Disclosure of Invention
Based on the technical problems in the background art, the invention provides an extraction method of essential oil from cigar tobacco leaves.
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding the leftovers of the cigar tobacco leaves, adjusting the water content, standing at room temperature for 2-6h at the temperature of-5 to-10 ℃, drying to constant weight, crushing and sieving, spraying an enzymolysis solution on the surface of the leftovers, performing enzymolysis for 5-10h at the temperature of 20-35 ℃, and performing high-temperature inactivation to obtain the enzymolysis tobacco leaves;
s2, adding the enzymolysis tobacco leaves into a tube furnace, heating to 160 ℃ under the protection of nitrogen, preserving the heat for 1-2h, slowly cooling to room temperature, grinding for 10-30min at the grinding speed of 10000-;
s3, adding the pre-crushed cigar tobacco leaves into an ultrasonic extraction tank, adding an organic solvent, soaking for 5-10h, performing ultrasonic extraction for 2-4h, collecting the extracting solutiona(ii) a Adding organic solvent into the residue, ultrasonic extracting for 4-10 hr, collecting extractive solutionb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1-1.5kPa, and collecting the fraction with boiling point lower than 175 ℃ to obtain the essential oil of the cigar tobacco leaves.
Preferably, the cigar tobacco offal is cigar tobacco stem, offal or powder.
Preferably, in S1, the biological enzyme in the enzymolysis solution is at least one of esterase, protease, amylase, hemicellulase, cellulase, ligninase, and pectin lyase.
Preferably, in S1, the mass ratio of the cigar tobacco leftovers to the enzymolysis solution is 5-10: 1-2, the specific activity of the enzymolysis solution is 10000-.
Preferably, in S1, the water content is adjusted to 10-20 wt%.
Preferably, in S1, the drying temperature is 70-80 ℃.
Preferably, in S1, the mixture is crushed and sieved by a 40-100 mesh sieve.
Preferably, the temperature reduction speed of the S2 is 1-2 ℃/min in the process of slowly reducing the temperature to the room temperature.
Preferably, in S3, the organic solvent is ethanol or glycerol.
The technical effects of the invention are as follows:
the method comprises the steps of shredding and freezing the leftovers of the cigar tobacco leaves, drying at 70-80 ℃ to thoroughly soften and embrittle macromolecules such as fibers in the leftovers of the cigar tobacco leaves, carrying out enzymolysis through an enzymolysis solution, ensuring that the dissolution degree of active ingredients is extremely high, carrying out heating treatment in a tube furnace to promote complex reaction processes such as cracking, Maillard and the like, promoting the obtained essential oil to reduce the burning fragrance of the cigar tobacco leaves to the maximum extent, and then matching with reduced pressure concentration distillation, wherein the extraction degree of the essential oil of the cigar tobacco leaves is extremely high, and by controlling the distillation temperature and the vacuum degree and collecting fractions, the macromolecules with weak polarity and negative influence on smoke can be removed, the removal and isolation are effectively realized, and the purity of.
The invention changes the wastes in the cigar processing process into valuable substances, makes full use of resources, extracts the essential oil to be the pure natural tobacco homologous spice, can reduce the smoke to the maximum extent, effectively makes up the defect of insufficient fragrance of tobacco products, achieves the effect of reducing the environmental pollution of the smoke of the cigarettes on the basis of not influencing the sense of the cigarettes, can obviously improve the smoking quality of the cigarettes, can generate good environmental benefit and economic benefit, and has great market potential.
The yield of the tobacco essential oil obtained by the invention is 2.72-3.15%, the yield of the cigar tobacco essential oil obtained by the invention can be improved by 1.5-1.7 times compared with a steam distillation extraction method, and can be improved by 1.2-1.4 times compared with a traditional petroleum ether extraction method, and the cigar tobacco essential oil prepared by the invention is suitable for industrial production.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding 0.5kg of cigar tobacco leftovers, adjusting the water content to 20wt%, standing at room temperature for 2h, freezing at minus 10 ℃ for 2h, heating to 80 ℃, drying to constant weight, crushing, sieving by a 40-mesh sieve, spraying 0.2kg of enzymolysis solution with the specific activity of 10000U/g on the surface of the enzymolysis solution, then placing the enzymolysis solution in a closed enzymolysis tank for enzymolysis for 10h, wherein the enzymolysis temperature is 20 ℃, and inactivating at high temperature to obtain enzymolysis tobacco leaves;
the biological enzyme in the enzymolysis solution comprises: protease, hemicellulase;
s2, adding the enzymolysis tobacco leaves into a tube furnace, heating to 160 ℃ under the protection of nitrogen, preserving heat for 1h, slowly cooling to room temperature at the cooling speed of 2 ℃/min, adding into a grinding kettle, grinding for 10min at the grinding speed of 15000r/min and the grinding pressure of 0.15MPa, and obtaining pre-ground cigar tobacco leaves;
s3, adding 100g of pre-crushed cigar tobacco leaves into an ultrasonic extraction tank, adding 100g of organic solvent, soaking for 10h, ultrasonically extracting for 2h, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting the extracta(ii) a Adding 100g organic solvent into the residue, ultrasonic extracting for 4 hr, opening the drain valve of the ultrasonic extraction tank, collecting extractive solutionb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1.5kPa, and collecting the fraction with the boiling point lower than 175 ℃ to obtain the cigar tobacco leaf essential oil.
