Preparation method of rose essential oil and rose hydrolat

By picking and salt sealing the rose petals in the early morning, combining double-distilled water distillation technology and controlling the heating speed, the complex and time-consuming problem of the existing rose essential oil and rose dew extraction process is solved, and efficient and high-quality rose essential oil and rose dew preparation is achieved.

CN120349830APending Publication Date: 2025-07-22LINFEN VOCATIONAL & TECH COLLEGE
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Patent Information

Application Number
CN202510547407.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-28
Publication Date
2025-07-22

AI Technical Summary

Technical Problem

The existing extraction methods of rose essential oil and rose puree are complex and time-consuming, which is not conducive to industrial production, and are prone to volatilization of aromatic substances and loss of aroma during the preparation process, affecting product quality and yield.

Method used

Roses are picked in the early morning and salt sealing are carried out. Combined with the double-distilling water distillation technology, distillation and re-steaming are carried out by controlling the heating speed and pressure to separate rose essential oil and rose puree, and a simple oil-water separator is used for separation.

Benefits of technology

It effectively shortens the distillation time, reduces the volatility of aromatic substances, improves the yield and quality of rose essential oil and rose puree, and the prepared products have a strong fragrance and meets cosmetic grade standards.

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Abstract

The invention discloses a preparation method of rose essential oil and rose hydrolat, and belongs to the technical field of plant essential oil extraction. The preparation method comprises the following steps: S1, picking fresh roses from four o'clock to nine o'clock in the early morning, picking roses with half-cup-shaped flowers and yellow stamens, and enabling the picked roses to be complete and full and not extruded; s2, removing calyx and impurities from the fresh roses to obtain rose petals, and immediately performing salt sealing treatment on the rose petals; s3, performing distillation treatment on the rose petals subjected to salt sealing in the step S2 by utilizing double distilled water to obtain rose essential oil and rose hydrolat containing trace rose essential oil; and S4, re-distilling the rose hydrolat containing trace rose essential oil and the distillation residue to obtain the rose hydrolat. According to the preparation method of the rose essential oil and the rose hydrolat, the obtained rose essential oil is rich in fragrance, the proportion of main components is proper, the cosmetic grade standard is met, and the obtained rose hydrolat is clear, transparent, free of impurities, rich in nutritional ingredients and suitable for various skin care and beauty products.
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Description

Technical Field

[0001] The present invention relates to the field of plant essential oil extraction, and particularly to a method for preparing rose essential oil and rose hydrosol. Background Art

[0002] Rose essential oil and rose hydrosol are treasures in the fields of aromatherapy and beauty skin care. Rose essential oil is the essence extracted from rose petals and is known as "liquid gold". Its extraction process is extremely delicate and consumes a large amount of materials. Only about two pounds of rose oil can be extracted from about five tons of rose petals. Rose hydrosol is a by-product separated during the distillation of rose essential oil, containing trace amounts of essential oil and a large amount of water-soluble substances in plants, and has the characteristics of natural purity.

[0003] The history of rose essential oil can be traced back to ancient China. There were records of using roses as early as the Northern Song Dynasty. Rose essential oil has been regarded as a precious item by successive imperial courts due to its excellent aroma and skin care effects. Kazanlak "Rose Valley" in Bulgaria has become a world-famous origin of rose essential oil due to its unique natural conditions. The roses here are picked in the early morning from late May to mid-June every year to ensure that the aroma and active ingredients of the flowers reach the best state.

[0004] In the field of beauty skin care, rose essential oil and rose hydrosol are widely used. Due to its high-concentration aromatic components and rich nutrients, rose essential oil is often used in high-end skin care products and has effects such as moisturizing, anti-aging, and soothing the skin. Rose hydrosol, due to its mild characteristics, is suitable for various skin types, especially outstanding in moisturizing and purifying the skin. Rose hydrosol can not only be used as a toner, but also provide deep nourishment for the skin by applying it to the face, spraying, etc.

[0005] In addition, rose hydrosol also has drinking value. Long-term drinking can improve bad breath, regulate endocrine, relieve constipation and other problems, and has the effect of prolonging life. Its natural aroma and mild characteristics make it an ideal choice in daily skin care and health conditioning. Whether used for facial care or whole-body maintenance, rose essential oil and rose hydrosol can bring significant beauty and health effects.

