CN115181607A - Production process for preparing pinecone essential oil by distillation method - Google Patents
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a production process for preparing pinecone essential oil by a distillation method, and relates to the technical field of pinecone essential oil; in order to ensure the efficacy of the product and facilitate the production; the method specifically comprises the following steps: taking out pine nuts of the pinecones to obtain pinecone peels; cleaning and airing the pinecone peels; slicing the pinecone peel, and secondarily airing to obtain dried peel slices; distilling the dried peel slices after secondary airing by a steam distillation method, wherein the distillation pressure is controlled to be 0.05-0.25 MPa, and the distillation time is 90-180 min; performing extractive fractionation to obtain the final product; wherein, the pinecone is the pinecone of Korean pine in lesser Khingan mountains. According to the invention, the pinecone peel, the loquat leaves and other components are added, and distillation extraction is carried out after slicing treatment, so that the effects of relieving cough and asthma and eliminating phlegm of the pinecone essential oil are effectively ensured, and the product quality is ensured.
Description
Technical Field
The invention relates to the technical field of pinecone essential oil, in particular to a production process for preparing pinecone essential oil by a distillation method.
Background
Pinecone is a fruit bearing on trees, and is named as pinecone because of being like pagoda; the appearance of the pine nut is dark brown, and a plurality of layers of scales are arranged, and pine nuts are clamped among the scales; the scale of the mountain pine is thin and dense, the rosin taste is strong, the scale of the pine cone of the subtropical pine is thick and is relatively loose, the rosin taste is not obvious, and the top of the scale of the fresh pine cone has small thorns; the pinecone has good effects of eliminating phlegm, relieving cough and relieving asthma; therefore, the product is processed into a product with a certain conditioning function, and can meet the requirements of partial markets.
Through search, a Chinese patent with the application number of CN202110750574.0 discloses a plant essential oil composition for benefiting lung and relieving cough and a preparation method and application thereof, the plant essential oil composition for benefiting lung and relieving cough utilizes a traditional Chinese medicine compatibility mode, adopts the formula principle of monarch, minister, triallen, quinquel and quinquel, selects lily essential oil as monarch, pinellia ternate essential oil and cardamon essential oil as minister, dried orange peel essential oil, costus root essential oil and nutgrass galingale rhizome essential oil as assistant, and matches tangerine leaf essential oil, magnolia obavata essential oil, bergamot essential oil, perilla seed essential oil and turmeric root-tuber essential oil as guide to prepare the plant essential oil composition for benefiting lung and relieving cough. The plant essential oil composition in the above patent has the following disadvantages: the formula has more components, more complex process, difficult production and processing and relatively higher cost.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a production process for preparing pinecone essential oil by a distillation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process for preparing pinecone essential oil by a distillation method comprises the following steps:
the method comprises the following steps:
s1: cleaning and airing the pinecone peel;
s2: slicing pinecone peel;
s3: drying in the sun for the second time to obtain dried peel slices;
s4: distilling the dried peel slices after secondary airing by a steam distillation method/pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.1-0.25 MPa, and the distillation time is 90-180 min;
s5: the water vapor is cooled to water with a water exchange condenser,
s6: and (5) taking oil by using an oil-water separator to obtain the oil.
Preferably: the pinecone is Korean pinecone from Xiaoxingan, and in step S3, the length, width and size of the slices are controlled to be 2mm-10 mm.
And further: the components are calculated by weight parts and replaced by the following components: 50-80 parts of pinecone peel, 12-18 parts of loquat leaf, 10-15 parts of white mulberry root-bark, 8-12 parts of tuckahoe and 5-8 parts of rhizoma polygonati.
Further preferred is: the production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried peel slices;
s4: drying in the sun for the second time to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a steam distillation method/pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.1-0.25 MPa, and the distillation time is 90-180 min;
s6: and (4) carrying out extraction and fractionation to obtain the product.
As a preferable aspect of the present invention: in the step S6, the extraction method adopts carbon dioxide supercritical extraction, the extraction pressure of the carbon dioxide supercritical extraction is 24-38 MPa, the extraction temperature is 48-58 ℃, the carbon dioxide flow is 18-36L/h, and the extraction time is 150-240 min.
Further preferred according to the invention are: the components of the paint comprise the following components in parts by weight: 65 parts of pinecone peel, 15 parts of loquat leaf, 12 parts of white mulberry root-bark, 10 parts of poria cocos and 6 parts of rhizoma polygonati.
