CN103074160A

CN103074160A - Extraction process for essential oil of Sabina vulgaris Ant. through distillation with water

Info

Publication number: CN103074160A
Application number: CN2009102543001A
Authority: CN
Inventors: 王林和; 张国盛; 郭秀艳; 包丽华
Original assignee: Individual
Current assignee: Individual
Priority date: 2009-12-10
Filing date: 2009-12-10
Publication date: 2013-05-01

Abstract

The invention discloses an extraction process for essential oil of Sabina vulgaris Ant. through distillation with water. The process comprises the following steps: a, cleaning, air-drying, crushing and sieving the raw material Sabina vulgaris Ant., placing obtained powder of Sabina vulgaris Ant. in a distilling flask, adding 7 to 9 times of water and 1 to 6% by mass of NaCl, and carrying out immersion for 2 to 8 h; b, connecting the flask to a steam distillation apparatus, carrying out extraction at a temperature of 100 to 120 DEG C for 2.0 to 4.0 h, carrying out standing for 0.5 to 2 h, carrying out cooling until temperature drops to normal temperature, then carrying out oil-water separation and discharging distillate according to reading to obtain the essential oil of Sabina vulgaris Ant. According to the invention, the steam distillation apparatus is employed in the invention, the advantages of easiness, easily practicable operation, easily controllable heating temperature, low production cost, high oil yield and the like are obtained, and plant essential oil in Sabina vulgaris Ant. can be rapidly extracted. The fragrant essential oil extracted from the branch, leaf, fruit, seed and root of Sabina vulgaris Ant. can be used for preparation of articles of everyday use, cosmetics, medicines, pesticides, etc., and has a wide application scope.

Description

Be total to the smelly cypress essential oil of water distillation and extraction technique

Technical field

The invention belongs to plants essential oil extraction process technology field, be specifically related to a kind of method of extracting smelly cypress essential oil.

Background technology

Smelly cypress can be used for induced labor, wind-damp dispelling, eases pain, calms the nerves, stomach invigorating, subside a swelling, invigorate blood circulation and the drug effects such as pain relieving, also has sterilization, insecticidal activity.Particularly podophyllum kind compound has significant broad spectrum anticancer activity and antiviral activity in the smelly cypress essential oil.But the oil yield of present smelly cypress essential oil is low, cost is high, and resource is caused very large waste.

Smelly cypress (Sabina vulgaris Ant.) is the evergreen shrub that crawls of Cupressaceae Sabina, also claims savin juniper, Sabina vulgaris, savin and climbs ground cypress etc., and rare is arbor, and branch is thin, and the then stink that sprig rubs, leaf are alternately to life; Dioecy, rare monoecism, the cone del has white powder, dun purple or atropurpureus when ripe; The nearly oval of seed, slightly flat, tool rib ridge has a small amount of resin storage tank, and 3 years are one ripe.Smelly Bai Shi is living, and scope is wide, the poor hemorrhoid of drought-enduring, cold-resistant, anti-soil etc., and well developed root system, with luxuriant foliage and spreading branches in leafy profusion, weatherproof sand buries, and smelly cypress group concentrates in flakes, and the coverage of smelly cypress shrubbery is up to 70%-95%, individual plant shrubbery area can reach 200m2, is good rare evergreen fixing the sand and bank protection soil conservation seeds and green tree species.Smelly cypress mainly is distributed in the stone matter hillside of arid, semiarid region in China, in addition, at Inner Mongol Mu Us Shadi and muddy Starch 1500 gram sand ground distribution is arranged also, also can grow in Loess Region after introducing a fine variety.From administrative division, smelly cypress can be settled down in " three Norths " area fully, its natural distributed is in the Inner Mongol, Xinjiang, Ningxia, Qinghai, Gansu and the Shaanxi in western part, and in Hebei, the provinces and cities such as Beijing, Shanxi and Liaoning are successfully introduced a fine variety is cities and towns and Landscape Trees, are a kind of seeds that can be introduced a fine variety on a large scale.Simultaneously, smelly cypress has very high economic use value.Smelly cypress is rich in essential oil, has aromatic odour, and its complex chemical composition is various, and the terpenes in the essential oil and podophyllotoxin analogue have antitumour activity and insecticidal activity, is the important physiologically active substance of a class.

The common practice that present steam distillation extracts smelly cypress essential oil is, the smelly cypress branch that has dried in the shade is suitably pulverized, extract its essential oil with the conventional wet distillation of volatile oil extractor, product is dissolved in ether, reclaim ether with anhydrous sodium sulfate drying and get essential oil, the gained essential oil is faint yellow transparent oily liquid, oil yield is generally about 0.5% of dried branches and leaves, one ton of essential oil of every production, incinerate distilled useless branches and leaves outer (200 tons), also to burn 360 tons in firewood, and thermo-efficiency only 20%, the essential oil loss is large.Heating temperature is too high easily to be made some composition decomposition of essential oil and makes the part material coking, thereby affects the quality of essential oil.And the residual recovery of chemical substance during extraction is incomplete, affects the quality of essential oil.Improve quality and the yield of essential oil, must study new distil process, based on the problem that steam distillation exists, people begin to be devoted to improve distillation plant and method, wish to improve quality and oil yield, reduce cost, but do not have up to now remarkable break-throughs.

The present invention adopts the electric mantle heating, can control temperature, and calorific loss is few, energy-conserving and environment-protective.Its principal feature is that common water steams straight run distillation, and for unstable chemcial property in the smelly pitch, still-process is the characteristics of loss easily, has taked can accelerate still-process like this to carrying out mechanical disintegration and use the sodium chloride aqueous solution immersion treatment before the smelly cypress material distillation.

