CN103143311B - Method for extracting lavender extract by adopting continuous countercurrent tube type ultrasonic waves - Google Patents
Method for extracting lavender extract by adopting continuous countercurrent tube type ultrasonic waves Download PDFInfo
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- CN103143311B CN103143311B CN201310105230.XA CN201310105230A CN103143311B CN 103143311 B CN103143311 B CN 103143311B CN 201310105230 A CN201310105230 A CN 201310105230A CN 103143311 B CN103143311 B CN 103143311B
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- extract
- lavender
- organic solvent
- herba lysimachiae
- lysimachiae foenumgraeci
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 229940083980 lavender extract Drugs 0.000 title abstract 6
- 235000020723 lavender extract Nutrition 0.000 title abstract 6
- 239000000284 extract Substances 0.000 claims abstract description 52
- 239000001102 lavandula vera Substances 0.000 claims abstract description 33
- 244000178870 Lavandula angustifolia Species 0.000 claims abstract description 32
- 235000010663 Lavandula angustifolia Nutrition 0.000 claims abstract description 32
- 235000018219 lavender Nutrition 0.000 claims abstract description 32
- 239000003960 organic solvent Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 238000001704 evaporation Methods 0.000 claims abstract description 11
- 230000008020 evaporation Effects 0.000 claims abstract description 11
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000011144 upstream manufacturing Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 7
- 239000003818 cinder Substances 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 5
- 239000003791 organic solvent mixture Substances 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 2
- 238000003306 harvesting Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000006210 lotion Substances 0.000 description 4
- 230000003020 moisturizing effect Effects 0.000 description 4
- 239000000344 soap Substances 0.000 description 4
- 150000001720 carbohydrates Chemical class 0.000 description 3
- 235000014633 carbohydrates Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229930182478 glucoside Natural products 0.000 description 3
- 150000008131 glucosides Chemical class 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000012165 plant wax Substances 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008278 cosmetic cream Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000015114 espresso Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Cosmetics (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for extracting a lavender extract by adopting continuous countercurrent tube type ultrasonic waves. The method comprises the following steps of: picking stems, leaves and petals of lavender, drying in the shade, and crushing the dried materials into powder with the particle size of 10-40 meshes; inputting the crushed lavender into a continuous countercurrent tube type ultrasonic extractor at a speed of 100kg/h, inputting an organic solvent reversely at a flow speed of 500-1000L/h, maintaining the temperature of an ultrasonic extraction tube to be 25-50 DEG C, and extracting for 20-40 minutes to obtain an extraction mixture of the lavender and the organic solvent; inputting the extraction mixture of the lavender and the organic solvent into a liquid residue squeeze-drying separator, separating residue materials, and performing squeezing separation at a speed of 20-100kg/h to obtain a mixture of the lavender extract and the organic solvent; and inputting the mixture of the lavender extract and the organic solvent into a dynamic loop low-temperature evaporation concentrator, reducing the pressure to -0.08MPa, performing evaporation concentration, maintaining the temperature to be 20-40 DEG C, recovering the organic solvent, and collecting a concentrated extract, thus obtaining the lavender extract, wherein the yield of the lavender extract is more than or equal to 15%.
Description
Technical field
The present invention relates to the extraction of lavender, especially utilize continuous flow upstream tubular ultrasonic extraction equipment to extract the method for Herba Lysimachiae foenumgraeci extract, quality and productive rate can be made to be significantly improved.
Background technology
Traditional lavender extracting method: (1) steam distillation obtains aromatic ester and the aromatic alcohol that single Lavender main component is effumability, now Lavender recovery rate≤0.9%.Lavender is aromatic plant, except containing except the Lavender of effumability, also containing a large amount of to human body very useful but not volatile plant wax, protein, glucoside, carbohydrate content etc., extraction and application cannot be realized by traditional way of distillation; (2) CO
2herba Lysimachiae foenumgraeci extract recovery rate≤5.6% that supercritical extraction obtains, final Extracting temperature>=50 DEG C, and adopt this extracting method recovery rate lower, and time more than 50 DEG C, Herba Lysimachiae foenumgraeci extract effective ingredient is easily destroyed; (3) fixed bed lixiviate is sent out and is extracted Herba Lysimachiae foenumgraeci extract recovery rate≤2.9%, and this method can not continuous seepage, and the organic solvent rate of recovery is low, and production process is in non-air-tight state, easily produces environment and pollutes.
The Herba Lysimachiae foenumgraeci extract that this method obtains, except containing except volatile Lavender, also containing compositions such as a large amount of not volatile plant wax, protein, glucoside, carbohydrates, account for 20 ~ 25% of extract total amount, and the composition that effectively value is high, cannot be realized by traditional extraction method, the value place of this namely this method application.
Summary of the invention
The object of the invention is to: adopt continuous flow upstream tubular ultrasonic extraction equipment to extract the method for Herba Lysimachiae foenumgraeci extract, adequately protected heat-sensitive substance, improves effective component content and quality, reduces energy consumption, have important promotional value.