As a still further scheme of the invention: the production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried pericarp slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.15MPa, and the distillation time is 150min;
s6: and (4) carrying out extraction and fractionation to obtain the product.
On the basis of the scheme: in the step S6, the carbon dioxide supercritical extraction is adopted as the extraction method, the extraction pressure of the carbon dioxide supercritical extraction is 32MPa, the extraction temperature is 52 ℃, the carbon dioxide flow is 28L/h, and the extraction time is 210min.
On the basis of the foregoing scheme, it is preferable that: in the step S3, the length, width and size of the slices and the blocks are controlled to be 6mm, 6mm.
It is further preferred on the basis of the foregoing scheme that: the production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried pericarp slices;
s4: drying in the sun for the second time to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.15MPa, and the distillation time is 150min;
s6: cooling the water vapor to water with a water exchange condenser;
s7: and (5) taking oil by using an oil-water separator to obtain the oil.
The beneficial effects of the invention are as follows:
1. according to the invention, the components such as the pinecone peel and the loquat leaf are added, and distillation extraction is carried out after slicing treatment, so that the effects of relieving cough and asthma, eliminating phlegm and the like of the pinecone essential oil are effectively ensured, and the product quality is ensured.
2. The invention has the effects of purging the lung, relieving asthma, inducing diuresis, reducing edema, tonifying spleen and calming the heart by adding the components of the white mulberry root-bark, the tuckahoe and the like; can effectively regulate the problems of lung heat cough and asthma, oliguria and edema and the like.
3. The sealwort and other components are added, so that the lung-nourishing health-care tea has the effects of tonifying the lung, promoting the production of body fluid and moistening dryness, has a good tonifying effect on the lung, spleen and kidney, and is matched with the rest components, so that the product effect is further improved.
Drawings
FIG. 1 is a comparative diagram showing the evaluation of products prepared by different schemes in the process for preparing pinecone essential oil by distillation according to the invention;
FIG. 2 is a diagram showing the relationship between the slice size and the product comprehensive efficacy of the process for preparing pinecone essential oil by distillation.
Detailed Description
The technical solution of the present patent will be further described in detail with reference to the following embodiments.
Example 1:
a production process for preparing pinecone essential oil by a distillation method comprises the following steps:
s1: cleaning pine cone peel and airing;
s2: slicing pinecone peel;
s3: drying in the sun for the second time to obtain dried peel slices;
s4: distilling the dried peel slices after secondary airing by a steam distillation method/pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.1-0.25 MPa, and the distillation time is 90-180 min;
s5: the water vapor is cooled to water with a water exchange condenser,
s6: and (5) taking oil by using an oil-water separator to obtain the oil.
Wherein, the pinecone is Pinus koraiensis of Xiaoxingan, and in the step S3, the length, width and size of the slices are controlled to be 2mm, 2mm-10mm, 10mm.
Example 2:
a production process for preparing pinecone essential oil by a distillation method comprises the following components in parts by weight: 50-80 parts of pinecone peel, 12-18 parts of loquat leaf, 10-15 parts of white mulberry root-bark, 8-12 parts of tuckahoe and 5-8 parts of rhizoma polygonati.
The production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried peel slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a steam distillation method/pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.1-0.25 MPa, and the distillation time is 90-180 min;
s6: and (4) carrying out extraction fractionation to obtain the product.
Wherein, the pinecone is Pinus koraiensis of Xiaoxingan, and in the step S3, the length, width and size of the slice and the block are controlled to be 2mm-10 mm.
In the step S6, the extraction method adopts carbon dioxide supercritical extraction, the extraction pressure of the carbon dioxide supercritical extraction is 24-38 MPa, the extraction temperature is 48-58 ℃, the carbon dioxide flow is 18-36L/h, and the extraction time is 150-240 min.
Example 3:
a production process for preparing pinecone essential oil by a distillation method comprises the following components in parts by weight: 75 parts of pinecone pericarp, 13 parts of loquat leaf, 12 parts of white mulberry root-bark, 9 parts of poria cocos and 6 parts of rhizoma polygonati.
The production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried peel slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a steam distillation method, wherein the distillation pressure is controlled to be 0.1MPa, and the distillation time is 120min;
s6: and (4) carrying out extraction and fractionation to obtain the product.
Wherein, the pinecone is Pinus koraiensis of Xiaoxingan, and in the step S3, the length, width and size of the slice and the block are controlled to be 2mm-10 mm.
