CN107536099A - A kind of nicotine salt and preparation method thereof - Google Patents
A kind of nicotine salt and preparation method thereof Download PDFInfo
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- CN107536099A CN107536099A CN201710828931.4A CN201710828931A CN107536099A CN 107536099 A CN107536099 A CN 107536099A CN 201710828931 A CN201710828931 A CN 201710828931A CN 107536099 A CN107536099 A CN 107536099A
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Abstract
The invention provides a kind of nicotine salt and preparation method thereof, comprise the following steps：Organic acid is mixed with nicotine, stirs and is reacted, obtains nicotine salt；In terms of mass fraction, the organic acid is 30 60 parts, and nicotine is 40 60 parts.This method is mixed using pure nicotine with organic acid, is had the advantages that simple to operate, convenient for production, safe.Prepared nicotine salt is in stable condition, the wherein stable content of nicotine, unattenuated, tobacco tar color change is not made, make the excitant of nicotine reduce, it is easier to be inhaled into, the soft aroma of electronic cigarette liquid and, to hit larynx sense comfortable, the advantages of being easier to be accessible to the user and being more beneficial for production and sales, it is adapted to widely promote in electronic cigarette field, prepared solid-state nicotine salt is not easy to reveal in packaging, in transport, preserves, using upper safer convenient.
Description
Technical field
The present invention relates to electronic cigarette liquid to allocate applied technical field, in particular to a kind of nicotine salt and its preparation
Method.
Background technology
Electronic cigarette is a kind of electronic product for imitating cigarette, there is outward appearance, smog, taste and the sensation as cigarette.
It is by the means such as being atomized, after nicotine etc. is become into steam, a kind of product for allowing user to suck.
Nicotine (Nicotine), popular name nicotine is the alkaloid that one kind is present in plant of Solanaceae (Solanum), Ye Shiyan
The important component of grass, or the representative of N choline receptor excitomotors, have effect, nothing to N1 and N2 acceptors and central nervous system
Clinical value.Nicotine can be addicting or produce dependence, and reusing nicotine also increases heart speed and rise
Blood pressure simultaneously reduces appetite.Heavy dose of nicotine can cause vomiting and nausea, and people can be dead when serious.
In order to mitigate the excitement of nicotine, make that electronic cigarette liquid mouthfeel is more preferable, is easier to be inhaled into, in tobacco, nicotine
Major part be with organic acid, the stable state as citric acid and malic acid are combined into salt is present, after being purified using industrialization
Nicotine is a kind of unpleasant, bitter, the oily liquid of clarification, high volatility, is easily oxidized in atmosphere and under illumination yellowish
Color liquid, content and color are extremely unstable.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of preparation method of nicotine salt, described to solve the above problems
The preparation method of nicotine salt, mixed using pure nicotine with organic acid, instead of nicotine, organic acid and pure nicotine are equal
For strong acid and highly basic, pH value is 5-3 faintly acid value after acid-base neutralization reaction, and the organic acid after heating is decomposed into titanium dioxide
Carbon and moisture content, the harm to body and environment is not caused, have the advantages that simple to operate, convenient for production, safe.
The second object of the present invention is to provide the nicotine salt prepared by a kind of preparation method of described nicotine salt,
The nicotine salt is in stable condition, wherein the stable content of nicotine, unattenuated, does not make tobacco tar color change, makes the thorn of nicotine
Swashing property reduces, it is easier to be inhaled into, the soft aroma of electronic cigarette liquid and, to hit larynx sense comfortable, it is easier to be accessible to the user and more favourable
In the production and sales the advantages of, it is adapted to widely promote in electronic cigarette field, prepared solid-state nicotine salt is not easy in packaging
Leakage, in transport, preserve, using upper safer convenient.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of preparation method of nicotine salt, comprises the following steps：
Organic acid is mixed with nicotine, stirs and is reacted, obtains nicotine salt；
In terms of mass fraction, the organic acid is 30-60 parts, and nicotine is 40-60 parts.