[0006] A method for extracting rose essential oil and rose hydrosol (Application No.: 202011615795.9), comprising the following steps: (1) At 5-7 am, at a temperature of 5-23 °C and a relative air humidity of 55%-70%, pick roses that have bloomed to a semi-cup shape and have yellow stamens, and select plump and uncrushed rose petals; (2) Place the rose petals and water into a distillation kettle, first use indirect steam to heat the temperature in the distillation kettle to 70-80 °C, then introduce direct steam to heat to boiling, and the internal pressure of the distillation device is 0.07-0.09 MPa; (3) Pass the mixture of rose oil and rose hydrosol produced by distillation and the distillation residue into a condenser and an oil-water separator for condensation and oil-water separation to obtain rose essential oil and rose hydrosol; (4) Pass the obtained rose hydrosol into a rectifying column and heat and rectify it for 10-20 min under the action of the steam rising in the distillation kettle, and then through condensation and oil-water separation to obtain refined rose hydrosol. This patent directly distills the picked rose petals, with multiple re-distillations during the process, the process is complex and time-consuming, which is not conducive to industrial production. Summary of the Invention

[0007] The object of the present invention is to provide a method for preparing rose essential oil and rose hydrosol. By pre-treating freshly picked roses, the subsequent distillation steps are effectively streamlined, the distillation time is shortened, and the prepared rose essential oil and hydrosol have a strong fragrance and a high yield.

[0008] To achieve the above object, the present invention provides a method for preparing rose essential oil and rose hydrosol, comprising the following steps: S1. Pick fresh roses from 4 am to 9 am, pick roses that have bloomed to a semi-cup shape and have yellow stamens, and the picked rose flowers are complete, plump and not squeezed; S2. Immediately seal the rose petals obtained after removing the sepals and impurities from the fresh roses with salt; S3. Distill the rose petals treated with salt sealing in S2 using double-distilled water to obtain rose essential oil and rose hydrosol containing trace amounts of rose essential oil; S4. Re-distill the rose hydrosol containing trace amounts of rose essential oil and the distillation residue to obtain rose hydrosol.

[0009] Preferably, in S2, the salt sealing includes: S21. Place the rose petals in a clean and disinfected container, add NaCl particles accounting for 1% of the mass of the rose petals, and stir to evenly cover the rose petals with the NaCl particles; S22. After the stirring in S21 ends, let it stand for 10-20 min to allow the NaCl to fully penetrate.

[0010] Preferably, in S21, the particle size of the NaCl particles is 0.1 - 0.5 mm, the stirring speed is 30 r / min, and care should be taken to avoid damaging the rose petals during stirring.

[0011] Preferably, in S2, the environmental temperature during the salt sealing treatment is controlled at 20 - 25 °C.

[0012] Preferably, in S3, the double-distilled water distillation includes: S31: Put the rose petals after salt sealing treatment into the distillation kettle, and add double-distilled water to the distillation kettle according to the weight ratio of petals to double-distilled water of 1:4. S32: Start the distillation equipment, heat the double-distilled water to boiling in two stages, and keep the temperature at 100 °C for distillation for 1 - 2 h after boiling. The internal pressure of the distillation device during the distillation process is 0.07 MPa.

[0013] Preferably, in S32, heating the double-distilled water to boiling in two stages includes: controlling the heating rate at 1 °C / min - 2.5 °C / min, and after heating to 90 °C - 95 °C, heating the double-distilled water to boiling at a heating rate of 0.5 °C / min.

[0014] Preferably, after S3, separate the rose essential oil and rose hydrosol through an oil-water separator to obtain rose essential oil and rose hydrosol containing trace amounts of rose essential oil, and perform preservation treatment on the rose essential oil.

[0015] Preferably, in S4, the re-distillation includes: S41: Put the rose hydrosol containing trace amounts of rose essential oil and the distillation residue into the distillation kettle, and add double-distilled water twice the volume of the rose hydrosol containing trace amounts of rose essential oil. S42: Start the distillation equipment, heat the double-distilled water to boiling in two stages, and keep the temperature at 100 °C for distillation for 1 - 2 h after boiling. The internal pressure of the distillation device during the distillation process is 0.07 MPa.

