Process method for treating natural aromatic plant essential oil after separation and purification
The treatment of aromatic vegetable primary oil through combined processes such as heating, ultrasonic, centrifugation, vacuum suction filtration and molecular distillation has solved the problem of removing moisture and impurities in primary oil, and achieved the production of high-quality essential oils, ensuring that the aroma and purity comply with international standards.
Patent Information
- Application Number
- CN202411602378.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-11
- Publication Date
- 2024-12-27
AI Technical Summary
In the prior art, natural aromatic plant primary oil contains a large amount of water and impurities, which is difficult to meet the purity and aroma requirements. The existing treatment methods such as filter cloth filtration and separating funnel separation method cannot completely remove impurities and moisture, resulting in essential oil pollution and aroma. Downgrade.
Using heating and ultrasonic liquid separation treatment, centrifugal treatment, vacuum suction filtration treatment and molecular distillation purification treatment, combined with gas chromatography, moisture and impurities are removed through a staged and combined process to obtain high-quality light and heavy-component essential oils, and Alcoholization treatment ensures that the finished essential oil meets international standards.
Effectively remove moisture and impurities in aromatic plant primary oils, maintain the aroma and physical and chemical properties of essential oils, and obtain stable, odor-free, high-quality aromatic plant essential oils, suitable for large-scale processing.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of aromatic plant primary oil processing, and in particular relates to a process for separating, purifying and post-processing natural aromatic plant essential oil. Background Art
[0002] In the prior art, steam distillation is often used to produce natural aromatic plant crude oil. However, the obtained crude oil contains a large amount of water and impurities, which is difficult to meet actual needs.
[0003] To reduce the amount of water or impurities in the primary oil, conventional methods often employ cloth filtration and separatory funnel separation for subsequent essential oil processing. However, cloth filtration cannot completely filter out impurities from the essential oil, leaving them in the oil for extended periods, contaminating the oil and reducing its apparent cleanliness. Separation funnel separation can only remove most of the visible water, leaving a significant amount of water remaining in the oil, affecting the purity and aroma of the essential oil.
[0004] Based on this, it is extremely important to effectively remove moisture and impurities from aromatic plant primary oils without affecting the physical and chemical properties of the primary oils, such as color and aroma. Summary of the Invention
[0005] The purpose of the present invention is to provide a process for separating, purifying and post-processing natural aromatic plant essential oils for the first time, so as to at least effectively remove moisture and impurities from the primary aromatic plant oils without affecting the physical and chemical properties of the primary oils, such as color and aroma.
[0006] The purpose of the present invention is achieved through the following technical solutions:
[0007] A process for separating, purifying and post-processing natural aromatic plant essential oils comprises the following steps:
[0008] S1 selects aromatic plant primary oil;
[0009] S2 heating and ultrasonic separation treatment;
[0010] S3 centrifugation;
[0011] S4 vacuum filtration treatment;
[0012] S5 molecular distillation purification process to obtain light component essential oil and heavy component essential oil;
[0013] S6 blends the light component essential oil and the heavy component essential oil;
[0014] S7 alcohol treatment.
[0015] As some possible implementation methods of the present application, in step S2, the heating temperature is 45-50°C, the ultrasonic frequency is 40-50KHZ, and the processing time is 20-30min.
[0016] As some possible implementation methods of the present application, the water content of the aromatic plant primary oil after treatment in step S2 is ≤5%, and the impurity content is ≤2%.
[0017] As some possible implementation methods of the present application, the water content of the aromatic plant primary oil after treatment in step S3 is ≤1%, and the impurity content is ≤5‰.
[0018] As some feasible implementation methods of the present application, in step S3, a glass sand filter element is used in combination with a slow filter paper for filtration. During filtration, the vacuum pump pressure is 0.03-0.04 MPA, and the filtration flow rate is 100-150 ML / min.
[0019] As some feasible implementation methods of the present application, the aromatic plant primary oil after processing in step S3 has a water content of ≤1%, does not contain impurities, and has a pure color.
[0020] As some feasible implementation methods of the present application, in step S5, the material heating temperature of the molecular distillation equipment is 35°C-40°C, the vacuum degree is 5-10mbar, the feed rate is 100-150rpm / min, the scraper speed is 150-160rpm / min, the heating evaporation temperature is 55-60°C, the condensation temperature is 10-15°C, and liquid nitrogen is used for cold hydrazine condensation.