The preparation method of nicotine salt provided herein, mixed using pure nicotine with organic acid, instead of
Nicotine, organic acid and pure nicotine are strong acid and highly basic, and pH value is 5-3 faintly acid value after acid-base neutralization reaction, is added
Organic acid after heat is decomposed into carbon dioxide and moisture content, does not cause the harm to body and environment, has simple to operate, producer
Just the advantages that, safe.
Preferably, it is described that organic acid is mixed with nicotine, stirs the process reacted, specifically include following steps：
Organic acid is mixed with organic solvent, it is heated, stirred, is mixed after cooling with nicotine, is carried out
Reaction, obtains liquid nicotine salt；
Wherein, the ratio of the organic solvent and the organic acid is (0.8-1)：1.
Preferably, it is described that organic acid is mixed with nicotine, stirs the process reacted, specifically include following steps：
Organic acid is mixed with solid-state nicotine, stirred, and obtained mixed liquor is viscous pasty state, is persistently stirred liquid, is mixed
Close liquid to start to react, generate heat, blocks of solid is crushed into blocks of solid, obtain powdered solid-state nicotine salt by final set.
Preferably, one or two kinds of combination of the organic acid in ethanedioic acid and malic acid.
Preferably, the temperature of the heating is 65-75 DEG C.
Preferably, during the heating, stirring, the time of stirring is 20-30 minutes.
Preferably, the time of the reaction is 3-3.5 hours.
Preferably, the mass ratio of the propane diols and the glycerine is 1:(0.9-1.1)；
The mass ratio of the preferred propane diols and the glycerine is 1:1.
Preferably, the mass ratio of the ethanedioic acid and the malic acid is 1:(0.9-1.1)；
It is furthermore preferred that the mass ratio of the ethanedioic acid and the malic acid is 1:1.
Nicotine salt prepared by the preparation method of described nicotine salt.
Compared with prior art, beneficial effects of the present invention are：
(1) preparation method of nicotine salt provided herein, mixed using pure nicotine with organic acid, generation
For nicotine, organic acid and pure nicotine are strong acid and highly basic, and pH value is 5-3 faintly acid value after acid-base neutralization reaction,
Organic acid after heating is decomposed into carbon dioxide and moisture content, does not cause the harm to body and environment, has simple to operate, production
The advantages that convenient, safe.
(2) nicotine salt prepared by method provided herein, it is the stable content of nicotine, unattenuated, do not make cigarette
Oily color change, makes the excitant of nicotine reduce, it is easier to be inhaled into, the soft aroma of electronic cigarette liquid and, to hit larynx sense comfortable.
(3) nicotine salt prepared by method provided herein, have and be easier to be accessible to the user and be more beneficial for
The advantages of production and sales, it is adapted to widely promote in electronic cigarette field.
(4) the solid-state nicotine salt prepared by method provided herein, is not easy to reveal in packaging, in transport, protects
Deposit, using upper safer convenient
Embodiment
Technical scheme is clearly and completely described below in conjunction with embodiment, but ability
Field technique personnel will be understood that following described embodiment is part of the embodiment of the present invention, rather than whole embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.Unreceipted actual conditions person in embodiment, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or instrument
Unreceipted production firm person, it is the conventional products that can be obtained by commercially available purchase.
A kind of preparation method of nicotine salt, comprises the following steps：
Organic acid is mixed with nicotine, stirs and is reacted, obtains nicotine salt；
In terms of mass fraction, the organic acid is 30-60 parts, and nicotine is 40-60 parts.
In this application, organic acid has acidity, and nicotine has strong basicity, is carried out after being mixed under certain proportion anti-
Should, the nicotine salt stablized.
