Essential oil preparation method capable of regulating and controlling components of clove bud oil on line and application

Abstract

The invention provides an essential oil preparation method capable of regulating and controlling components of clove bud oil on line. The invention also provides the clove bud oil prepared by the method and application thereof. The invention further provides the cigarette aroma raw material containing the clove bud oil and the cigarette. The essential oil preparation method and the application have the advantages of raw material advantages, mature technology, adjustable fragrance, simple operation, catalyst advantages, cost saving and wide application range, can obtain the required clove bud oil with an adjustable eugenol and isoeugenol ratio at a high yield, and can be used for preparing the essential oil with the adjustable eugenol and isoeugenol ratio. Therefore, the requirements of cigarette flavor blending application are met, and the practical application value is achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of flavor chemistry and fine chemical production, and relates to an essential oil preparation method and application of clove bud oil components that can be adjusted online, and specifically to an essential oil preparation method and device for adjusting the proportion of key aroma components in clove bud oil through online chemical catalytic reaction, and application in cigarettes. Background Art

[0002] Clove (Eugenia caryophyllata), belonging to the Myrtaceae family, is a plant that is widely grown in many tropical regions around the world, including Indonesia, Africa, Malaysia, and Guangdong, Guangxi and Hainan in China. Clove buds, after drying, not only have a spicy taste and mild nature, but are also highly regarded in traditional medicine for their significant medicinal value. Clove bud extract, clove bud oil, has become an extremely precious and important raw material in the spice industry with its unique aroma and wide application.

[0003] In industrial production, clove bud oil is mainly obtained through steam distillation. This process involves heating the clove buds, extracting the volatile essential oils with water vapor, and collecting them through condensation to obtain a yellow transparent liquid. Clove bud oil exudes a typical spicy, woody and eugenol aroma. The main components include eugenol, β-caryophyllene and eugenol acetate. In addition, it also contains trace components such as isoeugenol and α-caryophyllene, which are about 1% relative to the total content, but also have a great impact on its overall flavor characteristics.

[0004] Eugenol, as the main aroma component in clove bud oil, gives the essential oil a unique spicy smell. Recent studies have shown that isoeugenol, an isomer of eugenol, has a unique sweet, spicy and floral aroma with a hint of ambergris, musk, bean and cream, which can add complexity and richness to the overall aroma characteristics of clove bud oil.

[0005] Steam distillation is an effective essential oil extraction and preparation technology, but it is mainly based on physical processes and it is difficult to achieve more precise regulation of the chemical composition of essential oils. Summary of the invention

[0006] In view of the characteristics of the prior art described above, the purpose of the present invention is to provide an essential oil preparation method and application of an online adjustable clove bud oil component, aiming to provide a clove bud oil with an online adjustable or optimized aroma characteristic composition by controlling the ratio of eugenol and isoeugenol, thereby improving the application value of clove bud oil in cigarette flavoring, thereby meeting the needs of cigarette flavoring applications.

[0007] To achieve the above-mentioned object and other related objects, the first aspect of the present invention provides a method for preparing an essential oil with an online adjustable clove bud oil component, wherein an essential oil preparation device with an online adjustable clove bud oil component is used for online preparation, wherein the essential oil preparation device with an online adjustable clove bud oil component comprises a distillation chamber, a chemical reaction unit, a condenser and an oil-water separator which are sequentially connected online, and the method comprises the following steps:

[0008] 1) in a distillation chamber, passing water vapor into clove buds for heating and distillation to extract a water-oil liquid containing volatile components, wherein the volatile components include eugenol and isoeugenol;

[0009] 2) the water-oil liquid enters the chemical reaction unit online for distillation reaction, and the conversion between eugenol and isoeugenol is achieved under the action of a catalyst to achieve a desired ratio;

[0010] 3) The water-oil liquid containing eugenol and isoeugenol in the required ratio enters a condenser online for cooling and then enters an oil-water separator online for oil-water separation to obtain the required clove bud oil.

[0011] The second aspect of the present invention provides a clove bud oil prepared by the above method.

[0012] A third aspect of the present invention provides a use of clove bud oil in cigarette flavoring.

[0013] A fourth aspect of the present invention provides a cigarette flavor raw material, comprising the above-mentioned clove bud oil.

[0014] A fifth aspect of the present invention provides a cigarette comprising the above-mentioned cigarette flavor raw material.

[0015] As described above, the method for preparing an essential oil with online adjustable clove bud oil components and its application provided by the present invention have the following beneficial effects:

[0016] (1) The present invention provides an online method for preparing an essential oil with adjustable clove bud oil components and its application, which has the advantage of raw materials. Clove buds are used as the extraction raw materials. This natural product has a wide source, is economical, and has abundant resources, thus ensuring the sustainability and cost-effectiveness of the raw materials.

[0017] (2) The present invention provides an online method for preparing an essential oil with adjustable clove bud oil components and its application. The technology is mature and the extraction is carried out using mature steam distillation technology. The technology is easy to operate and control, can be produced quickly, and greatly reduces the production cycle and cost.

[0018] (3) The present invention provides an online method for preparing an essential oil with adjustable clove bud oil components and its application, wherein the aroma is adjustable. By accurately adjusting the ratio of eugenol to isoeugenol, the present invention can prepare clove bud oil with different aroma characteristics to meet different needs in cigarette flavoring.