[0021] As some possible implementation methods of the present application, in step S6, a gas chromatograph is used to perform component analysis on the light component essential oil and the heavy component essential oil, and then, according to the currently valid international, national or industry standards, the light and heavy component essential oils are combined and blended in different proportions according to the component index requirements that the aromatic plant essential oil needs to meet, and mixed to obtain a finished aromatic plant essential oil that meets the component standards; the combination method calculation formula is: A finished product essential oil composition = A1*% (light component essential oil*percentage) + A2*% (heavy component essential oil*percentage).
[0022] As some possible implementation methods of the present application, when the aromatic plant is rose, the percentage of light component essential oil in step S6 is 80-90%, and the percentage of heavy component essential oil is 10-20%. According to this ratio, the quality of the obtained rose essential oil component can meet the Bulgarian production area standard of ISO9842:2003 international standard.
[0023] As some possible implementation methods of the present application, in step S1, the aromatic plant primary oil is selected from the aromatic plant primary oil extracted and produced by steam distillation; the steam distillation method is distillation in water, distillation above water or reduced pressure distillation.
[0024] Compared with the prior art, the present invention has the following beneficial effects:
[0025] 1. The aromatic plant primary oil is treated by ultrasonic separation, centrifugation and vacuum filtration to separate and remove water and impurities in the essential oil, thereby obtaining essential oil with low water content and no impurities; the aromatic plant essential oil is then separated and purified by molecular distillation to remove odor molecules and water molecules, thereby obtaining high-quality light component essential oil and heavy component essential oil with pure aroma and no water and impurities; finally, the light and heavy component essential oils are blended and combined in different proportions, and then alcoholized to obtain high-quality aromatic plant essential oil with qualified ingredients and stable quality.
[0026] 2. This process uses physical methods for processing and does not contain any chemical additives. On the one hand, it makes the finished essential oil safe and reliable, and on the other hand, it does not affect or destroy the aroma and component quality of the essential oil, restoring the original aroma of the plant.
[0027] 3. This process is suitable for the deep processing of various aromatic plant primary oils (crude oils). The whole process has low processing temperature and high processing efficiency, and can be applied to the large-scale processing of aromatic plant essential oils. DETAILED DESCRIPTION
[0028] Currently, the natural aromatic plant crude oil produced by steam distillation contains a large amount of water and impurities, which is difficult to meet actual needs. In the existing technology, filter cloth filtration and separatory funnel separation are often used for subsequent processing of essential oils. However, the filter cloth filtration method cannot completely filter out impurities in the essential oil, and the impurities remain in the essential oil for a long time, causing the essential oil to be contaminated and reducing the appearance of the essential oil. The separatory funnel separation method is used to separate and dehydrate the essential oil, but it can only separate and remove most of the water in the essential oil that is visible to the naked eye. A large amount of water still remains in the essential oil, which affects the purity and aroma of the aromatic plant essential oil.
[0029] Based on this, the present invention provides a process for separating, purifying and post-processing natural aromatic plant essential oils, comprising the following steps:
[0030] S1 selects aromatic plant primary oil;
[0031] S2 heating and ultrasonic separation treatment;
[0032] S3 centrifugation;
[0033] S4 vacuum filtration treatment;
[0034] S5 molecular distillation purification process to obtain light component essential oil and heavy component essential oil;
[0035] S6 blends the light component essential oil and the heavy component essential oil;
[0036] S7 alcohol treatment.
[0037] In the present invention, a staged combined process is adopted to treat the aromatic plant crude oil, specifically as follows:
[0038] In the first stage, the aromatic plant crude oil is heated and subjected to ultrasonic separation treatment to separate and remove more water and some impurities in the aromatic plant crude oil; in the second stage, centrifugation and vacuum filtration are used to filter and remove most of the water and remaining impurities in the aromatic plant crude oil; after the water and impurity removal treatment in the first and second stages, conditions are provided for the third stage (molecular distillation purification treatment) (because without the treatment processes for impurities and water in the first and second stages, the third stage is difficult to achieve smoothly), and in the third stage, the crude oil is further purified and deodorized to produce light and heavy component essential oils; finally, the light and heavy component essential oils are blended in different proportions according to the component results to obtain aromatic plant essential oil that is water-free, impurity-free, odorless, and has qualified component indicators.
[0039] The present invention processes the aromatic plant primary oil through a staged combined process, which can effectively remove moisture and impurities in the aromatic plant primary oil, and at the same time, can also obtain aromatic plant essential oil with stable aroma, no odor and meeting quality requirements.