[0016] Preferably, in S42, heating the double-distilled water to boiling in two stages includes: controlling the heating rate at 1 °C / min - 2.5 °C / min, and after heating to 90 °C - 95 °C, heating the double-distilled water to boiling at a heating rate of 0.5 °C / min.

[0017] The application of rose essential oil and rose hydrosol prepared by the preparation method as described above in the fields of cosmetics and skin care products.

[0018] Therefore, the preparation method of a kind of rose essential oil and rose hydrosol of the present invention has the following beneficial effects: (1) The freshly picked rose flowers picked from 4 am to 9 am are immediately processed to avoid the volatilization of effective aromatic substances, thereby reducing the essential oil extraction amount; (2) Stir with salt to seal the fragrance of the rose flowers, prevent the loss of aroma, and at the same time, salt can also reduce the solubility of rose essential oil in water, facilitate subsequent distillation extraction, and further shorten the time required for distillation extraction; (3) Adopt the traditional distillation extraction process, use double-distilled water as an auxiliary material, the steam after steam heating is cooled and condensed to form distilled water, which enters the oil-water separator. At low temperature, the essential oil floats on the upper layer and the rose hydrosol is on the lower layer, so that the rose hydrosol and rose essential oil can be separated. The cost of the auxiliary material is low, the separation method is simple, and it is easy to promote the process; (4) Perform re-distillation treatment on the rose hydrosol and distillation residues containing trace amounts of rose essential oil to further improve the quality of the rose hydrosol; (5) No flavoring agents, moisturizers, preservatives, etc. are added during the extraction process, and the prepared rose essential oil and rose hydrosol are natural, high-quality, pure, and efficient.

[0019] The technical solution of the present invention will be further described in detail below with reference to the drawings and examples. Description of the Drawings

[0020] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments of the present invention will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0021] Figure 1 It is a schematic diagram of the preparation process of the rose essential oil and hydrosol of the present invention. Specific Embodiments

[0022] The technical solution of the present invention will be further described below with reference to the drawings and examples.

[0023] In order to make the purpose, technical solution and advantages of the present application clearer, more thorough and complete, the technical solution of the present invention will be clearly and completely described below with reference to the drawings and examples. The following detailed descriptions are all descriptions of embodiments, aiming to provide further detailed descriptions of the present invention. Unless otherwise specified, all technical terms used in the present invention have the same meaning as commonly understood by those of ordinary skill in the art to which this application belongs.

[0024] The instruments, equipment, reagents and materials used in the examples or comparative examples are all obtained through commercial channels. The roses used in the examples or comparative examples are all centifolia roses from the same rose garden, and there are no significant differences in the roses among the various examples or comparative examples.

[0025] Example 1 A method for preparing rose essential oil and rose hydrosol, the process is asFigure 1 As shown in the figure, it specifically includes the following steps: S1. Collection: Pick fresh roses from 4 am to 9 am. Pick roses that are half-cup shaped and have yellow stamens, ensuring that the picked rose flowers are complete, plump, and not squeezed.

[0026] S2. Petal pretreatment: Transport the picked fresh roses to the pretreatment area, remove the sepals and impurities of the fresh roses, put the rose petals into a clean and disinfected container, add NaCl particles accounting for 1% of the mass of the rose petals, stir for 10 minutes to seal the fragrance of the roses and prevent the loss of aroma. At the same time, NaCl can also reduce the solubility of rose essential oil in water, facilitating subsequent distillation extraction.

[0027] The time from rose picking to the start of pretreatment should not exceed 2 hours to avoid the volatilization of effective aromatic substances and reduce the essential oil extraction amount.

[0028] NaCl is a common commercially available product. Ensure that the NaCl particles are evenly covered on the rose petals during stirring. The stirring speed is 30 r / min, and the stirring speed is appropriate. Avoid being too fast, which may cause petal damage, and too slow, which may not achieve uniform mixing. After stirring, let the mixed petals stand for 10 minutes to allow the salt to fully penetrate.

[0029] The environmental temperature during pretreatment is controlled at 20 - 25 °C to avoid the influence of too high or too low temperature on the dissolution of NaCl and the aroma of the petals.

