CN1648223A - Rose oil and its producing process - Google Patents
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Abstract
The present invention relates to rose oil and its production process. The present invention uses rose of separated and screened Rosa Damascena Mill variety as material, and the rose oil contains cephrol 18-39 wt%, nerol 5-14 wt%, geraniol 14-29 wt%, paraffin 16-20 wt%, and phenylethanol <3.0 wt%. The present invention has high paraffin content and low phenylethanol content and scent lasting time as long as 48 hr, and features the sum of total geraniol and nerol content higher than cephrol content and thus special quality and scent. The present invention provides rose oil producing process with high production capacity, short processing time and rose oil yield as high as 0.035-0.050 %.
Description
Technical field
The present invention relates to a kind of rose oil and production technique thereof, belong to plant extract volatile oil field.
Background technology
Rose oil, Rose oil, yellow or orange transparent flow liquid refine from Rose and make refractive index 1.4568～1.4776, density 0.8478～0.9140, acid number 1.52～5.90, optically-active-4.272～-9.592.Rose oil is used for preparing perfume as the famous and precious spices in the world, also is commonly used for the spice additive of candy, cake, beverage, champagne, and rose oil is also had beautifying face and moistering lotion, an anti-aging effects.In recent years, the market demand of rose oil was ascendant trend year by year.
Rose variety is the principal element of decision rose oil quality.The main chemical compositions of rose is geraniol (rhodinol), Geraniol, vernol, phenylethyl alcohol.The difference of what and proportioning thereof on its chemical composition content of the rose of different varieties, the rose oil fragrance that causes producing has nothing in common with each other, and has produced delicate discrepancy.At present, the rose variety that is used for preparing rose oil mainly contains 4 classes system.Bulgaria and Turkey are the kind systems of pink damask rose (Rosa Damascena Mill) Tujue rose; France is Rosa gallica (Rosa gallica) and rose de mai (rose centifoila); Morocco is the cross-fertilize seed of (Rosa Gallicai) and (Rosa Centifolia); China then is to be main with Chinese rose (RosaChinesesa), comprises bitter water rose, Pingyin rose.Bulgarian and osmanli pink damask rose since each aroma substance distribute coordinate, harmony, its fragrance is fresh and sweet, pure, the Rose Essentielle that tool is fresh; And bitter water rose, Pingyin rose are satisfied inadequately on composition proportion, so that fragrance of a flower QI-insufficiency even apparent slightly assorted gas, and bitter water rose oil also contains more 2-dodecane ketone, methyl n-undecyl ketone, 2-tetradecane ketone, 2-pentadecanone, make it to show grease gas [Yu Zhen, Yi Yuanfen, Wu Yu etc., Yunnan plant research, 2002,24 (5), the chemical ingredients of several rose oil and fragrance are relatively].So far, do not see the value that " Geraniol %+ vernol %-geraniol % " in the open report rose oil main component arranged, and the height of this value has determined the quality of rose oil, expert [Ton Witmer Holland, Jan Danil France, Dogen Timer Turkey] think that Geraniol % and vernol % sum are given superior quality of rose oil and fragrance greater than geraniol %.The paraffin composition determines the lasting of rose oil fragrance, and at present, the rose oil fragrance time length commonly used was generally 24～36 hours.
At present, rose oil production mainly is divided into two kinds of extraction process and distillation method.
Extraction process has chemical extraction and carbon dioxide upercritical fluid extraction.Just begin the beginning of this century with contained volatile oil in the chemical solvents extraction plant.On the plant of desire extraction, spoon acetone, sherwood oil or hydrocarbon polymer derivative, obtain the product of newborn white shape.After utilizing alcohol dissolving and double filtration again, just pure volatile oil can have been obtained.But, the volatile oil that obtains of this method residual organic solvent still; Carbon dioxide upercritical fluid extraction is a research focus in recent years, and the process of extraction is to carry out under the supercritical temperature of carbonic acid gas, and the oil that extracts almost is indefective and oilyly itself also not contain any resistates.Shortcoming then is, required pressure is about 200MPa, and cost is very high.