[0019] (4) The present invention provides an online adjustable clove bud oil component essential oil preparation method and application, which is easy to operate, has a simple operation process, low industrial cost, easy to obtain clove buds, and high extraction efficiency.

[0020] (5) The method and application of preparing an essential oil with online adjustable clove bud oil components provided by the present invention have the advantages of catalysts, the catalysts used are cheap, easy to obtain, non-toxic, and have a high conversion rate. The solid-liquid separation process after the reaction is simple, which facilitates arbitrary control of the product ratio, has a low operating threshold, and does not require the use of organic solvents in the whole process, thereby reducing environmental pollution.

[0021] (6) The present invention provides an online method for preparing an essential oil with adjustable clove bud oil components and its application, and the water used in the reaction can be recycled and reused, further saving costs.

[0022] (7) The present invention provides an online method for preparing an essential oil with adjustable clove bud oil components and its application, which has a wide range of applications. Since clove bud oil can meet the tobacco industry's demand for high-quality spices due to its adjustable and optimized aroma characteristics, it has a wider range of applications and more significant application potential compared to traditional clove bud oil.

[0023] (8) The present invention provides an online method for preparing an essential oil with adjustable clove bud oil components and its application. Through steam distillation and online chemical catalytic reaction, the ratio of eugenol to isoeugenol can be adjusted to prepare clove bud oil with better aroma characteristics, thereby improving the application value of clove bud oil in cigarette flavoring. Clove bud oil with the required ratio of eugenol to isoeugenol can be obtained with a high yield, thereby meeting the application needs of cigarette flavoring.

[0024] (9) The present invention provides an online adjustable clove bud oil component essential oil preparation method and application, wherein the components in the preparation device are detachably connected, making the operation simple and easy to control, achieving the continuity and flexibility of the reaction, and being able to adjust and optimize the parameters such as the type, quantity, and reaction time of the catalyst in the active unit, thereby increasing the ratio of eugenol to isoeugenol in the clove bud oil, and better improving the quality and functionality of the clove bud oil, so as to achieve the best extraction effect.

[0025] (10) The present invention provides an online adjustable clove bud oil component essential oil preparation method and application. The preparation device uses water vapor as a heat source, allowing the temperature and flow rate of water vapor to be adjusted according to actual needs, which can meet the distillation requirements of clove buds and increase the scope of application. At the same time, it is more environmentally friendly and easier to control than other heating methods.

[0026] (11) The present invention provides an online adjustable clove bud oil component essential oil preparation method and application. By adjusting the aroma characteristics, the method may help meet the market demand for products with specific aroma characteristics and has practical application value. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 The structure diagram of the essential oil preparation device of the present invention with online adjustable clove bud oil components is shown. 1 is a water vapor source; 2 is a distillation chamber; 21 is a material partition; 211 is a first cavity; 212 is a second cavity; 3 is a chemical reaction unit; 31 is a movable unit; 4 is a connecting pipe; 5 is a condenser; 51 is a first pipe; 511 is a condensed water outlet; 512 is a condensed water inlet; 52 is a second pipe; 6 is an oil-water separator.

[0028] Figure 2 The chromatogram showing the ratio of eugenol to isoeugenol obtained in Example 1 of the present invention.

[0029] Figure 3 The chromatogram showing the ratio of eugenol to isoeugenol obtained in Example 2 of the present invention.

[0030] Figure 4 The chromatogram showing the ratio of eugenol to isoeugenol obtained in Example 3 of the present invention. DETAILED DESCRIPTION

[0031] The first aspect of the present invention provides a method for preparing an essential oil having an online controllable clove bud oil component, such as Figure 1 As shown, an essential oil preparation device with online adjustable clove bud oil components is used for online preparation, and the essential oil preparation device with online adjustable clove bud oil components includes a distillation chamber, a chemical reaction unit, a condenser and an oil-water separator which are connected in sequence online, and the method includes the following steps:

[0032] 1) in a distillation chamber, passing water vapor into clove buds for heating and distillation to extract a water-oil liquid containing volatile components, wherein the volatile components include eugenol and isoeugenol;

[0033] 2) the water-oil liquid enters the chemical reaction unit online for distillation reaction, and the conversion between eugenol and isoeugenol is achieved under the action of a catalyst to achieve a desired ratio;

[0034] 3) The water-oil liquid containing eugenol and isoeugenol in the required ratio enters a condenser online for cooling and then enters an oil-water separator online for oil-water separation to obtain the required clove bud oil.

[0035] In the above method, if Figure 1 As shown, the essential oil preparation device with online adjustable clove bud oil components also includes a water vapor source, and the distillation chamber is provided with a first cavity, a material partition, and a second cavity from bottom to top in sequence, and the material partition is provided with a plurality of through holes, the first cavity and the second cavity are separated by the material partition and connected through the through holes, the first cavity is connected to the water vapor source, and the second cavity is connected to the chemical reaction unit; a connecting pipe is provided between the chemical reaction unit and the condenser, and the chemical reaction unit is detachably arranged between the distillation chamber and the connecting pipe, and a movable unit is detachably installed inside the chemical reaction unit.

