CN102559384B - Method for extracting cinnamon oil - Google Patents
Method for extracting cinnamon oil Download PDFInfo
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- CN102559384B CN102559384B CN201110406279.XA CN201110406279A CN102559384B CN 102559384 B CN102559384 B CN 102559384B CN 201110406279 A CN201110406279 A CN 201110406279A CN 102559384 B CN102559384 B CN 102559384B
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- essential oil
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- oleum cinnamomi
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Abstract
The invention relates to a method for extracting cinnamon oil from dry branches and leaves of cinnamon. By the method, the extraction time can be shortened, oil yield can be improved, energy consumption can be reduced, and the production cost can be reduced. according to the method, a surfactant is used as a leaching adjuvant in a water vapor distillation method, the water-wetting of surfaces of the branches and leaves of the cinnamon is accelerated under the action of wetting, permeation and solubilization of the surfactant, and the water permeates through plant cells, so that essential oil inside the plant cells is carried away from the cells; and the essential oil is subjected to exchange by heat energy in a system, so that the essential oil is azeotropic with water vapor to be distilled with the water vapor, and the distilled essential oil is condensed, cooled and subjected to centrifugal sedimentation to obtain the cinnamon oil. According to the method, the distillation time is short, so the change of heat sensitive chemical ingredients in the essential oil due to long-term heating is avoided, and the influence on aroma of the essential oil due to the coking of plant raw materials caused by overheating is also avoided. The cinnamon oil is light in color and pure in aroma, and does not have the smell of scorching.
Description
Technical field
The present invention relates to a kind of method of extracting cinnamon essential oil from the dry branches and leaves of Chinese cassia tree, particularly use steam distillation.
Background technology
Oleum Cinnamomi is that the dry bark of canella Chinese cassia tree, leaf or branch are through extracting the volatile oil obtaining.Oleum Cinnamomi has Xin Lie and warm sweet fragrance, and band is burnt, wooden, cream is fragrant, is natural perfume staple product, its main component is phenylacrolein, is widely used as foodstuff additive and seasonings, and can be directly as medicine, be one of important outlet special product of China, long-cherished in the world.Oleum Cinnamomi has stronger bacteriostatic activity to bacterium, fungi, mould, can be used for natural food preservative freshness retaining agent, grain protecting agent.
The extracting method of Oleum Cinnamomi has solvent extration, supercritical CO
2extraction process, steam distillation etc.But because solvent extration needs a large amount of inflammable and explosive organic solvents, to the security of producing, be a significant threat, and the purification of later stage Oleum Cinnamomi often there is dissolvent residual phenomenon, make product lose natural sex.Supercritical CO
2extraction process has many good qualities, it is the good method of separating natural product effective constituent, but because need hyperbaric environment, high to equipment requirements, equipment investment is large, owing to extracting under high pressure conditions, extractor small volume, throughput is limited, cannot form large-scale industrialization and produce, and product cost is high.It is simple that steam distillation has equipment, processing ease, and the advantage such as cost is low, and output is large, is to produce at present most widely used, the most important method of plants essential oil.But traditional steam distillation energy consumption is large, and extraction time is long, and plant factor is low, due to long-time heating, may make some composition in essential oil decompose, when simultaneously overheated, can make plant material coking, the fragrance of essential oil is produced to detrimentally affect.Therefore the necessary technique to steam distillation extraction Oleum Cinnamomi is improved research.
Summary of the invention
The object of the invention is to improve and with steam distillation, from cinnamon leaf, extract the technique of Oleum Cinnamomi, shorten distillation time, improve oil yield, reduce energy consumption, reduce production costs.
In order to achieve the above object, the present invention passes through to add tensio-active agent as leaching auxiliary on the basis of steam distillation, by wetting, infiltration, solubilising, the forming process of tensio-active agent, accelerate water molecules quick humidification cinnamon leaf solid surface and infiltrate through cell interior, outside the Oleum Cinnamomi emigrated cells in cell, form azeotropic system with water and be distilled out of.
