阅读说明：本技术 一种玫瑰精油香膏的制备方法、玫瑰精油及其生产方法和应用 (Preparation method of rose essential oil balm, rose essential oil and production method and application of rose essential oil ) 是由 刘红 邵士俊 于 2019-10-22 设计创作，主要内容包括：本发明提供了一种玫瑰精油香膏的制备方法、玫瑰精油及其生产方法和应用,属于玫瑰加工技术领域。玫瑰精油香膏的制备方法,新鲜玫瑰鲜花和萃取溶剂混合,避光条件下进行亚临界萃取,去除所述萃取液中萃取溶剂得玫瑰精油香膏。玫瑰精油的生产方法,将制备的玫瑰精油香膏置于氮气循环气提装置的物料罐中,设置物料罐1.5～2kPa、60～80℃,氮气罐中氮气的压力2～4.5kPa,300～350℃,将氮气输入至物料罐中进行汽提；汽提物经过冷凝收集得到玫瑰精油。本发明通过亚临界萃取技术与氮气循环气提技术相结合,不但生产过程中无废水产生,而且能耗低、无污染、成本低,易于工业化生产；同时还具有玫瑰精油提取率高的特点。(The invention provides a preparation method of rose essential oil balm, rose essential oil, a production method and application thereof, and belongs to the technical field of rose processing. The preparation method of the rose essential oil balm comprises the steps of mixing fresh rose flowers with an extraction solvent, carrying out subcritical extraction under the condition of keeping out of the sun, and removing the extraction solvent in the extraction liquid to obtain the rose essential oil balm. The production method of the rose essential oil comprises the steps of placing the prepared rose essential oil balm into a material tank of a nitrogen circulating air stripping device, setting the material tank to be 1.5-2 kPa and 60-80 ℃, setting the pressure of nitrogen in a nitrogen tank to be 2-4.5 kPa and 300-350 ℃, and inputting the nitrogen into the material tank for steam stripping; condensing the stripped substance to obtain rose essential oil. By combining the subcritical extraction technology and the nitrogen circulating gas stripping technology, the method has the advantages of no waste water generation in the production process, low energy consumption, no pollution, low cost and easy industrial production; meanwhile, the rose essential oil has the characteristic of high extraction rate.)

1. A preparation method of rose essential oil balm comprises the following steps:

fresh rose flowers and extraction solvent were mixed in a 1 g: mixing 1-3 ml of the rose essential oil and the rose essential oil, performing subcritical extraction under a dark condition, collecting extract liquor, and removing an extraction solvent in the extract liquor to obtain the rose essential oil balm.

2. The production method according to claim 1, wherein the extraction solvent is one of propane, butane and tetrafluoroethane.

3. The preparation method according to claim 1, wherein the temperature of the subcritical extraction is 40-50 ℃, the pressure of the subcritical extraction is 0.40-0.50 MPa, the number of times of the subcritical extraction is 2-4, and the time of each extraction is 30-60 min.

4. The production method of the rose essential oil is characterized by comprising the following steps:

placing the rose essential oil balm prepared by the preparation method of any one of claims 1 to 3 in a material tank of a nitrogen circulating air stripping device, setting the pressure of the material tank to be 1.5 to 2kPa and the temperature to be 60 to 80 ℃, setting the pressure of nitrogen in a nitrogen tank to be 2 to 4.5kPa and the temperature to be 300 to 350 ℃, and then inputting the nitrogen into the material tank for steam stripping; and condensing and collecting the obtained stripping matter to obtain the rose essential oil.

5. The production method according to claim 4, wherein the pressure in the material tank is 1.8kPa, and the temperature in the material tank is 70 ℃.

6. The production method according to claim 4 or 5, wherein the pressure of the nitrogen gas in the nitrogen gas tank is 3kPa, and the temperature of the nitrogen gas in the nitrogen gas tank is 320 ℃.

7. The production method according to claim 4, wherein after the end of the stripping, the residue of the rose essential oil fragrance is collected in a heavy component collection tank, and the nitrogen gas is pumped into the nitrogen gas tank through a vacuum pump.

8. The rose essential oil obtained by the production method according to any one of claims 4 to 7, which is characterized by comprising the following components in percentage by mass: 40 to 50 percent of citronellol, 2 to 5.5 percent of nerol, 6 to 18 percent of geraniol, 0.45 to 3 percent of beta-phenethyl alcohol, 0.7 to 3 percent of heptadecane, 0.5 to 2 percent of nonadecane, 0.6 to 2 percent of heneicosane, 0.6 to 2 percent of tricosane, 2 to 3.5 percent of farnesol, 1 to 3.5 percent of linalool and 0.7 to 1 percent of eugenol; also contains trace components with the fragrance and quality of rose essential oil, including rose oxide, neryl oxide, rose furan and beta-ionone.