[0036] In a specific embodiment, Figure 1 As shown, the movable unit is connected from top to bottom and has a catalyst inside. According to the conversion of eugenol and isoeugenol in clove bud oil, the type, quantity, reaction time and other parameters of the catalyst are optimized to achieve the best extraction effect.

[0037] In a specific embodiment, Figure 1 As shown, the water vapor source is a water vapor generator, which is arranged outside the distillation chamber, and one end of which is connected to the first cavity. According to the water vapor flow rate, pressure and water vapor temperature required for distillation and purification, the flow rate entering the water vapor generator and the heating temperature of the water vapor generator are regulated, and high-temperature water vapor is generated in the water vapor generator, which directly enters the first cavity of the distillation chamber through the pipeline. The through holes on the material partition can allow water vapor to pass through, and the water vapor contacts and heats the plant material on the material partition. The volatile essential oil components in the plant material are rapidly vaporized under the high temperature and high heat of the water vapor, and enter the chemical reaction unit together with the water vapor. Those skilled in the art can also use water vapor sources with different settings and different settings as needed, such as setting a container for holding liquid water and a heating component for heating liquid water in the first cavity, which can achieve the same technical effect.

[0038] In a specific embodiment, Figure 1As shown, the movable unit and the chemical reaction unit are double-layer tube structures arranged from the inside to the outside, and the movable unit is detachably installed in the tube of the chemical reaction unit as an inner tube. The catalyst can be directly loaded into the movable unit, or placed in the movable unit through a support plate. The lower end of the chemical reaction unit is connected to the distillation chamber through a clamp, and the upper end of the chemical reaction unit is connected to the inlet end of the connecting pipe through a clamp. This arrangement is convenient for disassembly and cleaning, and is also convenient for replacing different materials and chemical reagents. After the water vapor carries the volatile clove bud oil component into the chemical reaction unit, the volatile clove bud oil component reacts with the catalyst in the movable unit to change the ratio of eugenol and isoeugenol in the volatile clove bud oil component, and the water vapor continues to carry the volatile clove bud oil component with the changed ratio of eugenol and isoeugenol into the connecting pipe.

[0039] In a specific embodiment, Figure 1 As shown, the outlet end of the connecting pipe is detachably connected to the upper end of the condenser through a clamp, which is convenient for maintaining or replacing the condenser and the connecting pipe. Water vapor carries the volatile clove bud oil component with a changed ratio of eugenol and isoeugenol through the connecting pipe and enters the condenser from the outlet end of the connecting pipe.

[0040] In a specific embodiment, Figure 1 As shown, the condenser includes a second tube body and a first tube body sleeved on the outside of the second tube body. The second tube body is detachably connected between the connecting pipe and the oil-water separator, which is convenient for maintaining and cleaning the condenser, the connecting pipe and the oil-water separator. The lower end of the first tube body is provided with a condensate inlet, and the upper end is provided with a condensate outlet. The condensate inlet is connected to the cooling water source. After the water vapor carrying the volatile clove bud oil component with a ratio of eugenol and isoeugenol enters the second tube body from the connecting pipe, the cooling water in the first tube body enters from the condensate inlet and flows out from the condensate outlet. With the flow of cooling water, the water vapor and the volatile clove bud oil component with a changed ratio of eugenol and isoeugenol gradually lose heat and condense into liquid and flow into the oil-water separator.

[0041] Those skilled in the art may also select other detachable connection methods to replace the above-mentioned clamp connection method as needed, such as threaded connection, etc.

[0042] In a specific embodiment, Figure 1 As shown, the oil-water separator is vertically arranged, including a transparent tube and a switch arranged at the lower end of the transparent tube. Under the action of gravity, clove bud oil and water with different densities will be stratified. The operator can clearly observe the boundary between the clove bud oil and the water layer through the transparent tube, and selectively release water or clove bud oil by controlling the switch of the transparent tube. The specific form of the switch is not limited, and it can be a knob switch, a valve, or a button switch. The transparent tube can be made of transparent materials such as glass and transparent ceramics.

[0043] The working principle of the above-mentioned essential oil preparation device with online adjustable clove bud oil components is as follows: before use, clove buds are first placed on the material partition, the catalyst is set in the movable unit, and then the movable unit is placed in the chemical reaction unit, and then the distillation chamber, the chemical reaction unit, the connecting pipe, the condenser and the oil-water separator are connected in sequence through clamps to form an online connection; when in use, the water vapor source inputs water vapor into the first cavity, and the water vapor passes through the through holes of the material partition and fully contacts the clove buds. The volatile essential oil components in the clove buds: eugenol and isoeugenol are vaporized due to the heating of the water vapor, and the water vapor carries the volatile essential oil components into the chemical reaction unit, and changes the ratio of eugenol and isoeugenol in the volatile clove bud oil components by chemical reaction with the catalyst in the movable unit, thereby realizing the selective conversion and optimization of the volatile clove bud oil components. After being processed by the chemical reaction unit, the water vapor carrying the volatile clove bud oil component with a changed ratio of eugenol and isoeugenol enters the second tube body of the condenser through the connecting pipe, and the cooling water flows in from the condensation water inlet, flows downward along the inside of the first tube body, and flows out from the condensation water outlet. As the cooling water flows, the water vapor and the volatile clove bud oil component with a changed ratio of eugenol and isoeugenol gradually lose heat and condense into a liquid and flow into the oil-water separator. After standing and stratifying, the clove bud oil and water layers are formed, and the boundary between the clove bud oil and the water layer can be clearly observed through the transparent tube. By switching the transparent tube, water or clove bud oil can be selectively released.

