CN105602719B - A kind of supercritical extraction method of tea oil - Google Patents

A kind of supercritical extraction method of tea oil Download PDF

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Publication number
CN105602719B
CN105602719B CN201610143939.2A CN201610143939A CN105602719B CN 105602719 B CN105602719 B CN 105602719B CN 201610143939 A CN201610143939 A CN 201610143939A CN 105602719 B CN105602719 B CN 105602719B
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time
tea
oil
tea oil
extraction
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CN105602719A (en
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刘汉槎
刘粤华
伍淑华
沈玉优
许建宇
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GUANGZHOU LYUHEYUAN BIO-TECHNOLOGY Co Ltd
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GUANGZHOU LYUHEYUAN BIO-TECHNOLOGY Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/006—Refining fats or fatty oils by extraction
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C11B1/04—Pretreatment of vegetable raw material
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/06—Production of fats or fatty oils from raw materials by pressing

Abstract

The present invention provides the supercritical extraction method of a kind of tea oil, comprises the steps: the pre-treatment of S1. raw material: take tea seed, shell, and after first time microwave drying and second time microwave drying, obtains dried tea seed kernel；S2. the preparation of tea oil crude oil: filtered after cold press by described tea seed kernel, obtains tea oil crude oil；S3. supercritical CO2Refining: described tea oil crude oil is sent into supercritical CO2In device, after extraction for the first time and second time extraction, collect raffinate, obtain finished product tea oil.The invention belongs to tea oil processing technique field, the method that the present invention provides decreases, while improving oil yield, the generation become sour, and while realizing Impurity removal, decreases the loss of the nutritional labelings such as vitamin E, and the tea oil quality stability obtained is good.