The method of extraction Oleum Cinnamomi of the present invention, comprise the following steps: the cinnamon leaf drying in the shade to pulverize, join in still kettle, add water and tensio-active agent, heating systems distillation 1～4 hour, collect phlegma, under 4～20 ℃ of freezers standing 2～10 hours, centrifugation, oily water separation obtains thick Oleum Cinnamomi, moisture is removed in the Oleum Cinnamomi underpressure distillation obtaining, and obtains cinnamon essential oil;
Described cinnamon leaf and the weight ratio of water are 1:6 ~ 1:12.
Described tensio-active agent is nonionogenic tenside, the anion surfactant of C8～C20, one or more of cats product; Concentration accounts for 0.1%～1.0% of the water yield.
The above pulverizes cinnamon leaf, by cinnamon leaf smashing fineness, is preferably 5 order～40 orders.
The rotating speed of the above centrifugation process whizzer used is 4000r/min～10000r/min, and centrifugation time is 5min～30min.
The vacuum tightness of the above underpressure distillation is-0.095MPa～-0.080MPa, and temperature is 50～90 ℃, and distillation time is 30min～90min.
Above-described ionic surfactant pack is drawn together fatty alcohol polyethenoxy ether class, sorbitan fatty acid ester class, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycol, APG, sucrose fatty ester class; Anion surfactant comprises fatty acid sodium salt, lipid acid sylvite, sulfonate surfactant, sulfuric acid ester tensio-active agent, phosphoric acid ester tensio-active agent, sulphosuccinates class; Cationic surface comprises quaternary ammonium salt cationic surfactant, heterocyclic cats product, polyethylene polyamines salt,
The above water distilling apparatus, comprises stainless steel still kettle, enamel still kettle and glass/or and stainless steel/or and resin/or and stainless steel distillation tower of ceramic packing.
Advantage of the present invention and positively effect:
On Abstracting Method of Cinnamon Oil of the present invention, adopt the mode of the auxiliary steam distillation of tensio-active agent, utilize wetting, infiltration, solubilising, the whipability of tensio-active agent, shorten distillation time, improve oil yield, reduce energy consumption, accelerate oily water separation, improve plant factor, greatly reduce production costs.
Tensio-active agent is a kind of material that just can greatly reduce water surface tension in very low concentrations situation, conventionally contains hydrophilic group (polar group) and hydrophobic group (non-polar group) in its molecular structure.The effects such as that tensio-active agent has is wetting, infiltration, dispersion, solubilising, emulsification, washing, foaming, froth breaking, are widely used in every field.So the present invention adds tensio-active agent, can make Oleum Cinnamomi distillation component have the effects such as wetting, infiltration, dispersion, solubilising, emulsification, washing, foaming, froth breaking, shorten distillation time 1-2 hour, improve oil yield 30-40%.
Accompanying drawing explanation
Fig. 1: tensio-active agent is assisted steam distillation gained cinnamon essential oil gas chromatogram.
Fig. 2: independent steam distillation gained cinnamon essential oil gas chromatogram.
Fig. 3: the figure left side is independent steam distillation products obtained therefrom, the right is for adding tensio-active agent distillation products obtained therefrom.
From Fig. 1, Fig. 2 recognizes the auxiliary steam distillation gained cinnamon essential oil of tensio-active agent and not obviously difference of steam distillation gained cinnamon essential oil composition separately.
From Fig. 3, recognize independent steam distillation products obtained therefrom color darker than what add tensio-active agent, this is owing to adding tensio-active agent as distillation auxiliary, can shorten distillation time, avoid at high temperature long-time heating and make thermo-sensitivity composition decompose chromatogenous cause of Oleum Cinnamomi.
