CN115868662A - Novel nicotine salt, preparation method thereof and atomized liquid - Google Patents

Novel nicotine salt, preparation method thereof and atomized liquid Download PDF

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Publication number
CN115868662A
CN115868662A CN202211668618.6A CN202211668618A CN115868662A CN 115868662 A CN115868662 A CN 115868662A CN 202211668618 A CN202211668618 A CN 202211668618A CN 115868662 A CN115868662 A CN 115868662A
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China
Prior art keywords
nicotine salt
acid
parts
electrolyzed water
nicotine
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CN202211668618.6A
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Chinese (zh)
Inventor
夏瑞
况利平
王华文
王晓莉
赵贯云
赵波洋
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Dongguan Jichun Biotechnology Co ltd
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Dongguan Jichun Biotechnology Co ltd
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Abstract

The invention relates to the field of electronic atomized liquid, in particular to a novel nicotine salt, a preparation method thereof and atomized liquid, wherein the novel nicotine salt is prepared by mixing and reacting 5-20 parts of acidic electrolyzed water, 1-10 parts of organic acid, 10-30 parts of nicotine and 40-80 parts of glycerol according to mass percentage; the preparation method comprises the following steps: (A) Adding acidic electrolyzed water and organic acid into nicotine, mixing and stirring; and (B) adding a glycerol magnetic stirrer for mixing and reacting. The novel nicotine salt is sequentially added with the propylene glycol and the glycerol to be mixed and stirred to obtain atomized liquid. Because the acidic electrolyzed water is colorless and tasteless, has acidic characteristics and enriched H +, and is used for replacing or partially replacing organic acid to generate nicotine salt, the acidic electrolyzed water is safer, has no peculiar smell and stimulation caused by the traditional organic acid, has better smoking experience and comfort, and generates nicotine salt by using water to directly react with acid and alkali, so the mist is more humid and more flexible, and the taste is better.

