Lilac bud oil for cigarettes and preparation method thereof

Abstract

The invention discloses clove bud oil for cigarettes and a preparation method of the clove bud oil. The preparation method comprises the following steps: (1) pretreating and crushing clove buds and mixing with vermiculite; (2) carrying out supercritical extraction without an entrainer to obtain clove bud oil 1; (3) adding an entrainer, and carrying out supercritical extraction to obtain clove bud oil 2; (4) purifying the clove bud oil 2 containing the entrainer through molecular distillation to obtain clove bud oil 3; and (5) adding the clove bud oil 3 purified by molecular distillation into the clove bud oil 1, and uniformly mixing to obtain the clove bud oil. The clove bud oil is obvious in clove characteristic fragrance, natural in fragrance, high in yield and high in product quality, the preparation method is practical and easy to implement, and the effect is good when the clove bud oil is applied to cigarettes.

Description

Technical Field

[0001] The invention relates to the technical field of tobacco flavor extraction, in particular to tobacco clove bud oil and a preparation method thereof. Background Art

[0002] Clove buds are the dried buds of the Myrtaceae family. They are both medicinal and edible, with a pungent flavor and warm properties. Clove bud oil, the primary extract from clove buds, and its main component, eugenol, are widely used in the tobacco industry and have promising market prospects.

[0003] Currently, the main methods for preparing clove bud oil are steam distillation and supercritical CO2 fluid extraction. In the steam distillation process, clove bud oil is a heavy oil with a density slightly greater than that of water, making it easy to form an emulsion with hot water. The clove bud oil droplets and water are difficult to separate, resulting in a complex extraction process and low efficiency. Clove bud oil prepared by supercritical CO2 extraction has a high essential oil content in the clove bud raw material. Although it can be extracted by supercritical extraction without an entrainer, the essential oil cannot be completely extracted and further extraction requires the addition of an entrainer. Clove bud oil extracted with an entrainer will contain entrainers, and further purification can be performed to improve the quality of the essential oil. Therefore, there is an urgent need for a preparation method for clove bud oil that effectively enhances its characteristic clove flavor, improves the yield and quality of the essential oil, and meets the demand for high-aroma, high-quality clove bud oil in cigarettes. Summary of the Invention

[0004] In view of the above deficiencies in the prior art, the technical problem solved by the present invention is to provide a clove bud oil for tobacco and a preparation method thereof. The clove bud oil is prepared by supercritical CO2 extraction and purified by molecular distillation to obtain clove bud oil with a distinct clove flavor and natural aroma. The product has a high yield and good quality. The method is practical, easy to implement, and has strong applicability.

[0005] In order to solve the above technical problems, the present invention provides a method for preparing clove bud oil for tobacco, comprising the following steps:

[0006] (1) Pre-treatment of clove buds by crushing and mixing with vermiculite;

[0007] (2) Clove bud oil 1 was obtained by supercritical CO2 extraction without entrainer;

[0008] (3) Adding an entrainer to extract clove bud oil 2 through supercritical CO2 extraction; the role of the entrainer is to extract the essential oil of clove bud oil as much as possible. After adding the entrainer, the essential oil extracted by supercritical extraction will contain a portion of the entrainer, so the subsequent separation and purification of the molecular distillation process is to separate the entrainer and some macromolecular substances that do not belong to the essential oil.

[0009] (4) Clove bud oil 2 containing an entrainer is purified by molecular distillation to obtain clove bud oil 3; the entrainer and some macromolecular substances that do not belong to the essential oil are removed and separated, which can improve the quality of the essential oil.

[0010] (5) Add the molecularly distilled purified clove bud oil 3 to the clove bud oil 1 and mix them evenly to obtain the clove bud oil.

[0011] As a preferred embodiment of the above technical solution, the preparation method of the tobacco clove bud oil provided by the present invention further includes some or all of the following technical features:

[0012] As an improvement to the above technical solution, in step (1), the pre-treatment of clove buds by crushing and mixing with vermiculite is to crush the dried clove buds into fine powder, add vermiculite and mix evenly; the particle size of the clove bud fine powder is 60-80 mesh, and the mass ratio of the clove bud fine powder to the vermiculite is 10-15:1.