[0030] S3. Distillation extraction: Put the pretreated rose petals into the distillation kettle, ensuring that the equipment is clean and free of impurities. Add double-distilled water to the distillation kettle according to the weight ratio of petals to double-distilled water of 1:4. Start the distillation equipment and heat the double-distilled water in the distillation kettle to gradually increase its temperature to the boiling point. Control the heating rate at 2 °C / min during the heating process. After heating to 90 - 95 °C, increase the temperature at a heating rate of 0.5 °C / min until boiling. Keep the temperature at 100 °C after the liquid boils and continue distillation for 2 hours. Keep the internal pressure of the distillation device at 0.07 MPa during the distillation process.

[0031] When the steam passes through the rose petals, it will carry the essential oil and aromatic components in the petals to form steam containing essential oil. The steam is cooled by the condenser tube and transformed into a liquid mixture. Since the density of rose essential oil is less than that of water, an oil film will form on the liquid surface, and the lower layer is rose hydrosol containing trace amounts of essential oil.

[0032] S4. Separation: Separate the upper-layer rose essential oil and the lower-layer rose hydrosol through an oil-water separator to obtain rose essential oil and rose hydrosol containing trace amounts of rose essential oil respectively. Store the rose essential oil in a dark glass bottle.

[0033] S5. Re-steaming: Put the rose hydrosol containing trace rose essential oil and the distillation residue back into the distillation kettle, add double-distilled water twice the volume of the rose hydrosol containing trace rose essential oil, and conduct re-steaming. The re-steaming conditions are the same as those in step S3. After re-steaming, separate the rose essential oil and rose hydrosol through an oil-water separator. Merge the rose essential oil into a dark glass bottle, and store the rose hydrosol in a clean glass bottle.

[0034] Example 2 A preparation method of rose essential oil and rose hydrosol specifically includes the following steps: S1. Collection: Pick fresh roses from 4 am to 9 am. Pick roses that are in a semi-cup shape and have yellow stamens, ensuring that the flowers are intact without damage.

[0035] S2. Petal pretreatment: Transport the picked fresh roses to the pretreatment area, remove the sepals and impurities of the fresh roses, put the rose petals into a clean container after disinfection, add NaCl particles accounting for 1% of the mass of the rose petals, stir for 10 minutes to seal the fragrance of the roses and prevent the loss of aroma. At the same time, NaCl can also reduce the solubility of rose essential oil in water, facilitating subsequent distillation extraction.

[0036] NaCl is a common commercially available product. Ensure that the NaCl particles are evenly covered on the rose petals during stirring. The stirring speed is 30 r / min, and the stirring speed is appropriate. Avoid being too fast, which may cause damage to the petals, and too slow, which may not result in uniform mixing. After stirring, let the mixed petals stand for 10 minutes to allow the salt to fully penetrate.

[0037] The environmental temperature during pretreatment should be controlled at 20-25°C to avoid the influence of too high or too low temperature on the dissolution of NaCl and the aroma of the petals.

[0038] S3. Distillation extraction: Put the rose petals after salt stirring treatment into the distillation kettle, ensuring that the equipment is clean without impurities. According to the weight ratio of petals to double-distilled water of 1:4, add double-distilled water to the distillation kettle. Start the distillation equipment and heat the double-distilled water in the distillation kettle to gradually increase its temperature to the boiling point. Control the heating rate at 1°C / min during the heating process. After heating to 90-95°C, increase the temperature at a heating rate of 0.5°C / min until boiling. Keep the temperature at 100°C after the liquid boils and continue distillation for 2 h. Keep the internal pressure of the distillation device at 0.07 MPa during the distillation process.

[0039] When the steam passes through the rose petals, it will carry the essential oil and aromatic components in the petals to form steam containing essential oil. The steam is cooled by the condenser and converted into a liquid mixture. Since the density of rose essential oil is less than that of water, an oil film will form on the liquid surface, and the lower layer is rose hydrosol containing trace essential oil.

[0040] S4. Separation: Separate the upper-layer rose essential oil and the lower-layer rose hydrosol through an oil-water separator to obtain rose essential oil and rose hydrosol containing trace amounts of rose essential oil respectively. Store the rose essential oil in a dark glass bottle.

