CN107446693A - A kind of method of ultrasonic wave vapour-liquid coexistence state ethanol fluid oil and grease extracting - Google Patents
A kind of method of ultrasonic wave vapour-liquid coexistence state ethanol fluid oil and grease extracting Download PDFInfo
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- CN107446693A CN107446693A CN201710816528.XA CN201710816528A CN107446693A CN 107446693 A CN107446693 A CN 107446693A CN 201710816528 A CN201710816528 A CN 201710816528A CN 107446693 A CN107446693 A CN 107446693A
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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
- 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
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
-
- 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
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- 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
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- 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
- C11B3/16—Refining fats or fatty oils by mechanical means
Abstract
The invention discloses a kind of method of ultrasonic wave vapour-liquid coexistence state ethanol fluid oil and grease extracting.The method of the present invention be first by nut through vacuum dehydrating at lower temperature, crush, then using ethanol as solvent, and sodium chloride is added in system, with reference to ultrasonic technology, realizes the oil extraction of nut raw material；The inventive method passes through the accurate control to extraction process heating-up temperature, feed temperature, reaction system pressure, ethanol is set to be in vapour-liquid admixture all the time in extraction process, solubility property of the ethanol to grease is greatly improved, so as to obtain higher extraction efficiency and extraction yield；Compared with other traditional pressing methods, solvent extraction process, extracting process, the present invention also has the advantages such as extraction temperature is relatively low, side reaction is few, extraction yield is high, oil quality is high, nontoxic no solvent residue, production cost are low.
Description
Technical field
The present invention relates to a kind of method of oil and grease extracting, specifically a kind of ultrasonic wave-vapour-liquid coexistence state ethanol fluid extraction
The method of grease, belong to organic matter abstraction technique field.
Background technology
It is a kind of growth in humans is developed, built up health, in advance rich in protein, grease, mineral matter, vitamin in nut
Anti- disease has the food of the effect of fabulous, and the fat that wherein nut contains may be up to more than 58.8%, by extracting in nut
Grease can be directly used for the fields such as food, daily use chemicals.
The extracting process of nut grease common are the methods of squeezing, solvent extraction, subcritical abstraction, supercritical extract.
Existing extracting process, in order to obtain higher oil yield, using be gasoline, n-hexane, isopropanol, liquefied gas, methane etc. make
For extractant, these extractants are not as thorough in removed, and can remain in oil product, influence oil quality, bring potential danger
Evil；Some extracting process, such as supercritical extract, need expensive extraction equipment so that cost increase, burden, skill are brought to enterprise
Art conversion faces awkward situation.
The content of the invention
For above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of ultrasonic wave-vapour-liquid coexistence state ethanol stream
The method of body oil and grease extracting.
Technical scheme is as follows：A kind of method of ultrasonic wave-vapour-liquid coexistence state ethanol fluid oil and grease extracting, including
Following steps：
（1）The pretreatment of raw material：The removal of impurities of nut kernel, vacuum dehydrating at lower temperature to water content are less than 12%；
（2）The crushing of raw material：Dried kernel is refrigerated to -10 to -20 DEG C, by air-stream type ultrafine pulverizer, by kernel
Granularity is crushed to as 100-300 μm, crushes temperature control less than 90 DEG C；
（3）Ultrasound-assisted extraction：Kernel after crushing and ethanol are pressed into solid-liquid ratio 1:1-1:After 15 are mixed, chlorination is added
Sodium, it is placed in ultrasonic response kettle, the mixed liquor in reactor is heated, carries out ultrasound-assisted extraction；
Wherein, hot water jacket's formula reactor is used in the reactor, condenser is set at the top of reactor；In the reactor
Mixed liquor heating is by the hot water heating in chuck, and the temperature of hot water is used with Gradient rate-determining steps in chuck：First will
Hot water temperature is controlled at 90-100 DEG C, when mixed liquor temperature is up to 70 ± 2 DEG C, is reduced hot water temperature to 80-95 DEG C, is passed through tune
The size of hot water inlet is saved, it is 75-90 DEG C to control mixed liquor temperature；
The ultrasound-assisted extraction, reacting system pressure is 0.1MPa, ultrasonic power 500W-1000W in reactor, extraction
Take time 30-120min；
（4）Extract separation of solid and liquid：When extraction terminates, stopping heating, reactor evaporator overhead condenser does not have condensed fluid to drip down
When, feed liquid separation is carried out, is comprised the concrete steps that：Extract is filtered using 50 μm of high pressure filter membrane or centrifuged by tubular type
Machine, separation of solid and liquid being carried out under centrifuge speed 18000r/min, the liquid obtained after separation is cooled further to 25-40 DEG C,
Stratification, upper strata are ethanol, and middle level is oil, and lower floor is salt deposit, collects oil reservoir, obtain crude oil, crude oil is again by decolourizing, at deodorization
Reason, obtain product oil.
