CN108277082A - One kind being suitable for industrial cinnamon oil extraction process - Google Patents

One kind being suitable for industrial cinnamon oil extraction process Download PDF

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Publication number
CN108277082A
CN108277082A CN201711247086.8A CN201711247086A CN108277082A CN 108277082 A CN108277082 A CN 108277082A CN 201711247086 A CN201711247086 A CN 201711247086A CN 108277082 A CN108277082 A CN 108277082A
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CN
China
Prior art keywords
oil
cinnamon oil
cassia tree
cinnamon
chinese cassia
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711247086.8A
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Chinese (zh)
Inventor
胡贤陈
邱远望
董银萍
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Fujian Zhongyi Pharmaceutical Co Ltd
Original Assignee
Fujian Zhongyi Pharmaceutical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fujian Zhongyi Pharmaceutical Co Ltd filed Critical Fujian Zhongyi Pharmaceutical Co Ltd
Priority to CN201711247086.8A priority Critical patent/CN108277082A/en
Publication of CN108277082A publication Critical patent/CN108277082A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/12Production of fats or fatty oils from raw materials by melting out
    • C11B1/16Production of fats or fatty oils from raw materials by melting out with steam
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/12Refining fats or fatty oils by distillation

Abstract

The present invention provides one kind being suitable for industrial cinnamon oil extraction process.First, it is compacted after cassia twig, the Gui Ye after crushing being added to extractor;Secondly, it is passed through vapor from extraction pot bottom, obtains milky oil water mixture liquid, milky oil water mixture liquid obtains cinnamon oil crude oil after oil water separator detaches;Finally, the cinnamon oil aqua aromatica after separation Chinese cassia tree crude oil is continued to concentrate by vacuum concentration pot, the cinnaldehydrum for remaining in remaining high-content in cinnamon oil aqua aromatica is kept completely separate;And after Chinese cassia tree crude oil is heated, the residual water molecules being wrapped in Chinese cassia tree crude oil can be detached thoroughly from Chinese cassia tree crude oil, obtain faint yellow supernatant liquid cinnamon oil.Cinnamon oil made from the method is better than the cinnamon oil color of traditional extraction by steam distillation, Determination of Cinnamaldehyde is high, yield is high, easy to operation, and not high to equipment requirement, suitable industrialized production.Gained cinnamon oil indices testing result meets 2015 editions《Chinese Pharmacopoeia》One ministerial standard.