9. The rose essential oil according to claim 8, wherein the density of the rose essential oil is 0.85 to 0.93, the refractive index is 1.468 to 1.480, and the ester number is 18 to 24 at 20 ℃.

10. Use of the rose essential oil according to claim 8 or 9 in cosmetics or daily necessities.

Technical Field

The invention belongs to the technical field of rose processing, and particularly relates to a preparation method of rose essential oil balm, rose essential oil, a production method and application of the rose essential oil.

Background

Rose (roses) is a precious natural spice plant belonging to the rosaceae, rosaceous and rosaceous genera. The rose has a history of more than two thousand and five hundred years in China, has various varieties and is widely distributed in Shandong, Gansu, Xinjiang, Beijing, Shanxi, Liaoning, Shaanxi and other places, wherein the Gansu rose and the Shandong Pingyin county rose are the most famous. The rose is one of four rose strains in China, belongs to the Rosaceae, is a natural hybrid of the rosa canina and the traditional rose in China, and is a rare plateau selenium-rich rose variety in the world.

The rose essential oil or rose extract is an active component extracted from rose of Rosa of Rosaceae, is colorless or yellow liquid with rose fragrance, and is called liquid gold. Rose essential oil is one of the most widely used spices in the world nowadays, and is mainly used for blending fragrance in cosmetics, food, pharmacy and high-grade cigarette production. Meanwhile, the rose essential oil has the effects of bacteriostasis, antioxidation, health care, beauty treatment, emotion regulation and the like.

The traditional rose extract production method mainly comprises a solvent extraction method, a supercritical carbon dioxide extraction method and the like. The solvent extraction method comprises soaking rose raw material with solvent to dissolve oil and fat in the solvent to form mixed oil, separating the mixed oil from solid residue, and evaporating and separating the mixture by using the difference of boiling points of the solvent and the oil and fat, wherein the oil and fat product is called rose extract. The main component of rose extract is a compound with fragrance, but also contains alkane, fatty acid methyl ester, terpene compound and pigment. To obtain a high quality product, a post-treatment step is required to produce the rose essential oil. In addition, the extract contains fatty acid methyl esters and diterpenoid compounds and other lipophilic compounds with high molecular weight. Because a large amount of wax covered on the surface of fresh flowers enters the extract in the leaching process, the wax content in the extract is higher and reaches 40 to 60 percent by weight, and the obtained rose extract is yellow, orange yellow or brown paste or wax solid and can be dissolved in ethanol and most of grease.

The basic steps of the industrial production of the extract at the present stage are solvent leaching, solvent filtration and extract concentration. The extraction method has relatively low temperature, and can reduce the loss of pyrolysis and hydrolysis of aromatic oil components, and the obtained rose oil has fragrance close to natural fragrance of flos Rosae Rugosae. Because the solvent has strong selectivity to the aromatic components in the roses, the main research direction lies in selecting proper solvents, the common solvents for extracting the rose essential oil at the present stage comprise petroleum ether and hexane, a single solvent often cannot extract comprehensive aromatic components, people try to use mixed solvents to exert the corresponding dissolving functions of the solvents on the aromatic components in the roses, so that the aromatic components in the roses can be thoroughly leached by the mixed solvents, and the yield and the flavor quality of the rose oil can be greatly improved. And how to select a proper solvent for extraction and reduce the content of lipid compounds in the rose extract as much as possible is an important problem of extract extraction. The rose extract obtained by extracting the fresh rose flowers with supercritical carbon dioxide has the characteristics of no solvent residue and no peculiar smell, is a pure natural product, and has natural and pure fragrance of the fresh rose flowers. However, the obtained rose extract contains more vegetable wax, and the melting point of part of the vegetable wax is higher, which increases the difficulty for further purification.

Disclosure of Invention

In view of the above, the present invention aims to provide a method for producing a rose essential oil balm, which not only has a low lipid content, but also is easy for industrial production.

The invention also aims to provide a method for producing the rose essential oil based on the rose essential oil balm, which not only has the characteristics of producing high-quality rose essential oil, but also has the characteristics of no wastewater discharge, low energy consumption and low cost.