Research contents

The purpose of this invention is to provide a kind of extraction process that can improve smelly cypress essential oil oil yield.

The technique that the present invention takes is as follows: gather → clean → dry in the shade → pulverize → pre-treatment → be total to water distillation → distillate to leave standstill → reading → minute filter → dehydration → preserve

At first clean after the bright branch of smelly cypress is plucked, then branches and leaves are separated, with branch classification, segment, dry in the shade and pulverize; First fruit is cleaned behind the smelly cypress picking fruit, and dried in the shade and pulverize; Smelly cypress root system gathers afterwash, classification, dries in the shade and pulverizes.Concrete grade scale is: withe leaf (branch and the leaf of giving birth to then), shoot (1-2 gives birth to), old branch (more than lifes in 2 years), radicula (D≤2.0mm) and root (D＞2.0mm) slightly.

1.. the smelly cypress of raw material is cleaned, and classification is dried in the shade, and pulverizes the 30--40 mesh sieve, places in the matrass, and adding 7-9 water and massfraction doubly is the NaCl of 1-6%, soaks 2-8h.

2.. connect altogether water-distillation unit, temperature is about 100-120 ℃, behind the extraction 2.0-4.0h, reflux cooling leaves standstill 1-2h until be cooled to room temperature, through oil, moisture is from obtaining smelly cypress essential oil, reading is emitted the essential oil in the volatile oil determination apparatus, removes moisture with anhydrous sodium sulphate, preserves.

Because this technique has been taked upper art technical scheme, compare with existing distillating method, have advantages of that oil yield is high, the oil quality index is high, energy-conserving and environment-protective, oil yield improves 50-100% than existing technique.

Description of drawings

Fig. 1 is ethereal oil determination of distillation device figure.Fig. 2 is temp. controllable electric mantle and distiller constitutional diagram.

Fig. 3 is smelly cypress distillation method extraction of essential oil artwork.

What hydrodistillation was altogether adopted in experiment is volatile oil determination apparatus, and such as figure, A is hard round-bottomed flask (2000mL), and B is volatile oil determination apparatus, and C is reflux condensing tube, and interface is smeared a small amount of Vaseline, guarantees resistance to air loss, prevents that steam and essential oil from overflowing.The density ratio water of essential oil is light, so it is an amount of to get trial-product, weighed weight is put in the flask, add water an amount of with granulated glass sphere number, behind the jolting mixing, connection volatile oil determination apparatus and reflux condensing tube.Self-condensation pipe upper end adds water makes the scale part that is full of volatile oil determination apparatus, and till overflow enters in the flask.Put to be heated in the electric mantle and boil, keep little certain hour that boils, oil mass no longer increases to the volatile oil determination apparatus, and stopped heating is placed a moment, opens tester lower end piston, and water is slowly emitted, and arrives to the oil reservoir upper end above scale 0 line till the 5mm place.Place more than the 1h, opening piston, to make oil reservoir drop to its upper end just concordant with scale 0 line again, reads the volatilization oil mass, emits the essential oil in the volatile oil determination apparatus, anhydrous sodium sulphate removal moisture.And be calculated as follows the oil yield (mL/100g) of essential oil in the trial-product.

Essential oil oil yield (mL/100g)=essential oil oil pump capacity (mL)/take by weighing sample size (100g)

Embodiment

Embodiment 1

At first with smelly CedarLeaves cleaning in the summer that gathers, dry in the shade, electric crusher is pulverized, and crosses the 30-40 mesh sieve, adds massfraction 6% sodium-chlor, soaks 2h, is total to water distillation 3h, and reflux cooling carries out oily water separation, uses anhydrous sodium sulfate drying again.Obtain having the yellowish green transparent flow liquid of aromatic odour.Oil yield 1.1% is that ortho-water is steam distilled more than 2 times.

Embodiment 2

With smelly cypress fruit cleaning in the autumn that gathers, dry, electric crusher is pulverized, and crosses the 30-40 mesh sieve, adds massfraction 2% sodium-chlor, soaks 4h, is total to water distillation 3h, and reflux cooling carries out oily water separation, uses anhydrous sodium sulfate drying again.Obtain having the water white transparency fluxion of aromatic odour.Oil yield 2.1%, ortho-water vapor distillation oil yield improves 35%.

Claims

One kind altogether water distill smelly cypress branches and leaves, fruit, extract the technique of smelly cypress essential oil, it is characterized in that smelly cypress raw material is cleaned, dry in the shade, crushing screening places in the matrass, adding 7-9 water and massfraction doubly is the NaCl of 1%-6%, soaks 2h.Connect the wet distillation device, temperature is 100 ℃--120 ℃, leave standstill 0.5-2h after extracting 2.0-4.0h, through oil, moisture from, reading is emitted distillate, obtains smelly cypress essential oil.
2. according to the method described in the right 1, it is characterized by smelly cypress branches and leaves, fruit was pulverized the 30-40 mesh sieve.
3. according to the method described in the right 1, it is characterized by adding sodium-chlor massfraction is 2%-6%.
4. according to the method described in the right 1, it is characterized by 7-9 times of water of adding pulverised material.
5. according to the method described in the right 1, it is characterized by soak time is 2-4 hour.
6. according to the method described in the right 1, it is characterized by distillation temperature is 100-120 ℃.
7. according to the method described in the right 1, it is characterized by distillation time is 2-4 hour.
8. according to the method described in the right 1, it is characterized by the determination of volatile oil device, the heating of temperature controllable electric mantle.