Description

One kind being suitable for industrial cinnamon oil extraction process
Technical field
The present invention relates to one kind being suitable for industrial cinnamon oil extraction process, is specifically carried existing there is provided one The equipment for taking cinnamon oil is transformed, introduces the technique of new cinnamon oil production equipment production cinnamon oil, not only increases Chinese cassia tree The recovery rate of oil, and also improve the quality of cinnamon oil.Cinnamon oil color and luster obtained is good, Determination of Cinnamaldehyde is high, by traditional meat Oil of bay industrialization yield is increased to 1.5%~2.0% from 0.8%~1.0%.Indices meet 2015 editions《Chinese Pharmacopoeia》One Standard.
Background technology
Cinnamon oil, English name Cinnamomum Oil are the dry of canella Chinese cassia tree Cinnamomum cassia Presl The volatile oil that dry branch, leaf are extracted through steam distillation.This product is the supernatant liquid of yellow or yellowish-brown;There is the special perfume (or spice) of Chinese cassia tree Gas, it is sweet, pungent.Main component has benzaldehyde, salicylide, acetophenone, benzyl carbinol, trans-cinnamic aldehyde, cinnamyl alcohol, eugenol, perfume (or spice) Legumin, cinnamyl acetate, trans- o-methoxy cinnamic aldehyde etc.;China Guangxi, Guangdong (accounting for about world wide production 80%) mainly are originated in, Vietnam, India also produce.According to the difference in growth geographical location, in physics and chemistry, different tank oil claims Sri Lanka osmanthus respectively in nature Leaf oil and Seychelles type bay leaves oil.Cinnamon oil is widely used:1. the fumet of food and beverage;It is carried 2. can also be detached from this oil Natural cinnamyl aldehyde is taken, and can further synthesize a variety of fragrance such as cinnamyl alcohol, benzaldehyde;3. having bactericidal effect, lead in medicine It to be used as the raw material of " essential wind oil " and " shangshi zhitong plaster, shangshi zhitong gao ".
The technique of industrial production cinnamon oil is mainly steam distillation extraction method and supercritical extraction at present.The invention is special It is sharp compared with existing steam distillation, have the advantage that:1. process contamination is small;2. recovery rate is high;3. product color is good. The patent of invention has the advantage that compared with existing supercritical extraction:1. equipment is simple, easy to clean, easy to operate;2. giving birth to It produces at low cost.
Invention content
The problem of for existing extraction by steam distillation cinnamon oil technique, is carried by the way that used equipment is transformed, introduces new equipment Being suitable for industrial cinnamon oil extraction process for one kind.The technique can not only improve the yield of cinnamon oil, but also product Color and luster is good;The advantages that equipment is easy to operate, easy cleaning.
Description of the drawings
Attached drawing 1 is extraction cinnamon oil process flow diagram
Attached drawing 2 is the result under TLC thin layers discriminating 365nm
Attached drawing 3 is the result under TLC thin layers discriminating 254nm
Attached drawing 4 is the assay of Cinnamaldehyde in Cinnamon Oil.
Specific implementation mode
Embodiment 1
The first step:After 1500kg cassia twig is selected removal of impurities, then coarse powder is broken into 1cm~3cm, obtains cassia twig particle 1342kg, then first In an input part to extractor, it is passed through steam wetting after compacting, is further continued for the compacting that feeds intake, until tank mouth is overflowed, covers extraction The lid of tank;
Second step:It is passed through steam from tank base, maintains Extracting temperature at 100 DEG C~108 DEG C, extraction time is 2.5 hours to 3 small When, obtain Chinese cassia tree oil/water mixed vapour;
Third walks:The condensed device condensation of Chinese cassia tree oil/water mixed vapour, obtains milky cinnamon oil/water cooling lime set;
4th step:Chinese cassia tree crude oil is obtained after 10 oil water separators separation that cinnamon oil/water cooling lime set is concatenated;
5th step:Cinnamon oil aqua aromatica after cinnamon oil/water cooling lime set separation Chinese cassia tree crude oil is concentrated through vacuum concentration equipment, is controlled Temperature is 65 DEG C~75 DEG C, and vacuum degree reading is -0.09Mpa~-0.1Mpa, obtains the higher Chinese cassia tree crude oil of amount containing cinnaldehydrum.
