CN103170294A - Method for extracting rose flower extractives by utilizing continuous countercurrent pipe type ultrasonic equipment - Google Patents
Method for extracting rose flower extractives by utilizing continuous countercurrent pipe type ultrasonic equipment Download PDFInfo
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- CN103170294A CN103170294A CN2013101026220A CN201310102622A CN103170294A CN 103170294 A CN103170294 A CN 103170294A CN 2013101026220 A CN2013101026220 A CN 2013101026220A CN 201310102622 A CN201310102622 A CN 201310102622A CN 103170294 A CN103170294 A CN 103170294A
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Abstract
The invention provides a method for extracting rose flower extractives by utilizing continuous countercurrent pipe type ultrasonic equipment. The method comprises the following steps of: drying picked fresh rose flower petals in the shade and crushing the petals to be 10-40 meshes; inputting the crushed petals into a continuous countercurrent pipe type ultrasonic extractor at a speed of 100kg/h; reversely inputting an organic solvent at a speed of 500-1000L/h; keeping the temperature of an ultrasonic extraction pipe at 25-50 DEG C for 20-40min to obtain a rose flower organic solvent extracted mixture; inputting the mixture into a liquid dreg squeezing and separating device; squeezing and separating materials and dregs at a speed of 20-100kg/h to obtain a rose flower extractive organic solvent mixture; inputting the mixture into a dynamic circulation low-temperature evaporation concentrating device, decompressing to -0.08MPa and keeping the temperature at 20-40 DEG C; and recycling an organic solvent and collecting concentrated extractives to obtain the rose flower extractives. The yield of the rose flower extractives is more than or equal to 12%.
Description
Technical field
The present invention relates to Flos Rosae Rugosae extract, especially utilize the method for continuous flow upstream tubular ultrasonic extraction equipment extraction Flos Rosae Rugosae extract, can significantly improve utilization rate and the quality of this material.
Background technology
Traditional rose extracting method: (1) steam distillation makes aromatic ester and the aromatic alcohol that single rose ethereal oil main component is effumability.Rose ethereal oil recovery rate≤0.03%.In this spices type of rose plant, except containing rose ethereal oil, also contain a large amount of to human body is very useful but the compositions such as not volatile plant wax, protein, glucoside, carbohydrate only can't be realized extraction and application by traditional way of distillation; (2) CO
2The resulting Flos Rosae Rugosae extract recovery rate of supercritical extraction≤1.6%.
Creativeness of the present invention: adopt continuous flow upstream tubular ultrasonic extraction equipment to extract the method for Flos Rosae Rugosae extract, by ultrasonic wave stretching shaking force can the rose compact tissue is loose, broken, plant cell wall is broken, make the compositions such as the stronger plant wax of the fragrant effective ingredients such as rose tissue space and intracellular ester class, alcohols and adhesive force, protein, glucoside, carbohydrate (account for extract total amount 15～20%), fully freed rear by organic solvent dissolution, extraction, improve effective component content and quality, reduce energy consumption, have important promotional value.
Summary of the invention
The object of the invention is to: adopt continuous flow upstream tubular ultrasonic extraction equipment to extract the method for Flos Rosae Rugosae extract, be that ultrasonic wave stretching shaking force is fully freed and by organic solvent dissolution and extraction effective ingredient, the method reduces energy consumption, has important production meaning.
The object of the present invention is achieved like this: a kind of method of utilizing continuous flow upstream tubular ultrasonic equipment to extract Flos Rosae Rugosae extract, step by step:
1) will pluck high-quality, without the fresh-rose petal that rots, be placed in the rear pulverizing of drying in the shade under natural conditions, wherein the water content of comminuting matter≤20%, granularity 10～40 orders;
2) rose of pulverizing is inputted in continuous flow upstream tubular ultrasonic extractor with 100kg/h speed, with the reverse input organic solvent of 500～1000L/h flow velocity, keep extracting 20～40min at 25～50 ℃ of ultrasonic extraction tube temperature, get the rose organic solvent and extract mixture;
3) the rose organic solvent is extracted mixture input melt cinder and extract separator, separate slag charge, carry out expression separation by 20～100kg/h, get the Flos Rosae Rugosae extract ORGANIC SOLVENT MIXTURES;
4) with in Flos Rosae Rugosae extract ORGANIC SOLVENT MIXTURES input dynamic circulation low-temperature evaporation inspissator, decompression is arrived-0.08MPa, and evaporation and concentration maintains the temperature at 20～40 ℃, reclaims organic solvent, collects concentrated extract, namely gets Flos Rosae Rugosae extract;
Wherein organic solvent is ethanol or ethyl acetate.