Description

Novel nicotine salt, preparation method thereof and atomized liquid
Technical Field
The invention relates to the field of electronic atomization, in particular to a novel nicotine salt, a preparation method thereof and an atomized liquid.
Background
The electronic atomization device atomizes atomized liquid by means of heating, atomization and the like so as to achieve the aim of absorbing nicotine by a human body. The electronic atomization equipment has the characteristics of zero tar, no suspended solid particles, no carbon monoxide and the like. The traditional atomized liquid solvents are mainly propylene glycol and glycerin, the mouth feel is good in reduction degree and less in irritation in the pumping process, but on one hand, as the boiling point of the glycerin is high and the glycerin is easy to absorb moisture, aerosol generated in the atomizing process is not easy to condense in the air and can be condensed into a plurality of tiny liquid drops to be suspended in the air, and obvious fog can be generated when a consumer uses the atomized liquid solvents, so that the appearance of a city is influenced in public places; on the other hand, the mists contain nicotine or nicotine salt and other substances, which also cause certain troubles to the public.
The nicotine reacts with acid to form nicotine salt, which can reduce throat feeling and discomfort caused by high concentration nicotine.
Chinese patent application CN 113880802A discloses a tartaric acid-nicotine salt, its preparation method and application, and preparation method of anhydrous tartaric acid crystal. The preparation method of the tartaric acid-nicotine salt comprises the following steps: mixing and stirring the anhydrous tartaric acid crystal and propylene glycol to prepare an anhydrous tartaric acid solution; nicotine is mixed with an anhydrous tartaric acid solution. The raw materials in the preparation method of the tartaric acid-nicotine salt adopt anhydrous tartaric acid crystals, propylene glycol and nicotine, and because the solubility, melting point, dissolution rate, biological effectiveness and other aspects of the anhydrous tartaric acid crystals are different from those of tartaric acid with crystal water on the market, carboxyl groups of the anhydrous tartaric acid crystals are more likely to be subjected to neutralization reaction with alkaline groups to generate salts, so that the pungent feeling or throat hitting feeling of users caused by nicotine can be eliminated, and the tartaric acid-nicotine salt prepared by the preparation method is particularly suitable for preparing non-combustion tobacco products.
Chinese patent application CN 114343229A discloses a preparation method of a novel nicotine salt. The preparation method comprises the following steps: s1, adding organic acid into a solvent, and heating to dissolve; s2, adding nicotine, heating and stirring to obtain nicotine salt; the organic acid used in the invention is one of benzoic acid, dihydroxybenzoic acid, vanillic acid, cinnamic acid, nicotinic acid, salicylic acid, sorbic acid, levulinic acid and lactic acid. The invention also takes the mixed acid as the raw material, adopts the mode of charging materials step by step, so that the prepared nicotine salt has unique flavor, the electronic atomized liquid is more similar to the taste of the traditional cigarette, and the nicotine salt can form a gel structure by adding the auxiliary acid, thereby increasing the stability and being convenient for storage; the preparation method is simple in preparation process, strong in operability and suitable for industrial production.
Chinese patent application CN 115251451A discloses an electronic atomized liquid and a preparation method thereof. An electronic atomized liquid comprises 20 to 50 parts of dimethyl sulfoxide, 30 to 100 parts of 3-methyl-2-butanol, 5 to 20 parts of water, 0.5 to 6 parts of nicotine and 0.4 to 7.5 parts of organic acid; the method comprises the following steps: mixing nicotine and organic acid, adding 40-50% of dimethyl sulfoxide, 3-methyl-2-butanol and water, heating and uniformly stirring, cooling to room temperature, standing to obtain nicotine salt, adding the rest components, and uniformly stirring at room temperature to obtain the electronic atomized liquid. The electronic atomization liquid can be used for obtaining similar effects such as smoke amount and taste, but the components are more harmless, micromolecular carbonyl compounds are not easy to generate, and the carcinogenicity of the electronic atomization liquid is greatly reduced.
However, the existing nicotine salt preparation method has the problems of unreasonable raw material selection, strong organic acid peculiar smell, insufficient suppleness, influence on the mouthfeel of atomized liquid and the like.
Disclosure of Invention
In order to overcome the defects that in the prior art, the organic acid reacts with nicotine to generate nicotine salt, the safety is low, the cost is high, and the taste is adversely affected by an external chemical reagent, so that the smoke has peculiar smell, the smoking experience is poor, and the taste is poor. The invention provides a novel nicotine salt, a preparation method thereof and atomized liquid.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a novel nicotine salt is prepared by mixing acidic electrolyzed water, organic acid, glycerol and nicotine, and reacting.
Preferably, the acidic electrolyzed water comprises 5-20 parts by mass of the acidic electrolyzed water, 1-10 parts by mass of the organic acid, 10-30 parts by mass of the nicotine and 40-80 parts by mass of the glycerol.
Preferably, the acidic electrolyzed water is obtained by adopting a salt electrolyte, adjusting the electrolysis time, electrolyzing by an electrolyzed water generator, and filtering by an anode membrane after H & lt + & gt is enriched.
Preferably, the salt electrolyte is food-grade potassium carbonate.
Preferably, the pH value of the acidic electrolyzed water is 2-5.
Preferably, the organic acid is one or more of benzoic acid, lactic acid, dihydroxybenzoic acid, vanillic acid, cinnamic acid, nicotinic acid, salicylic acid, sorbic acid and levulinic acid.
A preparation method of a novel nicotine salt comprises the following steps:
(A) Adding acidic electrolyzed water and organic acid into nicotine, mixing and stirring;
(B) Then adding glycerol, and mixing for reaction.
Preferably, step (B) is carried out for mixing reaction for 3-4h by using a magnetic stirrer.
An atomized liquid is prepared by sequentially adding propylene glycol and glycerol into novel nicotine salt, and mixing under stirring.
Preferably, the nicotine salt is 10-20 parts by mass, the propylene glycol is 50-60 parts by mass, and the glycerol is 30-40 parts by mass.
The acidic electrolyzed water is acidic water with pH value of 2-5, which is generated by adding a salt electrolyte (potassium carbonate) solution through electrolysis, adjusting electrolysis time and electrolysis pressure and enriching H + to an anode; the acidic property and the enriched H + of the nicotine salt have the condition that the nicotine salt can be generated through acid-base reaction with nicotine, water is colorless and tasteless, bad mouthfeel cannot be brought to atomized liquid, and the atomized liquid prepared by taking the nicotine salt as a raw material is more soft and smooth to suck and is moist and has better mouthfeel due to the addition of the water; the acidic electrolyzed water can replace or partially replace organic acid to react with nicotine to generate nicotine salt, and the atomized liquid prepared by the method has better taste and no peculiar smell.
Detailed Description
The following describes specific embodiments of the present invention in terms of raw material composition, formulation, specific preparation steps, test results, and the like.
Introduction of raw materials
Figure BDA0004015633130000031
1. The novel nicotine salt comprises the raw material components and the proportion of the components (by mass percent)
TABLE 1 Nicotine salt formulation
Examples Nicotine Acidic electrolyzed water Benzoic acid Glycerol
1 20 17 2 60
2 20 15 5 60
3 20 12 8 60
4 20 10 10 60
CK 20 0 20 60
Wherein CK represents a blank control comparative example, in which acidic electrolyzed water was not added at the time of mixing reaction.
2. The concrete preparation steps
(1) Preparing acidic electrolyzed water: adopting food-grade potassium carbonate, adjusting electrolysis time, electrolyzing by an electrolyzed water generator, and enriching H + into an anode membrane to filter to obtain acidic electrolyzed water with the pH value of 2-5;
(2) Adding 5-20 parts of acidic electrolyzed water and 1-10 parts of benzoic acid into 10-30 parts of nicotine, mixing and stirring, adding 40-80 parts of glycerol magnetic stirrer, and mixing and reacting for 3-4h;
(3) Mixing and stirring 10-20 parts of the prepared nicotine salt and 50-60 parts of propylene glycol;
(4) And (4) adding 30-40 parts of glycerol into the liquid obtained in the step (3), and uniformly mixing and stirring to obtain atomized liquid.
3. Sensory evaluation
The sensory evaluation mode and the score are described as follows:
appearance: the visual state of the atomized liquid when standing at room temperature, wherein the uniform and transparent time is 5 minutes, and the time is 0 minute when the atomized liquid is turbid or layered;
irritation: the irritation is mainly irritation to throat and nasal cavity, and has no irritation of 5-4 points, slight irritation of 4-3 points, moderate irritation of 3-2 points, and obvious irritation of 2-1 points;
visible degree of fog: the degree of visible fog generated by the atomized liquid during large-cycle suction or pulmonary suction is adopted, and the atomized liquid has 5 to 4 minutes of visual non-fog, 4 to 3 minutes of slight fog, 3 to 2 minutes of light fog and 2 to 1 minute of obvious fog;
the operation of the sensory evaluation is described below:
respectively mixing 15 parts of nicotine salt prepared in the above examples 1-4 and CK with 60 parts of propylene glycol, and stirring; then respectively adding 30 parts of glycerol, mixing and stirring uniformly to obtain 5 kinds of atomized liquid; sensory evaluation was performed on the above 5 kinds of atomized liquids by 30 panelists (male: female = 3). Wherein, each test technician adopts the lung suction method to suck 10 mouths of each atomized liquid, each mouth is separated by 10 seconds, and the interval time of sucking different atomized liquids is not less than 20 minutes, so as to avoid mutual influence. The sensory evaluation items included 5 items of throat hit sensation, irritation, softness, miscellaneous/aftertaste, and top sensation, and the comparison results are shown in table 2 below.
TABLE 2 sensory evaluation of Nicotine salts
Examples Sensory evaluation results
1 Strong throat-hitting feeling, no irritation, good compliance, no abnormal smell, moistening, and good feeling of the head.
2 Strong throat-hitting feeling, no irritation, good compliance, no odor, moistening, and strong feeling of feeling at the head.
3 Strong throat-hitting feeling, no irritation, good compliance, no odor, fineness, and moistening, and strong feeling of the upper head.
4 Strong throat-hitting feeling, no irritation, softness, no peculiar smell and strong feeling of feeling at the head.
CK The throat-hitting feeling is slightly weak, the throat-hitting feeling is slightly irritant, the throat-hitting feeling is relatively smooth, the throat-hitting feeling is slightly peculiar, and the feeling of the head-up is slightly weak.
Among them, 20 smoking technicians all selected the atomized liquid prepared by using nicotine salt prepared by using electrolyzed water in examples 1 to 4, had better smoking experience, strong throat hitting feeling, strong head feeling, fine and smooth fog and no peculiar smell, and the throat hitting feeling means that throat feels itchy or uncomfortable after smoking electronic cigarette smoke.
From the test results: 1. the nicotine salt prepared by adding the acidic electrolyzed water has stronger top feeling; 2. the nicotine salt mist prepared by using the acidic electrolyzed water is more flexible and moist; 3. the nicotine salt fog prepared by using the acidic electrolyzed water has no peculiar smell, is more delicate and has long-lasting fragrance.
The invention relates to a preparation method of a novel nicotine salt, which uses acidic electrolyzed water to carry out acid-base reaction, wherein the acidic electrolyzed water is acidic water which is generated by adding a salt electrolyte (potassium carbonate) solution through electrolysis, adjusting the electrolysis time and the electrolysis pressure, and enriching H + to an anode, wherein the pH value is 2-5; the acidic property and the enriched H + of the nicotine powder have the condition that the nicotine powder can generate acid-base reaction with nicotine to generate nicotine salt, meanwhile, water is colorless and tasteless, and does not bring bad taste to atomized liquid, and the atomized liquid prepared by taking the nicotine salt as a raw material is more smooth and soft to suck and is moist and has better taste due to the addition of the water; the acidic electrolyzed water can replace or partially replace organic acid to react with nicotine to generate nicotine salt, and the atomized liquid prepared by the method has better taste and no peculiar smell.
In the preparation of the acidic electrolyzed water, the potassium carbonate can be replaced by other salt-added electrolytes such as sodium carbonate, sodium bicarbonate, potassium bicarbonate and potassium hydroxide.
Variations and modifications to the above-described embodiments may occur to those skilled in the art based upon the disclosure and teachings of the above specification. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims (10)