[0013] As an improvement of the above technical solution, the step (2) of obtaining clove bud oil 1 by supercritical extraction without an entrainer specifically comprises preparing clove bud fine powder, supercritical extraction, and filtering to obtain clove bud oil 1.

[0014] As an improvement of the above technical solution, the step (3) of adding an entrainer for supercritical extraction to obtain clove bud oil 2 specifically comprises adding an entrainer, supercritical extraction, and filtration to obtain clove bud oil 2.

[0015] As an improvement of the above technical solution, the supercritical extraction solvent is CO2, the extraction pressure is 15-25MPa; the separation pressure is 5-8MPa; the supercritical extraction temperature is 40-45°C, and the separation temperature is 45-50°C; and filtration is performed using 0.8 micron qualitative filter paper.

[0016] As an improvement of the above technical solution, the extraction time without entrainer in step (2) is 1 hour, and the extraction time with entrainer added in step (3) is 1.5-2.0 hours.

[0017] As an improvement of the above technical solution, the additive is a polar solvent, and the addition ratio is 5-20% of the mass of the clove bud raw material.

[0018] As an improvement of the above technical solution, the polar solvent is one or more of methanol, ethanol, ethyl acetate, n-propanol, n-hexane, etc.

[0019] As an improvement to the above technical solution, in step (4), the clove bud oil 2 containing the entrainer is purified by molecular distillation to obtain the clove bud oil 3; the molecular distillation process conditions are as follows: a thin film evaporation temperature of 50-55°C, a condensation temperature of -5-10°C, a scraper speed of 300-350 r / min, a vacuum degree of 5-10 Pa, and a material flow rate of 3-4 mL / min.

[0020] As an improvement of the above technical solution, in step (5), the molecularly distilled and purified clove bud oil 3 is added to the clove bud oil 1 and mixed evenly to obtain the clove bud oil.

[0021] The present invention also provides a clove bud oil for tobacco use, which is prepared by any of the above methods. The clove bud oil of the present invention has a distinct and natural clove aroma, a high yield, and a high product quality. The preparation method is practical and easy, and the application in cigarettes is effective.

[0022] Compared with the prior art, the technical solution of the present invention has the following beneficial effects:

[0023] The invention discloses a clove bud oil for tobacco. The clove bud oil is prepared by supercritical CO2 extraction and purified by molecular distillation to obtain clove bud oil with obvious clove flavor and natural aroma. The product has high yield and good quality, and the method is practical, easy to implement and has strong applicability.

[0024] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention, it can be implemented in accordance with the contents of the specification. In order to make the above and other purposes, features and advantages of the present invention more obvious and easy to understand, the following is a detailed description in conjunction with the preferred embodiments. DETAILED DESCRIPTION

[0025] The specific embodiments of the present invention are described in detail below. As a part of this specification, the embodiments illustrate the principles of the present invention through examples. Other aspects, features and advantages of the present invention will become clear through the detailed description.

[0026] Example 1:

[0027] (1) Weigh 150 g of dried clove buds, crush them to 70 mesh, add 15 g of clean and dried vermiculite gravel, and mix well;

[0028] (2) The mixture of clove bud powder and vermiculite is put into a material bag, placed in a stainless steel material barrel of a supercritical CO2 extractor, and the parameters of the supercritical CO2 extractor are set to start extraction. The extraction kettle pressure is 20 MPa, the extraction temperature is 40°C, the separation kettle pressure is 7 MPa, the separation temperature is 45°C, and the extraction time is 1 h. After the extraction time is completed, the clove bud oil is filtered through a 0.8 micron qualitative filter paper to obtain clove bud oil 1, which is 18.8 g.

[0029] (3) 25 g of anhydrous ethanol was added to the supercritical CO2 extractor through an entrainer pump, and the supercritical CO2 extraction of the clove bud oil was continued for 2 h to obtain the clove bud oil, which was filtered through a 0.8 μm qualitative filter paper to obtain 23.4 g of clove bud oil 2.

