Ficus tikoua bur natural essential oil extraction method and special extraction equipment

Abstract

The invention discloses a wild sweet potato natural essential oil extraction method and special extraction equipment, and belongs to the technical field of natural perfume extraction. The extraction method comprises the steps of raw material pretreatment, crushing, extraction, separation, purification and aging, the extraction process covers all mainstream and novel processes such as steam distillation, ultrasonic-assisted extraction and subcritical extraction, the extraction temperature ranges from-20 DEG C to 120 DEG C, the pressure covers vacuum negative pressure to pressurization, and the raw materials cover fruits, stems, vines, leaves, roots, skins, milk and whole plants of ficus tikoua bur; the special extraction equipment comprises a crushing unit, an extraction unit, a temperature control unit, a pressure control unit, a condensation unit, an oil-water separation unit, a graded collection unit and a storage whole unit, the extraction unit can be flexibly switched and is adaptive to all extraction working conditions, and the condensation unit is a gradient / graded condensation system and can realize segmented collection of head incense, body incense and base incense. The technology covers the whole domain, equipment is exclusively matched, the technology and reported related patents of the ficus tikoua bur are coordinated and complemented, the situation that other people change the technology, parameters and equipment and select specific raw material parts to hit edge balls is thoroughly avoided, full blocking of the ficus tikoua bur natural essential oil extraction racing track is achieved, meanwhile, the extraction efficiency is high, fragrance is completely reserved, and the raw materials are completely utilized; the application range is wide.

Description

Technical Field

[0001] This invention belongs to the field of natural fragrance extraction technology, specifically relating to a method and specialized extraction equipment for extracting natural essential oil from wild jujube (Gnaphalium affine). It is applicable to the extraction of natural essential oil from the whole plant and various parts of wild jujube (Gnaphalium affine / Gnaphalium loquat), covering all scenarios including refined laboratory preparation, small-to-medium-scale industrial production, and high-end, high-fidelity essential oil preparation. It also extends its application to the extraction of essential oils from highly aromatic plants of the Moraceae family (Ficus and Morus). This invention complements existing extraction technologies such as deep processing, low-temperature aroma extraction, and atmospheric distillation of wild jujube, providing comprehensive technical coverage and improving the technical system for the extraction of natural essential oil from wild jujube. Background Technology

[0002] Wild jujube, a perennial creeping woody vine belonging to the genus Ficus of the Moraceae family, is rich in unique natural aromatic components in its fruits, stems, leaves, and latex. The extracted essential oil boasts a pure aroma and is naturally additive-free, making it widely used in perfumes, aromatherapy, car fragrances, cultural and creative fragrance products, and functional foods. Currently, existing wild jujube essential oil extraction technologies are mostly concentrated on single process routes, such as atmospheric distillation, low-temperature extraction, and coupling extraction with membrane separation. These methods suffer from incomplete extraction process coverage, poor equipment adaptability, and limited process parameter ranges. Furthermore, existing extraction equipment is mostly general-purpose distillation / extraction equipment, not specifically designed for the characteristics of wild jujube raw materials. This results in low aroma component retention, uneven extraction efficiency, and the inability to achieve graded aroma extraction. Simultaneously, existing technologies have limitations in utilizing different parts of the wild jujube raw material, failing to achieve whole-plant resource extraction and not covering novel extraction processes such as ultrasound, microwave, and subcritical extraction, making it difficult to meet the diverse and high-quality extraction needs of wild jujube essential oil.

[0003] To address the aforementioned technical challenges, this invention expands upon existing wild gooseberry essential oil extraction technologies (including low-temperature non-destructive aroma extraction, simplified atmospheric distillation, low-pressure fractional distillation, and membrane separation coupling) by comprehensively extending the process and designing dedicated equipment. It develops a complete method and specialized extraction equipment for extracting natural wild gooseberry essential oil, covering all processes, parameters, and raw material components. This achieves seamless coverage of the extraction process, dedicated equipment adaptation, and application across all scenarios, enhancing the comprehensiveness and adaptability of wild gooseberry essential oil extraction technology and meeting the extraction needs of different scales and quality requirements. Summary of the Invention

[0004] 1. Purpose of the invention The purpose of this invention is to provide a method and dedicated extraction equipment for extracting natural essential oil from wild jujube, which solves the technical defects of existing wild jujube essential oil extraction processes, such as limited parameter range, poor equipment adaptability, and ease of circumvention. This invention achieves full coverage of wild jujube essential oil extraction across all process paths, parameter ranges, and raw material parts. At the same time, it designs dedicated equipment adapted to all extraction processes to ensure high extraction efficiency, complete preservation of aroma components, and good graded aroma extraction effect. This invention forms a comprehensive technical protection with existing wild jujube extraction-related patents, completely locking down the wild jujube natural essential oil extraction market and leaving no loopholes for others to exploit.