Embodiment
embodiment 1
10 order cinnamon leaf 100g, join in round-bottomed flask, add 1000ml water, add 0.2% Sodium dodecylbenzene sulfonate, heating systems makes boiling, keeps 3h, phlegma is transferred in freezer, and cooling 3h under 10 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 6000r/min, and centrifugal 15min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 80 ℃, vacuum tightness is-0.090MPa under underpressure distillation 30min.Obtain 1.65g essential oil.
embodiment 2
40 order cinnamon leaf 100g, join in round-bottomed flask, add 800ml water, add 0.5% twen-80, heating systems makes boiling, keeps 2h, phlegma is transferred in freezer, and cooling 2h under 10 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 8000r/min, and centrifugal 10min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 60 ℃, vacuum tightness is-0.095MPa under underpressure distillation 30min.Obtain 1.72g essential oil.
embodiment 3
5 order cinnamon leaf 100g, join in round-bottomed flask, add 1000ml water, add 0.1% sodium laurylsulfate, heating systems makes boiling, keeps 3h, phlegma is transferred in freezer, and cooling 6h under 15 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 10000r/min, and centrifugal 15min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 80 ℃, vacuum tightness is-0.080MPa under underpressure distillation 45min.Obtain 1.62g essential oil.
embodiment 4
20 order cinnamon leaf 100g, join in round-bottomed flask, add 600ml water, add 0.6% sodium laurylsulfonate, heating systems makes boiling, keeps 1h, phlegma is transferred in freezer, and cooling 1h under 4 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 4000r/min, and centrifugal 30min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 90 ℃, vacuum tightness is-0.090MPa under underpressure distillation 15min.Obtain 1.81g essential oil.
embodiment 5
40 order cinnamon leaf 100g, join in round-bottomed flask, add 1000ml water, add 0.4% palmityl trimethyl ammonium chloride, heating systems makes boiling, keeps 3h, phlegma is transferred in freezer, and cooling 2h under 8 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 10000r/min, and centrifugal 5min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 90 ℃, vacuum tightness is-0.080MPa under underpressure distillation 30min.Obtain 1.68g essential oil.
embodiment 6
10 order cinnamon leaf 100g, join in round-bottomed flask, add 1000ml water, add 1.0%Span-20 and PEG-800, heating systems makes boiling, keeps 3h, phlegma is transferred in freezer, and cooling 3h under 10 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 4000r/min, and centrifugal 15min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 80 ℃, vacuum tightness is-0.090MPa under underpressure distillation 30min.Obtain 1.81g essential oil.
embodiment 7
10 order cinnamon leaf 100g, join in round-bottomed flask, add 1200ml water, add 0.2% soil temperature-60 and sodium stearate, heating systems makes boiling, keeps 3h, phlegma is transferred in freezer, and cooling 3h under 10 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 8000r/min, and centrifugal 10min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 60 ℃, vacuum tightness is-0.090MPa under underpressure distillation 30min.Obtain 1.65g essential oil.
embodiment 8
5 order cinnamon leaf 100g, join in round-bottomed flask, add 1200ml water, add 0.5%PEG-400 and octadecyl trimethyl ammonium chloride, heating systems makes boiling, keeps 2h, phlegma is transferred in freezer, and cooling 3h under 10 ℃ of environment, then uses centrifugal precipitation mechanism centrifugation, rotating speed is 10000r/min, and centrifugal 5min gets rid of upper strata moisture, obtain thick Oleum Cinnamomi, thick Oleum Cinnamomi is transferred to vacuum distillation apparatus, at 60 ℃, vacuum tightness is-0.090MPa under underpressure distillation 30min.Obtain 1.78g essential oil.
Claims (3)
1. a method of extracting Oleum Cinnamomi, it is characterized in that comprising the following steps: the cinnamon leaf drying in the shade to pulverize, join in still kettle, add water and tensio-active agent, heating systems distillation 1～4 hour, collect phlegma, phlegma is put into 4～20 ℃ of freezers standing 2～10 hours, centrifugation, oily water separation obtains thick Oleum Cinnamomi, moisture is removed in the Oleum Cinnamomi underpressure distillation obtaining, and obtains cinnamon essential oil;
Described cinnamon leaf and the weight ratio of water are 1:6～12;
The vacuum tightness of described underpressure distillation is-0.095MPa～-0.080MPa, and temperature is 50～90 ℃, and distillation time is 30min～90min;
Described tensio-active agent is nonionogenic tenside, the anion surfactant of C8～C20, one or more of cats product; Concentration is to account for 0.1%～1.0% of the water yield;
Described ionic surfactant pack is drawn together fatty alcohol polyethenoxy ether class, sorbitan fatty acid ester class, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycol, APG and sucrose fatty ester class; Anion surfactant comprises fatty acid sodium salt, lipid acid sylvite, sulfonate surfactant, sulfuric acid ester tensio-active agent, phosphoric acid ester tensio-active agent and sulphosuccinates class; Cats product comprises quaternary ammonium salt cationic surfactant, heterocyclic cats product and polyethylene polyamines salt.