In the step S6, carbon dioxide supercritical extraction is adopted as an extraction method, the extraction pressure of the carbon dioxide supercritical extraction is 26MPa, the extraction temperature is 50 ℃, the carbon dioxide flow is 22L/h, and the extraction time is 180min.
Example 4:
a production process for preparing pinecone essential oil by a distillation method comprises the following components in parts by weight: 55 parts of pinecone peel, 16 parts of loquat leaf, 13 parts of cortex mori, 11 parts of poria cocos and 7 parts of rhizoma polygonati.
The production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried peel slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.2MPa, and the distillation time is 150min;
s6: and (4) carrying out extraction fractionation to obtain the product.
Wherein, the pinecone is Pinus koraiensis of Xiaoxingan, and in the step S3, the length, width and size of the slices and the blocks are controlled to be 2mm-10mm.
In the step S6, carbon dioxide supercritical extraction is adopted as an extraction method, the extraction pressure of the carbon dioxide supercritical extraction is 26MPa, the extraction temperature is 55 ℃, the carbon dioxide flow is 32L/h, and the extraction time is 210min.
Example 5:
a production process for preparing pinecone essential oil by a distillation method comprises the following components in parts by weight: 65 parts of pine cone pericarp, 15 parts of loquat leaf, 12 parts of white mulberry root-bark, 10 parts of poria cocos and 6 parts of rhizoma polygonati.
The production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried pericarp slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.15MPa, and the distillation time is 150min;
s6: and (4) carrying out extraction and fractionation to obtain the product.
Wherein, the pinecone is Pinus koraiensis of Xiaoxingan, and in the step S3, the length, width and size of the slices and the blocks are controlled to be 2mm-10mm.
In the step S6, carbon dioxide supercritical extraction is adopted as an extraction method, the extraction pressure of the carbon dioxide supercritical extraction is 32MPa, the extraction temperature is 52 ℃, the carbon dioxide flow is 28L/h, and the extraction time is 210min.
Example 6:
a production process for preparing pinecone essential oil by a distillation method comprises the following components in parts by weight: 65 parts of pinecone peel, 15 parts of loquat leaf, 12 parts of white mulberry root-bark, 10 parts of poria cocos and 6 parts of rhizoma polygonati.
The production process of the pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried pericarp slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.15MPa, and the distillation time is 150min;
s6: cooling the water vapor to water with a water exchange condenser;
s7: and (5) taking oil by using an oil-water separator to obtain the oil.
Wherein, the pinecone is Pinus koraiensis of Xiaoxingan, and in the step S3, the length, width and size of the slices and the blocks are controlled to be 2mm-10mm.
Experiment one:
in order to guarantee the quality of the essential oil produced by the invention, the essential oil is prepared by adopting the schemes of example 3, example 4 and example 5 respectively, and the obtained essential oil is evaluated, so that the following conclusion is obtained:
| scheme(s) | Phlegm eliminating effect | Antitussive effect | Effect of invigorating spleen | Heat clearing effect | Lung moistening effect |
| Example 3 | 86 | 88 | 90 | 87 | 91 |
| Example 4 | 89 | 90 | 88 | 90 | 87 |
| Example 5 | 93 | 94 | 90 | 89 | 89 |
As can be seen from the above, the essential oils obtained by the production according to the protocol of example 5 are most effective in combination, and therefore, the production according to the protocol of example 5 is preferable.
Experiment two:
in order to guarantee the quality of the essential oil produced by the method, the essential oil is prepared by adopting the scheme of example 5, the sizes of the essential oil during slicing and dicing are changed, and the obtained essential oil is evaluated, so that the following conclusion is obtained:
| size of slice | 2mm*2mm | 4mm*4mm | 6mm*6mm | 8mm*8mm | 10mm*10mm |
| Combined effects | 86 | 92 | 94 | 91 | 83 |
From the above, it is known that the slice size has a certain influence on the overall efficacy of the product at the time of production, and that the overall efficacy of the product is optimal when the slice size is 6mm × 6mm, and therefore, it is preferable that the slice size (length × width) is controlled to be 6mm × 6mm.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (10)
1. The production process for preparing the pinecone essential oil by the distillation method is characterized by comprising the following steps:
the method comprises the following steps:
s1: cleaning and airing the pinecone peel;
s2: slicing pinecone peel;
s3: drying in the sun for the second time to obtain dried peel slices;
s4: distilling the dried peel slices after secondary airing by a steam distillation method/pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.1-0.25 MPa, and the distillation time is 90-180 min;
s5: the water vapor is cooled to water with a water exchange condenser,
s6: and (5) taking oil by using an oil-water separator to obtain the oil.
