CN1268726C - Technology of extracting rose oil by using two step variable distillation type back water distillation method - Google Patents
Technology of extracting rose oil by using two step variable distillation type back water distillation method Download PDFInfo
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- CN1268726C CN1268726C CN 200410073336 CN200410073336A CN1268726C CN 1268726 C CN1268726 C CN 1268726C CN 200410073336 CN200410073336 CN 200410073336 CN 200410073336 A CN200410073336 A CN 200410073336A CN 1268726 C CN1268726 C CN 1268726C
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Abstract
The present invention discloses a technology for extracting rose oil with a two-step water-return change distillation method, which comprises: pickled rose flowers is placed in a distillation tank, and water vapor is led in the distillation tank for heating the pickled rose flowers; when the temperature of flower water reaches 65 to 75 DEG C, condensed water is filled in the distillation tank; when boiled, the flower water is timed; the flower water is distilled for 3 hours at the distillation speed of 125 L/h, the temperature of the condensed water is kept at 35 to 37 DEG C; then the distillation speed is increased to 250 L/h, and the flower water is distilled again for 1 hour; the temperature of the condensed water can be moderately increased to about 40 DEG C; refined oil is separated at any time in the process of distillation, and a finished product is prepared after the materials are mixed. According to the multicomponent characteristic of rose oil, a traditional distillation process is divided into two stages by the present invention, wherein low distillation speed is adopted in the first stage, and high distillation speed is adopted in the second stage. Thus, the present invention ensures that high boiling components of a rose flower are largely extracted. Refined oil extracted by the technology for extracting rose oil with a two-step water-return change distillation method, which is provided by the present invention, has good effect and high quality, and achieves the requirements of ISO9842 standards and Bulgaria delta C653 standards. The present invention is suitable for extracting other rose oil varieties with a water vapor distillation method.
Description
Technical field
The present invention relates to the preparation of rose oil, relate to the water distillation method and extract the rose oil extracting method, definite says, be the technology that a kind of two step variable distillation type back water distillation method extracts rose oil, the present invention is divided into different two kinds of distillation speeds with traditional rose oil distillation method still-process, thus more the extracting of composition that can the Rose boiling point is higher.
Background technology
Flos Rosae Rugosae quintessence oil is a kind of special natural perfume, and its conventional preparation technology adopts steam distillation production." Ka Zanleke " rose is the main breed of Bulgarian Rose, and the Qin Wei rose is the offspring of this kind, belongs to pink damask rose (Rosa damascena Mill), and the cultivation history in more than 600 year is arranged.Its oil is pure, gives off a strong fragrance, and steady quality is one of best rose oil in the world
[1]The weinan tried to plant in 1985, beginning commerial growing in 1993, existing claim " (Qinwei rose)
[2,3]Cultivating the result for many years shows: the Qin Wei rose has not only kept the variety and quality of former Ka Zanleke rose, and adapt to the ecological condition in Shaanxi fully, it is healthy and vigorous to grow, flower amount big (a year per hectare is on average produced fresh flower 6900kg in the period of 7), oil length height (industrial oil yield 0.42 ‰).Now in the Weinan of Guanzhong, Shangzhou commerial growing of Shan Nan, become the main breed of Shaanxi rose
[2,4]For this reason, the applicant has carried out Qin Wei Flos Rosae Rugosae quintessence oil Research on processing technology on the basis that the success of above-mentioned area is cultivated.
The quality of Flos Rosae Rugosae quintessence oil not only depends on kind, ecological condition, and with complete processing certain relation is arranged.Present production technique abstraction process distillation speed is single, there is not the index of quantification, random big, essential oil quality instability, the present rose oil of China extracts and does not also have unified standard in addition, and the distil process of routine is not done further further investigation, and in Bulgaria, rose oil processing is not only with a long history, and has the certain height skill
[5]
The applicant retrieves in research process below with reference to document:
[1] LIWY (Li Wanying), WANGWZ (Wang Wenzhong).The rose of our country[C]。Plant introduction and acclimatization (plant introduction domestication collected papers), 3:1983.85-91(in Chinese)。
[2] Zhang Rui, Wei Anzhi etc.Qin Wei Flos Rosae Rugosae quintessence oil research [J].The northwest Botany Gazette, 2003,23 (11): 1991～1993.