Preferably, it is described that organic acid is mixed with nicotine, stirs the process reacted, specifically include following steps：
Organic acid is mixed with organic solvent, it is heated, stirred, is mixed after cooling with nicotine, is carried out
Reaction, obtains liquid nicotine salt；
Wherein, the ratio of the organic solvent and the organic acid is (0.8-1)：1, the preferred organic solvent with
The ratio of the organic acid is 1:1.
Organic solvent is added, makes reaction be more prone to carry out, obtains the nicotine salt of liquid.
Preferably, it is described that organic acid is mixed with nicotine, stirs the process reacted, specifically include following steps：
Organic acid is mixed with solid-state nicotine, stirred, and obtained mixed liquor is viscous pasty state, is persistently stirred liquid, is mixed
Close liquid to start to react, generate heat, blocks of solid is crushed into blocks of solid, obtain powdered solid-state nicotine salt by final set.
Preferably, one or two kinds of combination of the organic acid in ethanedioic acid and malic acid.
Ethanedioic acid refers to oxalic acid again, and the acidity of oxalic acid is stronger than acetic acid (acetic acid) 10000 times, is the strong acid in organic acid.One
Level dissociation constant Ka1=5.9 × 10-2, secondary ionization constant Ka2=6.4 × 10-5, there is the sour general character.
Malic acid has 3 kinds of L MALIC ACID, D-malic acid and DL-malic acid isomers.Naturally occurring malic acid is all L-type
, almost it is present in all fruits, with most in pomaceous fruit.Malic acid is colorless needle crystals, or white crystalline powder, nothing
Smelly, with irritant frank tart flavour, 127-130 DEG C of fusing point is soluble in water, 55.59/100mL (20 DEG C), is dissolved in ethanol, insoluble
In ether.There are hygroscopicity, the pH value 2.4 of 1% (quality) aqueous solution.
Ethanedioic acid and malic acid are all acid stronger acid, are swift in response with nicotine, stably, the two preferable equal proportion
Reacted after mixing with nicotine.
Preferably, the temperature of the heating is 65-75 DEG C.
Heating and temperature control is at 65-75 DEG C, and preferably 70 DEG C, organic acid is completely dissolved in organic solvent.
Preferably, during the heating, stirring, the time of stirring is 20-30 minutes.
Stirring is advantageous to radiate, and avoids excessive heat from influenceing the stability of nicotine salt.
Preferably, the time of the reaction is 3-3.5 hours.
Preferably, the mass ratio of the propane diols and the glycerine is 1:(0.9-1.1)；
The mass ratio of the preferred propane diols and the glycerine is 1:1.
Propane diols and glycerine are as solvent, and overall flow is good, and performance at high temperature is more stable.
Preferably, the mass ratio of the ethanedioic acid and the malic acid is 1:(0.9-1.1)；
It is furthermore preferred that the mass ratio of the ethanedioic acid and the malic acid is 1:1.
Nicotine salt prepared by the preparation method of described nicotine salt.
Nicotine salt stability prepared by the preparation method of nicotine salt provided herein is good, and content is not easy to decline
Subtract, tobacco tar is changed color.Nicotine salt after heating is decomposed into nicotine, carbon dioxide and moisture content, and Buddhist nun's Gu is reduced with this
The excitement that fourth is brought, make tobacco tar mouthfeel more preferable, it is easier to be inhaled into.Make the excitant of nicotine reduce, it is easier to it is inhaled into,
The soft aroma of electronic cigarette liquid and, to hit larynx sense comfortable.The advantages of with being easier to be accessible to the user and being more beneficial for production and sales, fit
Conjunction is widely promoted in electronic cigarette field.