[0041] S5. Re-distillation: Put the rose hydrosol containing trace amounts of rose essential oil and the distillation residue back into the distillation kettle, add double-distilled water twice the volume of the rose hydrosol containing trace amounts of rose essential oil, and conduct re-distillation. The re-distillation conditions are the same as those in step S3. After re-distillation, separate the rose essential oil and rose hydrosol through an oil-water separator, merge the rose essential oil into a dark glass bottle, and store the rose hydrosol in a clean glass bottle.

[0042] Comparative Example 1 A method for preparing rose essential oil and rose hydrosol specifically includes the following steps: S1. Collection: Pick fresh roses from 4 am to 9 am, pick roses with the flowers blooming to a semi-cup shape and the stamens being yellow, and ensure that the flowers are intact without damage.

[0043] S2. Petal pretreatment: Transport the picked fresh roses to the pretreatment area, remove the sepals and impurities of the fresh roses, put the rose petals into a clean container after disinfection, add NaCl particles accounting for 1% of the mass of the rose petals, stir for 10 minutes to seal the fragrance of the roses and prevent the loss of aroma. At the same time, NaCl can also reduce the solubility of rose essential oil in water, facilitating subsequent distillation extraction.

[0044] The time from rose picking to the start of pretreatment does not exceed 2 hours to avoid the volatilization of effective aromatic substances and reduce the essential oil extraction amount.

[0045] NaCl is a common commercially available product. Ensure that the NaCl particles evenly cover the rose petals during stirring. The stirring speed is 30 r / min, and the stirring speed is moderate. Avoid being too fast, which may cause damage to the petals, and too slow, which may not achieve uniform mixing. After stirring, let the mixed petals stand for 10 minutes to allow the salt to fully penetrate.

[0046] The environmental temperature during pretreatment should be controlled at 20 - 25 °C to avoid the influence of too high or too low temperature on the dissolution of NaCl and the aroma of the petals.

[0047] S3. Distillation extraction: Put the pretreated rose petals into the distillation kettle, ensuring that the equipment is clean without impurities. According to the weight ratio of petals to double-distilled water of 1:4, add double-distilled water to the distillation kettle. Start the distillation equipment, heat the water in the distillation kettle to gradually increase the temperature to the boiling point. During the heating-up process, control the heating-up speed at 2 °C / min, and after heating up to 90 - 95 °C, increase the temperature to boiling at a heating-up speed of 0.5 °C / min. After the liquid boils, keep the temperature at 100 °C and continue distillation for 2 h. During the distillation process, keep the internal pressure of the distillation device at 0.07 MPa.

[0048] When steam passes through rose petals, it will carry the essential oil and aromatic components in the petals, forming steam containing essential oil. The steam is cooled by a condenser tube and transformed into a liquid mixture. Since the density of rose essential oil is less than that of water, an oil film will form on the liquid surface, and the lower layer is rose hydrosol containing trace amounts of essential oil.

[0049] S4. Separation: Separate the upper-layer rose essential oil and the lower-layer rose hydrosol through an oil-water separator to obtain rose essential oil and rose hydrosol respectively. Store the rose essential oil in a dark glass bottle and the rose hydrosol in a clean glass bottle.

[0050] Comparative Example 2 A preparation method of rose essential oil and rose hydrosol specifically includes the following steps: S1. Collection: Pick fresh roses from 4 am to 9 am. Pick roses that have bloomed to a semi-cup shape and have yellow stamens, ensuring that the flowers are intact without damage.

[0051] S2. Petal pretreatment: Transport the picked fresh roses to the pretreatment area, remove the sepals and impurities of the fresh roses to obtain rose petals.

[0052] S3. Distillation extraction: Put the pretreated rose petals into a distillation kettle, ensuring that the equipment is clean without impurities. According to the weight ratio of petals to double-distilled water of 1:4, add double-distilled water to the distillation kettle. Start the distillation equipment and heat the water in the distillation kettle to gradually increase its temperature to the boiling point. Control the heating rate at 2 °C / min during the heating process, and after heating to 90 - 95 °C, increase the temperature at a heating rate of 0.5 °C / min until boiling. Keep the temperature at 100 °C after the liquid boils and continue distilling for 2 h. Keep the internal pressure of the distillation device at 0.07 MPa during the distillation process.