[0044] In the above method, in step 1), the clove buds are dried clove buds.

[0045] In the above method, in step 1), the ratio of the added weight g of the clove buds to the water vapor introduction pressure MPa is 900-1500: 0.5-15, specifically 900-1000: 0.5-1, 900-1000: 1-10, 900-1000: 10-15, 1000-1100: 0.5-1, 1000-1100: 1-10, 1000-1100: 10-15, preferably 1000: 1-10.

[0046] In the above method, in step 1), the clove buds are placed in a distillation chamber for heating and distillation in a manner of water distillation or water distillation.

[0047] In a specific embodiment, the clove buds are placed in a distillation chamber for heating and distillation in a water distillation manner.

[0048] In a specific embodiment, the distillation chamber is a reaction kettle into which water vapor can be introduced for heating and distillation.

[0049] In the above method, in step 1), the flow rate of the water vapor is 0.5 to 1200 L / min, specifically 0.5 to 1 L / min, 1 to 1000 L / min, 1000 to 1200 L / min, preferably 1 to 1000 L / min.

[0050] In the above method, in step 1), the temperature of the heating distillation is 70-100°C, specifically 70-80°C, 80-100°C, preferably 80-100°C.

[0051] In the above method, in step 1), the heating distillation time is 0.1 to 12 hours, specifically 0.1 to 0.5 hours, 0.5 to 10 hours, 10 to 12 hours, preferably 0.5 to 10 hours.

[0052] In the above method, the CAS number of the eugenol is 97-53-0, and the CAS number of the isoeugenol is 97-54-1.

[0053] In the above method, in step 2), the catalyst is selected from at least one of cobalt chloride, cobalt sulfate, ferric chloride or ferric sulfate.

[0054] In one embodiment, the catalyst is selected from cobalt chloride or ferric chloride.

[0055] In the above method, in step 2), the mass ratio of the catalyst to the clove buds is 0.001-1:1, specifically 0.001-0.005:1, 0.005-0.1:1, 0.01-1:1, 0.01-0.5:1, 0.5-1:1, preferably 0.01-0.5:1.

[0056] In a specific embodiment, the mass ratio of the catalyst to the clove buds is 0.001-1:1, and the conversion ratio between eugenol and isoeugenol is 99:1-15:85.

[0057] In a further embodiment, when the catalyst is cobalt chloride or ferric chloride, the mass ratio of the catalyst to the clove buds is 0.001-0.01:1, and the conversion ratio between eugenol and isoeugenol is 99:1-89:11; the mass ratio of the catalyst to the clove buds is 0.01-0.1:1, and the conversion ratio between eugenol and isoeugenol is 89:11-65:35; the mass ratio of the catalyst to the clove buds is 0.1-1:1, and the conversion ratio between eugenol and isoeugenol is 65:35-15:85.

[0058] The precise control of the ratio of eugenol to isoeugenol allows producers to adjust the ratio of the two compounds according to different application requirements, thereby creating clove bud oil with unique aroma characteristics. Moreover, its separation technology can effectively extract these two key components from clove buds without destroying their chemical structure, and does not change other chemical components, maintaining the natural properties of the essential oil.

[0059] In the above method, in step 3), the cooling temperature is 1-30°C, specifically 1-4°C, 4-25°C, 25-30°C, preferably 4-25°C.

[0060] The working mechanism of the method is as follows: clove buds are loaded onto a material partition in a distillation chamber, a certain proportion of catalyst is arranged in an active unit in a chemical reaction unit, after the device is started, water vapor generated by a water vapor source is introduced into a first cavity of the distillation chamber, and as the water vapor rises, it passes through a through hole on the material partition and enters a second cavity, the water vapor comes into direct contact with the clove buds, and the volatile essential oil components in the clove buds: eugenol and isoeugenol are vaporized due to the heating of the water vapor, and the water vapor carries the volatile clove bud oil components into the chemical reaction unit, and the volatile clove bud oil components react rapidly with the catalyst in the active unit to make the volatile clove buds Eugenol in the bud oil component is isomerized to produce a certain proportion of isoeugenol, and the water vapor carrying the volatile clove bud oil component with a changed ratio of eugenol and isoeugenol enters the second tube body of the condenser through the connecting pipe. Cooling water enters from the condensation water inlet and flows out from the condensation water outlet. With the flow of cooling water, the water vapor carrying the volatile clove bud oil component with a changed ratio of eugenol and isoeugenol is cooled and condensed into liquid in the condenser and flows into the oil-water separator for static stratification. Since clove bud oil is heavy oil, the switch is directly turned on to release part of the liquid, so as to obtain clove bud oil with a changed ratio of eugenol and isoeugenol.

[0061] The second aspect of the present invention provides a clove bud oil prepared by the above method.

[0062] A third aspect of the present invention provides a use of clove bud oil in cigarette flavoring.

[0063] A fourth aspect of the present invention provides a cigarette flavor raw material, comprising the above-mentioned clove bud oil.