Described method, the yield of Flos Rosae Rugosae extract are 〉=12%.
Know-why of the present invention and effect: (1) Flos Rosae Rugosae extract composition is except containing volatile rose ethereal oil, also contain the compositions such as not volatile plant wax, protein, glucoside, carbohydrate in a large number, and the high composition of these values can't be realized extraction and application by traditional extraction method.(2) owing to having adopted ultrasonic technology and continuous flow upstream technology, extraction tube whole process using adverse current state namely is extracted material and the agent solvent is arranged is to go in the same direction, it is maximum that each section concentration difference keeps, guaranteed to use the solvent of minimum to reach best extraction effect, the Flos Rosae Rugosae extract extraction rate reached is more than 12%.(3) continuous flow upstream tubular ultrasonic extraction equipment extracts Flos Rosae Rugosae extract extraction time and just can complete an extracting cycle at 40 minutes, and extraction temperature≤50 ℃ obtain the Flos Rosae Rugosae extract quality good.(4) continuous flow upstream tubular ultrasonic extraction equipment extracts the method for Flos Rosae Rugosae extract, systematically will extract, the functions such as melt cinder extruding separates, filter, concentrated, residual solvent Distillation recovery, solvent tail gas recovery organically combine, under low temperature, (≤40 ℃) have realized the continuous operations of full operation by automatic control in confined space, production efficiency is maximized, energy consumption minimized, reduced cost, Determination of Residual Organic Solvents is low, non-environmental-pollution shows technological progress.
Description of drawings
The present invention is further described by reference to the accompanying drawings.
Accompanying drawing is the schematic flow sheet that continuous flow upstream tubular ultrasonic equipment extracts Flos Rosae Rugosae extract;
---continuous flow upstream tubular ultrasonic extractor mixes with reverse input organic solvent, and---mixture input melt cinder is extracted separator, and--Flos Rosae Rugosae extract ORGANIC SOLVENT MIXTURES input dynamic circulation low-temperature evaporation inspissator---organic solvent recovery---gets Flos Rosae Rugosae extract except waste residue as shown in the figure: pulverize rose.
The specific embodiment
The present invention is further described in conjunction with the embodiments.
Embodiment
Raw material is disposed: will pluck high-quality, without rotten fresh-rose petal, and dry in the shade under field conditions (factors), during its water content≤20%, it be pulverized 20 mesh sieves;
Preparation scheme 1
Get the rose 100kg that pulverized 20 mesh sieves, meet in the continuous flow upstream tubular ultrasonic extractor of JB/T 20126-2009 national standard with the input of 100kg/h speed, organic solvent ethanol (95%) with the clean general happy bio tech ltd production in the reverse input of 800L/h flow velocity Xinjiang, keeping extracting 35min at 40 ℃ of ultrasonic extraction tube temperature, get the rose alcohol mixture; After this mixture input extraction melt cinder is extracted separator, isolate slag charge and extract mixture; To extract mixture input dynamic circulation low-temperature reduced-pressure and (0.08MPa) in the evaporation concentrator, keep 35 ℃ of temperature, recycling after the organic solvent ethanol evaporation reclaims.Collect residue extract 12.6kg, be Flos Rosae Rugosae extract, yield is 12.6%.
Preparation scheme 2
Get and pulverized 20 mesh sieve rose 100kg, meet in the continuous flow upstream tubular ultrasonic extractor of JB/T 20126-2009 national standard with the input of 100kg/ h speed, the organic solvent ethyl acetate of producing with the reverse input of 1000L/h flow velocity Tianjin Fu Yu Fine Chemical Co., Ltd, keeping extracting 40min under ultrasonic extraction tube temperature 45 C, get the rose ethyl acetate mixture; After this mixture input extraction melt cinder is extracted separator, isolate slag charge and extract mixture; (0.08MPa) in the evaporation concentrator, keep 40 ℃ of temperature, the evaporation of organic solvent ethyl acetate is recycled, and collects residue extract 12kg, is Flos Rosae Rugosae extract, and yield is 12% will to extract mixture input dynamic circulation low-temperature reduced-pressure.
This method obtains the effect of extract:
Production example 1
The interpolation of rose Manual perfumed soap:
During Manual perfumed soap was made, after the saponification process was completed, the saponification liquor temperature added rose extract 2.5%(kg/kg when remaining on 60 ℃), that constant temperature stirs is cooling in the injection moulding mould, cut apart, pack and to get the rose Manual perfumed soap.This rose extract is applied in the making of Manual perfumed soap, has replaced the use of chemical essence and pigment in common perfumed soap, after using more than the lasting 24h of body surface lasting, can play the effects such as tender white, moisturizing, moisturizing.