[0005] 2. Technical Solution

[0006] (a) A method for extracting natural essential oil from wild jujube. The process includes raw material pretreatment, crushing, extraction, separation, purification, and aging. The specific steps are as follows: ① Raw material pretreatment: Select any one or more combinations of fresh or preserved wild melon fruits, stems, vines, leaves, roots, peel, latex, or whole plant as raw materials. Remove mud, rotten parts, impurities, etc., rinse with clean water, and drain or air dry at -10℃~30℃ to remove surface free moisture and prevent raw material deterioration or loss of heat-sensitive aroma components; if the raw material is latex, filter directly to remove impurities before use. ② Crushing: Place the pretreated solid raw materials in an environment of -10℃ to 30℃ and crush or gently break down the cell walls using a crusher or grinder. The particle size after crushing is 10 to 80 mesh. The particle size can be adjusted according to the subsequent extraction process to avoid local overheating that could lead to the decomposition of aroma components. ③ Extraction: Place the crushed raw material or filtered milk in an extraction device and perform extraction using any one or more of the following methods: steam distillation, atmospheric distillation, vacuum distillation, low-pressure distillation, fractional distillation, gradient distillation, ultrasonic-assisted extraction, microwave-assisted extraction, subcritical extraction, supercritical CO2 extraction, cold grinding extraction, adsorption desorption, fermentation extraction, enzymatic extraction, and maceration. The extraction temperature should cover -20℃ to 120℃, and the extraction pressure should cover vacuum (≤0.01MPa), atmospheric pressure (0.1MPa), and pressurized pressure (0.1~0.5MPa). No organic solvents should be added during extraction, or only water or edible ethanol should be used as the extraction medium. The extraction time should be adjusted from 30min to 6h according to the extraction process to ensure sufficient enrichment of aroma components. ④ Separation: After extraction, solid-liquid separation or oil-water separation is carried out by any one of the following methods: centrifugation, filtration, sedimentation, membrane separation (molecular weight cutoff 1000-100000 Da), or oil-water separation, to remove raw material residues and solids, and obtain aroma-enriched liquid or crude essential oil. The temperature during the separation process is controlled between 0℃ and 40℃ to avoid loss of aroma components; ⑤ Purification and Pre-Aging: The separated aroma concentrate or crude essential oil is purified using any one or more of the following methods: molecular distillation, gradient condensation, staged condensation, low-temperature aging, and microfiltration (0.22–0.8 μm filter membrane). Gradient condensation and staged condensation allow for the segmented collection of top notes, middle notes, and base notes. Low-temperature aging is carried out at 2℃–8℃ for 7–30 days to ensure the purity and aroma stability of the essential oil. ⑥ Post-processing aging: Place the purified essential oil in a sealed container and age it for 7 to 30 days at 0℃~10℃ in the dark to make the aroma of the essential oil more mellow and stable, thus obtaining high-purity wild jujube natural essential oil.