For above-mentioned reasons, for routine is refined senior essential oil, seldom use extraction process, and adopt distillation method mostly.Each big and small rose oil manufacturer of the whole nation has many, but production technique is all relatively backward, and many is to adopt directly fire heating, the distillation of intermittent type water.The Gansu bitter water rose is the most well-known rose oil source of domestic maximum, its produce rose oil process using be: with directly fire heating, the distillation of intermittent type water, 1.2～1.8 cubic metres of steamer volumes, every pot was steamed 5～6 hours, 3 pots of every steamings put together fore-running water (twice of flower amount), and intermittently multiple again distillation once, handle 300～360 kilograms of flower amounts day, this distil process mode is backward in technique, complex operation, and it is few to handle the flower amount, can handle Wan the fresh flower peak period, and cause the fresh flower loss from spoilage, and time-consuming taking a lot of work and the gained rose oil is of poor quality, color is dark, sometimes also be with burning smell [Liu Yuchun, the development and use of rose for oil, Chinese forest-science academy chemistry of forest product chemical institute, 1988.6].The Gansu bitter water rose is owing to use ancient distillation method, and 1 kilogram of rose oil cost is up to more than 30,000 yuan, and oil yield is low, only is 1.8/10000ths～2.4.Overseas utilization " rose for oil " is produced mainly containing of Flos Rosae Rugosae quintessence oil: Bulgaria, France, Turkey, Morocco etc.Bulgarian Rose oil enjoys high reputation in the world, and lasting.It has three distinguishing features: the one, and fragrance is pure, and is strong; The 2nd, constant product quality; The 3rd, former plant is indigenous, and production cost is low.France: distillation legal system essential oil, what generally adopt is 500～10000 liters stainless steel distillation plant, typical batch distillation equipment, two condensers also have susceptor, separator, level of automation is also higher, and a workman can operate 4～6 equipment.Bulgaria uses second distillation equipment, in the recyclable distillate 85～90% of the rose oil total amount, and second distillation device diameter 500mm, the packing tower of the interior cloth Raschig ring of high 4600mm, distillation time is 2～2.5 hours, oil yield is 2.8/10000ths～3.5.And the oil yield of domestic other technology only has 1.8/10000ths～3.0[to open " rose " Chinese agriculture press such as Lu Jian].
Summary of the invention
The object of the present invention is to provide a kind of product of fine quality, fragrance uniqueness, the rose oil of fragrance longer duration; Provide working ability big simultaneously, the rose oil production technique that oil yield is high.
The rose oil that the present invention extracts, its raw material is that selecting for use with big horse scholar rose (Rosa Damascena Mill) is original seed, through separating, screen resulting rose variety, the rose oil main component and the weight percent that make are counted with the rose oil total amount: geraniol Citronellol:18%～39%; Vernol Nerol:5%～14%; Geraniol Geraniol:14%～29%; Paraffin paraffin:16%-20%; Phenylethyl alcohol Phen-ernyl alcohol:＜3.0%; Wherein, Geraniol %+ vernol %-geraniol %=8.68%～15.31%.
Further, rose oil main component and weight percent are counted with the rose oil total amount: geraniol 20%～30%, vernol 10%～14%, Geraniol 20%～28%, paraffin: 16%-20%.Phenylethyl alcohol＜3%; Wherein, Geraniol %+ vernol %-geraniol %=11%～15.31%.
Further, the weight percent of rose oil main component geraniol, vernol, Geraniol, paraffin, phenylethyl alcohol is counted with the rose oil total amount: 25.28%:11.73%:24.69%:19.7%:1.49%.
