CN116172236A - Composite nicotine salt and preparation method thereof - Google Patents

Abstract

The invention discloses a composite nicotine salt and a preparation method thereof, and relates to the technical field of nicotine product production. A method for preparing a composite nicotine salt, comprising the following steps: S1, mixing an organic acid, nicotine, and an organic solvent to obtain a single nicotine salt; S2, repeating step S1 to obtain a different single nicotine salt; S3, mixing a different single The nicotine salts are mixed to obtain a composite nicotine salt; the molar ratio of the organic acid to nicotine is 0.7-1.7:1. In the preparation method of the present invention, a single nicotine salt is obtained by mixing an organic acid with nicotine and an organic solvent, and then compounding different nicotine salts according to a specific ratio to obtain a compound nicotine salt with clear ingredients, bright taste and multiple layers of taste; the The preparation method has simple process operation and strong process repeatability, is suitable for industrial production, and can be mass-produced on a large scale.

Description

A composite nicotine salt and preparation method thereof

Technical Field

The present invention relates to the technical field of nicotine product production, and in particular to a composite nicotine salt and a preparation method thereof.

Background Art

Nicotine salt is the main component of electronic atomization liquid. Existing nicotine salts include single nicotine salt and compound nicotine salt. Among them, there are many existing single nicotine salt products with clear ingredients and distinct taste; but consumers' novelty has worn off and their acceptance has declined, and they are interested in compound nicotine salts with more distinct taste levels.

Most existing composite nicotine salts use mixed acids as raw materials, which are directly mixed with nicotine and heated to prepare. This can lead to problems such as unstable acid ratios, unclear nicotine salt composition, and poor process scale-up repeatability, making it impossible to mass-produce nicotine salts. It also affects the taste of the electronic atomization liquid and reduces consumer usage evaluation.

Therefore, in view of the existing preparation problems of composite nicotine salts, it is necessary to provide a simple and efficient preparation method of composite nicotine salts; the preparation method should be able to ensure a good taste and improve the smoking quality, while having clear ingredients and strong process repeatability, being suitable for industrial production and capable of large-scale mass production.

Summary of the invention

In view of the shortcomings of the prior art, the present invention provides a method for preparing a composite nicotine salt, wherein an organic acid is mixed with nicotine and an organic solvent to obtain a single nicotine salt, and then different nicotine salts are compounded in a specific ratio to obtain a composite nicotine salt with clear ingredients and a distinct taste; the preparation method has simple process operation and strong process repeatability, is suitable for industrial production, and can be mass-produced.

The present invention also provides a composite nicotine salt with clear ingredients, distinct taste, multiple taste levels, and high suction quality, which can improve consumers' evaluation of use.

Specifically, the present invention discloses a method for preparing a composite nicotine salt, comprising the following steps:

S1, mixing an organic acid, nicotine, and an organic solvent to obtain a single nicotine salt;

S2, repeating step S1 to obtain different single nicotine salts;

S3, mixing different single nicotine salts to obtain composite nicotine salts;

The molar ratio of the organic acid to nicotine is 0.7-1.7:1.

Preferably, the organic acid is selected from one of levulinic acid, benzoic acid, lactic acid, fumaric acid, salicylic acid, vanillic acid, gentisic acid, cinnamic acid and malic acid.

Preferably, the molar ratio of levulinic acid to nicotine is 1.2-1.4:1.

Preferably, the molar ratio of benzoic acid to nicotine is 1.1-1.3:1.

Preferably, the molar ratio of malic acid to nicotine is 1.5-1.7:1.

Preferably, the mass ratio of nicotine to organic solvent is 1:2-4.

Preferably, the different single nicotine salts include nicotine benzoate and nicotine levulinate.

Preferably, the mass ratio of the nicotine benzoate to the nicotine levulinate is 1-2:1.

Preferably, the different single nicotine salts further include at least one of lactic acid-nicotine salt, fumaric acid-nicotine salt, salicylic acid-nicotine salt, vanillic acid-nicotine salt, gentisic acid-nicotine salt, cinnamic acid-nicotine salt, and malic acid-nicotine salt, and the mass ratio of the content of lactic acid-nicotine salt to benzoic acid-nicotine salt is 1:6-15.