[0007] (ii) A special extraction device for wild yam natural essential oil that realizes the above extraction method It includes a crushing unit, an extraction unit, a temperature control unit, a pressure control unit, a condensation unit, an oil-water separation unit, a graded collection unit, and an essential oil storage unit. All units are connected sequentially. The entire device is made of stainless steel, resistant to low temperatures, high temperatures, and slight pressure. It is suitable for any operating condition, including normal pressure, low pressure, vacuum, ultrasonic, microwave, adsorption, fermentation, and distillation. The specific structure and functions are as follows: ① Crushing Unit: Includes feed inlet, low-temperature crusher, grinder, and discharge outlet. Equipped with a temperature control module, it can control the crushing environment temperature between -10℃ and 30℃, and can achieve adjustable crushing of raw materials from 10 to 80 mesh, adapting to the crushing needs of different parts of wild gourd. ② Extraction Unit: It can be any one of the following: distillation tank, ultrasonic extraction tank, microwave extraction chamber, subcritical extraction vessel, adsorption resin column, or fermentation tank. It is connected to the discharge port of the crushing unit. The extraction unit is equipped with a raw material stirring module and an extraction medium injection module. The stirring rate and extraction medium injection volume can be adjusted according to the extraction process to meet the extraction needs of wild gourd throughout the entire process. ③ Temperature control unit: Includes temperature sensor, heating module, and cooling module, connected to crushing unit, extraction unit, condensation unit, oil-water separation unit, and graded collection unit. It can independently control the operating temperature of each unit from -10℃ to 110℃, precisely matching the temperature requirements of the extraction process and avoiding the loss of aroma components due to temperature fluctuations; ④ Pressure control unit: Includes pressure sensor, vacuum pump, pressurizing pump, and pressure regulating valve. It is connected to the extraction unit and condensation unit and can accurately control the pressure of the extraction unit from vacuum negative pressure to 0.5MPa, realizing stepless adjustment of negative pressure, normal pressure, and pressurization to adapt to the pressure requirements of different extraction processes; ⑤ Condensation Unit: A gradient condensation or staged condensation system connected to the extraction unit, including at least two condensation chambers. The condensation temperature can be independently controlled between -10℃ and 40℃, enabling the segmented condensation and collection of the top, middle, and base aromas of wild radish essential oil, ensuring effective separation of different aroma fractions; ⑥ Oil-water separation unit: Connected to the condensation unit, it includes an oil-water separator, a liquid level sensor, and a slag discharge port. It can achieve efficient separation of crude refined oil and water phase after condensation, with a separation efficiency of ≥95%. The separation process temperature is controlled between 0℃ and 25℃. ⑦ Graded Collection Unit: Connected to the condensation unit and oil-water separation unit, it includes multiple independent essential oil collection tanks, corresponding to the top note, middle note, base note fractions and mixed essential oils respectively. The collection tanks are equipped with sealing, light-proof, and low-temperature storage functions, with the temperature controlled between 0℃ and 10℃; ⑧ Essential Oil Storage Unit: Connected to the graded collection unit, it includes a sealed, light-proof storage tank and a low-temperature constant-temperature module. The storage temperature is controlled between 0℃ and 10℃, enabling short-term or long-term storage of essential oils and preventing oxidation and aroma deterioration. The extraction method of this invention is compatible with dedicated extraction equipment. The dedicated extraction equipment serves as the exclusive carrier for the extraction method, allowing for flexible switching of extraction units and adjustment of temperature and pressure parameters according to extraction process requirements, achieving full-process, full-parameter, and full-raw-part extraction of wild yam essential oil.

[0008] 3. Beneficial effects

[0009] Compared with existing technologies, this invention has the following significant advantages: Complete process coverage, thoroughly avoiding risks: ① The extraction method of this invention covers all mainstream and novel extraction processes, including steam distillation, atmospheric distillation, vacuum distillation, low-pressure distillation, fractional distillation, gradient distillation, ultrasonic-assisted extraction, microwave-assisted extraction, subcritical extraction, supercritical CO2 extraction, cold grinding extraction, adsorption desorption, fermentation extraction, enzymatic extraction, and maceration. The extraction temperature covers -20℃ to 120℃, and the extraction pressure covers vacuum negative pressure to 0.5MPa. The raw materials include wild melon fruit, stems, vines, leaves, roots, peel, latex, and the whole plant. This completely prevents others from circumventing patent protection by changing processes, modifying temperatures, adjusting pressures, or selecting specific raw material parts. It complements the already submitted patents on low-temperature non-destructive aroma extraction of wild melon, simplified atmospheric distillation, low-pressure fractional distillation, and maceration membrane separation coupling, achieving full coverage and full protection of wild melon extraction technology. ② Dedicated equipment adaptation, compatible with all working conditions: The dedicated extraction equipment of this invention is specially designed for wild melon raw materials, integrating crushing, extraction, temperature control, pressure control, condensation, oil-water separation, graded collection, and storage units. It can flexibly switch between extraction units such as distillation tanks, ultrasonic extraction tanks, and microwave extraction chambers, and is adaptable to all working conditions including negative pressure, normal pressure, and pressurization. The temperature and pressure are precisely adjustable, solving the problems of poor compatibility and inability to grade and extract aroma from existing general-purpose equipment. At the same time, the equipment structure is a dedicated design, which can effectively prevent others from achieving equivalent technical solutions by simply modifying general-purpose equipment. ③ Complete aroma retention and high extraction efficiency: The entire extraction process of this invention can be controlled at low temperatures to avoid the decomposition of heat-sensitive aroma components. Gradient condensation and staged condensation are used to collect the top notes, middle notes, and base notes in stages, with an aroma component retention rate of ≥90%. At the same time, the extraction process and equipment are compatible with each other, the extraction time can be adjusted according to the process, and the solid-liquid separation and oil-water separation efficiency are high, which greatly improves the extraction efficiency and product quality of wild radish essential oil. ④ High utilization of the whole plant and high degree of resource utilization: This invention breaks through the limitations of existing technology in the utilization of wild melon raw materials, realizing the extraction of all parts of the fruit, stem, vine, leaf, root, peel, latex and whole plant, improving the resource utilization rate of wild melon raw materials and reducing extraction costs. At the same time, it can be extended to the extraction of essential oils from highly fragrant plants of the Ficus and Morus genera of the Moraceae family, with a wide range of applications; ⑤ Collaborating with prior patents to build a full-industry chain technological barrier: This invention expands upon the five wild gourd-related patents previously filed by the inventors, and develops related processes and equipment. All of these prior patents were primarily led by the inventors, some filed by the inventors personally, and some filed by companies in which the inventors are the legal representatives. This invention does not conflict with the prior patents; on the contrary, it forms a synergistic effect with the prior patents in terms of process complementarity, equipment adaptation, and comprehensive protection. From "specific process implementation" to "full-scenario coverage," it builds a full-industry chain technological barrier in the field of wild gourd natural essential oil extraction, achieving comprehensive technological protection. Detailed Implementation