Rose oil production technique provided by the invention may further comprise the steps:
The harvesting of a, Rose;
B, still kettle feed intake, and the weight ratio of Rose and water or oil-water mixture is 1: 1～4;
Feeding pressure in c, the still kettle is 4kg/cm
2Water vapor, be warming up to 130～142 ℃, heat-up rate is 2～5 ℃/min, carries out single flash, the temperature during distillation is 130～142 ℃, vapour pressure is 4～8kg/cm
2Mixed steam is collected phlegma I after condenser condenses, stop distillation after 2 hours, and single flash still discharging flower slag prepares to add the flower distillation next time;
Enter water-and-oil separator after d, the phlegma I cooling, collect oil reservoir wherein, get oily A; Remaining oil-water mixture enters distillation tower and carries out second distillation after the separating oil, and the second distillation temperature is: 130～142 ℃, oil-water mixture steam enters the after-condenser condensation, collects phlegma II;
Enter water-and-oil separator after e, the phlegma II cooling, collect oil reservoir wherein, get oily B, remaining mixture is sent to the single flash still and is mixed with fresh flower, recycles;
F, c step gained oil A and e step gained oil B is mixed becomes the finished product.
Wherein, the harvesting of Rose is 5 point～9 point in the morning, preferably plucks desire open flower or petal.
Further, the weight proportion of the described Rose of b step and water or oil-water mixture be preferably 1: 3～4.
Further, the described distillation temperature of c step is preferably: 137 ℃; Intensification degree speed is preferably: 3 ℃/min.
Wherein, temperature was controlled at about 30 ℃ before d step and the described phlegma of e step entered water-and-oil separator.
Wherein, for the first time and oily water separation for the second time be to look handleless cup through glass to separate, oil reservoir surpass place the fuel-displaced litmus mouth looked in the handleless cup the time, open valve, the automatic inflow of oil oil reservoir; When oil reservoir is brought down below fuel-displaced litmus mouth, by the flow of overflowing liquid in the upflow tube of regulating water-and-oil separator, last oil reservoir is risen to look the hydraucone in the handleless cup, flow into oil reservoir, oil is put clean back valve-off, separate and finish.
The rose oil that the present invention extracts is owing to use big horse scholar rose variety, at Xichang particular climate condition and soil cultivation, make it both have the traditional European odor type of big horse scholar rose, have again that disease resistance is strong, wide adaptability and the high characteristics of oil yield, therefore rose oil provided by the invention has its unique advantage.Analyze through censorship, the rose oil Geraniol content that the present invention extracts is slightly higher than Bulgarian national standard, vernol %+ Geraniol %-geraniol % reaches 8.68%, phenylethyl alcohol Phen-ernyl alcohol content is lower simultaneously, paraffin (C19) composition height, the fragrance time length reached more than 48 hours.
Rose oil production technique provided by the invention has following beneficial effect: 1, throughput is big, and every cover day processing Rose reaches 6～8 tons; 2, every still treatment time weak point, 1.5～2 hours promptly intact stills; 3, oil yield improves, and can reach 3.5/10000ths～5.
Below further specify beneficial effect of the present invention by embodiment, but should not be construed as is limitation of the present invention, and the technical scheme that modification, replacement or change realized of every other various ways of being made based on technology basic thought of the present invention all belongs to scope of the present invention.
Embodiment
The preparation of embodiment 1 rose oil of the present invention
The harvesting of Rose: 5 point～9 point in the morning must not have peculiar smell, foreign matter to sneak into.In principle, the same day, flower should be handled in the sky, as not finishing in the place same day, should be kept at freezer, in case temperature is too high, the oil-containing composition of flower volatilizees, and storage temperature should be at 2～3 ℃, and the shelf time is no more than 48 hours, otherwise oil yield can descend greatly.