The object of the present invention is achieved like this: a kind of continuous flow upstream tubular ultrasonic wave device extracts the method for Herba Lysimachiae foenumgraeci extract, step by step:
1) stem, leaf, the petal of the fresh lavender of harvesting high-quality, nothing being rotted, pulverize after drying in the shade, wherein water content≤20%, granularity 10 ~ 40 order of comminuting matter under being placed in natural conditions;
2) lavender 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 25 ~ 50 DEG C, extract 20 ~ 40min, obtain lavender Solvent Extract methods mixture;
3) lavender Solvent Extract methods mixture input melt cinder is extracted separator, be separated slag charge, carry out expression separation by 20 ~ 100kg/h, obtain Herba Lysimachiae foenumgraeci extract ORGANIC SOLVENT MIXTURES;
4) by Herba Lysimachiae foenumgraeci extract ORGANIC SOLVENT MIXTURES input dynamic circulation low-temperature evaporation inspissator, decompression is to-0.08MPa, and evaporation and concentration, maintains the temperature at 20 ~ 40 DEG C, reclaims organic solvent, collects concentrated extract, obtains Herba Lysimachiae foenumgraeci extract;
Wherein organic solvent is ethanol or ethyl acetate.
The yield of described method Herba Lysimachiae foenumgraeci extract is >=15%.
Know-why of the present invention and effect: Conventional espresso method is extracted Herba Lysimachiae foenumgraeci extract yield and is up to 0.9%; CO
2supercritical extraction extracts Herba Lysimachiae foenumgraeci extract yield and is up to 5.6%; Fixed bed restricted-access media Herba Lysimachiae foenumgraeci extract recovery rate is up to 2.9%.Have employed ultrasonic technology and continuous flow upstream technology, by ultrasonic wave stretching shaking force can by loose for lavender compact tissue, broken, plant cell wall is broken, the fragrant effective ingredient such as lavender tissue space and intracellular ester class, alcohols and the stronger composition such as plant wax, protein, glucoside, carbohydrate of adhesive force are fully freed, is extracted by organic solvent dissolution; Secondly extract the omnidistance reverse flow state that adopts namely be extracted material and have agent solvent to be go in the same direction, each section of concentration difference keeps maximum, ensure that and uses the solvent of minimum to reach best extraction effect, extraction rate reached more than 15%.
The technique effect of this method is, this Herba Lysimachiae foenumgraeci extract quality is good, adopts continuous flow upstream tubular ultrasonic extraction method to have adequately protected heat-sensitive substance, improves effective component content and quality; Secondly Determination of Residual Organic Solvents is low, extraction, melt cinder extruding are separated, filter, concentrated, residual solvent Distillation recovery, the function such as solvent tail gas recovery organically combine, reduce environmental pollution, the effective ingredient of the lavender simultaneously obtained, the input usefulness of great promotion industry, shows technological progress.
Accompanying drawing explanation
The present invention is further described by reference to the accompanying drawings.
Accompanying drawing is that continuous flow upstream tubular ultrasonic extraction equipment extracts Herba Lysimachiae foenumgraeci extract process flow diagram;
As shown in the figure: pulverize lavender--input continuous flow upstream tubular ultrasonic extractor--reverse input organic solvent--lavender ORGANIC SOLVENT MIXTURES---input melt cinder extracts separator--isolate slag charge and Herba Lysimachiae foenumgraeci extract ORGANIC SOLVENT MIXTURES---mixture input dynamic circulation low-temperature evaporation inspissator--organic solvent reclaims-obtain Herba Lysimachiae foenumgraeci extract.
Detailed description of the invention
The present invention is further described in conjunction with the embodiments.
Embodiment
Raw material is disposed: will pluck high-quality, without the fresh lavender stem, leaf, the petal that rot, dry in the shade under being placed in natural conditions, its water content≤20%, be pulverized 10 or 25 or 40 mesh sieves;
Preparation scheme 1
Get the lavender 100kg pulverizing 30 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; with the organic solvent ethanol (95%) that Jie Pule bio tech ltd, 800L/h flow velocity reverse input Xinjiang produces; at maintenance ultrasonic extraction tube temperature 40 DEG C, extract 35min, obtain lavender alcohol mixture; After this mixture input extraction melt cinder is extracted separator, isolate slag charge and extract mixture; To extract in mixture input dynamic circulation low-temperature reduced-pressure (-0.08MPa) evaporation concentrator, and keep temperature 35 DEG C, recycling after organic solvent ethanol evaporation reclaims, collect residue extract 17kg, be Herba Lysimachiae foenumgraeci extract, yield is 17%.
Preparation scheme 2
Get the lavender 100kg pulverizing 30 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, with the organic solvent ethyl acetate that the reverse input Tianjin Fu Yu Fine Chemical Co., Ltd of 1000L/h flow velocity produces, under the ultrasonic extraction tube temperature 45 C of maintenance, extract 40min, obtain lavender ethyl acetate mixture; After this mixture input extraction melt cinder is extracted separator, isolate slag charge and extract mixture, to extract in mixture input dynamic circulation low-temperature reduced-pressure (-0.08MPa) evaporation concentrator, keep temperature 40 DEG C, the evaporation of organic solvent ethyl acetate recycles after reclaiming, collect residue extract 15kg, be Herba Lysimachiae foenumgraeci extract, yield is 15%.