The present invention also discloses a composite nicotine salt, which is prepared by the preparation method of the composite nicotine salt.

Beneficial effects:

(1) The method for preparing a composite nicotine salt of the present invention comprises first mixing an organic acid with nicotine and an organic solvent to obtain a single nicotine salt, and then compounding different nicotine salts in a specific ratio to obtain a composite nicotine salt with clear ingredients and a distinct taste. Since the composite nicotine salt is compounded and mixed with a single synthesized stable nicotine salt instead of directly mixing a mixed acid with nicotine, the composite nicotine salt is more stable, which helps to prolong the shelf life and increase the flavor persistence. In addition, the preparation method has simple process operation and strong process repeatability, is suitable for industrial production, and can be mass-produced.

(1) The composite nicotine salt of the present invention has clear ingredients, a distinct taste, multiple taste levels, and high smoking quality, which can improve consumers' evaluation of its use.

BRIEF DESCRIPTION OF THE DRAWINGS

In order to more clearly illustrate the technical solution of the present invention, the accompanying drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings in the following description are some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying any creative work.

FIG1 is a schematic diagram of nicotine salt prepared from sample A2;

FIG2 is a schematic diagram of nicotine salt prepared from sample B2;

FIG3 is a schematic diagram of nicotine salt prepared from sample C3;

FIG4 is a schematic diagram of nicotine salt prepared from sample D1;

FIG5 is a schematic diagram of nicotine salt prepared from sample E2;

FIG6 is a schematic diagram of nicotine salt prepared from sample F3;

FIG7 is a schematic diagram of nicotine salt prepared from sample G3;

FIG8 is a schematic diagram of nicotine salt prepared from sample H2;

FIG9 is a schematic diagram of nicotine salt prepared from sample I3;

FIG10 is a schematic diagram of the composite nicotine salt prepared in Example 1 of the present invention;

FIG11 is a schematic diagram of the composite nicotine salt prepared in Example 2 of the present invention;

FIG12 is a schematic diagram of the composite nicotine salt prepared in Example 3 of the present invention;

FIG13 is a schematic diagram of the composite nicotine salt prepared in Example 4 of the present invention;

FIG14 is a schematic diagram of the composite nicotine salt prepared in Example 5 of the present invention;

FIG15 is a schematic diagram of the composite nicotine salt prepared in Example 6 of the present invention;

FIG. 16 is a schematic diagram of the nicotine salt prepared in Comparative Example 1.

DETAILED DESCRIPTION

The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

It should be understood that when used in this specification and the appended claims, the terms "include" and "comprises" indicate the presence of described features, integers, steps, operations, elements and/or components, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components and/or combinations thereof.

It should also be understood that the terms used in this specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. As used in the specification of the present invention and the appended claims, unless the context clearly indicates otherwise, the singular forms "a", "an" and "the" are intended to include plural forms.

It should be further understood that the term "and/or" used in the present description and the appended claims refers to and includes any and all possible combinations of one or more of the associated listed items.

It should be further understood that the term "concentration" used in the present specification and the appended claims refers to mass concentration, and "%" refers to mass percentage, unless otherwise explained.

A method for preparing a composite nicotine salt.

The following steps are involved:

S1, mixing an organic acid, nicotine, and an organic solvent to obtain a single nicotine salt;

S2, repeating step S1 to obtain different single nicotine salts;

S3, mixing different single nicotine salts to obtain composite nicotine salts;

The organic solvent is used to help the organic acid and nicotine mix. Preferably, the mass ratio of nicotine to the organic solvent is 1:2-4, more preferably 1:3. The organic solvent can be a food-grade organic solvent, such as glycerol.

The mixing operation may preferably be performed by heating in an oil bath at 70°C for 30 minutes.

The organic acid is selected from one of levulinic acid, benzoic acid, lactic acid, fumaric acid, salicylic acid, vanillic acid, gentisic acid, cinnamic acid and malic acid. The molar ratio of the organic acid to nicotine is 0.7-1.7:1.