Single flash:
Rose adds single flash still (3 cubic metres), and about 500 kilograms, add 1500 kilograms of hot water or second distillation liquid then, feeding pressure is 4kg/cm
2Steam taper heating coil to the still, temperature in the kettle rises to 137 ℃ with the heat-up rate of 3 ℃/min from 60 ℃.Steam (being that flower in the still, water mixture produce) enters primary condenser (6 square metres) by pipe connecting, collects the each 600kg of phlegma I, total amount 1200kg, and phlegma I temperature is controlled at about 30 ℃, enters water-and-oil separator and separates.Upper strata oil floats automatically to be looked in the handleless cup (cylindrical glass cover), and the fuel-displaced litmus mouth inflow oil reservoir from separator gets 0.095 kilogram of oily A; Collect the each 600kg of the remaining oil-water mixture of flash liberation, total amount 1200kg changes the once-run distillate storage tank over to, prepares to enter second distillation; The single flash still is stopped the supple of gas or steam, and discharging flower slag prepares to add the flower distillation next time.
Second distillation:
The profit miscellany of a storage tank is squeezed into well heater with pump, flowing into the packing tower shower nozzle after being heated to 60-70 ℃ is sprayed on the filler, contact with the steam of second distillation still, the profit mixing steam that produces enters condenser, get phlegma II, temperature is controlled at about 30 ℃ and flows into water-and-oil separator, carries out oily water separation, gets 0.13 kilogram of oily B; Collect the each 600kg of the remaining oil-water mixture of secondary separation, total amount 1200kg changes secondary distillate storage tank over to, sends to the single flash still and mixes with flower.
With oily A and oily B mixed after evenly 0.225 kilogram of finished product rose oil, oil yield is 4.5/10000ths.
Processed oil send French Robertet to detect, and detected result sees Table 1.
The basic index of rose oil of the present invention all reaches Bulgarian standard as can be seen from Table 1, and Geraniol content is also slightly higher than this standard, and vernol %+ Geraniol %-geraniol % reaches 8.68%, and the content of phenylethyl alcohol only has 1.37% simultaneously.Expert [Ton Witmer Holland, Jan Danil France, Dogen Timer Turkey] think, vernol % and Geraniol % sum make rose oil of the present invention give distinguished interesting quality and fragrance greater than this characteristic of geraniol %, are a kind of brand-new rose oil.Paraffin is the deciding factor that makes rose oil fragrance longer duration, Bulgaria's standard paraffin composition that do not appear in the newspapers, its composition may be very low, and paraffin composition of the present invention is up to 19.0%, the fragrance time length reached more than 48 hours, and external product was generally 24～36 hours.More sea nurse rose trading company overall evaluation oil quality is very good, really belongs to branded oil, is independent of Bulgaria and osmanli product, can be used to develop new perfume and makeup.
Table 1 processed oil send French detected result
The Bulgarian standard of main chemical compositions detected result (w%) (w%)
Geraniol % 28.79% 20%～37%
Vernol % 9.96% 6%～12%
Geraniol % 27.51% 14%～27%
Phenylethyl alcohol % 1.37%＜3.0%
Paraffin % 19.0%
The preparation of embodiment 2 rose oil of the present invention
The harvesting of Rose: 5 point～9 point in the morning, pluck the petal that not have opening, peculiar smell must not be arranged, foreign matter is sneaked into.
Single flash:
Rose adds single flash still (3 cubic metres), and about 500 kilograms, add 2000 kilograms of hot water or second distillation liquid then, feeding pressure is 4kg/cm
2Steam taper heating coil to the still, temperature in the kettle rises to 137 ℃ with the heat-up rate of 4 ℃/min from 60 ℃.Secondary steam (being that flower in the still, water mixture produce) enters primary condenser (6 square metres) condensation by pipe connecting, reservoir is collected the each 600kg of phlegma I, total amount 1200kg, and phlegma I temperature is controlled at about 30 ℃, enter water-and-oil separator and separate, get 0.075 kilogram of oily A; Collect the each 600kg of the remaining oil-water mixture of flash liberation, total amount 1200kg changes the once-run distillate storage tank over to, prepares to enter second distillation; The single flash still is stopped the supple of gas or steam, and discharging flower slag prepares to add the flower distillation next time.