[0040] In order to further improve the separation and purification effect of the aromatic plant crude oil, as some possible embodiments of the present application, the parameters in step S2 are further limited, that is, in step S2, the heating temperature is 45-50°C, the ultrasonic frequency is 40-50kHz, and the treatment time is 20-30min. Aromatic plant crude oils mostly contain alkane wax components, so it is necessary to heat to 45-50°C to fully dissolve the essential oil in liquid conditions to improve the separation effect of the essential oil and water. At the same time, this temperature range is relatively low and will not damage the aromatic components in the essential oil. According to the measured results, the ultrasonic frequency of 40-50kHz has the best separation effect on the essential oil.
[0041] To further enhance the separation and purification of the primary aromatic plant oil, as some possible implementations of this application, further limits are imposed on the water content and impurity content of the primary aromatic plant oil after treatment in step S2, namely, the water content and impurity content of the primary aromatic plant oil after treatment in step S2 are ≤ 5% and ≤ 2%. The treatment process in step S2 is a preliminary treatment involving ultrasonic and thermal separation, which only separates visible moisture and impurities. These limits ensure the effectiveness of step S3. Failure to do so would compromise the effectiveness of step S3.
[0042] In order to further improve the separation and purification effect of the aromatic plant crude oil, as some feasible embodiments of the present application, the water content and impurity content of the aromatic plant crude oil after step S3 treatment are further limited, that is, the water content of the aromatic plant crude oil after step S3 treatment is ≤1%, and the impurity content is ≤5‰. Simple centrifugation can only remove most of the water and impurities in the essential oil. The water and impurity content of the treated essential oil is directly related to the speed of the material feed flow rate. Therefore, by limiting the indicators of the treated crude oil, it is possible to ensure that the front-end processing requires an appropriate feed rate, and at the same time, it can ensure that the essential oil raw materials can meet the prerequisites for the back-end processing.
[0043] In order to further improve the separation and purification effect of the aromatic plant primary oil, as some embodiments of the present application, the parameters in step S3 are further limited, that is, in step S3, a glass sand filter element is used with a slow filter paper for filtration. During filtration, the vacuum pump pressure is 0.03-0.04MPA and the filtration flow rate is 100-150ML / min. The filtration quality of the vacuum-filtered essential oil is directly related to the vacuum pressure and filtration flow rate. High pressure and fast flow rate result in poor filtration quality. Low pressure and slow flow rate result in low filtration rate and large loss of aromatic components. Therefore, moderate parameters are required as key indicators for filtration.
[0044] To further improve the separation and purification of the virgin aromatic plant oil, as some possible embodiments of the present application, further limits are set on the water content and impurity content of the virgin aromatic plant oil after treatment in step S4. Specifically, the virgin aromatic plant oil after treatment in step S4 has a water content of ≤1%, is free of impurities, and has a pure color. Vacuum filtration can only filter out impurities in the essential oil, not the water content, so the impurity limit is set.
[0045] In order to further improve the separation and purification effect of aromatic plant primary oil, as some embodiments of the present application, the parameters in step S5 are further defined, that is, in step S5, the molecular distillation equipment material heating temperature is 35 ° C -40 ° C, the vacuum degree is 5-10mbar, the feed rate is 100-150rpm / min, the scraper speed is 150-160rpm / min, the heating evaporation temperature is 55-60 ° C, the condensation temperature is 10-15 ° C, and liquid nitrogen is used for cold hydrazine condensation. This parameter can separate the light and heavy components of the essential oil to the greatest extent, and collect the light component and the heavy component respectively. Using other parameters will cause the two components to be unable to be separated, affecting the back-end deployment.
[0046] In order to further improve the blending effect of the aromatic plant primary oil, as some embodiments of the present application, the specific steps in step S6 are further defined, that is, in step S6, a gas chromatograph is used to perform component analysis on the light component essential oil and the heavy component essential oil, and then, according to the component index requirements that the aromatic plant essential oil needs to meet, the light and heavy component essential oils are combined and blended in different proportions in accordance with the currently valid international, national or industry standards, and mixed to obtain an aromatic plant essential oil finished product that meets the component standards; wherein the combination method calculation formula is: A finished product essential oil composition = A1*% (light component essential oil* percentage) + A2*% (heavy component essential oil* percentage). Wherein, when the aromatic plant is rose, the light component essential oil percentage in step S6 is 80-90%, and the heavy component essential oil percentage is 10-20%. According to this proportion, the rose essential oil component quality obtained can reach the Bulgarian production area standard of the ISO9842:2003 international standard.
[0047] The separation and purification process of the natural aromatic plant essential oil described in this application will be further described in detail below in conjunction with specific embodiments.