[0064] A fifth aspect of the present invention provides a cigarette comprising the above-mentioned cigarette flavor raw material.

[0065] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0066] Example 1

[0067] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 1Mpa, the flow rate is 1L / min, the water vapor is ensured to pass through the clove buds evenly, the heating distillation temperature is 80°C, and the heating distillation time is 1h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0068] A chemical reaction unit is connected online above the reactor, and a movable unit is equipped in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is cobalt chloride with a mass of 10g, and the mass ratio of the catalyst to the clove bud is 0.01:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation passes through the reflux system in the reaction tube, and the clove bud oil and water are continuously refluxed, fully contacting with the catalyst, and a chemical reaction occurs to achieve the conversion between eugenol and isoeugenol in the essential oil, reaching the required ratio of 89:11. At the same time, the proportions of other components have not changed.

[0069] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification. After oil-water separation, 21.3g of clove bud oil sample 1# is collected.

[0070] The eugenol and isoeugenol in clove bud oil sample 1# were detected by gas chromatography-mass spectrometry. The specific test results are shown in Figure 2 , Table 1. Figure 2 As shown in Table 1, the ratio of eugenol to isoeugenol in clove bud oil sample 1# is about 89:11, and its specific value is similar to the conversion ratio obtained by the preparation method.

[0071] Table 1

[0072] Compound Retention time Compound peak area Peak area percentage Eugenol 17.951 374087220 88.777％ cis-Isoeugenol 18.755 13655272 3.241％ trans-isoeugenol 19.571 33635308 7.982％

[0073] Application Example 1

[0074] The clove bud oil sample 1# prepared in Example 1 was applied to cigarette flavoring evaluation to obtain a cigarette containing the clove bud oil sample 1# having a ratio of eugenol to isoeugenol of 89:11.

[0075] Aroma olfactory evaluation: The isomerized clove bud oil in Example 1 has obvious spicy and woody aromas.

[0076] Sensory evaluation of smoke: When the prepared clove bud oil is added to the cigarette for smoking, the spicy aroma of the smoke is significantly increased, with a slight woody smell, a slightly increased aroma volume, a slightly increased strength, a slightly increased aroma volume, a slightly soft and delicate smoke, and a slightly increased concentration.

[0077] Example 2

[0078] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 5Mpa, the flow rate is set to 5L / min, and the water vapor is ensured to pass through the clove buds evenly. The heating distillation temperature is 100°C and the heating distillation time is 2h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0079] A chemical reaction unit is connected online above the reactor. A movable unit is installed in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is cobalt chloride with a mass of 10g. The mass ratio of the catalyst to the clove bud is 0.05:1. The catalyst is fixed on the copper mesh in the reaction tube. The water-oil liquid containing volatile components distilled by water vapor heating passes through the reflux system in the reaction tube. The clove bud oil and water are continuously refluxed and fully contacted with the catalyst to produce a chemical reaction, thereby realizing the conversion between eugenol and isoeugenol and reaching the required ratio of 75:25. At the same time, the ratio of other components does not change.

[0080] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and 43.5g of clove bud oil sample 2# is collected.

[0081] The eugenol and isoeugenol in clove bud oil sample 2# were detected by gas chromatography-mass spectrometry. The specific test results are shown in Figure 3 , Table 2. Figure 3As shown in Table 2, the ratio of eugenol to isoeugenol in clove bud oil sample 2# is about 75:25, and its specific value is similar to the conversion ratio obtained by the preparation method.

[0082] Table 2

[0083] Compound Retention time Compound peak area Peak area percentage Eugenol 17.951 374607041 75.078％ cis-Isoeugenol 18.755 36342783 7.284％ trans-isoeugenol 19.571 88009773 17.639％

[0084] Application Example 2

[0085] The clove bud oil sample 2# prepared in Example 2 was applied to cigarette flavoring evaluation to obtain a cigarette containing the clove bud oil sample 2# having a ratio of eugenol to isoeugenol of 75:24.

[0086] Aroma olfactory evaluation: The isomerized clove bud oil in Example 2 has obvious spicy and woody aromas, slightly increased floral and green aromas, and a slightly sweet taste.

[0087] Sensory evaluation of smoke: When the prepared clove bud oil is added to the cigarette for smoking, the spicy aroma of the smoke is significantly increased, the woody and sweet aromas are increased, the strength is slightly increased, the aroma volume is increased, the smoke is soft and delicate, and the smoke concentration is increased.

[0088] Example 3

[0089] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 5Mpa, the flow rate is 5L / min, the water vapor is ensured to pass through the clove buds evenly, the heating distillation temperature is 100°C, and the heating distillation time is 9h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0090] A chemical reaction unit is connected online above the reactor, and a movable unit is equipped in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is cobalt chloride, with a mass of 100g, and the mass ratio of the catalyst to the clove bud is 0.5:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation passes through the reflux system in the reaction tube, and the clove bud oil and water are continuously refluxed, fully contacted with the catalyst, and a chemical reaction occurs to achieve the conversion between eugenol and isoeugenol in the essential oil, reaching the required ratio of 54:46. At the same time, the proportions of other components have not changed.

[0091] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and 121g of clove bud oil sample 3# is collected.