The invention provides a preparation method of rose essential oil balm, which comprises the following steps:

fresh rose flowers and extraction solvent were mixed in a 1 g: mixing 1-3 ml of the rose essential oil and the rose essential oil, performing subcritical extraction under a dark condition, collecting extract liquor, and removing an extraction solvent in the extract liquor to obtain the rose essential oil balm.

Preferably, the extraction solvent is one of propane, butane and tetrafluoroethane.

Preferably, the temperature of the subcritical extraction is 40-50 ℃, the pressure of the subcritical extraction is 0.40-0.50 MPa, the extraction times of the subcritical extraction are 2-4 times, and the time of each extraction is 30-60 min.

The invention provides a production method of rose essential oil, which comprises the following steps:

placing the rose essential oil balm prepared by the preparation method into a material tank of a nitrogen circulating air stripping device, setting the pressure of the material tank to be 1.5-2 kPa and the temperature to be 60-80 ℃, setting the pressure of nitrogen in a nitrogen tank to be 2-4.5 kPa, and inputting the nitrogen into the material tank for steam stripping after the temperature is 300-350 ℃; and condensing and collecting the obtained stripping matter to obtain the rose essential oil.

Preferably, the pressure in the material tank is 1.8kPa, and the temperature in the material tank is 70 ℃.

Preferably, the pressure of nitrogen in the nitrogen tank is 3kPa, and the temperature of nitrogen in the nitrogen tank is 320 ℃.

Preferably, after the stripping is finished, the residue of the rose essential oil balm is collected into a heavy component collecting tank, and the nitrogen is pumped into the nitrogen tank through a vacuum pump.

The invention provides rose essential oil obtained by the production method, which comprises the following components in percentage by mass: 40 to 50 percent of citronellol, 2 to 5.5 percent of nerol, 6 to 18 percent of geraniol, 0.45 to 3 percent of beta-phenethyl alcohol, 0.7 to 3 percent of heptadecane, 0.5 to 2 percent of nonadecane, 0.6 to 2 percent of heneicosane, 0.6 to 2 percent of tricosane, 2 to 3.5 percent of farnesol, 1 to 3.5 percent of linalool and 0.7 to 1 percent of eugenol; also contains trace components with the fragrance and quality of rose essential oil, including rose oxide, neryl oxide, rose furan and beta-ionone.

Preferably, under the condition of 20 ℃, the density of the rose essential oil is 0.85-0.93, the refractive index is 1.468-1.480, and the ester value is 18-24.

The invention provides application of the rose essential oil in cosmetics or daily necessities.

The invention provides a preparation method of rose essential oil balm, which comprises the following steps: fresh rose flowers and extraction solvent were mixed in a 1 g: mixing 1-3 ml of the rose essential oil and the rose essential oil, performing subcritical extraction under a dark condition, collecting extract liquor, and removing an extraction solvent in the extract liquor to obtain the rose essential oil balm. The invention produces an intermediate product for preparing rose essential oil, namely rose essential oil balm, and the production method adopts a subcritical extraction technology to obtain white or colorless volatile viscous paste rose essential oil balm which has the special fragrance and taste of rose, the fragrance of the rose essential oil balm is closer to the fragrance of fresh flowers than the fragrance of rose oil, but the fragrance of the rose essential oil balm is not elegant. 100 g of rose essential oil balsam is dissolved in 200 ml of hexane, and the obtained hexane solution is subjected to alkaline alumina column chromatography and washed by hexane to separate out all rose wax, so that the wax content of the rose essential oil balsam is found to be low, the wax content is about 10-30 percent and is far lower than 40-60 percent of the wax content in the rose extract prepared by the traditional process, and no waste water is generated in the whole production process of the rose essential oil balsam. The preparation method provided by the invention has the characteristics of low energy consumption, no pollution and low cost, and is easy for industrial production. Meanwhile, the preparation method of the rose essential oil balm provided by the invention has the characteristic of high extraction rate, the extraction rate of the rose essential oil balm is 21-25%, and a material basis is provided for extracting the rose essential oil.

The invention provides a production method of rose essential oil, which takes rose essential oil balm as a raw material and adopts a nitrogen circulating gas stripping technology to extract the rose essential oil, so that no waste water is generated in the whole production process, the energy consumption is low, no pollution is caused, the cost is low, and the industrial production is easy to realize; meanwhile, the solvent and the nitrogen can be recycled, so that the tedious operation of solvent recovery in the later period is reduced, and the production cost is reduced. Meanwhile, the production method provided by the invention has higher recovery rate, and experiments prove that the extraction rate of the rose essential oil reaches 2.5-3.2% and is 5-7 times of that (0.5%) of the rose essential oil prepared by traditional steam distillation.

