CN103756783A - Method for ultrasonic countercurrent extraction of tea seed and/or camellia seed soil - Google Patents
Method for ultrasonic countercurrent extraction of tea seed and/or camellia seed soil Download PDFInfo
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- CN103756783A CN103756783A CN201410009469.1A CN201410009469A CN103756783A CN 103756783 A CN103756783 A CN 103756783A CN 201410009469 A CN201410009469 A CN 201410009469A CN 103756783 A CN103756783 A CN 103756783A
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Abstract
The invention discloses a method for ultrasonic countercurrent extraction of tea seed and/or camellia seed soil, and the method comprises the following steps: putting the raw material treated tea seed and/or camellia seed oil into a feed device of a continuous countercurrent ultrasonic leacher, and inputting an extraction agent into the leacher from a slag outlet at the other end, and inputting the material and extraction liquid at the same time, wherein the ultrasonic frequency is 20-25KHz, the ultrasonic intensity is 50-600W, the extraction temperature is 30-60 DEG C, the material-liquid mass ratio is (1:2)-(1:12), and the leaching time is 10-30 minutes; separating to obtain tea seed and/or camellia seed residue and extract liquid; obtaining the tea seed and/or camellia seed raffinate from the slag outlet, and conveying to a solvent recycling system to recycle the extraction agent; obtaining the extraction liquid from a liquid outlet of the continuous countercurrent ultrasonic leacher; separating the tea seed and/or camellia seed crude oil from the extraction liquid while recycling the extraction agent. By adopting the continuous countercurrent ultrasonic technology to extract the tea seed and/or camellia seed crude oil, the method disclosed by the invention has the advantages of simple equipment, low energy consumption, high oil yield, short extraction time, low solvent consumption and the like, and is suitable for large-scale production.
Description
Technical field
The invention belongs to Vegetable oil lipoprotein extractive technique field, relate in particular to a kind of method of ultrasonic wave counter-current extraction tea-seed and/or camellia seed oil.
Background technology
China is the native place of tealeaves, and local tea variety is various, and tea-seed and/or tea seed are the fruits of tea tree, is the by product of Tea Production.Tea-seed and/or tea seed can extract oil, just on the books in the < < Compendium of Materia Medica > > showing as far back as China Ming Dynasty medicine scholar's LI Shi-Zhen (1518～1593).In in December, 2009 < < Ministry of Health of the People's Republic of China 2009 No. 18 bulletin > >, official approval tea-seed and/or camellia seed oil are new resource food.Within 2011, there are more than 3,165 ten thousand mu of tea places in China, and output is pressed 450kg/hm
2calculate, potential tea-seed and/or tea seed resource are about more than 95 ten thousand tons, as tea-seed and/or tea seed are made full use of, can turn waste into wealth, and increase tea grower's income, promote tea industry restructuring, keep the Sustainable development of Tea Production.
Grease is the main component of tea-seed and/or tea seed, accounts for the 25%-35% of tea-seed and/or tea seed dry weight, and tea-seed and/or camellia seed oil belong to nondrying oil, under normal temperature, is liquid, has the specific faint scent of this kind oil.Tea-seed and/or camellia seed oil are mainly containing palmitinic acid, stearic acid, eicosanoic acid, oleic acid, linolic acid etc., and wherein unsaturated fatty acids surpasses 80%, and especially linolic acid reaches more than 20%.The active class material of the functional living beings such as in addition, tea-seed and/or camellia seed oil contain abundant liposoluble vitamin, and are rich in tea-polyphenol, plant sterol, squalene, has very high nutritive value and nourishing function, and DEVELOPMENT PROSPECT is wide.
At present, tea-seed and/or tea seed or camellia seed oil are mainly to extract from tea-seed and/or tea seed by methods such as milling process, cold-press, organic solvent method, supercritical extractions.The tea-seed that milling process obtains and/or oil-tea camellia seed crude oil color and luster is dark, acid value is high, contain the solid impurities such as saponin, there is bitter taste and the squeezing time is long, residual oil content is high and oil expression process in have green compact high temperature to steam to fry operation, easily generate strong carcinogen benzopyrene; Although cold-press has been avoided the heat treatment process in traditional milling process, cake slag residual oil content is high, and the distinctive fragrance of tea-seed and/or camellia seed oil and local flavor are lighter; Organic solvent extractionprocess exists that extraction time is long, solvent-oil ratio is large, efficiency is low, crude oil inferior quality; Supercritical extraction rule requires high to plant and instrument, and cost is high, energy consumption is large, is not suitable for heavy industrialization consecutive production.
