Electronic atomizing liquid containing d-limonene and preparation method thereof

Abstract

This invention discloses an electronic atomizing liquid containing terpene-free sweet orange oil and its preparation method, relating to the field of electronic atomizing liquid technology. The electronic atomizing liquid containing terpene-free sweet orange oil is composed of the following components by weight percentage: 20-45% sweet orange flavoring, 0-5% nicotine salt, 0-10% sweetener, 0-10% acidulant, 0-10% cooling agent, 35-50% vegetable glycerin, and the balance propylene glycol. The electronic atomizing liquid containing terpene-free sweet orange oil of this invention is prepared by molecular distillation refining of natural sweet orange oil to remove some terpenes and other impurities, eliminating off-flavors and impurities, improving solubility, and then compounding it with some monomeric flavorings to prepare a high-quality electronic atomizing liquid containing terpene-free sweet orange oil. This results in a stable atomizing liquid with a rich and natural aroma, and the atomizing liquid will not easily leak into the electronic atomizer due to excessively low viscosity.

Description

Technical Field

[0001] This invention relates to the field of electronic atomizing fluid technology, and in particular to an electronic atomizing fluid containing terpene-free sweet orange oil and its preparation method. Background Technology

[0002] In recent years, sweet orange flavored e-cigarette liquids have become widely popular among consumers. However, the poor solubility of sweet orange flavoring and solvent system has led to quality problems such as turbidity, layering, and floating oil in the e-cigarette liquid. In addition, excessive ethanol has been added to increase solubility, resulting in excessively low viscosity of the e-cigarette liquid and leakage from the device. Alternatively, the sweet orange flavor may not be harmonious, rich, or natural enough. Summary of the Invention

[0003] To address the technical problems of existing sweet orange-flavored e-liquids, such as unstable quality, easy turbidity, layering, and floating oil; low viscosity leading to leakage during use; and weak, uncoordinated, and unnatural aroma, this invention provides an e-liquid containing terpene-free sweet orange oil and its preparation method. This involves refining natural sweet orange oil through molecular distillation to remove some terpenes and other impurities, eliminating off-flavors and impurities, and improving solubility. The oil is then compounded with some single-component fragrances to prepare a high-quality e-liquid containing terpene-free sweet orange oil. This results in a stable e-liquid with a rich, natural aroma, and prevents leakage in the e-atomizer due to low viscosity.

[0004] Specifically, the following technical solutions are included:

[0005] In one aspect, an electronic atomizing liquid containing terpene-free sweet orange oil is provided, which is composed of the following components by mass percentage: 20-45% sweet orange flavoring, 0-5% nicotine salt, 0-10% sweetener, 0-10% acidulant, 0-10% cooling agent, 35-50% vegetable glycerin, and the balance propylene glycol;

[0006] The sweet orange flavoring includes, in addition to terpene-containing sweet orange oil, ethyl butyrate, octyl acetate, citronellol, n-decanal, citral, n-octanol, nerol acetate, n-nonanol, citronellol, linalool, geraniol, geraniol acetate, nerol, n-octanol, n-decanoic acid, perillaldehyde, ethyl maltol, Valencia citrusene, benzyl alcohol, vanillin, edible ethanol, and propylene glycol.

[0007] The vegetable glycerin mentioned above is food-grade vegetable glycerin.

[0008] Furthermore, the sweet orange flavoring is composed of terpene-free sweet orange oil, ethyl butyrate, octyl acetate, citronellol, n-decanal, citral, n-octanol, nerol acetate, n-nonanol, citronellol, linalool, geraniol, geraniol acetate, nerol, n-octanol, n-decanoic acid, perillaldehyde, ethyl maltol, Valencia citrusene, benzyl alcohol, vanillin, edible ethanol, and propylene glycol.