[0092] The eugenol and isoeugenol in clove bud oil sample 3# were detected by gas chromatography-mass spectrometry. The specific test results are shown in Figure 4 , Table 3. Figure 4 As shown in Table 3, the ratio of eugenol to isoeugenol in clove bud oil sample 3# is about 55:45, and its specific value is similar to the conversion ratio obtained by the preparation method.

[0093] Table 3

[0094] Compound Retention time Compound peak area Peak area percentage Eugenol 17.951 803831168 54.605％ cis-Isoeugenol 18.755 277139038 18.826％ trans-isoeugenol 19.571 391104839 26.568％

[0095] Application Example 3

[0096] The clove bud oil sample 3# prepared in Example 3 was applied to cigarette flavoring evaluation to obtain a cigarette containing the clove bud oil sample 3# having a ratio of eugenol to isoeugenol of 54:46.

[0097] Aroma olfactory evaluation: The isomerized clove bud oil in Example 3 has spicy and bean aromas, obvious sweet aroma, obvious floral aroma, slightly increased green aroma, and a softer aroma.

[0098] Sensory evaluation of smoke: When the prepared clove bud oil was added to the cigarette for smoking, the spicy aroma of the smoke increased significantly, the woody and sweet aromas increased significantly, the strength was improved, the aroma volume was increased, the smoke was more delicate, the smoke concentration was increased, and the irritation was reduced.

[0099] Example 4

[0100] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 5Mpa, the flow rate is 1L / min, the water vapor is ensured to pass through the clove buds evenly, the heating distillation temperature is 95°C, and the heating distillation time is 8h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0101] A chemical reaction unit is connected online above the reactor, and a movable unit is equipped in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is cobalt chloride, with a mass of 900g, and the mass ratio of the catalyst to the clove bud is 0.9:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation is continuously refluxed by the reflux system in the reaction tube, and the clove bud oil and water are fully contacted with the catalyst to react chemically, so as to realize the conversion between eugenol and isoeugenol in the essential oil, and the required ratio is 15:85. At the same time, the proportions of other components have not changed.

[0102] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and 122g of clove bud oil sample 4# is collected.

[0103] Example 5

[0104] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 5Mpa, the flow rate is 1L / min, the water vapor is ensured to pass through the clove buds evenly, the heating distillation temperature is 95°C, and the heating distillation time is 12h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0105] A chemical reaction unit is connected online above the reactor, and a movable unit is equipped in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is cobalt chloride, with a mass of 900g, and the mass ratio of the catalyst to the clove bud is 0.9:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation is continuously refluxed by the reflux system in the reaction tube, and the clove bud oil and water are fully contacted with the catalyst to react chemically, so as to realize the conversion between eugenol and isoeugenol in the essential oil, and the required ratio is 15:85. At the same time, the proportions of other components have not changed.

[0106] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and 122.5g of clove bud oil sample 5# is collected.

[0107] Example 6

[0108] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 1Mpa, the flow rate is 1L / min, the water vapor is ensured to pass through the clove buds evenly, the heating distillation temperature is 80°C, and the heating distillation time is 1h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0109] A chemical reaction unit is connected online above the reactor, and a movable unit is equipped in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is ferric chloride with a mass of 10g, and the mass ratio of the catalyst to the clove bud is 0.01:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation passes through the reflux system in the reaction tube, and the clove bud oil and water are continuously refluxed, fully contacting with the catalyst, and a chemical reaction occurs to achieve the conversion between eugenol and isoeugenol in the essential oil, reaching the required ratio of 89:11. At the same time, the proportions of other components have not changed.

[0110] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and 21.1g of clove bud oil sample 6# is collected.

[0111] Example 7

[0112] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 1Mpa, the flow rate is 1L / min, the water vapor is ensured to pass through the clove buds evenly, the heating distillation temperature is 80°C, and the heating distillation time is 1h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0113] A chemical reaction unit is connected online above the reactor, and a movable unit is equipped in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is cobalt sulfate, with a mass of 10g, and the mass ratio of the catalyst to the clove bud is 0.01:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation passes through the reflux system in the reaction tube, and the clove bud oil and water are continuously refluxed, fully contacting with the catalyst, and a chemical reaction occurs to achieve the conversion between eugenol and isoeugenol in the essential oil, reaching the required ratio of 99:1. At the same time, the proportions of other components have not changed.

[0114] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and 20.2g of clove bud oil sample 7# is collected.

[0115] Example 8

[0116] 1000g of clove buds are weighed for online preparation, that is, they are evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of the online adjustable clove bud oil component. Water vapor is introduced for heating distillation by water distillation, the pressure of the water vapor is set to 1Mpa, the flow rate is 1L / min, the water vapor is ensured to pass through the clove buds evenly, the heating distillation temperature is 80°C, and the heating distillation time is 1h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, are vaporized due to the heating of the water vapor, so that the volatile components in the clove buds can be extracted, which is a water-oil liquid containing volatile components.

[0117] A chemical reaction unit is connected online above the reactor, and a movable unit is equipped in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is iron sulfate with a mass of 10g, and the mass ratio of the catalyst to the clove bud is 0.01:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation passes through the reflux system in the reaction tube, and the clove bud oil and water are continuously refluxed, fully contacting with the catalyst, and a chemical reaction occurs to achieve the conversion between eugenol and isoeugenol in the essential oil, reaching the required ratio of 99:1. At the same time, the proportions of other components have not changed.