[0048] Example 1
[0049] S1 selects the rose essential oil extracted by steam distillation (Damask rose flowers containing volatile components are co-distilled with pure water to distill the volatile components together with the water vapor. After condensation, the distillate enters a separator and is then separated from the oil and water to obtain rose essential oil).
[0050] In step S2, the raw rose essential oil is fed into a liquid separation device equipped with heating and ultrasonic functions. The liquid separation device is pear-shaped, larger at the top and smaller at the bottom. The heating temperature of the device is set at 50°C and the ultrasonic frequency is set at 45kHz. The raw rose essential oil is ultrasonically separated for 20 minutes. After the separation, the impurities and water separated from the raw rose essential oil are discharged from the bottom end, resulting in a pre-treated rose essential oil with a water content of ≤5% and an impurity content of ≤2%.
[0051] S3: feeding the rose essential oil after the liquid separation treatment into a tubular centrifuge, setting the centrifuge speed to 1950 r / min, and centrifuging the rose essential oil to obtain a rose essential oil with a water content of ≤1% and an impurity content of ≤5‰.
[0052] S4: Place the centrifuged rose essential oil into a vacuum filtration device, start the vacuum pump, control the vacuum pump pressure to 0.04 MPa, and the filtration flow rate to 100 ml / min. Use a glass sand filter element and slow filter paper to vacuum filter the rose essential oil to remove trace impurities. After treatment, the resulting rose essential oil has a water content of ≤1%, is free of impurities, and is pure in color.
[0053] S5 feeds the rose essential oil after vacuum filtration into a molecular distillation device for separation and purification, controls the material heating temperature of the molecular distillation device to be 40°C, the vacuum degree to be 8 mbar, the feed rate to be 100 rpm / min, the scraper speed to be 150 rpm / min, the heating evaporation temperature to be 60°C, the condensation temperature to be 10°C, and the molecular distillation process to be performed by cold hydrazine condensation using liquid nitrogen to avoid the loss of the aromatic aroma of the rose essential oil during the treatment process. After a certain treatment time, a rose light component essential oil and a rose heavy component essential oil that are free of water, impurities and odor are obtained.
[0054] S6 uses a gas chromatograph to analyze the components of the collected rose light component essential oil and rose heavy component essential oil to obtain the composition results of the two essential oils. According to the currently valid international, national or industry standards and the component index requirements that the aromatic plant essential oil needs to meet, the light and heavy components of the rose essential oil are combined and blended in different proportions to obtain a finished aromatic plant essential oil that meets the component standards. The combination method is calculated using the formula: A finished product essential oil composition = A1*% (light component essential oil* percentage) + A2*% (heavy component essential oil* percentage). In this embodiment, the composition is 83% light component essential oil and 17% heavy component essential oil.
[0055] S7 places the qualified rose essential oil in a cool, dry, dark refrigerator at 2-8°C for low-temperature alcoholization for 2 months. After alcoholization, a high-quality rose essential oil product with stable aroma and quality that meets the requirements is obtained.
[0056] Example 2
[0057] S1 is the same as Example 1.
[0058] In step S2, the virgin rose essential oil is fed into a liquid separation device equipped with heating and ultrasonic functions. The liquid separation device is pear-shaped, larger at the top and smaller at the bottom. The device is set to a heating temperature of 45°C and an ultrasonic frequency of 50 kHz. The virgin rose essential oil is ultrasonically separated for 28 minutes. Upon completion of the separation, the impurities and water separated from the virgin rose essential oil are discharged from the bottom end, resulting in a pre-treated rose essential oil with a water content of ≤5% and an impurity content of ≤2%.
[0059] S3: feeding the rose essential oil after the liquid separation treatment into a tubular centrifuge, setting the centrifuge speed to 2000 r / min, and centrifuging the rose essential oil to obtain a rose essential oil with a water content of ≤1% and an impurity content of ≤5‰.
[0060] S4: Place the centrifuged rose essential oil into a vacuum filtration device, start the vacuum pump, control the vacuum pump pressure to 0.035 MPa, and filter the flow rate to 150 ml / min. Use a glass sand filter element and slow filter paper to vacuum filter the rose essential oil to remove trace impurities. After treatment, the resulting rose essential oil has a water content of ≤1%, is free of impurities, and is pure in color.