[0053] When steam passes through rose petals, it will carry the essential oil and aromatic components in the petals, forming steam containing essential oil. The steam is cooled by a condenser tube and transformed into a liquid mixture. Since the density of rose essential oil is less than that of water, an oil film will form on the liquid surface, and the lower layer is rose hydrosol containing trace amounts of essential oil.

[0054] S4. Separation: Separate the upper-layer rose essential oil and the lower-layer rose hydrosol through an oil-water separator to obtain a mixture of rose essential oil and rose hydrosol. Store the rose essential oil in a dark glass bottle.

[0055] S5. Re-steaming: Put the mixture of rose hydrosol and rose essential oil and the distillation residue back into the distillation kettle again, add double-distilled water twice the volume of the mixture of rose hydrosol and rose essential oil, and conduct re-steaming. The re-steaming conditions are the same as those in step S3. After re-steaming, separate the rose essential oil and rose hydrosol through an oil-water separator. Combine the rose essential oil into a dark glass bottle, and store the rose hydrosol in a clean glass bottle.

[0056] Comparative Example 3 A method for preparing rose essential oil and rose hydrosol, specifically including the following steps: S1. Collection: Pick fresh roses from 4 am to 9 am. Pick roses that have bloomed to a semi-cup shape and have yellow stamens, ensuring that the flowers are intact without damage.

[0057] S2. Petal pretreatment: Transport the picked fresh roses to the pretreatment area, and remove the sepals and impurities of the fresh roses. The time from picking the roses to starting the pretreatment does not exceed 2 hours to avoid the volatilization of effective aromatic substances and reduce the essential oil extraction amount.

[0058] S3. Distillation extraction: Put the pretreated rose petals into the distillation kettle, ensuring that the equipment is clean without impurities. According to the weight ratio of petals to double-distilled water of 1:4, add double-distilled water to the distillation kettle. Start the distillation equipment and heat the water in the distillation kettle to gradually raise the temperature to the boiling point. Control the heating rate at 2.5 °C / min during the heating process. After raising the temperature to 90 - 95 °C, raise the temperature to boiling at a heating rate of 0.5 °C / min. Keep the temperature at 100 °C after the liquid boils and continue distilling for 2 hours. Keep the internal pressure of the distillation device at 0.07 MPa during the distillation process.

[0059] When the steam passes through the rose petals, it will carry the essential oil and aromatic components in the petals to form steam containing essential oil. The steam is cooled by the condenser tube and converted into a liquid mixture. Since the density of rose essential oil is less than that of water, an oil film will form on the liquid surface, and the lower layer is rose hydrosol containing a trace amount of essential oil.

[0060] S4. Separation: Separate the upper-layer rose essential oil and the lower-layer rose hydrosol through an oil-water separator to obtain rose essential oil and rose hydrosol containing a trace amount of essential oil respectively. Store the rose essential oil in a dark glass bottle.

[0061] S5. Re-steaming: Put the rose hydrosol containing a trace amount of essential oil and the distillation residue back into the distillation kettle again, add double-distilled water twice the volume of the rose hydrosol containing a trace amount of essential oil, and conduct re-steaming. The re-steaming conditions are the same as those in step S3. After re-steaming, separate the rose essential oil and rose hydrosol through an oil-water separator. Combine the rose essential oil into a dark glass bottle, and store the rose hydrosol in a clean glass bottle.

[0062] Comparative Example 4 A method for preparing rose essential oil and rose hydrosol, specifically including the following steps: S1. Collection: Fresh roses are picked from 4 am to 9 am. Pick roses that are in a semi-cup shape with yellow stamens, ensuring the flowers are intact without damage.

[0063] S2. Petal pretreatment: The picked fresh roses are transported to the pretreatment area, and the sepals and impurities of the fresh roses are removed. The time from rose picking to the start of pretreatment does not exceed 2 hours to avoid the volatilization of effective aromatic substances and reduce the essential oil extraction amount.

[0064] S3. Distillation extraction: The rose petals are put into a distillation kettle to ensure the equipment is clean without impurities. According to the weight ratio of petals to double-distilled water of 1:4, double-distilled water is added to the distillation kettle. Start the distillation equipment and heat the water in the distillation kettle to gradually increase the temperature to the boiling point. During the heating process, control the heating rate at 3°C / min. After heating to 90 - 95°C, increase the temperature at a heating rate of 0.5°C / min until boiling. After the liquid boils, keep the temperature at 100°C and continue distillation for 2 hours. During the distillation process, keep the internal pressure of the distillation device at 0.07 MPa.