[0118] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and 21.3g of clove bud oil sample 8# is collected.

[0119] Comparative Example 1

[0120] 1000g of clove buds were weighed and a clove bud oil sample 1* was prepared by conventional steam distillation, that is, clove buds were placed in a reactor serving as a distillation chamber, steam was introduced for heating and distillation, the steam pressure was set to 1Mpa, the flow rate was 1L / min, the heating and distillation temperature was 80°C, the heating and distillation time was 1h, and a water-oil liquid 1* containing volatile components was extracted without any chemical catalyst. The water-oil liquid 1* was then placed in a condenser for cooling at a cooling temperature of 10°C, condensed into a liquid, and then placed in an oil-water separator for standing and stratification. After oil-water separation, the clove bud oil sample 1* was obtained.

[0121] The obtained clove bud oil sample 1* was tested for the ratio of eugenol to isoeugenol by gas chromatography-mass spectrometry, and the conversion ratio of eugenol to isoeugenol in the clove bud oil sample 1* was determined to be about 99.9:0.1. Meanwhile, the ratios of other components did not change.

[0122] Comparative Example 2

[0123] Weigh 1000g of clove buds and use conventional steam distillation to prepare clove bud oil sample 2*, that is, put clove buds in a reactor serving as a distillation chamber, pass water vapor for heating distillation, set the water vapor pressure to 5Mpa, the flow rate to 5L / min, the heating distillation temperature to 100°C, the heating distillation time to 2h, and extract the water-oil liquid 2* containing volatile components without any chemical catalyst. Then, put the water-oil liquid 2* into a condenser for cooling at a cooling temperature of 10°C, condense into a liquid, and then put it into an oil-water separator for standing and stratification. After oil-water separation, the clove bud oil sample 2* is obtained.

[0124] The obtained clove bud oil sample 2* was tested for the ratio of eugenol to isoeugenol by gas chromatography-mass spectrometry, and the conversion ratio of eugenol to isoeugenol in the clove bud oil sample 2* was determined to be about 99.9:0.1. At the same time, the ratios of other components did not change.

[0125] Comparative Example 1

[0126] The clove bud oil sample 1-8# prepared in Example 1-8 was compared with the clove bud oil sample 1-2* prepared in Comparative Example 1-2. The specific data are shown in Table 4.

[0127] As shown in Table 4, when the catalyst is cobalt chloride or ferric chloride, the eugenol in the clove bud oil sample is isoeugenol, which has a higher conversion ratio, and the control and conversion of the conversion ratio can be achieved. When the catalyst is cobalt sulfate or ferric sulfate, the eugenol in the clove bud oil sample is isoeugenol, which has a lower conversion ratio. At the same time, in the clove bud oil sample prepared by the existing method, that is, without a catalyst, the conversion ratio of eugenol to isoeugenol is almost zero.

[0128] Table 4

[0129]

[0130]

[0131] Comparative Example 3

[0132] 1000g of clove buds were weighed to prepare clove bud oil sample 3* online, that is, they were evenly laid on the material partition in the reactor as the distillation chamber in the essential oil preparation device of online adjustable clove bud oil components. Water vapor was introduced for heating distillation by water distillation, the pressure of water vapor was set to 5Mpa, the flow rate was set to 5L / min, and the water vapor was ensured to pass through the clove buds evenly. The heating distillation temperature was 100°C and the heating distillation time was 9h, so that the volatile essential oil components in the clove buds, including eugenol and isoeugenol, were vaporized due to the heating of water vapor, so that the volatile components in the clove buds could be extracted, which was a water-oil liquid containing volatile components.

[0133] A chemical reaction unit is connected online above the reactor. A movable unit is installed in the chemical reaction unit. The movable unit is a reaction glass tube containing a catalyst that can be directly disassembled at will. The catalyst is sodium hydroxide with a mass of 100g. The mass ratio of the catalyst to the clove bud is 0.5:1. The catalyst is fixed on the copper mesh wire in the reaction tube. The water-oil liquid containing volatile components obtained by steam heating and distillation passes through the reflux system in the reaction tube. The clove bud oil and water are continuously refluxed, fully contacted with the catalyst, and a chemical reaction occurs.

[0134] After the catalytic reaction is completed, the water-oil liquid containing eugenol and isoeugenol enters the condenser online and is cooled at a cooling temperature of 10°C. It is condensed into a liquid and flows into the oil-water separator online for standing and stratification to separate the oil and water, and the clove bud oil sample 3* is collected.

[0135] Comparative Example 2

[0136] The clove bud oil sample 3# prepared in Example 3 and the clove bud oil sample 3* prepared in Comparative Example 3 were tested for eugenol and isoeugenol in the samples by gas chromatography-mass spectrometry. At the same time, other components in the samples, such as eugenol acetate, were tested. The specific data are shown in Table 5.

[0137] As can be seen from Table 5, compared with the method of the present invention, the use of existing strong bases such as sodium hydroxide as a catalyst can also change the conversion ratio of eugenol and isoeugenol, but its conversion ratio of eugenol and isoeugenol under the same conditions is worse than that of the present invention. At the same time, it will also change the proportion of other components in the clove bud oil sample. For example, the proportion of eugenol acetate in the clove bud oil sample 3* prepared in Comparative Example 3 changes, causing a fundamental change in the chemical composition of the clove bud oil sample, and the desired clove bud oil sample cannot be obtained.