Example 2
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding 1kg of cigar tobacco leftovers, adjusting the water content to 10wt%, standing at room temperature for 6h, freezing at-5 ℃ for 6h, heating to 70 ℃, drying to constant weight, crushing, sieving with a 100-mesh sieve, spraying 0.1kg of enzymolysis solution with the specific activity of 20000U/g on the surface of the enzymolysis solution, then placing the enzymolysis solution in a closed enzymolysis tank for enzymolysis for 5h at the enzymolysis temperature of 35 ℃, and inactivating at high temperature to obtain the enzymolysis tobacco leaves;
the biological enzyme in the enzymolysis solution comprises: esterase, cellulase;
s2, adding the enzymolysis tobacco leaves into a tubular furnace, heating to 120 ℃ under the protection of nitrogen, preserving heat for 2h, slowly cooling to room temperature at the cooling speed of 1 ℃/min, adding into a grinding kettle, grinding for 30min at the grinding speed of 10000r/min and the grinding pressure of 0.2MPa, and obtaining pre-ground cigar tobacco leaves;
s3, adding 80g of pre-crushed cigar tobacco leaves into an ultrasonic extraction tank, adding 200g of organic solvent, soaking for 5h, ultrasonically extracting for 4h, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting the extracta(ii) a Adding 40g organic solvent into the residue, ultrasonic extracting for 10 hr, opening the drain valve of the ultrasonic extraction tank, collecting the extractive solutionb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1kPa, collectingAnd (4) cutting the distillate with the boiling point lower than 175 ℃ to obtain the cigar tobacco essential oil.
Example 3
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding 0.6kg of cigar tobacco leftovers, adjusting the water content to 18wt%, standing at room temperature for 3h, freezing at-8 ℃ for 3h, heating to 77 ℃, drying to constant weight, crushing, sieving by a 60-mesh sieve, spraying 0.17kg of enzymolysis solution with the specific activity of 13000U/g on the surface of the enzymolysis solution, then placing the enzymolysis solution in a closed enzymolysis tank for enzymolysis for 8h, wherein the enzymolysis temperature is 25 ℃, and inactivating at high temperature to obtain enzymolysis tobacco leaves;
the biological enzyme in the enzymolysis solution comprises: protease, amylase, ligninase;
s2, adding the enzymolysis tobacco leaves into a tube furnace, heating to 150 ℃ under the protection of nitrogen, preserving heat for 1.3h, slowly cooling to room temperature at the cooling speed of 1.8 ℃/min, adding into a grinding kettle, grinding for 15min at the grinding speed of 14000r/min under the grinding pressure of 0.16MPa, and obtaining pre-ground cigar tobacco leaves;
s3, adding 95g of pre-crushed cigar tobacco leaves into an ultrasonic extraction tank, adding 130g of organic solvent, soaking for 8 hours, ultrasonically extracting for 2.5 hours, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting the extracta(ii) a Adding 80g organic solvent into the residue, ultrasonic extracting for 6 hr, opening the drain valve of the ultrasonic extraction tank, collecting extractive solutionb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1.3kPa, and collecting the fraction with the boiling point lower than 175 ℃ to obtain the cigar tobacco leaf essential oil.
Example 4
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding 0.8kg of cigar tobacco leftovers, adjusting the water content to 12wt%, standing at room temperature for 5h, freezing at minus 6 ℃ for 5h, heating to 73 ℃, drying to constant weight, crushing, sieving with a 80-mesh sieve, spraying 0.13kg of enzymolysis solution with specific activity of 18000U/g on the surface of the enzymolysis solution, then placing the enzymolysis solution in a closed enzymolysis tank for enzymolysis for 6h at the enzymolysis temperature of 30 ℃, and inactivating at high temperature to obtain the enzymolysis tobacco leaves;
the biological enzyme in the enzymolysis solution comprises: amylase, hemicellulase, cellulase, ligninase;
s2, adding the enzymolysis tobacco leaves into a tube furnace, heating to 130 ℃ under the protection of nitrogen, preserving heat for 1.7h, slowly cooling to room temperature at the cooling speed of 1.2 ℃/min, adding into a grinding kettle, grinding for 25min at the grinding speed of 12000r/min and the grinding pressure of 0.18MPa, and obtaining pre-ground cigar tobacco leaves;
s3, adding 85g of pre-crushed cigar tobacco leaves into an ultrasonic extraction tank, adding 170g of organic solvent, soaking for 6h, ultrasonically extracting for 3.5h, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting the extracta(ii) a Adding 60g organic solvent into the residual residue, ultrasonic extracting for 8 hr, opening the drain valve of the ultrasonic extraction tank, collecting the extractive solutionb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1.1kPa, and collecting the fraction with the boiling point lower than 175 ℃ to obtain the cigar tobacco leaf essential oil.