Preferably, the vacuum dehydrating at lower temperature condition is：50-60 DEG C of drying temperature, drying time 10-15h.
Preferably, the volumetric concentration of the ethanol is 80-100%.
Preferably, the addition of the sodium chloride is the 1-5% of ethanol addition.
Preferably, in step（3）During ultrasound-assisted extraction, when the temperature in reactor reaches the azeotropic of system
Point, ethanol start to evaporate, and steam state ethanol starts to condense in the presence of the condensing unit at the top of reactor, when being back in kettle,
The inflow of the cold water of condenser is controlled in 1-3Kg/min.
Found by years of researches, when ethanol is heated to 60-80 DEG C, and ethanol is in vapour-liquid coexistence state, in the temperature
Have very strong dissolubility in the range of degree to the fat in nut, based on this, the present invention by using ethanol as extractant,
Using the treatment conditions of the present invention, first by nut pretreatment of raw material, temperature is heated with reference to ultrasonic technology, and by accurately controlling
Degree, extraction temperature（Mixed liquor temperature）, the condition such as reaction system pressure, ethanol is mixed all the time in vapour-liquid in extraction process
Conjunction state, utilization can obtain higher oil yield and more preferably oil quality.The inventive method is particularly suitable for use in cashew nut, Australia
The oil extraction of one or more of nut raw materials in the grease type nuts such as nut, tea seed kernel.
Relative to prior art, the present invention has following advantageous effects：
（1）By nut raw material by vacuum dehydrating at lower temperature, brittle point is cooled to, particle diameter is broken into the presence of airslide disintegrating mill
Less particle, material temperature in pulverizer can be protected to be less than 100 DEG C, reduce the oxidation of raw oil material and other nutritional ingredients
Loss, improve the edible quality of grease；
（2）Using ultrasound-assisted extraction, the agent of ultrasonic wave facilitated extraction and the mixing of extract, promote the dissolution of grease, shorten
Extraction time, improve extraction efficiency；
（3）It with the addition of sodium chloride powder so that the azeotropic point increase of alcohol-water-sodium chloride mixed system, add pair of ethanol
The solubility of grease, ethanol are changed into vapour-liquid state coexistence state from liquid, and vapour-liquid coexistence state boiling point improves, and ethanol pair is greatly improved
The solubility property of grease；
（4）Compared with other traditional pressing methods, extraction temperature is relatively low, reduces nut oil and the reaction such as oxidation occurs, improve
The quality of oil, while the recovery rate of oil is higher；Nut grease is extracted using the method for the present invention, the yield of crude oil is up to 60%-
85%；
（5）With other traditional solvents（Gasoline, n-hexane, isopropanol）Extracting method and subcritical extraction method（Liquefied gas tank, first
Alkane etc.）Compare, using ethanol as solvent, ethanol is a kind of edible, nontoxic raw material, residual without poisonous and harmful solvent
Stay, improve the quality of oil；
（6）Compared with supercritical extraction method, the inventive method equipment investment cost is low, and cost is also low in extraction process, enters one
Step reduces the production cost of enterprise.
Embodiment
The present invention is described in further details below by embodiment, these embodiments are only used for illustrating the present invention, and
Do not limit the scope of the invention.
