of the first vacuum distillation is set as total reflux, further, the distillation is processed in a rectification mode, and as part of low-boiling-point impurities and organic solvent residues exist in an unprocessed sample, the total reflux is set in the first step, so that the impurities are distilled out twice at the temperature lower than the boiling point of nicotine and are separated from the nicotine, and the impurities cannot return to the reaction kettle again, and the separation effect in the first distillation process is ensured.
Step S3: the second step of vacuum distillation is to distill the residual undistilled nicotine again at 120-150 ℃ to obtain nicotine;
specifically, the temperature of the second vacuum distillation may be 120 ℃, 130 ℃, 140 ℃, 145 ℃ or 150 ℃.
The temperature range is the boiling point of nicotine, so that the temperature in the range selected by the second step of vacuum distillation can be used for distilling and collecting nicotine.
In one embodiment, the vacuum degree of the second vacuum distillation is 0.09MPa to 0.1 MPa. The vacuum degree is higher than the range, so that a large amount of nicotine is distilled off in the distillation process, and the waste and the loss of the nicotine are caused; when the degree of vacuum is less than this range, the efficiency of the distillation is reduced, the distillation time is prolonged, and the energy consumption is increased.
In one embodiment, the distillation is carried out by rectification, and the reflux ratio of the second step of vacuum distillation is 1: 2-1: 4. preferably 1:3, the reflux ratio is too low, the amount of nicotine flowing out in the distillation process is too high, the distillation process is insufficient, and the product purity is lost: too high a reflux ratio leads to too long distillation time, increased energy consumption and little production significance.
Step S4: and (4) carrying out reduced pressure distillation on the nicotine subjected to vacuum distillation in the second step to finally obtain the purified nicotine.
In one embodiment, the vacuum degree of the system is controlled to be 0.09MPa to 0.1MPa when the reduced pressure distillation is carried out, and the distillation temperature is 120 ℃ to 140 ℃.
The nicotine prepared by the method.
According to the method, the nicotine to be treated is distilled at the normal pressure at the temperature of 90-100 ℃, the distillation can ensure that the nicotine does not boil and is not heated to volatilize, but low-boiling-point impurities such as organic solvents and the like remained in the nicotine are continuously heated to volatilize at the temperature of 90-100 ℃, so that the low-boiling-point impurities are distilled out, and the low-boiling-point impurities are removed. The method can avoid the problems that the existing method has overhigh temperature, leads to nicotine volatilization, and can cause the cracking of residual organic solvent and the oxidation and degradation of nicotine due to the action of high temperature and oxygen, and simultaneously carries out two-step vacuum distillation on the nicotine after atmospheric distillation, wherein the temperature of the first-step vacuum distillation is controlled to be 110-150 ℃, so that the residual organic solvent (petroleum ether and the like) after atmospheric distillation can be thoroughly removed, and then the second-step distillation is carried out, the temperature is controlled to be 120-150 ℃, and the temperature range is the boiling point of the nicotine, therefore, the temperature in the range is selected for the second-step vacuum distillation, so that the nicotine can be distilled and collected. Finally, reduced pressure distillation and collection are carried out, and the nicotine obtained by the method is almost colorless and transparent, has pure smell and high purity of 99.693%; the related operation has less manual demand and large treatment capacity, the average daily nicotine treatment amount can reach 100L, and the method is suitable for large-scale production and use.
The invention is further illustrated, but not limited, by the following specific examples.
Example 1
The method for purifying nicotine of the present embodiment comprises the following steps:
1) putting 25L of nicotine into a 30L rectification reaction kettle, setting the temperature at 90 ℃, performing under normal pressure, setting the reflux ratio to be full outflow, keeping the nicotine not boiling in the reaction kettle, continuously introducing nitrogen by using a blowing device, keeping a certain amount of fresh nitrogen circulating in rectification equipment, and continuously performing for 3 hours to enable low-boiling-point substances such as organic solvents and the like to be continuously heated and volatilized, and flowing out along with airflow;
2) the method comprises the following steps of (1) carrying out vacuum distillation on nicotine distilled under normal pressure in two steps, wherein in the first step of distillation, the distillation temperature is raised to 110 ℃, the vacuum degree is 0.08Mpa, the reflux ratio is set to be full outflow, the distillation time is 40min, until no obvious oily matter (organic solvent residue such as petroleum ether) exists on the wall of a glass tube, residual nicotine volatilizes into a pipeline, condensation enters a collection bottle, a small amount of nicotine collected at the section is collected and discarded, and the residual nicotine which is not distilled is obtained;
3) after the collection device is replaced, the vacuum degree is 0.1Mpa, the reflux ratio is 1:3, the residual nicotine which is not distilled is distilled for 4 hours at 130 ℃, and the nicotine is collected.