Summary of the invention
The object of this part is to summarize some aspects of embodiments of the invention and briefly introduces some preferred embodiments.In this part and the application's specification digest and denomination of invention, may do a little simplification or omit to avoid the making object of this part, specification digest and denomination of invention fuzzy, and this simplification or omit can not be for limiting the scope of the invention.
The problem existing in method in view of above-mentioned and/or existing ultrasonic wave counter-current extraction tea-seed and/or camellia seed oil, has proposed the present invention.
Therefore, the object of the invention is to overcome the deficiency of existing organic solvent extraction tea-seed and/or camellia seed oil technique, improve tea-seed and/or camellia seed oil extraction yield, provide a kind of extraction yield high, save solvent, extraction time is short, cost is lower, crude oil quality better and applicable industrialization continuity are produced ultrasonic counter-current extraction tea-seed and/or the method for camellia seed oil.
For solving the problems of the technologies described above, the invention provides following technical scheme: a kind of method of ultrasonic wave counter-current extraction tea-seed and/or camellia seed oil, comprise the steps: step 1, tea-seed after processing and/or tea seed raw material are placed in the feeding unit of continuous countercurrent ultrasonic wave leacher, extraction agent is input in leacher from the slag notch of the other end, material and extracting solution are inputted simultaneously, wherein, ultrasonic frequency is 20～25KH, ultrasonic intensity 50～600W, extract 30 ℃～60 ℃ of temperature, feed liquid mass ratio is 1:2～1:12, leaching time 10～30min, separation obtains tea-seed and/or tea seed residue and extraction liquid, step 2, obtains tea-seed and/or tea seed extract remainder by slag notch, is delivered to solvent recovering system and carries out extraction agent recovery, and obtaining extracting solution by the leakage fluid dram of continuous countercurrent supersonic leaching device, extracting solution obtains tea-seed and/or oil-tea camellia seed crude oil after separation, reclaims extraction agent simultaneously.
As a kind of preferred version of the method for ultrasonic wave counter-current extraction tea-seed of the present invention and/or camellia seed oil, wherein: described extraction agent is normal hexane.
As a kind of preferred version of the method for ultrasonic wave counter-current extraction tea-seed of the present invention and/or camellia seed oil, wherein: described ultrasonic intensity scope is 50～250W, the ul-trasonic irradiation time is 10～120min.
As a kind of preferred version of the method for ultrasonic wave counter-current extraction tea-seed of the present invention and/or camellia seed oil, wherein: described temperature range is 30 ℃～45 ℃, and feed liquid mass ratio is 1:6.
As a kind of preferred version of the method for ultrasonic wave counter-current extraction tea-seed of the present invention and/or camellia seed oil, wherein: described tea-seed and/or its moisture controlled of tea seed raw material, 2%～8%, are crushed to 16 order～60 orders.
Beneficial effect of the present invention:
(1) the present invention adopts continuous countercurrent ultrasonic extraction tea-seed and/or oil-tea camellia seed crude oil, has the advantages such as equipment is simple, energy consumption is low, oil yield is high, extraction time is short, solvent-oil ratio is low, is applicable to scale operation;
(2) tea-seed and/or the oil-tea camellia seed crude oil quality better that by present method extraction, are obtained, its phospholipids content, acid number and peroxide value are low, lighter color;
(3) in China, belong to " little kind " oil plant, but the rare pollution of its growing environment, suitable exploitation becomes high added value fine work tea-seed and/or camellia seed oil product, tea-seed and/or camellia seed oil local flavor are fine, contain abundant fatty accompaniment (as plant sterol, squalene, tocopherol, polyphenol etc.), nutritive value is higher, the present invention has improved the oil extracting rate of tea-seed and/or tea seed, obtain high-quality tea-seed and/or oil-tea camellia seed crude oil, made up traditional tea seed and/or camellia seed oil milling process and solvent extration not enough.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with specific embodiment, the specific embodiment of the present invention is described in detail.