Embodiment 1
A kind of preparation method of liquid nicotine salt, is comprised the following steps that：
(1) 1 kilogram of nicotine salt is prepared；
(2) it is 300g to weigh ethanedioic acid 30%, and it is 300g to weigh propane diols 30%, and ethanedioic acid is 1 with propane diols proportioning:1；
(3) ethanedioic acid and propane diols are added into glass beaker；
(4) glass beaker is placed on heater, started to warm up up to constant temperature after 70 degree；20 points are stirred since heating process
Clock stops heating after reaching fully dissolving, and ethanedioic acid solution is made；
(5) after ethanedioic acid solution is down to normal temperature, it is 400g to weigh pure nicotine 40%, is added in ethanedioic acid solution；
(6) after ethanedioic acid solution and pure nicotine mix, mixed liquor shows cloudy state and spontaneous heating, starts response procedures.
Mixed liquor stops reacting and is cooled to normal temperature state after 3 hours, now shows clear yellow liquid, the preparation of nicotine salt
Process is completed.
Embodiment 2
A kind of preparation method of liquid nicotine salt, specifically includes following steps：
(1) 1 kilogram of nicotine salt is prepared；
(2) it is 300g to weigh malic acid 30%, and it is 300g to weigh propane diols 30%, and malic acid is 1 with propane diols proportioning:1；
(3) malic acid and propane diols are added into glass beaker；
(4) glass beaker is placed on heater, started to warm up up to constant temperature after 70 degree；20 points are stirred since heating process
Clock stops heating after reaching fully dissolving, and malic acid solution is made；
(5) after malic acid solution is down to normal temperature, it is 400g to weigh pure nicotine 40%, is added in malic acid solution；
(6) after malic acid solution and pure nicotine mix, mixed liquor shows cloudy state and spontaneous heating, starts response procedures.
Mixed liquor stops reacting and is cooled to normal temperature state after 3 hours, now shows clear yellow liquid, the preparation of nicotine salt
Process is completed.
Embodiment 3
A kind of preparation method of liquid nicotine salt, is comprised the following steps that：
(1) 1 kilogram of nicotine salt is prepared；
(2) it is 300g to weigh ethanedioic acid 30%,
(3) it is 100g to weigh propane diols 10%, and it is 200g to weigh glycerine 20%, and propane diols is mixed with glycerine
It is even；
(4) ethanedioic acid and solvent (propane diols, glycerine) proportioning are 1:1；
(5) ethanedioic acid and solvent are added into glass beaker；
(6) glass beaker is placed on heater, started to warm up up to constant temperature after 70 degree；20 points are stirred since heating process
Clock stops heating after reaching fully dissolving, and ethanedioic acid solution is made；
(7) after ethanedioic acid solution is down to normal temperature, it is 400g to weigh pure nicotine 40%, is added in ethanedioic acid solution；
(8) after ethanedioic acid solution and pure nicotine mix, mixed liquor shows cloudy state and spontaneous heating, starts response procedures.
Mixed liquor stops reacting and is cooled to normal temperature state after 3 hours, now shows clear yellow liquid, the preparation of nicotine salt
Process is completed.
Embodiment 4
A kind of preparation method of liquid nicotine salt, is comprised the following steps that：
(1) 1 kilogram of nicotine salt is prepared；
(2) it is 100g to weigh ethanedioic acid 10%, weighs malic acid 10%100g；
(3) it is 200g to weigh propane diols 20%, and organic acid (ethanedioic acid, malic acid) is 1 with propane diols proportioning:1；
(7) organic acid and propane diols are added into glass beaker；
(8) glass beaker is placed on heater, started to warm up up to constant temperature after 70 degree；20 points are stirred since heating process
Clock stops heating after reaching fully dissolving, and organic acid soln is made；
(9) after organic acid soln is down to normal temperature, it is 600g to weigh pure nicotine 60%, is added in organic acid soln；
(10) after organic acid soln and pure nicotine mix, mixed liquor shows cloudy state and spontaneous heating, starts response procedures.
Mixed liquor stops reacting and is cooled to normal temperature state after 3 hours, now shows clear yellow liquid, the preparation of nicotine salt
Process is completed.