Production example 2
The interpolation of cosmetics creme class skin care item rose hand lotion:
When making skin care item hand lotion emulsification process and finish, add rose extract 1.0%(kg/kg when keeping 40 ℃ of temperature), be down to room temperature after constant temperature stirs, after packing, packing both the rose hand lotion.This rose extract is applied to the use that hand lotion has replaced chemical essence and pigment in common perfumed soap, and the sustainable lasting of body surface after using can play the effects such as tender white, moisturizing, moisturizing.
Claims (2)
1. method of utilizing continuous flow upstream tubular ultrasonic equipment to extract Flos Rosae Rugosae extract is characterized in that: step by step:
1) will pluck high-quality, without the fresh-rose petal that rots, be placed in the rear pulverizing of drying in the shade under natural conditions, wherein the water content of comminuting matter≤20%, granularity 10～40 orders;
2) rose of pulverizing is inputted in continuous flow upstream tubular ultrasonic extractor with 100kg/h speed, with the reverse input organic solvent of 500～1000L/h flow velocity, keep ultrasonic extraction tube temperature to extract 20～40min at 25～50 ℃, get the rose organic solvent and extract mixture;
3) the rose organic solvent is extracted mixture input melt cinder and extract separator, separate slag charge, carry out expression separation by 20～100kg/h, get the Flos Rosae Rugosae extract ORGANIC SOLVENT MIXTURES;
4) with in Flos Rosae Rugosae extract ORGANIC SOLVENT MIXTURES input dynamic circulation low-temperature evaporation inspissator, decompression is arrived-0.08MPa, and evaporation and concentration maintains the temperature at 20～40 ℃, reclaims organic solvent, collects concentrated extract, namely gets Flos Rosae Rugosae extract;
Wherein organic solvent is ethanol or ethyl acetate.
2. method according to claim 1, it is characterized in that: the yield of Flos Rosae Rugosae extract is 〉=12%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409239A (en) * | 2013-07-26 | 2013-11-27 | 郑刚 | Method for extracting chamomile extract by using countercurrent tube type ultrasonic device |
| CN103756783A (en) * | 2014-01-09 | 2014-04-30 | 江南大学 | Method for ultrasonic countercurrent extraction of tea seed and/or camellia seed soil |
| CN108191805A (en) * | 2018-03-06 | 2018-06-22 | 云南华测检测认证有限公司 | A kind of method that natural procyanidins are extracted in the rose from polyphyll |
| CN113214900A (en) * | 2021-05-12 | 2021-08-06 | 劲牌有限公司 | Preparation process of rose essence base suitable for blending wine body |
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| CN101954200A (en) * | 2009-07-14 | 2011-01-26 | 张娟 | Vertical countercurrent extracting method and device thereof |
| CN102166039A (en) * | 2011-04-08 | 2011-08-31 | 深圳波顿香料有限公司 | Method for extracting roselle extractive and application in cigarettes as well as cigarettes |
| CN102433018A (en) * | 2011-11-17 | 2012-05-02 | 安徽杜鹃花生物科技有限公司 | Method for extracting azalea pigment |
| CN102851118A (en) * | 2011-06-27 | 2013-01-02 | 湖北中烟工业有限责任公司 | Extraction process of rose essence for cigarette |
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2013
- 2013-03-27 CN CN2013101026220A patent/CN103170294A/en active Pending
Patent Citations (4)
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| CN101954200A (en) * | 2009-07-14 | 2011-01-26 | 张娟 | Vertical countercurrent extracting method and device thereof |
| CN102166039A (en) * | 2011-04-08 | 2011-08-31 | 深圳波顿香料有限公司 | Method for extracting roselle extractive and application in cigarettes as well as cigarettes |
| CN102851118A (en) * | 2011-06-27 | 2013-01-02 | 湖北中烟工业有限责任公司 | Extraction process of rose essence for cigarette |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409239A (en) * | 2013-07-26 | 2013-11-27 | 郑刚 | Method for extracting chamomile extract by using countercurrent tube type ultrasonic device |
| CN103756783A (en) * | 2014-01-09 | 2014-04-30 | 江南大学 | Method for ultrasonic countercurrent extraction of tea seed and/or camellia seed soil |
| CN108191805A (en) * | 2018-03-06 | 2018-06-22 | 云南华测检测认证有限公司 | A kind of method that natural procyanidins are extracted in the rose from polyphyll |
| CN113214900A (en) * | 2021-05-12 | 2021-08-06 | 劲牌有限公司 | Preparation process of rose essence base suitable for blending wine body |
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Application publication date: 20130626 |