[0010] The present invention will be further described in detail below with reference to specific embodiments. These embodiments are only used to explain the present invention and are not intended to limit the scope of protection of the present invention. All simple modifications based on the present invention are within the scope of protection of the present invention.

[0011] Example 1: Extraction of essential oil from wild jujube fruit by atmospheric distillation ① Raw material pretreatment: Select fresh wild melon fruits as raw materials, remove rotten fruits and impurities, rinse with clean water and drain at 25℃ to remove surface free moisture; ② Crushing: Place the drained wild melon fruit in a 25℃ environment and crush it to 40 mesh to obtain fruit pulp; ③ Extraction: Place the fruit pulp in the distillation tank of a dedicated extraction device, add water at a mass ratio of 1:3, start atmospheric distillation (0.1MPa), extract at 95℃ for 2 hours, use water as the extraction medium, and do not add any organic solvents. ④ Separation: After extraction, an oil-water separator is used to separate the oil and water at a temperature of 20℃ to obtain crude essential oil from wild melon fruit; ⑤ Purification: The crude essential oil was purified by filtration through a 0.45μm micropore filter to remove impurities; ⑥ Aging: The purified essential oil is aged at 5℃ in the dark for 15 days to obtain high-purity wild melon fruit essential oil; The specialized extraction equipment used in this embodiment has an extraction unit that is a distillation tank, a temperature control unit that controls the distillation temperature at 95°C, a pressure control unit that maintains atmospheric pressure, and a gradient condensation system that enables the segmented collection of top notes, body notes, and base notes.

[0012] Example 2: Extraction of essential oil from the whole plant of wild jujube using ultrasound-assisted extraction method ① Raw material pretreatment: Select the whole wild melon plant (fruit + stems and leaves + roots) as raw material, remove impurities and mud, rinse with clean water and air dry at 15℃; ② Crushing: Place the air-dried wild melon plant in a 10℃ environment and crush it to 60 mesh to obtain whole plant powder; ③ Extraction: Place the whole plant powder in the ultrasonic extraction vessel of a special extraction device, add 10 times the amount of edible ethanol as the extraction medium, turn on ultrasonic-assisted extraction, extraction temperature 40℃, extraction pressure normal pressure, ultrasonic power 300W, extraction time 1h; ④ Separation: After extraction, the solids are removed by centrifugation (3000 r / min) to obtain the aroma-enriched solution; ⑤ Purification: The aroma-enriched liquid was purified by molecular distillation at 50℃ and a vacuum of 0.05MPa to obtain crude essential oil from the whole plant of *Gnaphalium affine*. ⑥ Aging: The crude essential oil is aged at 2℃ in the dark for 20 days to obtain high-purity wild jujube whole plant essential oil; The specialized extraction equipment used in this embodiment consists of an ultrasonic extraction tank, a temperature control unit that controls the extraction temperature at 40°C, a pressure control unit that maintains normal pressure, and a graded collection unit that collects the mixed essential oils.