1. A novel nicotine salt is characterized by being prepared by mixing acidic electrolyzed water, organic acid, glycerol and nicotine for reaction.
2. A novel nicotine salt according to claim 1, wherein the acidic electrolyzed water is 5-20 parts, the organic acid is 1-10 parts, the nicotine is 10-30 parts, and the glycerol is 40-80 parts by mass.
3. The novel nicotine salt according to claim 1 or 2, wherein the acidic electrolyzed water is obtained by electrolyzing the acidic electrolyzed water by an electrolyzed water generator by adding a salt electrolyte, and enriching H + into an anode membrane for filtration.
4. A novel nicotine salt as claimed in claim 3, wherein the salt electrolyte is food grade potassium carbonate.
5. A novel nicotine salt according to claim 1 or 2, characterised in that the acidic electrolyzed water has a pH value of 2-5.
6. A novel nicotine salt according to claim 1 or 2, wherein the organic acid is one or more of benzoic acid, lactic acid, dihydroxybenzoic acid, vanillic acid, cinnamic acid, nicotinic acid, salicylic acid, sorbic acid, levulinic acid.
7. A preparation method of a novel nicotine salt comprises the following steps:
(A) Adding acidic electrolyzed water and organic acid into nicotine, mixing and stirring;
(B) Then adding glycerol, and mixing for reaction.
8. The method for preparing a novel nicotine salt according to claim 7, wherein step (B) is carried out by mixing and reacting for 3-4h with a magnetic stirrer.
9. An atomized liquid, which is obtained by adding the novel nicotine salt as claimed in any one of claims 1 to 6 to propylene glycol and glycerol in sequence, mixing and stirring.
10. The atomized liquid of claim 9, wherein the nicotine salt is 10 to 20 parts by mass, the propylene glycol is 50 to 60 parts by mass, and the glycerol is 30 to 40 parts by mass.
CN202211668618.6A 2022-12-24 2022-12-24 Novel nicotine salt, preparation method thereof and atomized liquid Pending CN115868662A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006004646A1 (en) * 2004-06-28 2006-01-12 Nektar Therapeutics Aerosol formulation comprising nicotine salt
CN102423110A (en) * 2011-07-24 2012-04-25 红云红河烟草(集团)有限责任公司 Method for improving smoking quality of high-nicotine cigarettes
US20120255567A1 (en) * 2009-09-16 2012-10-11 Philip Morris Products S.A. Improved device and method for delivery of a medicament
CN111039715A (en) * 2019-12-20 2020-04-21 西南科技大学 Multi-effect nicotine water aqua and preparation method thereof
CN111187250A (en) * 2020-01-08 2020-05-22 深圳黑尔格科技有限公司 Method for preparing optically active nicotine in split mode
CN114343229A (en) * 2022-01-24 2022-04-15 深圳市真味生物科技有限公司 Preparation method of novel nicotine salt
EP4094594A1 (en) * 2021-05-25 2022-11-30 Consumer Brands International s.r.o. A filing of a nicotine formulation, in particular a nicotine sachet and the method of its manufacture, and a mixture of nicotine salts and the method of its manufacture
CZ2021255A3 (en) * 2021-05-25 2022-12-07 Consumer Brands International s.r.o. Mixture of nicotine salts and producing it