Second distillation:
The profit miscellany of once-run distillate storage tank is squeezed into well heater with pump, flowing into the packing tower shower nozzle after being heated to 60～70 ℃ is sprayed on the filler, contact with the steam of second distillation still, the profit steam that produces enters condenser, get phlegma II, temperature is controlled at about 30 ℃ and flows into water-and-oil separator, carries out oily water separation, gets 0.17 kilogram of oily B; Collect the each 600kg of the remaining oil-water mixture of secondary separation, total amount 1200kg changes secondary distillate storage tank over to, sends to the single flash still and mixes with flower.
With oily A and the mixed evenly back of oily B packing, get 0.245 kilogram of finished product rose oil, oil yield is 4.9/10000ths.
Send osmanli oil product inspection center to detect the finished product rose oil, as a result table 2:
Table 2 rose oil main component of the present invention analysis report
Standard Beige ﹠ Rose essential oil
Project
Rose oil % of the present invention
The highest % of minimum %
CITRONELLOL geraniol 33.9 37.9 28.9
NEROL vernol 7.2 8.4 13.5
GERANIOL Geraniol 14.6 18.7 25.2
PE ALCOHOL phenylethyl alcohol 1.6 1.8 1.3
Paraffin paraffin (C19) 8.3 10.0 19.7
METHYL?EUGENOL
2.0 3.4 1.5
Methyleugenol
C20 0.7 0.8
C21 1.7 3.6 2.6
EUGENOL oxymethoxyallylbenzene 1.5 1.8 1.3
ETHANOL ethanol 2.6 4.8 0.1
Density density 0.8638 0.8705 0.8702
Refraction?Index
1.4560 1.4618 1.4654
Refractive index
Rotation Index specific rotation-4.44-3.85-3.80
The sense of smell report of rose oil of the present invention:
Compare with its essential oil of Tu Er of standard, rose oil of the present invention has the feature of branch/bud point, and sweet taste is less, is the high reason of level owing to kind vernol Nerol and Geraniol Geraniol.As can be seen from Table 2, vernol %+ Geraniol %-geraniol % reaches 9.8%, and the Beige ﹠ Rose essential oil can not reach far away.The level of compositions such as phenylethyl alcohol, methyleugenol, oxymethoxyallylbenzene, ethanol is lower simultaneously, gives rose oil fine quality of the present invention; Owing to high-caliber paraffin (C19), help the lasting stability of fragrance in addition, the time length reached more than 48 hours.Simultaneously because the low characteristics of contents level that wet distillation technology is given ethanol in the rose oil of the present invention.
In a word, rose oil of the present invention is best in quality, and vernol %+ Geraniol %～geraniol % reaches 9.8%, and this has given should special, interesting quality of oil and fragrance; And because paraffin composition height, the fragrance time length reached more than 48 hours, was a kind of new rose oil.In addition, it is big that rose oil production technique provided by the invention has throughput, the characteristics that oil yield is high, and oil yield is up to 4.9/10000ths.
Claims (10)
1, it is original seed that a kind of rose oil, its raw material are selected for use with pink damask rose (Rosa Damascena Mill), through separating, screen the flower of resulting rose variety; Rose oil main component and weight percent are counted with the rose oil total amount: geraniol: 18%～39%; Vernol: 5%～14%; Geraniol: 14%～29%; Paraffin: 16%-20%; Phenylethyl alcohol:＜3.0%; Wherein, Geraniol %+ vernol %-geraniol %=8.68%～15.31%.
2, according to the described rose oil of claim 1, it is characterized in that: rose oil main component and weight percent are counted with the rose oil total amount: geraniol: 20%～30%; Vernol: 10%～14%; Geraniol: 20%～29%; Paraffin: 16%-20%, phenylethyl alcohol:＜1.5; Wherein, Geraniol %+ vernol %-geraniol %=11%～15.31%.