[0009] Furthermore, the sweet orange flavoring is composed of the following components in weight percentages:

[0010] The composition includes: 10-50% sweet orange oil (excluding terpenes), 0.01-3.0% ethyl butyrate, 0.05-2.0% octyl acetate, 0.05-2.0% citronellol, 0.02-2.0% n-decanal, 0.02-1.0% citral, 0.02-1.0% n-octanol, 0.02-0.9% nerol acetate, 0.02-0.9% n-nonanol, 0.02-2.0% citronellol, 0.02-5.0% linalool, and 0% geraniol. 0.02-1.5%, Geraniol 0.02-1.0%, Nerol 0.02-0.5%, Octal 0.02-1.0%, Decanoic acid 0.02-2.0%, Perillaldehyde 0.01-0.9%, Ethyl maltol 0.02-2.0%, Valencian citric acid 0.01-0.8%, Benzyl alcohol 0.02-0.9%, Vanillin 0.02-0.4%, Edible ethanol 10-30%, Propylene glycol balance.

[0011] Furthermore, the method for preparing the terpene-free sweet orange oil includes the following steps:

[0012] S1. Natural sweet orange oil is subjected to first molecular distillation. The conditions for first molecular distillation are: vacuum degree 100-2000Pa, main evaporator temperature 40-90℃, roller speed 60-400rpm, and feed rate 200-2000mL / h. Collect the heavy components to obtain sweet orange oil 1.

[0013] S2. Mix sweet orange oil 1 with propylene glycol at a mass ratio of 1:(4-99), and then sonicate for 0.5-1h to obtain sweet orange oil 2.

[0014] S3. The sweet orange oil 2 is subjected to a second molecular distillation. The conditions for the second molecular distillation are: vacuum degree 0.1-50 Pa, main evaporator temperature 50-150℃, roller speed 60-400 rpm, and feed rate 500-5000 mL / h. The light components are collected to obtain sweet orange oil 3, which is the terpene-free sweet orange oil.

[0015] Preferably, in the method for preparing the terpene-free sweet orange oil, the natural sweet orange oil is one of American sweet orange oil, Brazilian sweet orange oil, or domestic sweet orange oil.

[0016] Sweet orange (Citrus sinensis (Linn.) Osb.) is a fruit tree belonging to the genus Citrus in the subfamily Citrus of the family Rutaceae. It is an evergreen shrub or small tree. It is mainly produced in Brazil, the United States, Israel, and southern and eastern China. The pulp can be eaten directly or used to make orange juice, while the peel is rich in flavonoids, carotenoids, and limonoids. Natural sweet orange oil, extracted from the whole fruit or peel using cold milling, cold pressing, steam distillation, or supercritical CO2 extraction, is one of the three most commonly used fruit flavorings and is widely used in medicine, food, daily chemicals, and tobacco.

[0017] Chemical analysis of natural sweet orange oil revealed that its main components are terpenes and their oxidized derivatives, such as limonene, myrcene, pinene, decanal, octanal, linalool, and citral. Limonene accounts for 90% of the total composition, but contributes very little to the essential oil's aroma and is easily oxidized to carvone and carvacrol upon exposure to light and heat, which is a major cause of spoilage in natural sweet orange oil. Other components, such as decanal, octanal, and linalool, are present in lower amounts but are the main sources of the characteristic aroma of citrus essential oils. Especially when used as flavor enhancers, it is desirable to have as many of these low-content components as possible. Therefore, enriching the characteristic aroma components in natural sweet orange oil and reducing the limonene content is crucial for improving its stability and flavor quality. Furthermore, higher terpene content also leads to poor water solubility, resulting in poor or unstable performance when used in e-liquids.

[0018] Furthermore, unlike traditional distillation which relies on boiling point differences for separation, molecular distillation utilizes the difference in the mean free path of molecular motion of different substances to achieve separation. Its lower pressure and boiling temperature make it ideal for separating heat-sensitive, high-boiling-point substances. It also offers advantages such as short material heating time, low operating pressure, high separation degree and yield, good product quality, minimal changes in composition before and after distillation, and the avoidance of organic solvents in the separated product.