Description

A kind of supercritical extraction method of tea oil
Technical field
The invention belongs to tea oil processing technique field, particularly relate to the supercritical extraction method of a kind of tea oil.
Background technology
Tea oil, i.e. camellia seed oil, tea-seed oil, camellia oil, processed for the mature seed of Theaceae Camellia Plants tea oil tree The grease arrived.Tea oil look clear, taste is fragrant, and the content of the unrighted acid such as oleic acid, linoleic acid plus linolenic acid reaches more than 90%, also Containing nutritional labelings such as more rich vitamin E, vitamin D, squalene, sterol, phosphatide.The water content of fresh tea seed is led to It is often 20～30%, owing to water content is higher, therefore preserves for a long time and be susceptible to become sour, generally require after carrying out rapid draing Liquefaction or Cord blood immediately.
The tradition processing of tea oil mainly uses milling process and solvent extraction method liquefaction to dry tea seed, then through " five take off " technique Refining prepares finished product tea oil." five take off " technique refers to degumming, depickling, decolouring, deodorization and dewaxing.Not only complex process, five take off In, need to add alkali lye and carry out chemical reaction generation soap with the acid in oil, need washing to produce a large amount of waste water, in addition it is also necessary in oil Add bleaching earth adsorption to refilter out, produce waste residue, thus there is three wastes problem.Milling process is with applying physical pressure grease Separate from oil plant, derive from the method for producing oil in tradition workshop, the most again through " five take off " technique refining.Solvent extraction method one As use n-hexane make the grease in extraction tea seed, though solvent extraction method can extract liquefaction in high volume, but in the crude oil produced Impurity is many, tea oil lacks tea seed kernel fragrance.
Supercritical extract has the feature of rectifying and liquid-solid extraction concurrently, utilizes the pressure and temperature impact on supercritical fluid solvability And carry out the separation of material.Supercritical carbon dioxide fluid has the advantages such as safe noresidue, is to apply most supercritical fluids, It is widely used in preparation or the refining of tea oil.Chinese patent application CN 105018218 discloses the overcritical of a kind of tea-seed oil Extraction process, comprises the following steps: tea seed is dried, and removes tea seed episperm；The tea seed that will shell is pulverized；CO2Supercritical extract, stream Body extracting pressure is 20～40MPa, and temperature is 35～40 DEG C, and fluid flow is 700～800L/h, and the time is 1～5h, obtains tea Seed crude oil, the most again refrigerated centrifuge, obtain tea-seed oil.By this extraction process, tea oil can be extracted from tea seed powder, Owing to being to extract tea seed powder, the handling of solid material are more difficult, and extraction process needs higher pressure, therefore, deposits , service life disadvantageous problem to equipment big in equipment investment, is unfavorable for that large-scale industrialization produces.
Chinese patent application CN 103289816 discloses a kind of tea oil processing method, comprises the following steps: the low temperature drying of tea seed, Shell；Tea oil crude oil is prepared in cold press；Supercritical CO2Refining, pressure is 15～25MPa, and temperature is 30～60 DEG C, overcritical CO2Resolve in 7～12MPa and go the removal of impurity, it is thus achieved that finished product tea oil.This processing method is by extracting the tea oil crude oil of liquid The mode of impurity elimination obtains tea oil, although pressure is reduced to a certain extent, but has also extracted more while extracting impurities Active component, the yield causing tea oil is relatively low, loses more serious, and in tea oil, the content of the nutritional labeling such as vitamin E is managed not Think.
Summary of the invention
For solving problems of the prior art, pre-treatment and the super of tea oil crude oil of tea seed are faced by inventor by lot of experiments Boundary's extraction conditions is studied, unforeseeable discovery: is dried by the secondary microwave of specific wavelength and can realize the quick of tea seed Be dried and curing, decrease, improving while oil yield, the generation become sour, by the extraction of secondary different condition, realize miscellaneous While matter is removed, decreasing the loss of the nutritional labelings such as vitamin E, the tea oil quality stability obtained is good.Based on above-mentioned Existing, thus complete the present invention.
The purpose of the present invention will be further described in detail below reflect and description.
The present invention provides the supercritical extraction method of a kind of tea oil, comprises the steps:
The pre-treatment of S1 raw material: take tea seed, shell, after first time microwave drying and second time microwave drying, obtains dried tea Seed benevolence；
The preparation of S2 tea oil crude oil: filtered after cold press by described tea seed kernel, obtains tea oil crude oil；
S3 supercritical CO2Refining: described tea oil crude oil is sent into supercritical CO2In device, through extraction for the first time and second time extraction After, collect raffinate, obtain finished product tea oil.
Microwave has high frequency and fluctuation, and heating using microwave can be to hydrogen bond, hydrophobic bond and Van der Waals force generation effect so that it is weight New distribution, and then change the immanent structure of tea seed, causing cell rupture, drying efficiency is high, and follow-up squeezing is fuel-displaced.Additionally, The present invention is found through experiments, and needs to avoid long heating using microwave, to avoid the carbonization of tea seed.
Prior art is often by supercritical CO2Fluid is directly obtained by extraction finished product tea oil to tea seed kernel, mainly living of extraction Property composition, and the present invention is that tea oil crude oil is carried out supercritical CO2Fluid extraction removes the impurity such as malodorous elements, and raffinate is only Target product.