Example 5
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding 0.7kg of cigar tobacco leftovers, adjusting the water content to 15wt%, standing at room temperature for 4h, freezing at-7 ℃ for 4h, heating to 75 ℃, drying to constant weight, crushing, sieving with a 70-mesh sieve, spraying 0.15kg of enzymolysis solution with the specific activity of 15000U/g on the surface of the enzymolysis solution, then placing the enzymolysis solution in a closed enzymolysis tank for enzymolysis for 7h at the enzymolysis temperature of 28 ℃, and inactivating at high temperature to obtain the enzymolysis tobacco leaves;
the biological enzyme in the enzymolysis solution comprises: esterase, protease, amylase, hemicellulase, cellulase, ligninase, pectin lyase;
s2, adding the enzymolysis tobacco leaves into a tubular furnace, heating to 140 ℃ under the protection of nitrogen, preserving heat for 1.5h, slowly cooling to room temperature at the cooling speed of 1.5 ℃/min, adding into a grinding kettle, grinding for 20min at the grinding speed of 13000r/min under the grinding pressure of 0.17MPa, and obtaining pre-ground cigar tobacco leaves;
s3, adding 90g of pre-crushed cigar tobacco leaves into an ultrasonic extraction tank, adding 150g of organic solvent, soaking for 7h, ultrasonically extracting for 3h, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting the extracta(ii) a Adding 70g of organic solvent into the residual slag, performing ultrasonic extraction for 7h, and opening a drain valve of an ultrasonic extraction tankCollecting extractive solutionb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1.2kPa, and collecting the fraction with the boiling point lower than 175 ℃ to obtain the cigar tobacco leaf essential oil.
Comparative example 1
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding 0.7kg of cigar tobacco leftovers, adding the shredded leftovers into a tubular furnace, heating to 140 ℃ under the protection of nitrogen, keeping the temperature for 1.5h, slowly cooling to room temperature at the cooling speed of 1.5 ℃/min, adding the leftovers into a grinding kettle, grinding for 20min at the grinding speed of 13000r/min under the grinding pressure of 0.17MPa, and obtaining pre-ground cigar tobacco;
s2, adding 90g of pre-crushed cigar tobacco leaves into an ultrasonic extraction tank, adding 150g of organic solvent, soaking for 7h, ultrasonically extracting for 3h, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting the extracta(ii) a Adding 70g organic solvent into the residual residue, ultrasonic extracting for 7 hr, opening the drain valve of the ultrasonic extraction tank, collecting the extractive solutionb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1.2kPa, and collecting the fraction with the boiling point lower than 175 ℃ to obtain the cigar tobacco leaf essential oil.
Comparative example 2
A method for extracting essential oil from cigar tobacco leaves comprises the following steps:
s1, shredding 0.7kg of cigar tobacco leftovers, adjusting the water content to 15wt%, standing at room temperature for 4h, freezing at-7 ℃ for 4h, heating to 75 ℃, drying to constant weight, crushing, sieving with a 70-mesh sieve, spraying 0.15kg of enzymolysis solution with the specific activity of 15000U/g on the surface of the enzymolysis solution, then placing the enzymolysis solution in a closed enzymolysis tank for enzymolysis for 7h at the enzymolysis temperature of 28 ℃, and inactivating at high temperature to obtain the enzymolysis tobacco leaves;
the biological enzyme in the enzymolysis solution comprises: esterase, protease, amylase, hemicellulase, cellulase, ligninase, pectin lyase;
s2, adding 90g of enzymolysis tobacco leaves into an ultrasonic extraction tank, adding 150g of organic solvent, soaking for 7h, performing ultrasonic extraction for 3h, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting extracta(ii) a Adding 70g of organic solvent into the residual slag, and performing ultrasonic extractionTaking for 7h, opening a liquid discharge valve of the ultrasonic extraction tank, and collecting the extractb(ii) a Mixing extractive solutionsaWith an extract liquidbConcentrating under reduced pressure, maintaining the vacuum pressure of the system at 1.2kPa, and collecting the fraction with the boiling point lower than 175 ℃ to obtain the cigar tobacco leaf essential oil.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.