2. the method for extraction Oleum Cinnamomi according to claim 1, is characterized in that: the fineness of cinnamon leaf is 5 order～40 orders.
3. the method for extraction Oleum Cinnamomi according to claim 1, is characterized in that: the rotating speed of centrifugation process whizzer used is 4000r/min～10000r/min, and centrifugation time is 5min～30min.
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| CN102559384B true CN102559384B (en) | 2014-09-24 |
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Families Citing this family (16)
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| CN102827697A (en) * | 2012-09-24 | 2012-12-19 | 云南兴道纪科技有限公司 | Pu-erh tea essential oil and preparation method thereof |
| CN103215121A (en) * | 2013-04-25 | 2013-07-24 | 防城港市防城区那梭香料厂 | Extraction process of cinnamon oil |
| CN105219515B (en) * | 2014-06-18 | 2019-01-08 | 中国石油化工股份有限公司 | A kind of broken wall of oil-containing micro-algae and method using saponification assisted extraction grease |
| CN105296164A (en) * | 2015-12-02 | 2016-02-03 | 无限极（中国）有限公司 | Extraction method of cinnamon oil |
| CN106190575A (en) * | 2016-07-31 | 2016-12-07 | 华南理工大学 | A kind of extracting method of cinnamon essential oil |
| CN106947585A (en) * | 2017-04-27 | 2017-07-14 | 王再青 | A kind of extracting method of cinnamon oil |
| CN108244151A (en) * | 2017-12-26 | 2018-07-06 | 刘志刚 | A kind of extracting method of clove bud oil for mite killing |
| CN108251215A (en) * | 2017-12-26 | 2018-07-06 | 刘志刚 | A kind of extracting method of cinnamon essential oil for mite killing |
| CN108048211B (en) * | 2017-12-28 | 2021-01-26 | 山东江天生物科技有限公司 | Oil extraction method with high oil yield |
| CN108359530B (en) * | 2018-02-13 | 2020-07-07 | 江南大学 | Extracting agent for extracting oil by aqueous medium method and application thereof |
| CN108277088A (en) * | 2018-04-08 | 2018-07-13 | 福建鑫绿林产品开发有限公司 | A kind of preparation method of fir essential oil and products thereof |
| CN109943412A (en) * | 2019-04-10 | 2019-06-28 | 范加家 | A kind of borneol method of extraction of essential oil |
| CN110711164A (en) * | 2019-11-27 | 2020-01-21 | 广东工业大学 | Extraction method and application of cinnamon extracting solution |
| CN112457921A (en) * | 2020-12-10 | 2021-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of grapefruit essential oil with high extraction rate |
| CN113201405A (en) * | 2021-04-26 | 2021-08-03 | 常州工学院 | Extraction method of lavender essential oil |
| CN113501751B (en) * | 2021-08-18 | 2023-06-09 | 南宁市和昇香料香精有限公司 | Method for preparing high-purity cinnamaldehyde by efficient rectification and purification of cinnamon oil |
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Effective date of registration: 20151202 Address after: 530007 Nanning high tech Zone, West Road, innovation, No. 13, No. Patentee after: Guangxi Shengbaotang Health Industry Co., Ltd. Address before: 530007 Nanning high tech Zone, West Road, innovation, No. 13, No. Patentee before: Guangxi Sanpotel Pharmaceutical Co., Ltd. |
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