Under normal circumstances, supercritical CO2The extraction efficiency of the material that fluid is less to non-polar and polar is than the extraction of polar substances In hgher efficiency, solute is at supercritical CO2Solubility in fluid is easily stressed and the impact of temperature.The present invention is by difference After the parsing product of extraction conditions is studied, have found surprisingly that supercritical CO2Fluid is in the condition of low pressure (8～10MPa) Lower first extraction 30～50min, then pressure be 12MPa, temperature be 42 DEG C under conditions of extract 15～30min, free-fat The impurity solubility with this understanding such as acid are relatively big, and the solubility of vitamin E is less, can while realizing deacid-deodoring, Reduce the loss of the nutritional labelings such as vitamin E.Under conditions of pressure >=13MPa, temperature are 40 DEG C, free fatty and dimension Raw element E is at supercritical CO2Solubility in fluid is more or less the same, and while deacid-deodoring, the loss of vitamin E is bigger.
For small-sized supercritical CO2Device: dress tea oil crude oil 1～2kg, CO every time2Rate of flow of fluid is preferably 10～20L/h；Right In medium-sized supercritical CO2Device: dress tea oil crude oil 16～22kg, CO every time2Rate of flow of fluid is preferably 160～260L/h；For The large and super-critical CO of industrialization2Device: dress tea oil crude oil 200～400kg, CO every time2Rate of flow of fluid is preferably: 2000～3000L/h.
Preferably, the frequency of described first time microwave drying is 800～1000MHz, and drying time is 2～4min；Described second The frequency of secondary microwave drying is 800～1000MHz, and drying time is 1～2min；Described first time microwave drying and described second 5～20min it are spaced between secondary microwave drying；The water content of the tea seed after first time microwave drying and second time microwave drying is 5～8%.
Preferably, the frequency of described first time microwave drying is 912MHz, and the frequency of described second time microwave drying is 912MHz.
Preferably, the pressure of extraction of described first time be 8～10MPa, temperature be 32～36 DEG C, the time be 30～50min.
Tea oil crude oil is pumped into equipped with in the extraction column of filler by extraction column top, super faces with entered in extraction column by extraction column bottom Boundary CO2Fluid contacts, and the impurity in crude oil is dissolved in supercritical CO2In fluid, then supercritical CO2Fluid enters extraction-container In, by pressure drop as little as 5.5～7MPa, impurity then separates out, and discharges from floss hole, CO2Enter after condenser condenses again CO2Storage tank is used for recycle.By extracting for the first time, malodorous elements (such as low grade aldehyde etc.) can be removed, partly dissociate The impurity such as aliphatic acid.
It is highly preferred that the pressure of extraction of described first time be 9MPa, temperature be 35 DEG C, the time be 40min.
Preferably, the pressure of described second time extraction be 12～13MPa, temperature be 38～45 DEG C, the time be 15～30min. Extracted by second time, the impurity such as peroxide and remaining free fatty can be removed.
It is highly preferred that the pressure of described second time extraction be 12MPa, temperature be 42 DEG C, the time be 20min.
Preferably, described supercritical CO2Device includes the extraction column equipped with filler.It is highly preferred that described filler is stainless steel west Tower ring filler.
Preferably, the oil outlet temperature of described cold press is 40～55 DEG C.
Preferably, described tea seed is fresh tea seed or antistaled tea seed, and the water content of tea seed is 10～30%.Due to present invention offer Pre-treating method drying efficiency is high, directly can be dried fresh tea seed, the generation become sour with minimizing.
Compared with prior art, the invention has the beneficial effects as follows: the present invention is dried by the secondary microwave of specific wavelength, it is achieved that The rapid draing of tea seed and curing, drying efficiency is greatly improved, and decreases, while improving oil yield, the generation become sour；Pass through The extraction of secondary different condition, while realizing deacid-deodoring, decreases the loss of the nutritional labelings such as vitamin E, obtains Tea oil quality better, rich in nutrition content, quality stability is good.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail.
In the embodiment of the present invention, the mensuration of acid number uses GB/T 5530-2005 (animal and plant fat: acid number and acidity assaying), The mensuration of peroxide value uses GB/T 5538-2005 (animal and plant fat: peroxide value), and the mensuration of vitamin E uses height Effect liquid phase chromatogram method NY/T 1598-2008 (vitamin E prescription and the mensuration of content in edible vegetable oil), the mensuration of squalene Use high performance liquid chromatography.
The preparation of embodiment one tea oil crude oil
Taking fresh tea seed, water content is 20.6%, shells, through first time microwave drying and second time microwave drying, the most micro- The frequency that ripple is dried is 912MPa, and the time is 3min, after the 20min of interval, carries out second time microwave drying, for the first time microwave The frequency being dried is 912MPa, and the time is 1min, obtains dried tea seed kernel, and the water content of dried tea seed is 7.2%； Being pulverized by tea seed kernel and filter after cold press, oil outlet temperature is 50 DEG C, obtains tea oil crude oil.Tea oil crude oil is detected, acid number Being 3.2, peroxide value is 5.7.
The preparation of embodiment two tea oil crude oil
Taking fresh tea seed, water content is 20.6%, through first time microwave drying and second time microwave drying, for the first time microwave drying Frequency be 912MPa, the time is 2min, interval 15min after, carry out second time microwave drying, microwave drying for the first time Frequency is 912MPa, and the time is 2min, and the water content of dried tea seed is 7.0%, shells, obtains tea seed kernel；By tea seed Benevolence is pulverized, and filters after cold press, and oil outlet temperature is 50 DEG C, obtains tea oil crude oil.Detecting tea oil crude oil, acid number is 3.0, Peroxide value is 5.4.
The preparation of comparative example one tea oil crude oil
Taking fresh tea seed, water content is 20.6%, and through microwave drying, the frequency of microwave drying is 912MPa, and the time is 4min, The water content of dried tea seed is 7.3%, shells, obtains tea seed kernel；Tea seed kernel is pulverized, filters after cold press, go out oil temperature Degree is 50 DEG C, obtains tea oil crude oil.Detecting tea oil crude oil, acid number is 3.3, and peroxide value is 7.1.
Comparative example one is to be carried out continuously microwave drying with the difference of embodiment two.
The means of supercritical extraction of embodiment three tea oil