6th step:Chinese cassia tree crude oil heats in heat insulation tank, control temperature at 70 DEG C~80 DEG C, heating time be 30min~ 40min.The water wrapped up in Chinese cassia tree crude oil is kept completely separate, cinnamon oil 24.15kg, yield 1.80% are obtained.
Embodiment 2
The first step:After the osmanthus 1500kg leaf is selected removal of impurities, then coarse powder is broken into 1cm~3cm, obtains osmanthus leaf particle 1275kg, then first In an input part to extractor, it is passed through steam wetting after compacting, is further continued for the compacting that feeds intake, until tank mouth is overflowed, covers extraction The lid of tank;
Second step:It is passed through steam from tank base, maintains Extracting temperature at 100 DEG C~108 DEG C, extraction time is 2.5 hours to 3 small When, obtain Chinese cassia tree oil/water mixed vapour;
Third walks:The condensed device condensation of Chinese cassia tree oil/water mixed vapour, obtains milky cinnamon oil/water cooling lime set;
4th step:Chinese cassia tree crude oil is obtained after 10 oil water separators separation that cinnamon oil/water cooling lime set is concatenated;
5th step:Cinnamon oil aqua aromatica after cinnamon oil/water cooling lime set separation Chinese cassia tree crude oil is concentrated through vacuum concentration equipment, is controlled Temperature is 65 DEG C~75 DEG C, and vacuum degree reading is -0.09Mpa~-0.1Mpa, obtains the higher Chinese cassia tree crude oil of amount containing cinnaldehydrum.
6th step:Chinese cassia tree crude oil heats in heat insulation tank, control temperature at 70 DEG C~80 DEG C, heating time be 30min~ 40min.The water wrapped up in Chinese cassia tree crude oil is kept completely separate, cinnamon oil 19.56kg, yield 1.53% are obtained.
Embodiment 3
The first step:By 1500kg cassia twig and osmanthus leaf mixture(Cassia twig 900kg, Gui Ye 600kg)After selecting removal of impurities, then coarse powder is broken into 1cm~3cm obtains cassia twig/osmanthus leaf hybrid particles 1308kg, and steam is first then passed through after compacting in an input part to extractor Wetting, is further continued for the compacting that feeds intake, until tank mouth is overflowed, covers the lid of extractor;
Second step:It is passed through steam from tank base, maintains Extracting temperature at 100 DEG C~108 DEG C, extraction time is 2.5 hours to 3 small When, obtain Chinese cassia tree oil/water mixed vapour;
Third walks:The condensed device condensation of Chinese cassia tree oil/water mixed vapour, obtains milky cinnamon oil/water cooling lime set;
4th step:Chinese cassia tree crude oil is obtained after 10 oil water separators separation that cinnamon oil/water cooling lime set is concatenated;
5th step:Cinnamon oil aqua aromatica after cinnamon oil/water cooling lime set separation Chinese cassia tree crude oil is concentrated through vacuum concentration equipment, is controlled Temperature is 65 DEG C~75 DEG C, and vacuum degree reading is -0.09Mpa~-0.1Mpa, obtains the higher Chinese cassia tree crude oil of amount containing cinnaldehydrum.
6th step:Chinese cassia tree crude oil heats in heat insulation tank, control temperature at 70 DEG C~80 DEG C, heating time be 30min~ 40min.The water wrapped up in Chinese cassia tree crude oil is kept completely separate, cinnamon oil 22.12kg, yield 1.69% are obtained.
The present invention extracts cinnamon oil process flow diagram
Attached drawing 1
By 2015 editions《Chinese Pharmacopoeia》One ministerial standard method detects quality and technical index respectively, and every testing result conforms to It asks.
The thin layer discrimination test of cinnamon oil:
(1)Configuration proportion is n-hexane:Petroleum ether:Ethyl acetate:Acetic acid=6:2:3:0.2 solvent;
(2)Prepare sample:It takes 1ml cinnamon oils in test tube, adds 10ml methanol, shake up spare.
(3)TLC thin layers differentiate, as a result as follows:
365nm:Attached drawing 2
254nm:Attached drawing 3
According to National Standard of the People's Republic of China's GB 1886.207-2016 Chinese cinnamon oil appendix A characteristic component assays Prescriptive procedure area normalization method carries out the assay of Cinnamaldehyde in Cinnamon Oil, and measurement result is as follows:
Attached drawing 4.