The extract effect example that this method obtains.
1) daily use chemicals articles for washing class is as the application example of lavender Manual perfumed soap:
In Manual perfumed soap manufacture craft, after its saponification process completes, saponification liquor temperature adds Herba Lysimachiae foenumgraeci extract 0.1 or 3 or 5%(kg/kg when remaining on 40 or 60 or 80 DEG C), constant temperature stir cooling in injection moulding mould, segmentation, packaging both lavender Manual perfumed soap.This Herba Lysimachiae foenumgraeci extract is applied to Manual perfumed soap, uses sustainable more than the 24h of the fragrant fragrance remaining time of rear body surface lavender, can play the effect such as moisturizing, moisturizing.
2) application example of Cosmetic cream class skin care item lavender hand lotion:
At the end of making skin care item hand lotion emulsification process, add Herba Lysimachiae foenumgraeci extract 0.01 or 1.6 or 3%(kg/kg when keeping temperature 30 or 45 or 60 DEG C), be down to room temperature after constant temperature stirs, after packing, packaging, both obtain lavender hand lotion.This Herba Lysimachiae foenumgraeci extract is applied to hand lotion, uses the sustainable lasting of rear body surface, can play the effect such as moisturizing, moisturizing.
Claims (1)
1. adopt continuous flow upstream tubular ultrasonic ripple to extract a method for Herba Lysimachiae foenumgraeci extract, it is characterized in that: step by step:
1) stem, leaf, the petal of the fresh lavender of harvesting high-quality, nothing being rotted, pulverize after drying in the shade, wherein water content≤20%, granularity 10 ~ 40 order of comminuting matter under being placed in natural conditions;
2) lavender 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 25 ~ 50 DEG C, extract 20 ~ 40min, obtain lavender Solvent Extract methods mixture;
3) lavender Solvent Extract methods mixture input melt cinder is extracted separator, be separated slag charge, carry out expression separation by 20 ~ 100kg/h, obtain Herba Lysimachiae foenumgraeci extract ORGANIC SOLVENT MIXTURES;
4) by Herba Lysimachiae foenumgraeci extract ORGANIC SOLVENT MIXTURES input dynamic circulation low-temperature evaporation inspissator, decompression is to-0.08MPa, and evaporation and concentration, maintains the temperature at 20 ~ 40 DEG C, reclaims organic solvent, collects concentrated extract, obtains Herba Lysimachiae foenumgraeci extract;
Wherein organic solvent is ethanol or ethyl acetate;
The yield of Herba Lysimachiae foenumgraeci extract is >=15%.
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| CN201310105230.XA CN103143311B (en) | 2013-03-28 | 2013-03-28 | Method for extracting lavender extract by adopting continuous countercurrent tube type ultrasonic waves |
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| CN201310105230.XA CN103143311B (en) | 2013-03-28 | 2013-03-28 | Method for extracting lavender extract by adopting continuous countercurrent tube type ultrasonic waves |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103385832B (en) * | 2013-07-24 | 2015-09-23 | 云南西草资源开发有限公司 | A kind of take Herba Lysimachiae foenum-graeci extract as the anti-aging cosmetics of main active |
| CN103409240A (en) * | 2013-07-26 | 2013-11-27 | 郑刚 | Method for extracting chamomile extract by using pot-type ultrasonic device |
| CN103409239A (en) * | 2013-07-26 | 2013-11-27 | 郑刚 | Method for extracting chamomile extract by using countercurrent tube type ultrasonic device |
| CN106512467A (en) * | 2015-09-13 | 2017-03-22 | 王建卫 | Economical solid-liquid transfer method |
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- 2013-03-28 CN CN201310105230.XA patent/CN103143311B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 李紫薇等.超声波辅助提取狭叶薰衣草总黄酮的研究.《伊犁师范学院学报(自然科学版)》.2012,(第3期),第53-56页. * |
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Effective date of registration: 20150910 Address after: 835000 Bayan Dai village, Dai Town, Yining, Yili Kazakh Autonomous Prefecture, the Xinjiang Uygur Autonomous Region, Bayan Patentee after: Yili lavender products Co. Ltd. Mayila St. Address before: 835000 the Xinjiang Uygur Autonomous Region Yili Kazak Autonomous Prefecture of Yining City, Bayan Dai Zhen Yili lavender products Co. Ltd. Mayila St. Patentee before: Zheng Gang Patentee before: Wang Yubiao |
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| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20130612 Assignee: Yili lavender products Co. Ltd. Mayila St. Assignor: Zheng Gang|Wang Yubiao Contract record no.: 2015650000037 Denomination of invention: Method for extracting lavender extract by adopting continuous countercurrent tube type ultrasonic waves Granted publication date: 20150708 License type: Exclusive License Record date: 20150831 |
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