The tea oil crude oil 20kg that Example two prepares, is pumped into tea oil crude oil equipped with stainless steel western tower ring filler by extraction column top Extraction column in, supercritical CO2Entered in extraction column by extraction column bottom, after extraction for the first time and second time extraction, collect Raffinate, obtains finished product tea oil.The pressure extracted for the first time is 9MPa, temperature is 35 DEG C, CO2Flow velocity be 240L/h, time Between be 40min；The pressure of second time extraction is 12MPa, temperature is 42 DEG C, CO2Flow velocity is 240L/h, the time is 20min. In terms of tea oil crude oil, the mass yield of finished product tea oil is 98.5%.
The means of supercritical extraction of embodiment four tea oil
The tea oil crude oil 20kg that Example two prepares, is pumped into tea oil crude oil equipped with stainless steel western tower ring filler by extraction column top Extraction column in, supercritical CO2Entered in extraction column by extraction column bottom, after extraction for the first time and second time extraction, collect Raffinate, obtains finished product tea oil.The pressure extracted for the first time is 10MPa, temperature is 35 DEG C, CO2Flow velocity be 240L/h, time Between be 40min；The pressure of second time extraction is 12MPa, temperature is 42 DEG C, CO2Flow velocity is 240L/h, the time is 20min. In terms of tea oil crude oil, the mass yield of finished product tea oil is 97.7%.
The means of supercritical extraction of comparative example two tea oil
Take the tea oil crude oil that comparative example one prepares, tea oil crude oil is pumped into the extraction equipped with stainless steel western tower ring filler by extraction column top Take in post, supercritical CO2Entered in extraction column by extraction column bottom, after extraction for the first time and second time extraction, collect raffinate Liquid, obtains finished product tea oil.The pressure extracted for the first time is 9MPa, temperature is 35 DEG C, CO2Flow velocity is 240L/h, the time is 40min；The pressure of second time extraction is 12MPa, temperature is 42 DEG C, CO2Flow velocity is 240L/h, the time is 20min.
With the difference of embodiment three, comparative example two is that tea oil crude oil is prepared by comparative example one.In terms of tea oil crude oil, finished product tea oil Mass yield is 98.0%.
The means of supercritical extraction of comparative example three tea oil
The tea oil crude oil that Example two prepares, is pumped into the extraction equipped with stainless steel western tower ring filler by tea oil crude oil by extraction column top Take in post, supercritical CO2Entered in extraction column by extraction column bottom, after extraction, collect raffinate, obtain finished product tea oil. The pressure of extraction is 12MPa, temperature is 42 DEG C, CO2Flow velocity is 240L/h, the time is 60min.
Comparative example three is to carry out single extraction with the difference of embodiment three, and pressure is 12MPa, temperature is 42 DEG C.With tea oil hair Oil meter, the mass yield of finished product tea oil is 96.8%.
The means of supercritical extraction of comparative example four tea oil
The tea oil crude oil that Example two prepares, is pumped into the extraction equipped with stainless steel western tower ring filler by tea oil crude oil by extraction column top Take in post, supercritical CO2Entered in extraction column by extraction column bottom, after extraction, collect raffinate, obtain finished product tea oil. The pressure of extraction is 9MPa, temperature is 35 DEG C, CO2Flow velocity is 240L/h, the time is 60min.
Comparative example four is to carry out single extraction with the difference of embodiment three, and pressure is 9MPa, temperature is 35 DEG C.With tea oil hair Oil meter, the mass yield of finished product tea oil is 99.2%.
The means of supercritical extraction of comparative example five tea oil
The tea oil crude oil that Example two prepares, is pumped into the extraction equipped with stainless steel western tower ring filler by tea oil crude oil by extraction column top Take in post, supercritical CO2Entered in extraction column by extraction column bottom, after extraction for the first time and second time extraction, collect raffinate Liquid, obtains finished product tea oil.The pressure extracted for the first time is 9MPa, temperature is 35 DEG C, CO2Flow velocity is 240L/h, the time is 40min；The pressure of second time extraction is 16MPa, temperature is 42 DEG C, CO2Flow velocity is 240L/h, the time is 20min.
With the difference of embodiment three, comparative example five is that the pressure that second time extracts is 16MPa.In terms of tea oil crude oil, finished product tea oil Mass yield be 95.3%.
Test example one: the detection of finished product tea oil
The finished product tea oil preparing embodiment three, comparative example two, comparative example three, comparative example four and comparative example five detects, knot Fruit is as shown in table 1.
The finished product tea oil detection that table 1 Different Extraction Method obtains
Acid number Peroxide value Vitamin E (mg/kg) Squalene (mg/kg)
Embodiment three 0.3 3.9 252 168
Comparative example two 0.4 5.2 237 161
Comparative example three 0.3 4.0 191 153
Comparative example four 1.2 6.3 205 174
Comparative example five 0.3 3.6 146 133
As known from Table 1, acid number and the peroxide value of the finished product tea oil that the embodiment of the present invention two prepares are relatively low, reach GB Primary standard in 11765-2003 (camellia seed oil standard test), and the content of vitamin E and squalene is higher.
Test example two: the stability of finished product tea oil
The finished product tea oil preparing embodiment three, comparative example two, comparative example three, comparative example four and comparative example five carries out stability and examines Examining, result is as shown in table 2.
The finished product tea oil stability that table 2 Different Extraction Method obtains
As known from Table 2, the good stability of the finished product tea oil that the embodiment of the present invention two prepares, remain to reach GB after preserving 18 months Primary standard in 11765-2003 (camellia seed oil standard test), acid number and peroxide value are relatively low.
Above content is to combine concrete preferred embodiment further description made for the present invention, it is impossible to assert the present invention Be embodied as be confined to these explanations.For general technical staff of the technical field of the invention, without departing from this On the premise of inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.