[0019] The main solvents in electronic atomizing fluid systems are propylene glycol and glycerol, which contain multiple hydroxyl groups and are primarily water-soluble. Terpenes, belonging to hydrocarbons, can be classified as monoterpenes, sesquiterpenes, diterpenes, etc., and have poor solubility in water-soluble systems. This invention utilizes molecular distillation technology to process natural sweet orange oil, removing some terpenes and improving its solubility. This ensures that the oil remains stable in electronic atomizing fluids, without becoming cloudy, separating, or floating. Simultaneously, it reduces the amount of low-viscosity solvent—alcohol—used in the flavoring system, keeping the viscosity of the electronic atomizing fluid within a certain range and reducing the risk of leakage in electronic atomizers.

[0020] Furthermore, the electronic atomizing liquid containing terpene-free sweet orange oil is composed of the following components by mass percentage: 20-45% sweet orange flavoring, 0.01-5% nicotine salt, 0.01-10% sweetener, 0.01-10% acidulant, 0.01-10% cooling agent, 35-50% vegetable glycerin, and the balance propylene glycol.

[0021] Furthermore, the sweetener is one or more of sucralose, neotame, steviol glycosides, and maltitol.

[0022] Furthermore, the acidulant is one or more of acetic acid, propionic acid, malic acid, etc.

[0023] Furthermore, the cooling agent is one or more of WS-23 (N,2,3-trimethyl-2-(1-methylethyl)butanamide), WS-5 (N-(ethoxycarbonylmethyl)-p-alkyl-3-carboxamide), WS-3 (N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide), and menthone.

[0024] Furthermore, the nicotine salt is one or more of benzoic acid nicotine salt, malic acid nicotine salt, tartaric acid nicotine salt, oxalic acid nicotine salt, and lactic acid nicotine salt.

[0025] Secondly, a method for preparing an electronic atomizing liquid containing terpene-free sweet orange oil as described in the first aspect is provided, comprising the following steps: mixing sweet orange flavoring, nicotine salt, sweetener, acidulant, cooling agent, vegetable glycerin and propylene glycol, letting stand for 0.5-1 h, and passing through a 200-1000 mesh sieve to obtain an electronic atomizing liquid containing terpene-free sweet orange oil.

[0026] The beneficial effects of this invention are as follows:

[0027] This invention provides an electronic atomizing liquid containing terpene-free sweet orange oil and its preparation method. Utilizing molecular distillation technology, some terpenoids in natural sweet orange oil can be removed, preserving as many characteristic aroma compounds as possible. It also removes flavonoids and other substances that may be carried from the peel during extraction, eliminating any bitter aftertaste or off-flavors. Simultaneously, combining fragrance technology, the physicochemical properties and volatility of different monomeric fragrances under heat are utilized. By adding appropriate monomeric fragrance substances, the aroma of the electronic atomizing liquid containing terpene-free sweet orange oil becomes harmonious, rich, and natural. Detailed Implementation

[0028] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0029] It should be understood that, when used in this specification and the appended claims, the terms "comprising" and "including" indicate the presence of the described features, integrals, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components and / or collections thereof.

[0030] It should also be understood that the terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. As used in this specification and the appended claims, the singular forms “a,” “an,” and “the” are intended to include the plural forms unless the context clearly indicates otherwise.

[0031] It should also be further understood that the term "and / or" as used in this specification and the appended claims refers to any combination of one or more of the associated listed items and all possible combinations, and includes such combinations.

[0032] To better understand the technical content of the present invention, the technical solution of the present invention will be further introduced and explained below with reference to specific embodiments.

[0033] Preferably, in the sweet orange flavorings of the embodiments and comparative examples of the present invention, the sweet orange flavoring includes, in addition to, terpene-containing sweet orange oil, a variety of monomeric flavorings, edible ethanol, and propylene glycol. The monomeric flavorings include one or more of the following: ethyl butyrate, octyl acetate, citronellol, n-decanal, citral, n-octanol, nerol acetate, n-nonanol, citronellol, linalool, geraniol, geraniol acetate, nerol, n-octanol, n-decanoic acid, perillaldehyde, ethyl maltol, Valencia citrus, benzyl alcohol, and vanillin. All monomeric flavorings are prepared into a 1% (w / w) dilution using propylene glycol or a mixture of propylene glycol and 95% (v / v) edible ethanol as a solvent.