4) Distilling the nicotine obtained by vacuum distillation in the second step under reduced pressure at a vacuum degree of 0.1Mpa and a distillation temperature of 120 ℃, collecting the purified nicotine, and storing at low temperature.
The nicotine obtained by the preparation of this example and the untreated nicotine product were subjected to component analysis by a mass spectrometer, and the measurement method was as follows:
GC-MS detection conditions:
furnace temperature: 40 ℃ (2min) -250 ℃ (3min), heating rate: 10 ℃/min;
sample inlet temperature: 250 ℃;
helium as carrier gas;
carrier gas flow: 1 ml/min;
a sample introduction system: split flow 50: 1
Sample introduction amount: 2 mu l of the solution;
MS SCAN: 40-500amu solvent extension: 2 min;
the test results of this example 1 are shown in table 1 and fig. 1, and the test results of untreated nicotine are shown in table 2 and fig. 2.
TABLE 1
TABLE 2
As can be seen from the detection results, the purity of the nicotine is improved from 93.089% to 99.693% by processing the nicotine by the method disclosed by the invention.
Example 2
The method for purifying nicotine of the present embodiment comprises the following steps:
1) putting 25L of nicotine into a 30L rectification reaction kettle, setting the temperature at 100 ℃, performing under normal pressure, setting the reflux ratio to be full outflow, keeping the nicotine not boiling in the reaction kettle, continuously introducing nitrogen by using a blowing device, keeping a certain amount of fresh nitrogen circulating in rectification equipment, and continuously performing for 4 hours to enable low-boiling-point substances such as organic solvents and the like to be continuously heated and volatilized, and flowing out along with airflow;
2) the nicotine after atmospheric distillation is subjected to vacuum distillation in two steps, wherein the distillation temperature in the first step is increased to 120 ℃, the vacuum degree is 0.085Mpa, the distillation time is 1h, no obvious oily substance (organic solvent residue such as petroleum ether) on the wall of a glass tube is left, the residual nicotine volatilizes into a pipeline, the nicotine is condensed into a collecting bottle, a small amount of nicotine collected in the section is collected and discarded, and the residual nicotine which is not distilled is obtained;
3) after the collection device is replaced, the vacuum degree is 0.095Mpa, and the residual nicotine which is not distilled is subjected to the second step of distillation at 140 ℃ for 6h, and the nicotine is collected.
4) Distilling the nicotine obtained by vacuum distillation in the second step under vacuum degree of 0.095Mpa and distillation temperature of 130 deg.C, collecting purified nicotine, and storing at low temperature.
The nicotine purity of this example was found to be 99.547%
Example 3
The method for purifying nicotine of the present embodiment comprises the following steps:
1) putting 25L of nicotine into a 30L rectification reaction kettle, setting the temperature at 100 ℃, performing under normal pressure, setting the reflux ratio to be full outflow, keeping the nicotine not boiling in the reaction kettle, continuously introducing argon by using a blower, keeping a certain amount of fresh nitrogen circulating in rectification equipment, and continuously performing for 5 hours to enable low-boiling-point substances such as organic solvents and the like to be continuously heated and volatilized, and flowing out along with airflow;
2) the nicotine after atmospheric distillation is subjected to vacuum distillation in two steps, wherein the distillation in the first step raises the distillation temperature to 150 ℃, the distillation time is 30min at the vacuum degree of 0.085Mpa, no obvious oily substance (organic solvent residue such as petroleum ether) on the wall of a glass tube is left, the residual nicotine volatilizes into a pipeline, the nicotine is condensed into a collecting bottle, and a small amount of nicotine A collected in the section is collected and discarded to obtain the non-distilled nicotine;
3) after the collection device is replaced, the vacuum degree is 0.09Mpa, and the residual nicotine which is not distilled is subjected to the second step of distillation for 5 hours at the temperature of 150 ℃, and the nicotine is collected.
4) Distilling the nicotine obtained by vacuum distillation in the second step under reduced pressure at vacuum degree of 0.095MPA and distillation temperature of 135 deg.C, collecting the purified nicotine, and storing at low temperature.
The nicotine purity of this example was found to be 99.441%.