Claims (7)

1. the supercritical extraction method of a tea oil, it is characterised in that: comprise the steps:
The pre-treatment of S1 raw material: take tea seed, shell, after first time microwave drying and second time microwave drying, To dried tea seed kernel；
The preparation of S2 tea oil crude oil: filtered after cold press by described tea seed kernel, obtains tea oil crude oil；
S3 supercritical CO2Refining: described tea oil crude oil is sent into supercritical CO2In device, through for the first time extraction and After second time extraction, collect raffinate, obtain finished product tea oil；
The frequency of described first time microwave drying is 800～1000MHz, and drying time is 2～4min；Described second The frequency of secondary microwave drying is 800～1000MHz, and drying time is 1～2min；Described first time microwave is done 5～20min it are spaced between dry and described second time microwave drying；
The pressure of extraction of described first time is 8～10MPa, temperature is 32～36 DEG C, the time is 30～50min；
The pressure of described second time extraction is 12～13MPa, temperature is 38～45 DEG C, the time is 15～30min.
The supercritical extraction method of tea oil the most according to claim 1, it is characterised in that: described first time is micro- The frequency that ripple is dried is 912MHz, and the frequency of described second time microwave drying is 912MHz.
The supercritical extraction method of tea oil the most according to claim 1, it is characterised in that: described first time extracts The pressure taken is 9MPa, temperature is 35 DEG C, the time is 40min.
The supercritical extraction method of tea oil the most according to claim 1, it is characterised in that: described second time extracts The pressure taken is 12MPa, temperature is 42 DEG C, the time is 20min.
The supercritical extraction method of tea oil the most according to claim 1, it is characterised in that: described supercritical CO2 Device includes the extraction column equipped with filler.
The supercritical extraction method of tea oil the most according to claim 1, it is characterised in that: going out of described cold press Oil temperature is 40～55 DEG C.
The supercritical extraction method of tea oil the most according to claim 1, it is characterised in that: described tea seed is new Fresh tea seed or antistaled tea seed, the water content of tea seed is 10～30%.
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CN106433985B (en) * 2016-10-12 2018-06-29 广东聿津食品有限公司 A kind of ginger essential oil and preparation method thereof
CN109593596A (en) * 2018-12-19 2019-04-09 浙江晟泰茶油科技有限公司 A kind of extraction process of high quality tea oil
CN110106015A (en) * 2019-05-15 2019-08-09 诸暨市众创机械设备厂 A kind of refining technique of tea-seed oil and its application in health-care oil
CN110791376B (en) * 2019-10-22 2024-02-06 广东轻工职业技术学院 Supercritical CO 2 Method for removing free fatty acid in camellia seed oil by microemulsion
CN112831368A (en) * 2021-01-07 2021-05-25 吉林农业大学 Preparation method of cyperus esculentus oil

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