2. The process for producing an essential oil of pinecone by distillation as claimed in claim 1, wherein the pinecone is pinecone of Pinus koraiensis from Xiaoxingan, and the length and width of the slices are controlled to be about 2mm to about 10mm in step S3.
3. The production process for preparing pinecone essential oil by using the distillation method according to claim 1, wherein the components in parts by weight are replaced by the components comprising: 50-80 parts of pinecone peel, 12-18 parts of loquat leaf, 10-15 parts of white mulberry root-bark, 8-12 parts of tuckahoe and 5-8 parts of rhizoma polygonati.
4. The production process for preparing pinecone essential oil by a distillation method according to claim 3, wherein the production process for pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried peel slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a steam distillation method/a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.1-0.25 MPa, and the distillation time is 90-180 min;
s6: and (4) carrying out extraction fractionation to obtain the product.
5. The production process for preparing pinecone essential oil by a distillation method according to claim 4, wherein in the step S6, carbon dioxide supercritical extraction is adopted as an extraction method, the extraction pressure of the carbon dioxide supercritical extraction is 24-38 MPa, the extraction temperature is 48-58 ℃, the carbon dioxide flow is 18-36L/h, and the extraction time is 150-240 min.
6. The production process for preparing pinecone essential oil by using the distillation method according to claim 5, wherein the pinecone essential oil comprises the following components in parts by weight: 65 parts of pinecone peel, 15 parts of loquat leaf, 12 parts of white mulberry root-bark, 10 parts of poria cocos and 6 parts of rhizoma polygonati.
7. The production process for preparing pinecone essential oil by a distillation method according to claim 3, wherein the production process for pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried peel slices;
s4: secondary airing to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.15MPa, and the distillation time is 150min;
s6: and (4) carrying out extraction and fractionation to obtain the product.
8. The production process of pinecone essential oil by distillation as claimed in claim 7, wherein in the step S6, carbon dioxide supercritical extraction is adopted as the extraction method, the extraction pressure of carbon dioxide supercritical extraction is 32MPa, the extraction temperature is 52 ℃, the flow rate of carbon dioxide is 28L/h, and the extraction time is 210min.
9. The process of claim 8, wherein the length and width of the slices and blocks are controlled to 6mm in step S3.
10. The production process for preparing pinecone essential oil by a distillation method according to claim 3, wherein the production process for pinecone essential oil specifically comprises the following steps:
s1: cleaning and airing the raw materials;
s2: slicing pinecone peel;
s3: slicing and dicing other raw materials according to the specification of dried peel slices;
s4: drying in the sun for the second time to obtain a dry mixed raw material;
s5: distilling the dried mixed raw material after secondary airing by a pressurized steam distillation method, wherein the distillation pressure is controlled to be 0.15MPa, and the distillation time is 150min;
s6: cooling the water vapor to water with a water exchange condenser;
s7: and (5) taking oil by using an oil-water separator to obtain the oil.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101461853A (en) * | 2007-12-20 | 2009-06-24 | 广西壮族自治区花红药业股份有限公司 | Chinese medicine granular formulation for relieving cough, dispelling phlegm and calming panting and preparation method thereof |
| CN101773527A (en) * | 2010-03-04 | 2010-07-14 | 大理学院 | Pinecone extractive of Yunnan Pinus and preparation method and medicinal application thereof |
| CN111437312A (en) * | 2020-04-08 | 2020-07-24 | 刘佳 | Formula of natural compound essential oil for improving reproductive system |
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- 2022-06-21 CN CN202210707782.7A patent/CN115181607A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101461853A (en) * | 2007-12-20 | 2009-06-24 | 广西壮族自治区花红药业股份有限公司 | Chinese medicine granular formulation for relieving cough, dispelling phlegm and calming panting and preparation method thereof |
| CN101773527A (en) * | 2010-03-04 | 2010-07-14 | 大理学院 | Pinecone extractive of Yunnan Pinus and preparation method and medicinal application thereof |
| CN111437312A (en) * | 2020-04-08 | 2020-07-24 | 刘佳 | Formula of natural compound essential oil for improving reproductive system |
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| 周秋丽等主编: "《现代中药基础研究与临床》", vol. 1, 天津科技翻译出版公司, pages: 366 * |
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