Among them, preferably, the molar ratio of levulinic acid to nicotine is 1.2-1.4:1, the molar ratio of benzoic acid to nicotine is 1.1-1.3:1, the molar ratio of lactic acid to nicotine is 1.0-1.3:1, the molar ratio of fumaric acid to nicotine is 0.7-0.9:1, the molar ratio of salicylic acid to nicotine is 1.1-1.2:1, the molar ratio of vanillic acid to nicotine is 1.2-1.3:1, the molar ratio of gentisic acid to nicotine is 0.8-1.0:1, the molar ratio of cinnamic acid to nicotine is 1.0-1.2:1, and the molar ratio of malic acid to nicotine is 1.5-1.7:1.

The different single nicotine salts include nicotine benzoate salt and nicotine levulinate salt. Preferably, the mass ratio of the nicotine benzoate salt to the nicotine levulinate salt is 1-2:1.

The different single nicotine salts also include at least one of lactic acid-nicotine salt, fumaric acid-nicotine salt, salicylic acid-nicotine salt, vanillic acid-nicotine salt, gentisic acid-nicotine salt, cinnamic acid-nicotine salt, and malic acid-nicotine salt, and the mass ratio of the total content thereof to benzoic acid-nicotine salt is preferably 1:4-15. The content is the sum of at least one of lactic acid-nicotine salt, fumaric acid-nicotine salt, salicylic acid-nicotine salt, vanillic acid-nicotine salt, gentisic acid-nicotine salt, cinnamic acid-nicotine salt, and malic acid-nicotine salt.

In some specific embodiments of the present invention, different single nicotine salts include nicotine benzoate salt and nicotine levulinate salt, and also include nicotine lactate salt and nicotine malate salt; wherein the mass ratio of the total content of nicotine lactate salt and nicotine malate salt to nicotine benzoate salt is 1:5.5.

A single nicotine salt, prepared as follows:

An organic acid, nicotine and an organic solvent are mixed and reacted to obtain a single nicotine salt; specifically, nicotine-organic acid salt is prepared according to the organic acid-nicotine molar ratio (0.7-1.7:1), the organic acid is dissolved in 15g of glycerol, 5g of nicotine is added dropwise, and the mixture is heated in an oil bath at 70°C for 30min until completely dissolved to obtain a homogeneous oily nicotine salt.

Sensory evaluation test: The prepared nicotine salt is configured into electronic atomizer liquid according to the requirements of the electronic atomizer, loaded into the same cartridge equipment, and a number of professional evaluators conduct sensory analysis. The evaluation indicators include throat hit, irritation, smoothness, off-flavor and aroma, each with 10 points, and the evaluation screens out the best ratio of organic acid to nicotine. Specifically, the evaluation indicators are shown in Table 1.

Table 1 Evaluation indicators

Specifically, a single nicotine salt sample A-I was prepared according to the above preparation method and configured into an electronic atomization liquid for sensory evaluation test. 20 evaluators evaluated each sample 3 times, and the results were averaged. The results are shown in Table 2 below.

Table 2 Samples A-I and their sensory evaluation results

Among them, in sample C1, the mass ratio of nicotine to organic solvent is 1:2, specifically, 10g of glycerol; in sample H3, the mass ratio of nicotine to organic solvent is 1:4, specifically, 20g of glycerol.

Figures 1-9 are all homogeneous oily nicotine salts, which are brown-yellow in color, with the shades shown in the figures.

As can be seen from Table 2, preferably, the molar ratio of levulinic acid to nicotine is 1.2-1.4:1, the molar ratio of benzoic acid to nicotine is 1.1-1.3:1, the molar ratio of lactic acid to nicotine is 1.0-1.3:1, the molar ratio of fumaric acid to nicotine is 0.7-0.9:1, the molar ratio of salicylic acid to nicotine is 1.1-1.2:1, the molar ratio of vanillic acid to nicotine is 1.2-1.3:1, the molar ratio of gentisic acid to nicotine is 0.8-1.0:1, the molar ratio of cinnamic acid to nicotine is 1.0-1.2:1, and the molar ratio of malic acid to nicotine is 1.5-1.7:1.