A lot of details have been set forth in the following description so that fully understand the present invention, but the present invention can also adopt other to be different from alternate manner described here and implement, those skilled in the art can do similar popularization without prejudice to intension of the present invention in the situation that, so the present invention is not subject to the restriction of following public specific embodiment.
Secondly, alleged " embodiment " or " embodiment " refers to special characteristic, structure or the characteristic that can be contained at least one implementation of the present invention herein.Different local in this manual " in one embodiment " that occur not all refer to same embodiment, neither be independent or the embodiment mutually exclusive with other embodiment optionally.
Embodiment 1
In this embodiment, comprise the following steps:
(1) tea-seed and/or tea seed after cleaning removal of impurities are dried at 60 ℃ of temperature, moisture content is controlled at 4% left and right, is crushed to 16 order～60 orders, obtains tea-seed and/or tea seed raw material.
(2) get and process rear tea-seed and/or tea seed raw material 13g, put into the reactor of ultrasonic wave backflow device, extracted rear separated tea-seed and/or tea seed residue and extraction liquid, extraction liquid obtains tea-seed and/or oil-tea camellia seed crude oil after reclaiming solvent.Extraction conditions is: at ultrasonic frequency 20～25KH, and ultrasound intensity 65W, solid-liquid ratio 1:4, leaching time 10min, extracts 30 ℃ of temperature (recirculated water temperature control), and separation obtains tea-seed and/or oil-tea camellia seed crude oil, reclaim normal hexane, obtain tea-seed and/or camellia seed oil 3.29g.
Embodiment 2
Get and process rear tea-seed and/or tea seed raw material 13g, put into the reactor of ultrasonic backflow device, extracted rear separated tea-seed and/or tea seed residue and extraction liquid, extraction liquid obtains tea-seed and/or oil-tea camellia seed crude oil after reclaiming solvent.Extraction conditions is: at ultrasonic frequency 20～25KH, and ultrasound intensity 130W, solid-liquid ratio 1:4, leaching time 10min, extracts 30 ℃ of temperature (recirculated water temperature control), and separation obtains tea-seed and/or oil-tea camellia seed crude oil, reclaim normal hexane, obtain tea-seed and/or camellia seed oil 3.63g.
Embodiment 3
(1) tea-seed and/or tea seed after cleaning removal of impurities are dried at 60 ℃ of temperature, moisture content is controlled at 4% left and right, is crushed to 16 order～60 orders, obtains tea-seed and/or tea seed raw material.
(2) get and process rear tea-seed and/or tea seed raw material 13g, put into the reactor of ultrasonic backflow device, extracted rear separated tea-seed and/or tea seed residue and extraction liquid, extraction liquid obtains tea-seed and/or oil-tea camellia seed crude oil after reclaiming solvent.Extraction conditions is: at ultrasonic frequency 20～25KH, and ultrasound intensity 200W, solid-liquid ratio 1:6, leaching time 20min, extracts temperature 50 C (recirculated water temperature control), and separation obtains tea-seed and/or oil-tea camellia seed crude oil, reclaim normal hexane, obtain tea-seed and/or camellia seed oil 3.86g.
As can be seen here, the extracting method of tea-seed of the present invention and/or oil-tea camellia seed crude oil, the United Technologies that adopt organic solvent extraction and low frequency ultrasound counter-current extraction, it is first clean tea-seed and/or tea seed are dried or naturally dried, moisture controlled is 2%～8%, be crushed to 16 order～60 orders, obtain tea-seed and/or tea seed raw material; Tea-seed after processing and/or tea seed raw material are placed in the feeding unit of continuous countercurrent supersonic leaching device, and extraction agent is input to the slag notch from the other end in leacher, and material and extracting solution are inputted simultaneously; Concrete working parameter under normal pressure: ultrasonic frequency 20～25KH, ultrasound intensity 50～600W, extracts 30 ℃～60 ℃ of temperature, solid-liquid ratio 1:2～1:12, leaching time 10～30min, separation obtains tea-seed and/or tea seed residue and extraction liquid; After above-mentioned steps extraction finishes, by slag notch, obtain tea-seed and/or tea seed extract remainder and be delivered to solvent recovering system and carry out solvent recuperation; Leakage fluid dram by continuous countercurrent supersonic leaching device is extracted liquid, and extraction liquid obtains tea-seed and/or oil-tea camellia seed crude oil after solvent recuperation, reclaims extraction agent simultaneously.