Claims (10)

1. one kind being suitable for industrial cinnamon oil extraction process, which is characterized in that include the following steps:By the osmanthus of Chinese cassia tree Branch, cassia bark be crushed to 1~3cm, be added in extractor, be passed through after compacting vapor wetting, continuously add crush after cassia twig, Gui Ye, until closeing the lid after overflowing extractor, being passed through vapor from extraction pot bottom is distilled, the mixing of cinnamon oil and water Milky Chinese cassia tree oil water mixture, water-oil separating of the Chinese cassia tree oil water mixture through successively successively decreasing are obtained after the condensed device condensation of steam After device standing separation, Chinese cassia tree crude oil is obtained;Cinnamon oil aqua aromatica after separation Chinese cassia tree crude oil continues to concentrate by vacuum concentration pot, The cinnaldehydrum for remaining in remaining high-content in cinnamon oil aqua aromatica is kept completely separate;Last Chinese cassia tree crude oil further heats progress It is separated off and is wrapped in remaining water in cinnamon oil, finally obtain faint yellow, clear cinnamon oil.
2. as described in claim 1 a kind of suitable for industrial cinnamon oil extraction process, it is characterised in that:The osmanthus Drying branch, the leaf of branch, osmanthus leaf canella Chinese cassia tree Cinnamomum cassia Presl derive from " township of Chinese cinnamon " sieve Determine city.
3. as described in claim 1 a kind of suitable for industrial cinnamon oil extraction process, it is characterised in that:The raw material Cassia twig, osmanthus leaf can individually feed intake, can also mixed material feeding;When mixed material feeding, the weight ratio of cassia twig and osmanthus leaf is 6 to 4.
4. the cassia twig to feed intake, osmanthus leaf length are 1~3cm.
5. as described in claim 1 a kind of suitable for industrial cinnamon oil extraction process, it is characterised in that:The extraction Tank material is 304 stainless steels, and specification is 1.6 tons;Extractor mode of heating is that tank base leads directly to steam heating tank base Water generates new steam after bottom water ebuillition of heated.
6. as described in claim 1 a kind of suitable for industrial cinnamon oil extraction process, it is characterised in that:The technique Temperature when extracting Chinese cassia tree crude oil is 100 DEG C~108 DEG C, and extraction time is 2.5 hours to 3 hours.
7. as described in claim 1 a kind of suitable for industrial cinnamon oil extraction process, it is characterised in that:It is concentrated in vacuo Shi Wendu is 65 DEG C~75 DEG C, and vacuum degree reading is -0.09Mpa~-0.1Mpa.
8. as described in claim 1 a kind of suitable for industrial cinnamon oil extraction process, it is characterised in that:The grease Separator material is 304 stainless steels, and quantity is 10, is used in series.
9. number is 1#, 2#, 3#, 4#, 5#, 6#, 7#, 8#, 9#, 10#, wherein 1#~7# pot bottoms are big cone, specification 2 Ton;Tri- tank specifications of 8#, 9#, 10# are 1.6 tons, and bottom is flat;1#~8# top discharges mouth is reduced step by step as next The feed inlet of tank, the height and 8# tanks of two tanks of 9#, 10# are consistent, and bottom discharge mouth is ganged up connected.
10. as described in claim 1 a kind of suitable for industrial cinnamon oil extraction process, it is characterised in that:Heating point Temperature from the water wrapped up in Chinese cassia tree crude oil is 70 DEG C~80 DEG C, and heating time is 30min~40min.
CN201711247086.8A 2017-12-01 2017-12-01 One kind being suitable for industrial cinnamon oil extraction process Pending CN108277082A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711247086.8A CN108277082A (en) 2017-12-01 2017-12-01 One kind being suitable for industrial cinnamon oil extraction process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711247086.8A CN108277082A (en) 2017-12-01 2017-12-01 One kind being suitable for industrial cinnamon oil extraction process

Publications (1)

Publication Number Publication Date
CN108277082A true CN108277082A (en) 2018-07-13

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106350214A (en) * 2016-09-19 2017-01-25 罗定市荣兴香料有限公司 Cinnamon oil extraction method
CN107034011A (en) * 2017-06-09 2017-08-11 广东心宝药业科技有限公司 The continuous preparation method of cinnamon oil

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106350214A (en) * 2016-09-19 2017-01-25 罗定市荣兴香料有限公司 Cinnamon oil extraction method
CN107034011A (en) * 2017-06-09 2017-08-11 广东心宝药业科技有限公司 The continuous preparation method of cinnamon oil

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Application publication date: 20180713

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