[0061] S5 feeds the rose essential oil after vacuum filtration into a molecular distillation device for separation and purification, controls the material heating temperature of the molecular distillation device to be 35° C., the vacuum degree to be 10 mbar, the feed rate to be 150 rpm / min, the scraper speed to be 160 rpm / min, the heating evaporation temperature to be 55° C., the condensation temperature to be 13° C., and the molecular distillation process to be performed by cold hydrazine condensation using liquid nitrogen to avoid the loss of the aroma of the rose essential oil during the treatment process. After a certain treatment time, a rose light component essential oil and a rose heavy component essential oil that are free of water, impurities, and odor are obtained.
[0062] S6 is the same as in Example 1.
[0063] S7 is the same as in Example 1.
[0064] Comparative Example 1
[0065] The rose essential oil used in Example 1 was filtered through a 400-mesh filter cloth.
[0066] Comparative Example 2
[0067] The rose essential oil used in Example 1 was treated by a separating funnel separation method.
[0068] Experimental example
[0069] The quality (appearance, physicochemical properties, and essential oil components) of the rose essential oils treated in Examples 1-2 and Comparative Examples 1-2 were compared, and the results are shown in Tables 1 and 2. The adopted standard was the Bulgarian ISO 9842:2003 standard.
[0070] Table 1: Appearance and physical and chemical comparison
[0071]
[0072]
[0073] Table 2: Comparison of essential oil components.
[0074]
[0075] As shown in Table 2, after the rose essential oil prepared by the purification method of the present invention is subsequently treated, the aromatic components of the rose essential oil finally prepared can fully meet the ISO 9842:2003 Bulgarian standard, and the fragrance is purer.
Claims
1. A process for separating, purifying and post-processing natural aromatic plant essential oils, characterized in that: The steps include: S1 selects aromatic plant virgin oil; S2 heating and ultrasonic separation treatment; S3 centrifugation; S4 vacuum filtration treatment; S5 molecular distillation purification process to obtain light component essential oil and heavy component essential oil; S6 blends the light component essential oil and the heavy component essential oil; S7 alcohol treatment.
2. A process for separating and purifying natural aromatic plant essential oils after treatment according to claim 1, characterized in that: In step S2, the heating temperature is 45-50°C, the ultrasonic frequency is 40-50KHZ, and the processing time is 20-30min.
3. A process for separating and purifying natural aromatic plant essential oils after treatment according to claim 2, characterized in that: The water content of the aromatic plant primary oil after being processed in step S2 is ≤5%, and the impurity content is ≤2%.
4. A process for separating and purifying natural aromatic plant essential oil after treatment according to claim 1, characterized in that: The water content of the aromatic plant primary oil after being processed in step S3 is ≤1%, and the impurity content is ≤5‰.
5. A process for separating and purifying natural aromatic plant essential oil after treatment according to claim 1, characterized in that: In step S4, a glass sand filter element is used in combination with a slow filter paper for filtration. During filtration, the vacuum pump pressure is 0.03-0.04 MPa, and the filtration flow rate is 100-150 ML / min.
6. A process for separating and purifying natural aromatic plant essential oil after treatment according to claim 5, characterized in that: The aromatic plant primary oil treated in step S4 has a water content of ≤1%, contains no impurities, and has a pure color.
7. A process for separating and purifying natural aromatic plant essential oil after treatment according to claim 1, characterized in that: In step S5, the material heating temperature of the molecular distillation equipment is 35°C-40°C, the vacuum degree is 5-10mbar, the feed rate is 100-150rpm / min, the scraper speed is 150-160rpm / min, the heating evaporation temperature is 55-60°C, the condensation temperature is 10-15°C, and liquid nitrogen is used for cold hydrazine condensation.
8. A process for separating and purifying natural aromatic plant essential oil after treatment according to claim 1, characterized in that: In step S6, a gas chromatograph is used to perform component analysis on the light component essential oil and the heavy component essential oil, and then the light and heavy component essential oils are combined and blended in different proportions according to the component index requirements that the aromatic plant essential oil needs to meet, and the aromatic plant essential oil finished product that meets the component standards is obtained by mixing; wherein the matching method calculation formula is: A finished product essential oil composition = A1*% (light component essential oil* percentage) + A2*% (heavy component essential oil* percentage).
9. A process for separating, purifying and post-processing natural aromatic plant essential oil according to claim 8, characterized in that: When the aromatic plant is rose, the percentage of light component essential oil in step S6 is 80-90%, and the percentage of heavy component essential oil is 10-20%.
10. A process for separating, purifying and post-processing natural aromatic plant essential oil according to claim 1, characterized in that: In step S1, the aromatic plant primary oil is selected from the aromatic plant primary oil extracted by steam distillation; the steam distillation method is distillation in water, distillation on water or reduced pressure distillation.