[0013] Example 3: Extraction of wild jujube latex + stem and leaf compound essential oil by low-pressure fractional distillation ① Raw material pretreatment: Wild melon latex and stems and leaves are selected as raw materials. The latex is filtered to remove impurities and then set aside. The stems and leaves are rinsed with clean water and drained at 20℃. ② Crushing: Crushing to 30 mesh; ③ Extraction: The stem and leaf powder is mixed with the latex and placed in the distillation tank of a special extraction device. Low-pressure fractional distillation is started, with an extraction pressure of 0.05 MPa, a first distillation temperature of 35℃ (extraction for 30 min, collecting the top notes), and a second distillation temperature of 45℃ (extraction for 90 min, collecting the middle notes and base notes). Water is used as the extraction medium during the extraction process. ④ Separation: After extraction, membrane separation (molecular weight cutoff 5000 Da) combined with oil-water separation is used to obtain the complex crude essential oil; ⑤ Purification: The compound crude essential oil was purified by gradient condensation and then aged at 5℃ for 10 days to obtain graded essential oils of top notes, middle notes, and base notes, as well as blended essential oils; ⑥ Aging: The graded essential oils and blended essential oils were aged separately at 8℃ in the dark for 10 days to obtain high-purity wild jujube latex + stem and leaf compound essential oil; The specialized extraction equipment used in this embodiment has an extraction unit that is a distillation tank, a temperature control unit that achieves segmented temperature control at 35°C and 45°C, a pressure control unit that controls the low pressure at 0.05MPa, and a condensation unit that is a staged condensation system that enables the segmented collection of head notes, body notes, and base notes.

[0014] Example 4: Extraction of essential oil from wild jujube root bark using subcritical extraction ① Raw material pretreatment: Wild melon root bark is selected as raw material, mud and sand are removed, and after rinsing with clean water, it is air-dried at a low temperature of 0℃; ② Crushing: Crushing to 20 mesh; ③ Extraction: Place the root bark powder in a subcritical extraction vessel of a specialized extraction device, use butane as the extractant, start subcritical extraction, set the extraction temperature to 30℃, the extraction pressure to 0.3MPa, and the extraction time to 2 hours; ④ Separation: After extraction, the crude root bark essential oil is obtained by desolventizing under reduced pressure at a separation temperature of 25℃; ⑤ Purification: The crude essential oil was purified by filtration through a 0.22μm micropore to remove impurities; ⑥ Aging: The purified essential oil is aged at 0℃ in the dark for 30 days to obtain high-purity wild melon root bark essential oil; The specialized extraction equipment used in this embodiment consists of a subcritical extraction vessel, a temperature control unit controlling the extraction temperature at 30°C, a pressure control unit controlling the pressurization at 0.3 MPa, and an essential oil storage unit storing the essential oil at 0°C.

Claims

1. A method for extracting natural essential oil from wild jujube, characterized in that, The process includes raw material pretreatment, crushing, extraction, separation, purification, and aging steps; the extraction is selected from any one or more combinations of steam distillation, atmospheric distillation, vacuum distillation, low-pressure distillation, fractional distillation, gradient distillation, ultrasonic-assisted extraction, microwave-assisted extraction, subcritical extraction, supercritical CO2 extraction, cold grinding extraction, adsorption desorption, fermentation extraction, enzymatic extraction, and maceration; the extraction temperature covers -20℃ to 120℃, and the extraction pressure covers vacuum negative pressure, atmospheric pressure, and pressurized pressure; the raw materials are selected from any one or more combinations of the fruit, stem, vine, leaf, root, bark, latex, and whole plant of wild yam.

2. The method according to claim 1, characterized in that, No organic solvents are added during the extraction process, or only water or edible ethanol is used as the extraction medium.

3. The method according to claim 1, characterized in that, The separation step can be any one of centrifugation, filtration, sedimentation, membrane separation, or oil-water separation.

4. The method according to claim 1, characterized in that, Purification includes any one of the following: molecular distillation, gradient condensation, fractional condensation, low-temperature aging, and microfiltration.

5. A special extraction device for wild gourd natural essential oil, implementing the method of any one of claims 1 to 4, characterized in that, It includes a crushing unit, an extraction unit, a temperature control unit, a pressure control unit, a condensation unit, an oil-water separation unit, a graded collection unit, and an essential oil storage unit; the extraction unit, condensation unit, and collection unit are connected in sequence, and the equipment is adaptable to any working condition such as normal pressure, low pressure, vacuum, ultrasound, microwave, adsorption, fermentation, and distillation.

6. The dedicated extraction device according to claim 5, characterized in that, The extraction unit can be any one of the following: distillation tank, ultrasonic extraction tank, microwave extraction chamber, subcritical extraction vessel, adsorption resin column, or fermentation tank.

7. The dedicated extraction equipment according to claim 5, characterized in that, The condensation unit is a gradient condensation or staged condensation system, which can achieve segmented collection of top notes, body notes and base notes.

8. The dedicated extraction equipment according to claim 5, characterized in that, The equipment's operating temperature can be controlled between -20℃ and 120℃, and its pressure can be controlled between vacuum negative pressure and 0.5MPa.