[3] Zhang Rui, Wei Anzhi etc.3 kinds of different flavor Flos Rosae Rugosae quintessence oil The Characteristic Study [J].The northwest Botany Gazette, 2003,23 (10): 1768～1771.
[4] Zhang Rui, Wei Anzhi etc.Qin Wei rose and cultivation processing [J] thereof.Fragrance flavor and cosmetic, 2003,5:13-15.
[5] Zhang Cheng once edited. natural perfume handbook [M], Beijing: light industry press, 1989:281-283.
[6] yellow insighted writing. perfume oil chemistry [M], Shanghai: Shanghai science tech publishing house, 1959:122-123.
Summary of the invention
Defective or deficiency at above-mentioned conventional rose oil steam distillation existence, the object of the present invention is to provide a kind of two step variable distillation type back water distillation method to extract the technology of rose oil, the present invention is according to the multicomponent characteristics of rose oil, traditional still-process is divided into two sections, adopt different distillation speeds respectively, more the extracting of composition that can the Rose boiling point is higher.
Realize that the technical solution that above-mentioned purpose is taked is, two step variable distillation type back water distillation method extracts the technology of rose oil, it is characterized in that, comprises the following steps:
1) fresh rose flower of plucking is spread in the place, cool place, and in time adopt 20% salt salt marsh to be stored in the encloses container;
2) fresh rose flower that salt marsh was handled, in the retort of packing into, and with routine cleaning water or the distillate of adding of 4 multiple proportions of flower;
3) airtight retort is fed steam heating, open water of condensation when the flower water temp reaches 70 ± 5 ℃;
When 4) Hua Shui comes to life, adopt the distillation speed of 125L/h to distill, distillation time is 3 hours, and condensed water temperature remains on 35 ℃～37 ℃; Adopt the distillation speed of 250L/h then, continue distillation 1 hour, condensed water temperature remains on 40 ℃; When Hua Shui comes to life, adopt lower distillation speed to distill, distillation time is 2～3 hours, and condensed water temperature remains on 35 ℃～37 ℃; Adopt higher distillation speed to continue distillation 1～2 hour then, condensed water temperature remains on 40 ℃;
5) in still-process, constantly carry out oily water separation, and take out that essential oil is stored in Glass Containers or, make with extra care after distillation is all over and to obtain finished product not by in the essential oil dissolved container.
Two step variable distillation type back water distillation method of the present invention extracts the technology of rose oil, show according to the extraction to the Qin Wei Flos Rosae Rugosae quintessence oil: it is respond well to adopt two step variable distillation type backwater water distillation method technology to extract the Qin Wei Flos Rosae Rugosae quintessence oil, essential oil quality height has reached ISO9842 and Б А С 653 standard-requireds.Technology of the present invention is suitable for adopting steam distillation to extract other rose for oil kind.
Description of drawings
Fig. 1 is preparation technology's schema of the present invention;
Fig. 2 is the processing units synoptic diagram that preparation technology uses;
Fig. 3 is a Qin Wei Flos Rosae Rugosae quintessence oil gas chromatogram.
The embodiment that provides below in conjunction with accompanying drawing and contriver is described in further detail the present invention.
Embodiment
Kind: Qin Wei rose (Rosa damascene Miller).
1 fresh flower collection, preservation and processing units
1.1 fresh flower collection and preservation
1.1.1 fresh flower collection
Before 10 o'clock every mornings of florescence, open and semi-open flower taken take back source mill into cage and preserve processing.
1.1.2 fresh flower is preserved
Fresh rose flower mixed with 20% salt and stir and put into airtight container and preserve.