[0138] Table 5

[0139]

[0140] The above is only a preferred embodiment of the present invention, and is not any formal or substantial limitation of the present invention. It should be pointed out that ordinary technicians in this technical field can make several improvements and supplements without departing from the method of the present invention, and these improvements and supplements should also be regarded as the protection scope of the present invention. Any technician familiar with this profession, without departing from the spirit and scope of the present invention, can make some changes, modifications and evolutions of the technical content disclosed above, which are equivalent embodiments of the present invention; at the same time, any changes, modifications and evolutions of any equivalent changes made to the above embodiments based on the essential technology of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A method for preparing an essential oil having an online adjustable clove bud oil component, wherein the essential oil is prepared online using an essential oil preparation device having an online adjustable clove bud oil component, wherein the essential oil preparation device having an online adjustable clove bud oil component comprises a distillation chamber (2), a chemical reaction unit (3), a condenser (5) and an oil-water separator (6) which are connected in sequence online, and the method comprises the following steps: 1) in a distillation chamber (2), steam is introduced into clove buds for heating and distillation to extract a water-oil liquid containing volatile components, wherein the volatile components include eugenol and isoeugenol; 2) the water-oil liquid enters the chemical reaction unit (3) online for distillation reaction, and the conversion between eugenol and isoeugenol is achieved under the action of a catalyst to achieve a desired ratio; 3) The water-oil liquid containing eugenol and isoeugenol in the required ratio enters the condenser (5) online for cooling, and then enters the oil-water separator (6) online for oil-water separation to obtain the required clove bud oil.

2. The method for preparing an essential oil having an online controllable clove bud oil component according to claim 1, characterized in that: The essential oil preparation device with online adjustable clove bud oil components also comprises a water vapor source (1); a first cavity (211), a material partition (21), and a second cavity (212) are sequentially arranged from bottom to top in the distillation chamber (2); the material partition (21) is provided with a plurality of through holes; the first cavity (211) and the second cavity (212) are separated by the material partition (21) and are connected via the through holes; the first cavity (211) is connected to the water vapor source (1), and the second cavity (212) is connected to a chemical reaction unit (3); a connecting pipe (4) is arranged between the chemical reaction unit (3) and the condenser (5); the chemical reaction unit (3) is detachably arranged between the distillation chamber (2) and the connecting pipe (4), and a movable unit (31) is detachably installed inside the chemical reaction unit (3).

3. The method for preparing an essential oil having an online controllable clove bud oil component according to claim 2, characterized in that: The essential oil preparation device with online adjustable clove bud oil components also includes any one or more of the following conditions: A1) The movable unit (31) is connected vertically and has a catalyst inside; A2) the water vapor source (1) is a water vapor generator, one end of the water vapor generator is connected to the first cavity (211); A3) the movable unit (31) and the chemical reaction unit (3) are double-layer tube structures arranged from the inside to the outside, and the movable unit (31) is detachably installed in the tube of the chemical reaction unit (3) as an inner tube; A4) the outlet end of the connecting pipe (4) is detachably connected to the upper end of the condenser (5) via a clamp; A5) the condenser (5) comprises a second tube body (52) and a first tube body (51) sleeved on the outside of the second tube body (52), the second tube body (52) is detachably connected between the connecting pipe (4) and the oil-water separator (6), the lower end of the first tube body (51) is provided with a condensed water inlet (512), and the upper end is provided with a condensed water outlet (511); A6) The oil-water separator (6) is arranged vertically, and comprises a transparent tube and a switch arranged at the lower end of the transparent tube.

4. The method for preparing an essential oil having an online controllable clove bud oil component according to claim 1, characterized in that: Step 1) includes any one or more of the following conditions: B1) the clove buds are dried clove buds; B2) the ratio of the added weight of the clove buds to the water vapor pressure Mpa is 900-1500: 0.5-15, g / Mpa; B3) the clove buds are placed in a distillation chamber for heating and distillation in a way of water distillation or water distillation; B4) the flow rate of the water vapor is 0.5-1200 L / min; B5) the temperature of the heating distillation is 70-100°C; B6) The heating distillation time is 0.1 to 12 hours.

5. The method for preparing an essential oil having an online controllable clove bud oil component according to claim 1, characterized in that: Step 2) includes any one or more of the following conditions: C1) the catalyst is selected from at least one of cobalt chloride, cobalt sulfate, ferric chloride or ferric sulfate; preferably, the catalyst is selected from one of cobalt chloride or ferric chloride; C2) The mass ratio of the catalyst to the clove buds is 0.001 to 1:

1.

6. The method for preparing an essential oil having an online controllable clove bud oil component according to claim 1, characterized in that: In step 3), the cooling temperature is 1-30°C.

7. A clove bud oil prepared by the essential oil preparation method of online adjustable clove bud oil components according to any one of claims 1 to 6.

8. Use of the clove bud oil according to claim 7 in cigarette flavoring.

9. A cigarette flavor raw material, comprising the clove bud oil according to claim 7.

10. A cigarette comprising the cigarette flavor raw material according to claim 9.

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