Example 4
The method for purifying nicotine of the present embodiment comprises the following steps:
1) putting 25L of nicotine into a 30L rectification reaction kettle, setting the temperature at 100 ℃, performing under normal pressure, setting the reflux ratio to be full outflow, keeping the nicotine not boiling in the reaction kettle, continuously introducing argon by using a blower, keeping a certain amount of fresh nitrogen circulating in rectification equipment, and continuously performing for 5 hours to enable low-boiling-point substances such as organic solvents and the like to be continuously heated and volatilized, and flowing out along with airflow;
2) the nicotine after atmospheric distillation is subjected to vacuum distillation in two steps, wherein the distillation temperature in the first step is increased to 120 ℃, the vacuum degree is 0.09Mpa, the distillation time is 50min, no obvious oily substance (organic solvent residue such as petroleum ether) on the wall of a glass tube is left, the residual nicotine volatilizes into a pipeline, the nicotine is condensed into a collecting bottle, and a small amount of nicotine A collected in the section is collected and discarded to obtain the non-distilled nicotine;
3) after the collection device is replaced, the vacuum degree is 0.09Mpa, and the residual nicotine which is not distilled is distilled for 5 hours at 120 ℃ to obtain the nicotine.
4) Distilling the nicotine obtained by vacuum distillation in the second step under reduced pressure at vacuum degree of 0.1Mpa and distillation temperature of 140 deg.C, collecting nicotine D, and storing at low temperature.
The nicotine content of this example was found to be 99.397%.
Comparative example 1
Putting 25L of untreated nicotine into 50L of reduced pressure distillation equipment, and distilling under reduced pressure at 145 ℃ under vacuum; the final nicotine product with high purity was obtained and analyzed by GC-MS according to the detection method in example 1. The results are shown in table 3 and fig. 3.
TABLE 3
As can be seen from table 3 and fig. 3, the conventional distillation process produces more nicotine oxidation products, such as octagon, macrantine, neonicotinoid, dehydroneonicotinoid, cotinine, and the purity of nicotine can be only increased from 93.089% to 97.699%. The traditional nicotine distillation process is under the conditions of reduced pressure and high temperature, the purification treatment of nicotine is carried out, under the condition that the guarantee of complete vacuum cannot be guaranteed, the residual of oxygen components can be avoided in equipment, the nicotine structure is formed by two nitrogen heterocycles, pyridine and hydrogenated pyrrole which are connected through a single bond, the device has instability and is easy to oxidize in air, so that the effects of two factors, namely high temperature and oxygen, in the traditional distillation process are realized, the nicotine is easy to oxidize and crack, new impurities are generated, a large amount of organic solvents are used in the extraction process of the nicotine, the residual organic solvents are also easy to crack and cannot be completely removed in the traditional distillation process, and therefore, the finished product of the nicotine is treated through the conventional reduced pressure distillation process, and the improvement of the purity is. Compared with the traditional nicotine purification process, the nicotine obtained by adopting the nicotine purification process disclosed by the invention is higher in purity, less in nicotine derivatives, and obviously improved in color, smell, taste and the like.
Comparative example 2
This comparative example differs from example 1 only in that the temperature of atmospheric distillation in step 1) was set to 80 ℃. The nicotine content of this comparative example was measured to be 97.82%.
Comparative example 3
This comparative example differs from example 1 only in that the temperature of atmospheric distillation in step 1) was set to 110 ℃. The nicotine content of this comparative example was measured to be 98.34%. From the results, it is understood that the purity of nicotine is reduced due to the high temperature, which causes volatilization of nicotine, and the high temperature and oxygen cause the problems of cracking of residual organic solvent and oxidation and degradation of nicotine itself.
Comparative example 4
This comparative example differs from example 1 only in that step 2) was not included and the nicotine content of the comparative example was measured to be 98.67%.
Comparative example 5
This comparative example differs from example 1 only in that in step 2, the first distillation time was 15 min; the nicotine content of this comparative example was measured to be 98.97%.
Effect examples sensory evaluation test of tobacco juice
Test samples: comparative examples 1-5, examples 1-4, control (untreated nicotine).
The experimental method comprises the following steps: preparing tobacco absolute oil of a test sample into electronic cigarette liquid with the concentration of 1% according to a conventional method, adding 1.5 electronic cigarette liquid into the electronic cigarette, and performing evaluation on color, irritation and offensive odor by professional evaluation personnel.
Grading standard: wherein the color and luster is divided into 20 points, 40 points of irritation and 40 points of miscellaneous qi.
The better the color of the appearance, the higher its score; the smaller the impact of the tobacco liquid on the throat is, the lower the irritation is, and the higher the comfort index score is; the less the miscellaneous gas, the purer the taste and the higher the miscellaneous gas fraction.