[0065] When the steam passes through the rose petals, it will carry the essential oil and aromatic components in the petals to form steam containing essential oil. The steam is cooled by a condenser and transformed into a liquid mixture. Since the density of rose essential oil is less than that of water, an oil film will form on the liquid surface, and the lower layer is rose hydrosol containing trace amounts of essential oil.

[0066] S4. Separation: The upper-layer rose essential oil and the lower-layer rose hydrosol are separated through an oil-water separator to obtain rose essential oil and rose hydrosol containing trace amounts of essential oil respectively. The rose essential oil is stored in a dark glass bottle.

[0067] S5. Re-distillation: The rose hydrosol containing trace amounts of essential oil and the distillation residue are put into the distillation kettle again, and double-distilled water twice the volume of the rose hydrosol containing trace amounts of essential oil is added for re-distillation. The re-distillation conditions are the same as those in step S3. After re-distillation, the rose essential oil and rose hydrosol are separated through an oil-water separator. The rose essential oil is combined and stored in a dark glass bottle, and the rose hydrosol is filled into a clean glass bottle for storage.

[0068] Test Example 1 (1) Physical property detection of the rose hydrosol and rose essential oil prepared in Example 1: The colors of both the rose essential oil and the rose hydrosol are light yellow; the rose essential oil has a strong rose aroma, and the aroma of the rose hydrosol is relatively light.

[0069] (2)Chemical composition analysis of the rose hydrosol and rose essential oil prepared in Example 1: The gas chromatography-mass spectrometry (GC-MS) analysis results of the rose essential oil showed that the main component contents were within the standard range, and the proportions of components such as citronellol, geraniol, and phenethyl alcohol were appropriate. The HPLC analysis results of the rose hydrosol showed that the main component contents accounted for 96% of the total amount, the proportions of components such as citronellol, geraniol, and phenethyl alcohol were appropriate, arsenic (mg / L, calculated as As) ≤ 0.8, lead (mg / L, calculated as Pb) ≤ 2, and mercury (mg / L, calculated as Hg) < 0.8.

[0070] (3)Escherichia coli or Staphylococcus aureus was not detected in the rose hydrosol and rose essential oil prepared in Example 1, meeting the cosmetic-grade standard.

[0071] (4)Yield analysis: The yields of the rose essential oil and rose hydrosol in Example 1, Example 2, Comparative Example 1 to Comparative Example 4 were tested, and the results are shown in Table 1 below: Table 1

[0072] Comparing Example 1 with Example 2, it can be seen that by reducing the heating rate in the first stage of heating during distillation and double distillation, the yield of rose essential oil can be increased, and there is almost no impact on the yield of rose hydrosol. Comparing Example 1 with Comparative Example 1, it can be seen that double distillation can effectively increase the yield of rose hydrosol. Comparing Example 1 with Comparative Example 2, it can be seen that salt sealing can make the extraction of rose essential oil and rose hydrosol more complete and effectively increase the yields of rose essential oil and rose hydrosol. Comparing Example 1, Example 2 with Comparative Example 3, Comparative Example 4, it can be seen that when the heating rate in the first stage of heating during distillation and double distillation is increased between 1 - 2.5 °C / min, the yields of rose essential oil and rose hydrosol are relatively high. Exceeding 2.5 °C / min will reduce the yields of rose essential oil and rose hydrosol. This may be because the salt increases the osmotic pressure of the rose flower cells, causing cell rupture, thereby improving the extraction efficiency of rose hydrosol and rose essential oil. However, this also makes the rose petals more sensitive to temperature, and rapid heating may cause some rose essential oil to deteriorate or decompose.

[0073] Therefore, in the preparation method of a rose essential oil and rose hydrosol of the present invention, the freshly picked rose flowers are sealed with salt to lock in the fragrance, reduce the dissipation of the rose flower fragrance, and can improve the efficiency of extracting rose essential oil and rose hydrosol during subsequent distillation, shortening the time of distillation and double distillation; the obtained rose essential oil has a strong fragrance, the proportion of main components is appropriate, and it meets the cosmetic-grade standard. The obtained rose hydrosol is clear and transparent, free of impurities, and contains rich nutritional components, and is suitable for various skin care and beauty products.