[0030] (4) The clove bud oil 2 containing the entrainer was purified by molecular distillation. The working parameters of the molecular distillation instrument were set as vacuum degree 10 Pa, thin film evaporation temperature 50°C, condensation temperature -8°C, scraper speed 350 r / min, and the material valve was adjusted to maintain the material flow rate at 3 mL / min. After the molecular distillation was completed, the light component was collected to obtain clove bud oil 3, a total of 8.16 g.

[0031] (5) Clove bud oil 3 purified by molecular distillation was added to clove bud oil 1 and mixed evenly to obtain 26.96 g of clove bud oil with an essential oil yield of 17.97%.

[0032] Example 2:

[0033] (1) Weigh 200 g of dried clove buds, crush them to 60 mesh, add 16 g of clean and dried vermiculite gravel, and mix well;

[0034] (2) The mixture of clove bud powder and vermiculite is put into a material bag, placed in a stainless steel material barrel of a supercritical CO2 extractor, and the parameters of the supercritical CO2 extractor are set to start extraction. The extraction kettle pressure is 25 MPa, the extraction temperature is 45°C, the separation kettle pressure is 6 MPa, the separation temperature is 50°C, and the extraction time is 1 h. After the extraction time is completed, the clove bud oil is filtered through a 0.8 micron qualitative filter paper to obtain clove bud oil 1, which is 23.7 g.

[0035] (3) 15 g of n-propanol was added to the supercritical CO2 extractor through an entrainer pump, and the supercritical CO2 extraction of the clove bud oil was continued for 1.5 h to obtain the clove bud oil, which was filtered through a 0.8 μm qualitative filter paper to obtain 17.3 g of clove bud oil 2.

[0036] (4) The clove bud oil 2 containing the entrainer was purified by molecular distillation. The working parameters of the molecular distillation instrument were set as vacuum degree 10 Pa, thin film evaporation temperature 50°C, condensation temperature -10°C, scraper speed 300 r / min, and the material valve was adjusted to maintain the material flow rate at 4 mL / min. After the molecular distillation was completed, the light component was collected to obtain clove bud oil 3, a total of 11.31 g.

[0037] (5) Clove bud oil 3 purified by molecular distillation was added to clove bud oil 1 and mixed evenly to obtain 25.01 g of clove bud oil with an essential oil yield of 17.51%.

[0038] Example 3:

[0039] (1) Weigh 180 g of dried clove buds, crush them to 65 mesh, add 15 g of clean and dried vermiculite gravel, and mix well;

[0040] (2) The mixture of clove bud powder and vermiculite is put into a material bag, placed in a stainless steel material barrel of a supercritical CO2 extractor, and the parameters of the supercritical CO2 extractor are set to start extraction. The extraction kettle pressure is 24 MPa, the extraction temperature is 40°C, the separation kettle pressure is 6.5 MPa, the separation temperature is 45°C, and the extraction time is 1 h. After the extraction time is completed, the clove bud oil is filtered through a 0.8 micron qualitative filter paper to obtain clove bud oil 1, which is 23.1 g.

[0041] (3) 18 g of ethyl acetate was added to the supercritical CO2 extractor through an entrainer pump, and the supercritical CO2 extraction of the clove bud oil was continued for 2 h to obtain clove bud oil, which was filtered through a 0.8 μm qualitative filter paper to obtain 23.3 g of clove bud oil 2.

[0042] (4) The clove bud oil 2 containing the entrainer was purified by molecular distillation. The working parameters of the molecular distillation instrument were set as vacuum degree 5 Pa, thin film evaporation temperature 50°C, condensation temperature -10°C, scraper speed 350 r / min, and the material valve was adjusted to maintain the material flow rate at 3 mL / min. After the molecular distillation was completed, the light component was collected to obtain clove bud oil 3, a total of 9.57 g.

[0043] (5) Clove bud oil 3 purified by molecular distillation was added to clove bud oil 1 and mixed evenly to obtain 32.67 g of clove bud oil with an essential oil yield of 18.15%.