In the present invention,
1. peroxide value is pressed GB/T5538-2005 < < animal-plant oil determination of POV > >
2. acid number is pressed GB/T5530-2005 < < animal-plant oil acid number and acid test > >
3. phospholipids content is pressed GB/T5537---the mensuration > > of 2008 < < grain and oil detection phospholipids content
4. oxidation-stabilized index (OSI), with reference to the mensuration > > of GB/T21121-2007 < < animal-plant oil oxidative stability, is measured with the oxidation-stabilized instrument of Rancimat743.
5. phospholipids content is pressed GB/T22460---the mensuration > > of 2008 < < animal-plant oil Lovibond color and lusters
6. adopt HPLC method to measure.Take 1.0g oil sample, be accurate to 0.001g and be placed in the brown volumetric flask of 10mL, with n-hexane dissolution, ultrasonic rear constant volume, centrifugal, get 20 μ L sample introductions.Sehperisorb Silica post, moving phase is normal hexane: Virahol=98: 2,0.5mL/min, 25 ℃ of column temperatures, detect wavelength 295nm.The hexane solution of preparation mixed tocopherol standard substance, concentration is 1mg/mL.External standard method tocopherol content, standard specimen and three sample difference sample introductions, by standard specimen, determine the retention time of each tocopherol, according to standard specimen total concn and total peak area relation, can calculate the tocopherol content of four kinds of configurations in sample and total tocopherol content simultaneously.
Tea-seed and/or the oil-tea camellia seed crude oil of the plant produced of the tea-seed that ultrasonic countercurrent extraction is obtained and/or oil-tea camellia seed crude oil and same batch carry out quality comparison:
As can be seen here, the tea-seed and/or the oil-tea camellia seed crude oil quality better that by present method extraction, are obtained, its phospholipids content, acid number and peroxide value are low, lighter color.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (5)
1. a method for ultrasonic wave counter-current extraction tea-seed and/or tea seed, is characterized in that, comprises the steps:
Step 1, tea-seed after processing and/or tea seed raw material are placed in the feeding unit of continuous countercurrent ultrasonic wave leacher, extraction agent is input in leacher from the slag notch of the other end, material and extracting solution are inputted simultaneously, and wherein, ultrasonic frequency is 20～25KH, ultrasonic intensity 50～600W, 30 ℃～60 ℃ of temperature of extraction, feed liquid mass ratio are 1:2～1:12, leaching time 10～30min, and separation obtains tea-seed and/or tea seed residue and extraction liquid;
Step 2, obtains tea-seed and/or tea seed extract remainder by slag notch, is delivered to solvent recovering system and carries out extraction agent recovery; And obtaining extracting solution by the leakage fluid dram of continuous countercurrent supersonic leaching device, extracting solution obtains tea-seed and/or oil-tea camellia seed crude oil after separation, reclaims extraction agent simultaneously.
2. the method for ultrasonic wave counter-current extraction tea-seed according to claim 1 and/or camellia seed oil, is characterized in that, described extraction agent is normal hexane.
3. the method for ultrasonic wave counter-current extraction tea-seed according to claim 1 and/or camellia seed oil, is characterized in that, described ultrasonic intensity scope is 50～250W, and the ul-trasonic irradiation time is 10～120min.
4. the method for ultrasonic wave counter-current extraction tea-seed according to claim 1 and/or camellia seed oil, is characterized in that, described temperature range is 30 ℃～45 ℃, and feed liquid mass ratio is 1:6.
5. the method for ultrasonic wave counter-current extraction tea-seed according to claim 1 and/or camellia seed oil, is characterized in that, described tea-seed and/or its moisture controlled of tea seed raw material, 2%～8%, are crushed to 16 order～60 orders.
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| CN110721240A (en) * | 2019-11-29 | 2020-01-24 | 江南大学 | Method for extracting fat-soluble polyphenols with different forms in camellia oleosa seed oil |
| CN110923058A (en) * | 2019-12-24 | 2020-03-27 | 贵州航天乌江机电设备有限责任公司 | Method for controlling harmful substances in edible vegetable oil |
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Application publication date: 20140430 |