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006004646A1 (en) * 2004-06-28 2006-01-12 Nektar Therapeutics Aerosol formulation comprising nicotine salt
US20060018840A1 (en) * 2004-06-28 2006-01-26 Nektar Therapeutics Aerosolizable formulation comprising nicotine
US20120255567A1 (en) * 2009-09-16 2012-10-11 Philip Morris Products S.A. Improved device and method for delivery of a medicament
CN102423110A (en) * 2011-07-24 2012-04-25 红云红河烟草(集团)有限责任公司 Method for improving smoking quality of high-nicotine cigarettes
CN111039715A (en) * 2019-12-20 2020-04-21 西南科技大学 Multi-effect nicotine water aqua and preparation method thereof
CN111187250A (en) * 2020-01-08 2020-05-22 深圳黑尔格科技有限公司 Method for preparing optically active nicotine in split mode
EP4094594A1 (en) * 2021-05-25 2022-11-30 Consumer Brands International s.r.o. A filing of a nicotine formulation, in particular a nicotine sachet and the method of its manufacture, and a mixture of nicotine salts and the method of its manufacture
CZ2021255A3 (en) * 2021-05-25 2022-12-07 Consumer Brands International s.r.o. Mixture of nicotine salts and producing it
CN114343229A (en) * 2022-01-24 2022-04-15 深圳市真味生物科技有限公司 Preparation method of novel nicotine salt

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