Embodiment 5
A kind of preparation method of solid-state nicotine salt, is comprised the following steps that：
(1) 1 kilogram of solid-state nicotine salt is prepared；
(2) it is 600g to weigh ethanedioic acid 60%；
(3) it is 400g to weigh pure nicotine 40%, and ethanedioic acid is 1 with pure nicotine proportioning:1.5；
(4) ethanedioic acid and pure nicotine are added into stainless steel measuring cup；
(5) ethanedioic acid starts to react and generated heat after adding stainless steel measuring cup with pure nicotine, is now viscous liquid, leads to
Crossing to be stirred continuously makes it fully react to close solidification；
(6) block nicotine salt is taken out after it is fully cured and crushed；
(7) the solid-state nicotine salt after crushing is white powdered, and preparation process is completed；
The solid-state nicotine salt prepared by this method, fragrance is clear, and excitant is very small, convenient to preserve transport.
Embodiment 6
A kind of preparation method of solid-state nicotine salt, is comprised the following steps that：
(1) 1 kilogram of solid-state nicotine salt is prepared；
(2) it is 250g to weigh malic acid 25%；
(3) it is 250g to weigh ethanedioic acid 25%；
(4) it is 500g to weigh pure nicotine 50%, and organic acid (malic acid, ethanedioic acid) is 1 with pure nicotine proportioning：1；
(5) organic acid and pure nicotine are added into stainless steel measuring cup；
(6) organic acid starts to react and generated heat after adding stainless steel measuring cup with pure nicotine, is now viscous liquid, leads to
Crossing to be stirred continuously makes it fully react to close solidification；
(7) block nicotine salt is taken out after it is fully cured and crushed；
(8) the solid-state nicotine salt after crushing is white powdered, and preparation process is completed.
The rat airway smooth muscle cells proliferative effect of experimental example 1
(1) material
Male SD rat is purchased from Guangdong Province medical faunae center；Nicotine is purchased from German Meck companies；DMEM/F12 is cultivated
Base, hyclone are purchased from Gibco companies；MCA, MG624, small anti-rat α-SMA antibody, FITC mark goat anti-mouse iggs
It is purchased from Sigma companies；HRP- goat anti-rabbit igg antibodies, WesternBlottingLuminolReagent are purchased from SantaCruz
Company；EDU kits are purchased from RiboBio companies；CyclinD1 rabbit-antis monoclonal antibody is purchased from CST companies；Triumphant base holoprotein carries
Kit, triumphant base determination of protein concentration kit, GAPDH rabbit-anti monoclonal antibodies is taken to be purchased from KeygenBio companies.
(2) method
(1) cell primary culture and cellular immunofluorescence identification：Cell primary culture and cellular immunofluorescence identification cleaning
4~8 weeks SD male rats of level, 2% amobarbital intraperitoneal injection of anesthesia, under rapid aseptic condition separation take out bronchus, application
Enzyme digestion and the tissue Explant culture culture Primary rat airway smooth muscle cells of improvement
(ratairwaysmoothmusclecells, RASMCs).The 3rd~6 generation cell is taken to be applied to experiment, 4% paraformaldehyde is fixed
Cell, 0.3%triton-X-100 penetration cells, 3%BSA closings, small anti-rat α-actin monoclonal primary antibodies are added dropwise,
FITC marks goat anti-mouse IgG secondary antibody, and DAPI is redyed, lucifuge fluorescence microscope, film making.Every piece takes 5 to regard at random
200 cells are detected in open country, each visual field.Calculate α-actin expression positive cell in each visual field and account for the visual field total cell number
Ratio, it is smooth muscle cell purity.