[0044] The clove bud oil prepared by the present invention has a higher essential oil yield than that prepared by steam distillation. The oil has a distinct and natural characteristic clove aroma, exhibiting four aroma notes: spicy, floral, woody, and sour. Sensory evaluation of the clove bud oil of the present invention showed an improvement of 1-2 points out of 5 in the olfactory aroma evaluation score, 1-2 points out of 5 in the smoke aroma richness evaluation score, and 1-2 points out of 5 in the smoke softness evaluation score.

[0045] The raw materials listed in the present invention, as well as the upper and lower limits and interval values ​​of the raw materials, and the upper and lower limits and interval values ​​of the process parameters (such as temperature, time, etc.) can all realize the present invention, and the embodiments are not listed one by one here.

[0046] The above description is only a preferred embodiment of the present invention, which certainly cannot be used to limit the scope of rights of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and changes can be made without departing from the principles of the present invention. These improvements and changes are also considered to be within the scope of protection of the present invention.

Claims

1. A method for preparing clove bud oil for tobacco, characterized in that: The following steps are included: (1) Pre-treatment of clove buds by crushing and mixing with vermiculite; (2) Clove bud oil 1 was obtained by supercritical CO2 extraction without entrainer; (3) adding an entrainer and extracting clove bud oil 2 through supercritical CO2; (4) purifying the clove bud oil 2 containing the entrainer by molecular distillation to obtain clove bud oil 3; (5) Add the molecularly distilled purified clove bud oil 3 to the clove bud oil 1 and mix them evenly to obtain the clove bud oil.

2. The method for preparing clove bud oil for tobacco according to claim 1, wherein: In the step (1), the pre-treatment of clove buds by crushing and mixing with vermiculite is to crush the dried clove buds into fine powder, and add vermiculite to mix evenly; the particle size of the clove bud fine powder is 60-80 mesh, and the mass ratio of the clove bud fine powder to the vermiculite is 10-15:

1.

3. The method for preparing clove bud oil for tobacco according to claim 1, wherein: The step (2) of obtaining clove bud oil 1 by supercritical extraction without entrainer specifically comprises preparing clove bud fine powder, supercritical extraction, and filtering to obtain clove bud oil 1.

4. The method for preparing clove bud oil for tobacco according to claim 1, wherein: The step (3) of adding an entrainer for supercritical extraction to obtain clove bud oil 2 specifically comprises adding an entrainer, supercritical extraction, and filtration to obtain clove bud oil 2.

5. The method for preparing the tobacco clove bud oil according to claim 3 or 4, wherein: The supercritical extraction solvent is CO2, the extraction pressure is 15-25 MPa; the separation pressure is 5-8 MPa; the supercritical extraction temperature is 40-45°C, and the separation temperature is 45-50°C; and filtration is performed using 0.8 micron qualitative filter paper.

6. The method for preparing clove bud oil for tobacco according to claim 1, wherein: The extraction time in step (2) without entrainer is 1 hour, and the extraction time in step (3) with entrainer added is 1.5-2.0 hours.

7. The method for preparing clove bud oil for tobacco according to claim 4, wherein: The entrainer is a polar solvent, and the addition ratio is 5-20% of the mass of the clove bud raw material.

8. The method for preparing clove bud oil for tobacco according to claim 7, wherein: The polar solvent is one or more of methanol, ethanol, ethyl acetate, n-propanol, and n-hexane.

9. The method for preparing clove bud oil for tobacco according to claim 1, wherein: In the step (4), the clove bud oil 2 containing the entrainer is purified by molecular distillation to obtain the clove bud oil 3; the molecular distillation process conditions are as follows: a thin film evaporation temperature of 50-55°C, a condensation temperature of -5-10°C, a scraper speed of 300-350 r / min, a vacuum degree of 5-10 Pa, and a material flow rate of 3-4 mL / min.

10. A clove bud oil for tobacco, characterized by: The tobacco clove bud oil is prepared by the method according to any one of claims 1 to 9.