The evaluation results are shown in table 4:
TABLE 4
| Group of | Color | Irritation property | Miscellaneous qi | Total up to |
| Example 1 | 20 | 38.56 | 36.34 | 94.9 |
| Example 2 | 20 | 37.12 | 32.15 | 89.27 |
| Example 3 | 20 | 38.74 | 37.78 | 96.52 |
| Example 4 | 20 | 38.21 | 33.42 | 91.63 |
| Control group | 12 | 25.54 | 20.45 | 57.99 |
| Comparative example 1 | 15 | 30.15 | 28.57 | 73.72 |
| Comparative example 2 | 18 | 33.58 | 29.45 | 81.03 |
| Comparative example 3 | 18 | 34.57 | 30.15 | 82.72 |
| Comparative example 4 | 17 | 33.89 | 30.47 | 81.36 |
| Comparative example 5 | 18 | 37.45 | 32.78 | 88.23 |
As can be seen from table 4, compared with untreated nicotine, the nicotine treated by the method of the present invention has significantly improved sensory quality, especially significantly reduced chemical off-gases, and is more suitable for application in electronic cigarettes. The method adopted in the comparative example 1 is a traditional method, and results show that the method is not as good as the method in aspects of color, irritation and miscellaneous gas, and the purity of the obtained nicotine finished product is generally 95-98% by adopting the reduced pressure distillation at 140 ℃, the color is yellowish, the appearance is not good, and the application of the nicotine in the field of biological medicine is limited. The methods of comparative examples 2 to 3 differ from example 1 in that the distillation temperature in step 1) is outside the range of the present invention, and it can be seen from the results that nicotine prepared at too high or too low a temperature experiences a decrease in color, odor, and taste. The method of comparative example 4 is different from example 1 in that step 4) is not included, and it is known from the results that there is a certain reduction in the experience in terms of color, smell, and taste because it is certain that the organic solvent (petroleum ether, etc.) remaining after atmospheric distillation cannot be completely removed by this step, thereby affecting the sensory experience; the first step distillation time of comparative example 5 was less than 30min, and the residue in the pipeline was not handled cleanly, resulting in an adverse sensory experience.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method of purifying nicotine comprising the steps of:
under the condition of introducing protective gas, carrying out normal pressure distillation on the nicotine to be treated at the temperature of 90-100 ℃ to remove low-boiling-point impurities; the protective gas is continuously introduced to keep the gas circulation;
the nicotine after atmospheric distillation is subjected to vacuum distillation in two steps, wherein the first step of vacuum distillation is distillation at the temperature of 110-150 ℃, the distillation is carried out for 30 min-1 h, a small amount of nicotine is obtained by distillation, the small amount of nicotine obtained by distillation is discarded, the residual nicotine which is not distilled is obtained, the reflux ratio of the first step of vacuum distillation is set to be total outflow, and the vacuum degree of the first step of distillation is 0.08-0.09 Mpa;
and the second step of vacuum distillation is to distill the residual undistilled nicotine again at 120-150 ℃ to obtain nicotine, wherein the reflux ratio of the second step of vacuum distillation is 1: 2-1: 4, the vacuum degree of the second step of distillation is 0.09Mpa to 0.1 Mpa;
carrying out reduced pressure distillation on the nicotine subjected to vacuum distillation in the second step to finally obtain purified nicotine; when the reduced pressure distillation is carried out, the vacuum degree of the system is controlled to be 0.09 Mpa-0.1 Mpa, and the distillation temperature of the reduced pressure distillation is 120 ℃ to 140 ℃.
2. The method according to claim 1, wherein the atmospheric distillation reaction time is 3 to 5 hours.
3. The method of claim 1, wherein the protective gas is nitrogen or argon.
4. The process of claim 1, wherein the reflux ratio of the second vacuum distillation is 1: 3.
5. The method according to claim 1, wherein the reduced pressure distillation has a distillation temperature of 120 ℃ and a vacuum degree of 0.1 MPa; or the distillation temperature of the reduced pressure distillation is 130 ℃, and the vacuum degree is 0.095 Mpa; or the distillation temperature of the reduced pressure distillation is 135 ℃, and the vacuum degree is 0.095 Mpa; or the distillation temperature of the reduced pressure distillation is 140 ℃, and the vacuum degree is 0.1 Mpa.
6. The method of claim 1, wherein the atmospheric distillation is atmospheric distillation and the atmospheric distillation reflux ratio is set to a total outflow.
7. The method of claim 1, wherein the vacuum distillation is vacuum distillation.
8. The method according to claim 1, wherein the time of the second vacuum distillation is 4 to 6 hours.
9. The process according to claim 1, characterized in that the atmospheric distillation temperature is 90 ℃ and the protective gas circulation time is 3 h; and/or, the second step vacuum distillation temperature is 130 ℃.
10. The process according to claim 1 or 9, wherein the temperature of the first vacuum distillation is 110 ℃.
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