[0034] Preparation method of terpene-free sweet orange oil:

[0035] S1. Natural sweet orange oil is subjected to first molecular distillation. The conditions for first molecular distillation are: vacuum degree 100-2000Pa, main evaporator temperature 40-90℃, roller speed 60-400rpm, and feed rate 200-2000mL / h. Collect the heavy components to obtain sweet orange oil 1.

[0036] S2. Mix sweet orange oil 1 with propylene glycol at a mass ratio of 1:(4-99), and then sonicate for 0.5-1h to obtain sweet orange oil 2.

[0037] S3. The sweet orange oil 2 is subjected to a second molecular distillation. The conditions for the second molecular distillation are: vacuum degree 0.1-50 Pa, main evaporator temperature 50-150℃, roller speed 60-400 rpm, and feed rate 500-5000 mL / h. The light components are collected to obtain sweet orange oil 3, which is the terpene-free sweet orange oil.

[0038] This invention utilizes molecular distillation technology to remove some terpenoids while preserving characteristic aroma compounds as much as possible. It also removes flavonoids and other substances that may be brought out from the fruit peel during extraction, eliminating any bitter aftertaste or off-flavors. Simultaneously, by combining fragrance technology and utilizing the physicochemical properties and volatility of different monomeric fragrances under heat, appropriate monomeric fragrance substances are added to make the aroma of the electronic atomized liquid containing terpene-free sweet orange oil harmonious, rich, and natural.

[0039] Preparation method of e-liquid containing terpene-free sweet orange oil:

[0040] Mix sweet orange flavoring, nicotine salt, sweetener, acidulant, cooling agent, vegetable glycerin and propylene glycol, let stand for 0.5-1 hour, and pass through a 200-1000 mesh sieve to obtain an electronic atomizing liquid containing terpene-free sweet orange oil.

[0041] Example

[0042] Example 1

[0043] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0044] The sweet orange flavoring is composed of the following components by weight percentage:

[0045] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0046] The method for preparing the terpene-free sweet orange oil includes the following steps:

[0047] S1. Natural sweet orange oil is subjected to first molecular distillation. The conditions for first molecular distillation are: vacuum degree 900 Pa, main evaporator temperature 60℃, roller speed 200 rpm, feed rate 300 mL / h, and heavy components are collected to obtain sweet orange oil 1; the natural sweet orange oil is Brazilian sweet orange oil.

[0048] S2. Mix sweet orange oil 1 with propylene glycol at a mass ratio of 1:49, and then sonicate for 0.5 h to obtain sweet orange oil 2.

[0049] S3. The sweet orange oil 2 is subjected to a second molecular distillation. The conditions for the second molecular distillation are: vacuum degree 15 Pa, main evaporator temperature 90 ℃, roller speed 300 rpm, and feed rate 1000 mL / h. The light components are collected to obtain sweet orange oil 3, which is the terpene-free sweet orange oil.

[0050] The preparation method of the electronic atomizing liquid containing terpene-free sweet orange oil includes the following steps: mixing sweet orange flavoring, nicotine salt, sweetener, acidulant, cooling agent, vegetable glycerin and propylene glycol, letting stand for 0.5 hours, and passing through an 800-mesh sieve to obtain the electronic atomizing liquid containing terpene-free sweet orange oil.

[0051] Example 2

[0052] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 20% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0053] The sweet orange flavoring is composed of the following components by weight percentage:

[0054] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0055] Example 3

[0056] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 45% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0057] The sweet orange flavoring is composed of the following components by weight percentage:

[0058] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0059] The preparation methods of the terpene-free sweet orange oil in Examples 2-3 are the same as those in Example 1. The preparation methods of the electronic atomizing liquid containing the terpene-free sweet orange oil in Examples 2-3 are the same as those in Example 1.

[0060] Comparative Example 1

[0061] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0062] The sweet orange flavoring is composed of the following components by weight percentage:

[0063] Ethyl butyrate 1.0%, octyl acetate 0.2%, citronellol 0.6%, n-decanal 0.8%, citral 0.2%, n-octanol 0.4%, nerol acetate 0.1%, n-nonanol 0.2%, citronellol 0.25%, linalool 1.0%, geraniol 0.05%, geraniol acetate 0.05%, nerol 0.2%, n-octanol 0.5%, n-decanoic acid 0.4%, perillaldehyde 0.2%, ethyl maltol 0.8%, Valencia citrusene 0.1%, benzyl alcohol 0.5%, vanillin 0.1%, edible ethanol 20%, propylene glycol balance.