(2) BeckmanZ2 cell analysis calculating instrument detection cell quantity：Vitellophag passes on, and each 2ml cell suspensions are uniform
Assign to and grown in each hole of six orifice plates.Using containing 1% hyclone culture medium starved cells 24h, make cell growth synchronous, be in
The G0 phases.Experiment packet：Control group, nicotine independent role group (comparative example group), embodiment 1-6 groups.The tire ox of the control group 1%
Blood serum medium, other groups are prepared using 1% hyclone culture medium, and the propagation feelings of cell are detected using the 24h periods
Condition.Pancreatin digests, and collects cell suspension and is managed to each 1.5mlEP for carrying out mark, instrument meter is counted using BeckmanZ2 cell analysis
Number.
Experimental result is as shown in table 1.
Influence of the nicotine salt of table 1 to rat airway smooth muscle cells quantity
Note：Compared with alone nicotine group,aP ＜ 0.05；Compared with control group,bP ＜ 0.05.
Test result indicates that nicotine salt provided herein has weaker stimulation to rat airway smooth muscle cells
Property, it is statistically significant that comparing difference is individually organized with nicotine.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that various embodiments above is only used
To illustrate technical scheme, rather than its limitations；It will be understood by those within the art that：Without departing substantially from this hair
In the case of bright spirit and scope, the technical scheme described in foregoing embodiments can be modified, or to wherein
Some or all of technical characteristic carries out equivalent substitution；And these are changed or are replaced, the essence of appropriate technical solution is not made
Depart from the scope of various embodiments of the present invention technical scheme；It is, therefore, intended that include belonging to the present invention in the following claims
In the range of all these substitutions and modifications.
Claims (10)
1. a kind of preparation method of nicotine salt, it is characterised in that comprise the following steps：
Organic acid is mixed with nicotine, stirs and is reacted, obtains nicotine salt；
In terms of mass fraction, the organic acid is 30-60 parts, and nicotine is 40-60 parts.
2. the preparation method of nicotine salt according to claim 1, it is characterised in that described to mix organic acid and nicotine
Close, the process that stirring is reacted, specifically include following steps：
Organic acid is mixed with organic solvent, it is heated, stirred, mixes, is reacted with nicotine after cooling,
Obtain liquid nicotine salt；
Wherein, the ratio of the organic solvent and the organic acid is (0.8-1)：1.
3. the preparation method of nicotine salt according to claim 1, it is characterised in that described to mix organic acid and nicotine
Close, the process that stirring is reacted, specifically include following steps：
Organic acid is mixed with solid-state nicotine, stirred, and obtained mixed liquor is viscous pasty state, is persistently stirred liquid, mixed liquor
Start to react, generate heat, blocks of solid is crushed into blocks of solid, obtain powdered solid-state nicotine salt by final set.
4. the preparation method of nicotine salt according to claim 1, it is characterised in that the organic acid be selected from ethanedioic acid and
One or two kinds of combination in malic acid.
5. the preparation method of nicotine salt according to claim 2, it is characterised in that the temperature of the heating is 65-75
℃。
6. the preparation method of nicotine salt according to claim 2, it is characterised in that during the heating, stirring,
The time of stirring is 20-30 minutes.
7. the preparation method of nicotine salt according to claim 2, it is characterised in that the time of the reaction is 3-3.5
Hour.
8. the preparation method of nicotine salt according to claim 2, it is characterised in that the organic solvent is selected from propane diols
With one or two kinds of combination in glycerine；
Preferably, the mass ratio of the propane diols and the glycerine is 1:(0.9-1.1)；
The mass ratio of the preferred propane diols and the glycerine is 1:1.
9. the preparation method of nicotine salt according to claim 4, it is characterised in that the ethanedioic acid and the malic acid
Mass ratio be 1:(0.9-1.1)；
Preferably, the mass ratio of the ethanedioic acid and the malic acid is 1:1.
10. the nicotine salt prepared by the preparation method of the nicotine salt according to claim any one of 1-9.
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| CN114868955A (en) * | 2022-05-09 | 2022-08-09 | 深圳市吉迩技术有限公司 | Preparation method of nicotine salt, nicotine salt and aerosol product |
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