[0074] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit them. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions of the present invention or make equivalent replacements, and these modifications or equivalent replacements cannot make the modified technical solutions deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A preparation method of rose essential oil and rose hydrosol, characterized in that, It includes the following steps: S1. Pick fresh roses from 4 am to 9 am. Pick the roses when the flowers bloom to a semi-cup shape and the stamens are yellow. The picked rose flowers are complete, plump, and not squeezed. S2. Immediately perform salt sealing on the rose petals obtained by removing the sepals and impurities from the fresh roses. S3. Distill the rose petals after salt sealing in S2 with double-distilled water to obtain rose essential oil and rose hydrosol containing trace amounts of rose essential oil. S4. Re-distill the rose hydrosol containing trace amounts of rose essential oil and the distillation residue to obtain rose hydrosol.

2. The preparation method of a kind of rose essential oil and rose hydrosol according to claim 1, wherein, In S2, the salt sealing includes: S21. Place the rose petals in a clean and disinfected container, add NaCl particles accounting for 1% of the mass of the rose petals, and stir to evenly cover the rose petals with the NaCl particles. S22. After the stirring in S21 ends, let it stand for 10 - 20 min to allow the NaCl to fully penetrate.

3. The preparation method of a rose essential oil and rose hydrosol according to claim 2, characterized in that: In S21, the particle size of the NaCl particles is 0.1 - 0.5 mm, the stirring speed is 30 r / min, and avoid damaging the rose petals during stirring.

4. The preparation method of a kind of rose essential oil and rose hydrosol according to claim 1, characterized in that: In S2, the environmental temperature during salt sealing treatment is controlled at 20 - 25 °C.

5. A method for preparing rose essential oil and rose hydrosol according to claim 1, characterized in that: In S3, distillation with double-distilled water includes: S31. Put the rose petals after salt sealing into the distillation kettle, and add double-distilled water to the distillation kettle according to the weight ratio of petals to double-distilled water of 1:

4. S32. Start the distillation equipment, heat the double-distilled water in two stages to boiling, and keep the temperature at 100 °C for distillation for 1 - 2 h after boiling. The internal pressure of the distillation device during the distillation process is 0.07 MPa.

6. The preparation method of a kind of rose essential oil and rose hydrosol according to claim 5, characterized in that, In S32, heating the double-distilled water in two stages to boiling includes: controlling the heating rate at 1 °C / min - 2.5 °C / min, and after heating to 90 °C - 95 °C, heating the double-distilled water to boiling at a heating rate of 0.5 °C / min.

7. The preparation method of a kind of rose essential oil and rose hydrosol according to claim 1, characterized in that: In S3, after distillation ends, separate the rose essential oil and rose hydrosol through an oil-water separator to obtain rose essential oil and rose hydrosol containing trace amounts of rose essential oil, and perform preservation treatment on the rose essential oil.

8. The preparation method of a kind of rose essential oil and rose hydrosol according to claim 1, characterized in that, In S4, the re-distillation includes: S41. Put the rose hydrosol containing trace amounts of rose essential oil and the distillation residue into the distillation kettle, and add double-distilled water twice the volume of the rose hydrosol containing trace amounts of rose essential oil. S42. Start the distillation equipment, heat the double-distilled water in two stages to boiling, and keep the temperature at 100 °C for distillation for 1 - 2 h after boiling. The internal pressure of the distillation device during the distillation process is 0.07 MPa.

9. A method for preparing rose essential oil and rose hydrosol according to claim 8, characterized in that: In S42, heating the double-distilled water in two stages to boiling includes: controlling the heating rate at 1 °C / min - 2.5 °C / min, and after heating to 90 °C - 95 °C, heating the double-distilled water to boiling at a heating rate of 0.5 °C / min.

10. Application of the rose essential oil and rose hydrosol prepared by the preparation method according to any one of claims 1 - 9 in the fields of cosmetics and skin care products.

Citation Information

Patent Citations

  • Extraction method of rose essential oil and rose hydrolat

    CN112662477A