[0064] The difference between Comparative Example 1 and Example 1 is that the sweet orange flavoring of the e-cigarette containing deterpenoid sweet orange oil does not contain deterpenoid sweet orange oil, while all other conditions are the same.

[0065] Comparative Example 2

[0066] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0067] The sweet orange flavoring is composed of 30% terpene-free sweet orange oil, 20% edible ethanol, and the remainder propylene glycol.

[0068] Compared with Example 1, Comparative Example 2 differs in that the sweet orange flavoring of the electronic atomizing liquid containing deterpenoid sweet orange oil is composed of deterpenoid sweet orange oil, edible ethanol and propylene glycol, while all other conditions are the same.

[0069] Comparative Example 3

[0070] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0071] The sweet orange flavoring is composed of the following components by weight percentage:

[0072] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0073] The method for preparing the terpene-free sweet orange oil includes the following steps:

[0074] S1. Natural sweet orange oil is subjected to first molecular distillation. The conditions for first molecular distillation are: vacuum degree 900 Pa, main evaporator temperature 60℃, roller speed 200 rpm, feed rate 300 mL / h, and heavy components are collected to obtain sweet orange oil 1; the natural sweet orange oil is Brazilian sweet orange oil.

[0075] S2. Mix sweet orange oil 1 with propylene glycol at a mass ratio of 1:49, and then sonicate for 0.5 h to obtain sweet orange oil 2, which is the terpene-free sweet orange oil.

[0076] The preparation method of the electronic atomizing liquid containing terpene-free sweet orange oil in Comparative Example 3 is the same as that in Example 1.

[0077] The only difference between Comparative Example 3 and Example 1 is the preparation method of the terpene sweet orange oil; all other conditions are the same.

[0078] Comparative Example 4

[0079] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0080] The sweet orange flavoring is composed of the following components by weight percentage:

[0081] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0082] The method for preparing the terpene-free sweet orange oil includes the following steps:

[0083] S1. Natural sweet orange oil and propylene glycol are mixed in a mass ratio of 1:49, and then the mixture is ultrasonicated for 0.5 h to obtain sweet orange oil 1; the natural sweet orange oil is Brazilian sweet orange oil.

[0084] S2. The sweet orange oil 1 is subjected to a second molecular distillation. The conditions for the second molecular distillation are: vacuum degree 15 Pa, main evaporator temperature 90 ℃, roller speed 300 rpm, and feed rate 1000 mL / h. The light components are collected to obtain sweet orange oil 2, which is the terpene-free sweet orange oil.

[0085] The preparation method of the electronic atomizing liquid containing terpene-free sweet orange oil in Comparative Example 4 is the same as that in Example 1.

[0086] The only difference between Comparative Example 4 and Example 1 is the preparation method of the terpene sweet orange oil; all other conditions are the same.

[0087] Comparative Example 5

[0088] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0089] The sweet orange flavoring is composed of the following components by weight percentage:

[0090] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0091] The method for preparing the terpene-free sweet orange oil includes the following steps:

[0092] S1. Natural sweet orange oil and propylene glycol are mixed at a mass ratio of 1:49, and then ultrasonically mixed for 0.5 hours to obtain sweet orange oil 1, which is the terpene-free sweet orange oil. The natural sweet orange oil mentioned is Brazilian sweet orange oil.

[0093] The preparation method of the electronic atomizing liquid containing terpene-free sweet orange oil in Comparative Example 5 is the same as that in Example 1.

[0094] The only difference between Comparative Example 5 and Example 1 is the preparation method of the terpene sweet orange oil; all other conditions are the same.