The above-mentioned single nicotine salt has clear ingredients, distinct taste and good sensory evaluation; however, the taste level is not rich enough and the long-term consumer acceptance is not high; therefore, in the present invention, the single nicotine salt is used as a raw material to prepare a composite nicotine salt with more taste levels.

The prepared different single nicotine salt samples A-I were mixed to obtain composite nicotine salt Examples 1-7. The specific preparation method was the same as that of Example 1.

Example 1

1.1 g of sample A2, 0.7 g of sample B1, 0.08 g of sample C2, and 0.12 g of sample I3 were taken and stirred at room temperature for 20 min to obtain a homogeneous orange-yellow oily composite nicotine salt.

The composite nicotine salts prepared in Examples 1-7 were configured into electronic atomization liquids, and then a sensory evaluation test was conducted. 20 evaluators evaluated each sample 3 times, and the results were averaged. The results obtained are shown in Table 3 below.

Table 3 Ingredients and sensory test evaluation results of Examples 1-7

Figures 10-15 are all homogeneous orange-yellow oily or brown-yellow oily composite nicotine salts.

Comparative Examples 1-5 are set according to the above-mentioned Example 1; the differences between Comparative Examples 1-5 and Example 1 are shown in Table 4 below.

Table 4 Comparative Examples 1-5 and Example 1

The nicotine salts prepared in Comparative Examples 1-5 were configured into electronic atomization liquids for sensory evaluation tests. 20 evaluators evaluated each sample 3 times, and the results were averaged. The results are shown in Table 5 below.

Table 5 Sensory test evaluation results of Example 1 and Comparative Examples 1-5

FIG16 is a nicotine salt prepared in Comparative Example 1, which is a homogeneous brown oily nicotine salt.

As shown in Tables 2-5, the composite nicotine salts prepared in Examples 1-7 have a soft taste, multiple layers, a full and delicate aroma, a good throat hit, and produce a sense of pleasure and physiological satisfaction, and the overall evaluation is good.

In the above embodiments, the description of each embodiment has its own emphasis. For parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims (10)

1. A method for preparing a compound nicotine salt, comprising the steps of:

s1, mixing organic acid, nicotine and an organic solvent to obtain single nicotine salt;

s2, repeating the step S1 to obtain different single nicotine salts;

s3, mixing different single nicotine salts to obtain compound nicotine salt;

the molar ratio of the organic acid to the nicotine is 0.7-1.7:1.

2. The method for preparing a compound nicotine salt according to claim 1, wherein the organic acid is one selected from levulinic acid, benzoic acid, lactic acid, fumaric acid, salicylic acid, vanillic acid, gentisic acid, cinnamic acid and malic acid.

3. A method of preparing a complex nicotine salt according to claim 2, wherein the molar ratio of levulinic acid to nicotine is 1.2-1.4:1.

4. A method of preparing a complex nicotine salt according to claim 2, characterized in that the molar ratio of benzoic acid to nicotine is 1.1-1.3:1.

5. A method of preparing a complex nicotine salt according to claim 2, wherein the molar ratio of malic acid to nicotine is 1.5-1.7:1.

6. The method for preparing the compound nicotine salt according to claim 2, wherein the mass ratio of the nicotine to the organic solvent is 1:2-4.

7. A method of preparing a complex nicotine salt as claimed in claim 2, wherein said different single nicotine salts comprise benzoic acid-nicotine salt and levulinic acid-nicotine salt.

8. The method of preparing a complex nicotine salt of claim 7, wherein the mass ratio of benzoic acid-nicotine salt to levulinic acid-nicotine salt is 1-2:1.

9. The method for preparing composite nicotine salt of claim 8, wherein the different single nicotine salts further comprise at least one of lactate-nicotine salt, fumarate-nicotine salt, salicylate-nicotine salt, vanilla-nicotine salt, gentisic acid-nicotine salt, cinnamic acid-nicotine salt, malic acid-nicotine salt, and the mass ratio of the content to benzoic acid-nicotine salt is 1:4-15.

10. A compound nicotine salt prepared by the preparation method of any one of claims 1-9.

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