3, according to the described rose oil of claim 1, it is characterized in that: rose oil main component and weight percent are counted with the rose oil total amount: geraniol 25.28%, vernol 11.73%, Geraniol 24.69%, paraffin 19.7%, phenylethyl alcohol 1.49%.
4, a kind of preparation method who prepares the described rose oil of claim 1, it is characterized in that: it may further comprise the steps:
The harvesting of a, Rose;
B, still kettle feed intake, and the weight ratio of Rose and water or oil-water mixture is 1: 1～4;
Feeding pressure in c, the still kettle is 3～5kg/cm
2Water vapor, be warming up to 130～142 ℃ with the heat-up rate of 2～5 ℃/min, carry out single flash; Temperature during distillation is 130～142 ℃, and vapour pressure is 4～8kg/cm
2Mixed steam is collected phlegma I after condenser condenses, stopped distillation in 2 hours, and still kettle discharging flower slag prepares to add the flower distillation next time;
Enter water-and-oil separator after d, the phlegma I cooling, collect oil reservoir wherein, get oily A; Remaining oil-water mixture enters distillation tower and carries out second distillation after the separating oil, and the second distillation temperature is: 130～142 ℃, oil-water mixture steam enters the after-condenser condensation, collects phlegma II;
Enter water-and-oil separator after e, the phlegma II cooling, collect oil reservoir wherein, get oily B, remaining mixture is sent to the single flash still and is mixed with fresh flower, recycles;
F, c step gained oil A and e step gained oil B is mixed becomes the finished product.
5, according to the described preparation method of claim 4, it is characterized in that: the harvesting of Rose is 5 point～9 point in the morning, plucks desire open flower or petal.
6, according to the described preparation method of claim 4, it is characterized in that: the weight proportion of the described Rose of step b and water or oil-water mixture is 1: 3～4.
7, according to the described preparation method of claim 4, it is characterized in that: the described heat-up rate of step c is: 3 ℃/min, described distillation temperature is: 137 ℃.
8, according to the described preparation method of claim 4, it is characterized in that: the temperature that the described phlegma I of steps d enters before the water-and-oil separator is controlled at 30 ℃.
9, according to the described preparation method of claim 4, it is characterized in that: the temperature that the described phlegma II of step e enters before the water-and-oil separator is controlled at 30 ℃.
10, according to Claim 8 or 9 described preparation methods, it is characterized in that: oily water separation is to look handleless cup through the glass of water-and-oil separator to separate.
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| CN101353611A (en) * | 2008-08-21 | 2009-01-28 | 许向梅 | Rose essential oil and rose pure dew extraction equipment |
| CN101157882B (en) * | 2007-11-16 | 2010-06-23 | 牛江林 | Method for abstracting manchu rose oil and dew from manchu rose flowers |
| CN103897807A (en) * | 2014-04-24 | 2014-07-02 | 四川银谷玫瑰科技有限公司 | Method for extracting rose essential oil |
| CN105249476A (en) * | 2015-11-13 | 2016-01-20 | 合肥金源生物科技有限公司 | Rose water extract and preparation method thereof |
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| CN101157882B (en) * | 2007-11-16 | 2010-06-23 | 牛江林 | Method for abstracting manchu rose oil and dew from manchu rose flowers |
| CN101353611A (en) * | 2008-08-21 | 2009-01-28 | 许向梅 | Rose essential oil and rose pure dew extraction equipment |
| CN103897807A (en) * | 2014-04-24 | 2014-07-02 | 四川银谷玫瑰科技有限公司 | Method for extracting rose essential oil |
| CN105249476A (en) * | 2015-11-13 | 2016-01-20 | 合肥金源生物科技有限公司 | Rose water extract and preparation method thereof |
| CN105249476B (en) * | 2015-11-13 | 2018-04-06 | 合肥金源生物科技有限公司 | Rose water extract and preparation method thereof |
| CN105779133A (en) * | 2016-05-26 | 2016-07-20 | 陕西恒芳玫瑰开发有限公司 | Stage extraction method for rose essential oil |
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