[0095] Comparative Example 6

[0096] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0097] The sweet orange flavoring is composed of the following components by weight percentage:

[0098] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0099] The method for preparing the terpene-free sweet orange oil includes the following steps:

[0100] S1. Natural sweet orange oil is subjected to first molecular distillation. The conditions for first molecular distillation are: vacuum degree 900 Pa, main evaporator temperature 110 ℃, roller speed 200 rpm, feed rate 300 mL / h, and heavy components are collected to obtain sweet orange oil 1; the natural sweet orange oil is Brazilian sweet orange oil.

[0101] S2. Mix sweet orange oil 1 with propylene glycol at a mass ratio of 1:49, and then sonicate for 0.5 h to obtain sweet orange oil 2.

[0102] S3. The sweet orange oil 2 is subjected to a second molecular distillation. The conditions for the second molecular distillation are: vacuum degree 15 Pa, main evaporator temperature 170℃, roller speed 300 rpm, and feed rate 1000 mL / h. The light components are collected to obtain sweet orange oil 3, which is the terpene-free sweet orange oil.

[0103] The preparation method of the electronic atomizing liquid containing terpene-free sweet orange oil in Comparative Example 6 is the same as that in Example 1.

[0104] The only difference between Comparative Example 6 and Example 1 is the preparation method of the terpene sweet orange oil; all other conditions are the same.

[0105] Comparative Example 7

[0106] An electronic atomizing liquid containing terpene-free sweet orange oil comprises the following components by mass percentage: 30% sweet orange flavoring, 1.8% nicotine salt, 4% sweetener, 3% acidulant, 3% cooling agent, 40% vegetable glycerin, and the balance being propylene glycol; wherein the sweetener is composed of sucralose, neotame, and maltitol in a mass ratio of 3:3:2; the acidulant is composed of acetic acid, propionic acid, and malic acid in a mass ratio of 3:3:2; the cooling agent is composed of WS-23, WS-5, WS-3, and menthone in a mass ratio of 3:3:2:1; and the nicotine salt is composed of benzoic acid nicotine salt, oxalate nicotine salt, and lactate nicotine salt in a mass ratio of 1:1:1.

[0107] The sweet orange flavoring is composed of the following components by weight percentage:

[0108] The composition includes 30% sweet orange oil (excluding terpenes), 1.0% ethyl butyrate, 0.2% octyl acetate, 0.6% citronellol, 0.8% n-decanal, 0.2% citral, 0.4% n-octanol, 0.1% nerol acetate, 0.2% n-nonanol, 0.25% citronellol, 1.0% linalool, 0.05% geraniol, 0.05% geraniol acetate, 0.2% nerol, 0.5% n-octanol, 0.4% n-decanoic acid, 0.2% perillaldehyde, 0.8% ethyl maltol, 0.1% Valencia citrusene, 0.5% benzyl alcohol, 0.1% vanillin, 20% edible ethanol, and the remainder propylene glycol.

[0109] The method for preparing the terpene-free sweet orange oil includes the following steps:

[0110] S1. Natural sweet orange oil is subjected to first molecular distillation. The conditions for first molecular distillation are: vacuum degree 1500 Pa, main evaporator temperature 60℃, roller speed 200 rpm, feed rate 300 mL / h, and heavy components are collected to obtain sweet orange oil 1; the natural sweet orange oil is Brazilian sweet orange oil.

[0111] S2. Mix sweet orange oil 1 with propylene glycol at a mass ratio of 1:49, and then sonicate for 0.5 h to obtain sweet orange oil 2.

[0112] S3. The sweet orange oil 2 is subjected to a second molecular distillation. The conditions for the second molecular distillation are: vacuum degree 100 Pa, main evaporator temperature 90 ℃, roller speed 300 rpm, and feed rate 1000 mL / h. The light components are collected to obtain sweet orange oil 3, which is the terpene-free sweet orange oil.

[0113] The preparation method of the electronic atomizing liquid containing terpene-free sweet orange oil in Comparative Example 7 is the same as that in Example 1.

[0114] The only difference between Comparative Example 7 and Example 1 is the preparation method of the terpene sweet orange oil; all other conditions are the same.