1.2 processing units
The Rose essential oil extracts and adopts production unit shown in Figure 3, this equipment is the stainless steel distiller that designs voluntarily, horizontal condensation, backwater distillation, the about 3000L of volume, each retortable Rose 500kg.
2 complete processings
2.1 technical process
On the basis of repetition test, found out the method that a cover lowly earlier heats up in a steamer, the back height heats up in a steamer backwater distillation Rose essential oil in the water, comparable single conventional distillation improves 27%.Be that a production technique is simple, be easy to grasp effective novel process (table 1).Its production process is referring to shown in Figure 1:
2.2 key points for operation
The salt marsh rose is put into retort, feed the water vapor heating, when the flower water temp reaches 70 ℃ of left and right sides, open water of condensation, timing when coming to life, with low distillation speed distillation 3h, condensed water temperature keeps 35～37 ℃ earlier; Appropriateness increases distillation speed and continues distillation 1h then, and condensed water temperature can appropriateness be brought up to about 40 ℃, and condensed water temperature remains on 40 ℃.In still-process, separate essential oil at any time, be finished product after the mixing.
2.3 optimal processing parameter
| Essential oil yield, outward appearance and fragrance are relatively under table 1 different condition | |||||
| Sequence number | Material quantity is (in fresh flower, kg) | The distillation mode | Oil offtake (g) | Oil yield (‰) | Outward appearance and fragrance |
| 1 | 500 | Routine is heated up in a steamer fast 4h | 165 | 0.33 | Weak yellow liquid, rose feature flavor, but wax is on the low side. |
| 2 | 500 | Higherly heat up in a steamer fast 4h | 310 | 0.62 | Yellow thickness body has the boiling peculiar smell. |
| 3 | 500 | Lowly heat up in a steamer fast 2h, higherly heat up in a steamer fast 2h | 240 | 0.48 | Weak yellow liquid, slightly boiling peculiar smell |
| 4 | 500 | Lowly heat up in a steamer fast 3h, higherly heat up in a steamer fast 1h | 210 | 0.42 | Weak yellow liquid, rose feature flavor. |
| Annotate: routine is heated up in a steamer speed=200L/h, the higher speed=250L/h that heats up in a steamer, the low speed=125L/h that heats up in a steamer | |||||
20% salt marsh is preserved 1～25d be advisable (table 2).Flower: water=1: 4 (table 3).Conventional distillation speed (200L/h) 3h, higher distillation speed (250L/h) 1h.
Embodiment:
1. salt marsh is preserved the Rose 500kg (in fresh flower) of 1～25d, in the extractor 1 of packing into (referring to Fig. 2), added 2000kg water, covered and enclosed.
2. feed steam and heat, when treating that temperature rises to 70 ℃ of left and right sides, open water of condensation and cool off.
3. when seething with excitement fully, adopt 125L/h to heat up in a steamer speed earlier, distilled 3 hours, adopt 250L/h to heat up in a steamer speed then, distilled about 1 hour, finish distillation.
4. in still-process, constantly separate essential oil, merge the gained essential oil, refining getting final product.
5. adopt the Flos Rosae Rugosae quintessence oil of this law production, according to ISO 9842:1991 standard detection, every index is qualified.
Fresh flower inlet 2 and vapour inlet 3 are arranged on the extractor 1, and the bottom of extractor has snifting valve 4, and slag-drip opening 5 is arranged at the bottom, and the upper end of its extractor connects condenser 6, and is communicated with by return line 7 and oil trap 8, and an end of condenser 6 is connected with oil trap 8; Get hydraulic fluid port 9 on the oil trap 8, also have water inlet 10 and water outlet 11 on the condenser.