Detailed Description

The invention provides a preparation method of rose essential oil balm, which comprises the following steps:

fresh rose flowers and extraction solvent were mixed in a 1 g: mixing 1-3 ml of the rose essential oil and the rose essential oil, performing subcritical extraction under a dark condition, collecting extract liquor, and removing an extraction solvent in the extract liquor to obtain the rose essential oil balm.

The invention relates to a method for extracting fresh rose flowers and an extraction solvent, wherein the extraction solvent comprises the following components in parts by weight of 1 g: mixing at a mass-to-volume ratio of 1-3 ml. The extraction solvent is preferably one of propane, butane and tetrafluoroethane. The fresh rose flowers and the extraction solvent are preferably 1 g: 2 ml.

After mixing, the mixture is subjected to subcritical extraction under the condition of keeping out of the sun, and the extract liquor is collected. The temperature of the subcritical extraction is preferably 40-50 ℃, and more preferably 45 ℃. The pressure of the subcritical extraction is preferably 0.40-0.50 MPa, and more preferably 0.45 MPa. The extraction frequency of the subcritical extraction is preferably 2-4 times, and the time of each extraction is preferably 30-60 min, and more preferably 40 min. The subcritical extraction instrument is a subcritical extraction tank. The subcritical extraction tank is not particularly limited in the model and specification, and a subcritical extraction tank known in the art can be adopted.

After the extraction liquid is obtained, the extraction solvent in the extraction liquid is removed, and the rose essential oil balm is obtained.

In the present invention, the method for removing the extraction solvent from the extract preferably comprises evaporation desolventizing. And compressing and liquefying the solvent obtained by evaporation by a diaphragm compressor, and then recovering the solvent, wherein the solid phase obtained by evaporation is the rose essential oil balm.

The invention provides a production method of rose essential oil, which comprises the following steps:

placing the rose essential oil balm prepared by the preparation method into a material tank of a nitrogen circulating air stripping device, setting the pressure of the material tank to be 1.5-2 kPa and the temperature to be 60-80 ℃, setting the pressure of nitrogen in a nitrogen tank to be 2-4.5 kPa, and inputting the nitrogen into the material tank for steam stripping after the temperature is 300-350 ℃; and condensing and collecting the obtained stripping matter to obtain the rose essential oil.

In the present invention, the pressure in the material tank is preferably 1.8kPa, and the temperature in the material tank is preferably 70 ℃. The pressure of nitrogen in the nitrogen tank is preferably 3kPa, and the temperature of nitrogen in the nitrogen tank is preferably 320 ℃. After the stripping is completed, the residue of the rose essential oil balm is preferably collected in a heavy component collection tank, and the nitrogen is preferably pumped into the nitrogen tank through a vacuum pump. The nitrogen circulating stripping device is not particularly limited, and the nitrogen circulating stripping device known in the field can be adopted.

The prepared rose essential oil is subjected to physical and chemical analysis, is yellow liquid in shape and has strong rose fragrance, and through GC-MS analysis, the rose essential oil obtained by the production method provided by the invention comprises the following components in percentage by mass: 40 to 50 percent of citronellol, 2 to 5.5 percent of nerol, 6 to 18 percent of geraniol, 0.45 to 3 percent of beta-phenethyl alcohol, 0.7 to 3 percent of heptadecane, 0.5 to 2 percent of nonadecane, 0.6 to 2 percent of heneicosane, 0.6 to 2 percent of tricosane, 2 to 3.5 percent of farnesol, 1 to 3.5 percent of linalool and 0.7 to 1 percent of eugenol; also contains trace components with the fragrance and quality of rose essential oil, including rose oxide, neryl oxide, rose furan and beta-ionone.

Preferably, under the condition of 20 ℃, the density of the rose essential oil is 0.85-0.93, the refractive index is 1.468-1.480, and the ester value is 18-24.

The invention provides application of the rose essential oil in cosmetics or daily necessities.

In the present invention, the cosmetics include smoothing toner, lotion, essence cream, etc. The daily necessities preferably comprise perfumed soaps, air fresheners and the like.

The following examples are provided to illustrate the preparation of a rose essential oil balm, the production of the rose essential oil and the application of the rose essential oil, but they should not be construed as limiting the scope of the present invention.