[0115] Performance testing

[0116] 1. Stability test of electronic atomizing fluid

[0117] The e-liquids prepared in the examples and comparative examples were placed in the same environment (temperature, humidity, etc.), and the appearance of the products was observed on days 1, 3, 7, 15, and 30 to check for turbidity, layering, or floating oil (+ and - indicate the presence and absence of this phenomenon, respectively). The stability of the e-liquids in Examples 1-3 and Comparative Examples 1-7 was tested, and the results are shown in Table 1 below.

[0118] Table 1. Stability test results of electronic atomizing liquids in Examples 1-3 and Comparative Examples 1-7

[0119]

[0120] As can be seen from the test results in Table 1, the electronic atomizing liquid containing terpene-free sweet orange oil prepared in the embodiments of the present invention has strong stability. This is because the present invention reduces the content of terpenoids and increases their solubility in solvents by molecular distilling natural sweet orange oil, thereby improving the stability of the electronic atomizing liquid containing terpene-free sweet orange oil and reducing the occurrence of turbidity, layering, and floating oil phenomena in the atomizing liquid.

[0121] 2. Viscosity test of electronic atomizing fluid

[0122] The viscosity of the e-liquids prepared in the examples and comparative examples was measured using a viscometer. Based on experience with e-liquids in e-atomizers, when the viscosity is below 60 mPa·s, there is a certain risk of leakage in the e-liquid, and the risk of leakage increases with lower viscosity. Viscosity tests were conducted on the e-liquids of Examples 1-3 and Comparative Examples 1-7, and the test results are shown in Table 2 below.

[0123] Table 2. Viscosity test results of electronic atomizing liquids in Examples 1-3 and Comparative Examples 1-7.

[0124]

[0125]

[0126] As shown in Table 2, the electronic atomizing liquid containing terpene-removed sweet orange oil prepared in this embodiment of the invention can reduce the content of terpenoids and increase its water solubility by performing molecular distillation on natural sweet orange oil. This reduces the use of low-viscosity solvent in the flavoring—95% edible alcohol—and thus increases the viscosity of the atomizing liquid, reducing the risk of leakage of the electronic atomizing liquid containing terpene-removed sweet orange oil in the electronic atomizer.

[0127] 3. Sensory evaluation test

[0128] A panel of 20 professional e-liquid tasters evaluated the samples from the examples and comparative examples. Each indicator was scored from 0 to 100 points, with higher scores indicating stronger responses. The average results were taken. Sensory evaluation tests were conducted on the e-liquids containing terpene-free sweet orange oil from Examples 1-3 and Comparative Examples 1-7. The test results are shown in Table 3 below.

[0129] Table 3 Sensory evaluation test results of Examples 1-3 and Comparative Examples 1-7

[0130]

[0131]

[0132] As shown in Table 3, the electronic atomizing liquid containing terpene-removed sweet orange oil prepared in this embodiment of the invention has a significant improvement in flavor. Due to the molecular distillation of natural sweet orange oil, terpenoids that contribute less to the aroma can be removed, thus improving its stability. It can also remove impurities and off-flavors. Then, in synergy with the monomeric fragrance, it can significantly improve the experience quality of the electronic atomizing liquid containing terpene-removed sweet orange oil during atomization.

[0133] In summary, this invention provides an electronic atomizing liquid containing terpene-free sweet orange oil and its preparation method. Utilizing molecular distillation technology to process natural sweet orange oil not only preserves its flavor as much as possible but also removes some terpenes and impurities, eliminates off-gassing, and improves the solubility of sweet orange oil in the atomizing liquid system, resulting in a stable atomizing liquid that is clear, does not separate, and does not float. During the preparation of the sweet orange flavoring, the amount of ethanol added is strictly controlled to regulate the viscosity at an appropriate level, reducing the risk of leakage in the electronic atomizer. By employing fragrance blending techniques, natural flavoring substances such as aldehydes and alcohols are added to create a harmonious, rich, and natural aroma in the electronic atomizing liquid containing terpene-free sweet orange oil.

[0134] This invention selects ethyl butyrate, octyl acetate, citronellol, n-decanal, citral, n-octanol, nerol acetate, n-nonanol, citronellol, linalool, geraniol, geraniol acetate, nerol, n-octanol, n-decanoic acid, perillaldehyde, ethyl maltol, Valencia orangeene, benzyl alcohol, and vanillin as monomeric fragrances. By adding monomeric fragrances to terpene-free sweet orange oil using fragrance blending techniques, the components work synergistically during atomization, resulting in a harmonious, rich, and natural aroma in the electronic atomized liquid.