| The different salt marsh times of table 2 are to the influence of essential oil yield | ||||
| Fresh flower amount (kg) | The salt marsh time | Distil process | Get oil mass (g) | Oil yield (‰) |
| 500 | Straight run distillation | Two steps became the method for heating up in a steamer | 190 | 0.38 |
| 500 | Salt marsh 1d | 205 | 0.41 | |
| 500 | Salt marsh 5d | 210 | 0.42 | |
| 500 | Salt marsh 25d | 205 | 0.41 | |
| 500 | Salt marsh 30d | 180 | 0.36 | |
| The do not suit influence of water comparison essential oil yield of table 3 | |||||
| Material quantity (kg) 500 500 500 | Amount of water (kg) 1,500 2,000 2500 | Flower: water 1: 31: 41: 5 | Distillation time 4h 4h 4h | Oil yield (‰) 0.36 0.42 0.39 | Evaluation temperature rises fast, have caking to be uniformly dispersed the temperature rising slowly, energy consumption increases |
3 product quality analysis
Flos Rosae Rugosae quintessence oil is a weak yellow liquid, and after tested, it has reached international standard ISO9842 and Bulgarian standard Б Д С 653 requirements about quality, sees table 4 for details.
| Table 4 Qin Wei Flos Rosae Rugosae quintessence oil index | |||
| Project | The Qin Wei Flos Rosae Rugosae quintessence oil | ISO9842 | БДС653 |
| Outward appearance | Liquid, | Liquid, more or less crystallization | Liquid, more or less crystallization |
| Color | Faint yellow | Faint yellow | Faint yellow |
| Fragrance | Natural Rose Essentielle is arranged, fragrance exquisiteness, soft, elegant | The feature Muscat Hamburg | The feature Muscat Hamburg |
| 20/20 ℃ of relative density | 0.8593 | 0.848-0.862 | 0.848-0.861 |
| 20 ℃ of refractive indexs | 1.4610 | 1.4530-1.4640 | 1.4530-1.4640 |
| 20 ℃ of specific rotatioies | -4.2° | -5°-2° | -2.2-4.6° |
| Congealing point (℃) | 21.2 | About 20 | 16.5-23 |
| Ester value | 20.0 | 7.5-23.5 | 7.3-17.1 |
| Ester value after the acetylize | 226.2 | 204-231 | 202.6-224.8 |
With capillary gas chromatography the Qin Wei Chemical Components of Rose Essential is analyzed, isolated 115 components altogether, require to have detected the position and the content (Fig. 3) of 15 kinds of main components according to ISO 9842, its position and standard diagram comparing result are in full accord.As can be seen from Table 5, geraniol (Citronellol), vernol (Nerol), 3 kinds of main component content of Geraniol (Geraniol) of ISO 9842 regulations, the Qin Wei Flos Rosae Rugosae quintessence oil is all within scope.Phenylethyl alcohol (Phenylethyl alcohol) is water-soluble extremely strong composition, and the rose oil of various places differs greatly, and this material of Qin Wei Flos Rosae Rugosae quintessence oil that this experiment records is 1.03%, though be lower than the regulation of ISO 8942, consistent with the regulation of Б Д С 653.
Rose oil contains solid hydrocarbon compound, is called Si Diluoboting (stearoptene), the popular name stearoptene
[6]Main component is n-C
17+ C
19+ C
21+ C
23, the content difference is bigger, and is subjected to multiple factor affecting, and as then weather, degree that the flowers are in blossom puts and the influence of complete processing, ISO 9842 does not stipulate.Composition requirement by Б Д С 653 regulations is 14%～33%, and the content of Qin Wei Flos Rosae Rugosae quintessence oil is 15.7%, meets the requirements.