[0135] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the technical scope disclosed in the present invention, and these modifications or substitutions should all be covered within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. An electronic atomized liquid containing d-limonene-free sweet orange oil, characterized in that, It is composed of the following components by weight percentage: sweet orange flavor 20-45%, nicotine salt 0-5%, sweetener 0-10%, acidulant 0-10%, cooling agent 0-10%, vegetable glycerin 35-50%, and propylene glycol balance; The sweet orange flavoring is composed of the following components by weight percentage: 10-50% terpene-free sweet orange oil, 0.01-3.0% ethyl butyrate, 0.05-2.0% octyl acetate, 0.05-2.0% citronellol, 0.02-2.0% n-decanal, 0.02-1.0% citral, 0.02-1.0% n-octanol, 0.02-0.9% nerol acetate, 0.02-0.9% n-nonanol, 0.02-2.0% citronellol, and 0.0% linalool. 2-5.0%, Geraniol 0.02-1.5%, Geraniyl acetate 0.02-1.0%, Nerol 0.02-0.5%, Octal 0.02-1.0%, Decanoic acid 0.02-2.0%, Perillaldehyde 0.01-0.9%, Ethyl maltol 0.02-2.0%, Valencian citric acid 0.01-0.8%, Benzyl alcohol 0.02-0.9%, Vanillin 0.02-0.4%, Edible ethanol 10-30%, Propylene glycol balance; The method for preparing the terpene-free sweet orange oil includes the following steps: S1. Natural sweet orange oil is subjected to first molecular distillation. The conditions for first molecular distillation are: vacuum degree 100-2000Pa, main evaporator temperature 40-90℃, roller speed 60-400rpm, and feed rate 200-2000mL / h. Collect the heavy components to obtain sweet orange oil 1. S2. Mix sweet orange oil 1 with propylene glycol at a mass ratio of 1:(4-99), and then sonicate for 0.5-1h to obtain sweet orange oil 2. S3. The sweet orange oil 2 is subjected to a second molecular distillation. The conditions for the second molecular distillation are: vacuum degree 0.1-50 Pa, main evaporator temperature 50-150℃, roller speed 60-400 rpm, and feed rate 500-5000 mL / h. The light components are collected to obtain sweet orange oil 3, which is the terpene-free sweet orange oil.

2. The electronic atomizing liquid containing d-limonene orange oil according to claim 1, wherein It consists of the following components by weight percentage: sweet orange flavor 20-45%, nicotine salt 0.01-5%, sweetener 0.01-10%, acidulant 0.01-10%, cooling agent 0.01-10%, vegetable glycerin 35-50%, and propylene glycol balance.

3. The electronic atomizing liquid containing d-limonene orange oil according to claim 1, wherein The sweetener is one or more of sucralose, neotame, steviol glycosides, and maltitol.

4. The electronic atomizing liquid containing d-limonene orange oil according to claim 1, wherein The acidulant is one or more of acetic acid, propionic acid, and malic acid.

5. The electronic atomizing liquid containing diterpene sweet orange oil according to claim 1, wherein The cooling agent is one or more of WS-23, WS-5, WS-3, and menthone.

6. The electronic atomizing liquid containing diterpene sweet orange oil according to claim 1, wherein The nicotine salt is one or more of the following: benzoic acid nicotine salt, malic acid nicotine salt, tartrate nicotine salt, oxalate nicotine salt, and lactate nicotine salt.

7. The method of claim 1-6, wherein the electronic atomizing liquid containing diterpene sweet orange oil is prepared by the steps of, The process includes the following steps: mixing sweet orange flavoring, nicotine salt, sweetener, acidulant, cooling agent, vegetable glycerin and propylene glycol, letting stand for 0.5-1 hour, and passing through a 200-1000 mesh sieve to obtain an electronic atomizing liquid containing terpene-free sweet orange oil.

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