| Table 5 Qin Wei Flos Rosae Rugosae quintessence oil main chemical | ||||
| Measure number | The compound title | Relative content (%) | Standard-required | |
| ISO 9842(％) | БДС653(％) | |||
| 1 | Ethanol | 0.037 | —— | —— |
| 2 | The cis-trans rose oxide | 0.1067 | —— | —— |
| 3 | Phantol | 1.3223 | —— | —— |
| 4 | Geraniol | 34.65 | 34～44 | 17～37 |
| 5 | Vernol | 9.77 | 6～9 | 5～16 |
| 6 | Geraniol | 16.80 | 12～18 | 12～27 |
| 7 | Phenylethyl alcohol | 1.03 | ～2 | ～1 |
| 8 | Carbon-19 alkane n-C 19 | 10.75 | —— | n-C 17+C 19+C 21+C 23 |
| 9 | Carbon-19 alkene n-C 19 | 0.01 | —— | 14～33 |
| 10 | The cloves methyl ether | 2.38 | —— | |
| 11 | Carbon-20 alkane n-C 20 | 0.87 | —— | |
| 12 | Carbon-20 alkene n-C 20 | 0.14 | —— | |
| 13 | Carbon-21 alkane n-C 21 | 3.86 | —— | |
| 14 | Carbon-21 alkene n-C 21 | 0.07 | —— | |
| 15 | Eugenol | 0.81 | —— | |
Conclusion
Two step variable distillation type backwater method distillation extraction Flos Rosae Rugosae quintessence oil technology of the present invention, when not increasing distillation time, industrial oil yield improves 27% than the normal conventional distillation method.And essential oil quality height, about index has reached ISO9842 and Б Д С 653 requirements.
The two step variable distillation type back water distillation method that the present invention adopts extracts Flos Rosae Rugosae quintessence oil technology optimum producting condition: preserve 1-25d with 20% salt salt marsh; The Hua Shui ratio is 1: 4; Distillation time 4h wherein earlier with 125L/h distillation speed distillation 3h, continues distillation 1h with the 250L/h distillation speed again, and after the oily water separation, dehydration is refining can to obtain quality products.
Claims (2)
1. two step variable distillation type back water distillation method extracts the technology of rose oil, it is characterized in that, comprises the following steps:
1) fresh rose flower of plucking is spread in the place, cool place, and in time adopt 20% salt salt marsh to be stored in the encloses container;
2) fresh rose flower that salt marsh was handled, in the retort of packing into, and with routine cleaning water or the distillate of adding of 4 multiple proportions of flower;
3) airtight retort is fed steam heating, open water of condensation when the flower water temp reaches 70 ± 5 ℃;
When 4) Hua Shui comes to life, adopt the distillation speed of 125L/h to distill, distillation time is 3 hours, and condensed water temperature remains on 35 ℃～37 ℃; Adopt the distillation speed of 250L/h then, continue distillation 1 hour, condensed water temperature remains on 40 ℃;
5) in still-process, constantly carry out oily water separation, and take out that essential oil is stored in Glass Containers or, make with extra care after distillation is all over and to obtain finished product not by in the essential oil dissolved container.
2. technology as claimed in claim 1 is characterized in that, the salt marsh shelf time of described fresh rose flower is 1～25 day, and the Hua Shui ratio is 1: 4.
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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 |
| CN102851121A (en) * | 2012-10-18 | 2013-01-02 | 云南悦馨香料科技有限公司 | Preparation method of rose oil |
| 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 |
| CN108102785A (en) * | 2018-01-04 | 2018-06-01 | 湖北瑞晟生物有限责任公司 | A kind of extraction of Rosa Damascana and preparation method |
| CN109554229A (en) * | 2018-11-19 | 2019-04-02 | 江西省林业科学院 | A kind of method of extraction of essential oil and device of high-content linalool |
| CN111363626B (en) * | 2020-01-19 | 2024-01-26 | 宁波市妇女儿童医院 | Holographic rose essential oil and green preparation method thereof |
| CN111778108A (en) * | 2020-07-05 | 2020-10-16 | 王瑞雪 | Rose essential oil extraction production system and extraction production method |
| CN112662476A (en) * | 2020-12-30 | 2021-04-16 | 小金县夹金山清多香野生资源开发有限责任公司 | Extraction method of rose essential oil with high oil yield |
| CN113293059A (en) * | 2021-06-04 | 2021-08-24 | 成都全美生物科技有限公司 | Method for separating rhodinol from rose essential oil |
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