Embodiment 1 realizes the present invention using following steps：
（1）The pretreatment of raw material：Queensland nut kernel is taken, is cleaned, vacuum dehydrating at lower temperature to water content is less than 12%；What is used is true
Empty low temperature drying condition is：50-60 DEG C of drying temperature, drying time 12h；
（2）The crushing of raw material：Dried kernel is refrigerated to -10 DEG C, by air-stream type ultrafine pulverizer, kernel be crushed to
Granularity is 200 μm, crushes temperature control less than 90 DEG C；
（3）Ultrasound-assisted extraction：Kernel after crushing and volumetric concentration are pressed into solid-liquid ratio 1 for 90% ethanol:10 are mixed
Afterwards, the sodium chloride powder of ethanol addition 2.5% is added, is placed in ultrasonic response kettle, the mixed liquor in reactor is added
Heat, carry out ultrasound-assisted extraction；
Wherein, hot water jacket's formula reactor is used in reactor, condenser is set at the top of reactor；Mixing in the reactor
Feed liquid heating is by the hot water heating in chuck, and the temperature of hot water is used with Gradient rate-determining steps in chuck：First by hot water
Temperature control is at 90-100 DEG C, when mixed liquor temperature is up to 70 ± 2 DEG C, hot water temperature is reduced to 80-95 DEG C, by adjusting heat
The size of water inlet, it is 75-90 DEG C to control mixed liquor temperature；
Ultrasound-assisted extraction process, it is 0.1MPa, ultrasonic power 800W to control reacting system pressure in reactor, is extracted
Time 90min；
In step（3）During ultrasound-assisted extraction, when the temperature in reactor reaches the azeotropic point of system, ethanol starts to steam
Hair, steam state ethanol starts to condense in the presence of the condensing unit at the top of reactor, when being back in kettle, controls the cold of condenser
The inflow of water is in 1-3kg/min；
（4）Extract separation of solid and liquid：When extraction terminates, stopping heating, reactor evaporator overhead condenser does not have condensed fluid to drip down
When, feed liquid separation is carried out, is comprised the concrete steps that：Extract is filtered using 50 μm of high pressure filter membrane or centrifuged by tubular type
Machine, separation of solid and liquid being carried out under centrifuge speed 18000r/min, the liquid obtained after separation is cooled further to 25-40 DEG C,
Stratification, upper strata are ethanol, and middle level is oil, and lower floor is salt deposit, collects oil reservoir, obtain crude oil, crude oil is again by decolourizing, at deodorization
Reason, obtain product oil, recovery rate 75.24%.
Embodiment 2 realizes the present invention using following steps：
（1）The pretreatment of raw material：Queensland nut kernel is taken, is cleaned, vacuum dehydrating at lower temperature to water content is less than 12%；What is used is true
Empty low temperature drying condition is：50-60 DEG C of drying temperature, drying time 15h；
（2）The crushing of raw material：Dried kernel is refrigerated to -20 DEG C, by air-stream type ultrafine pulverizer, kernel be crushed to
Granularity is 300 μm, crushes temperature control less than 90 DEG C；
（3）Ultrasound-assisted extraction：Kernel after crushing and volumetric concentration are pressed into solid-liquid ratio 1 for 80% ethanol:15 are mixed
Afterwards, the sodium chloride powder of ethanol addition 5% is added, is placed in ultrasonic response kettle, the mixed liquor in reactor is heated,
Carry out ultrasound-assisted extraction；
Wherein, hot water jacket's formula reactor is used in reactor, condenser is set at the top of reactor；Mixing in the reactor
Feed liquid heating is by the hot water heating in chuck, and the temperature of hot water is used with Gradient rate-determining steps in chuck：First by hot water
Temperature control is at 90-100 DEG C, when mixed liquor temperature is up to 70 ± 2 DEG C, hot water temperature is reduced to 80-95 DEG C, by adjusting heat
The size of water inlet, it is 75-90 DEG C to control mixed liquor temperature；
Ultrasound-assisted extraction process, it is 0.1MPa, ultrasonic power 1000W to control reacting system pressure in reactor, is extracted
Take time 120min；
In step（3）During ultrasound-assisted extraction, when the temperature in reactor reaches the azeotropic point of system, ethanol starts to steam
Hair, steam state ethanol starts to condense in the presence of the condensing unit at the top of reactor, when being back in kettle, controls the cold of condenser
The inflow of water is in 1-3kg/min；
（4）Extract separation of solid and liquid：When extraction terminates, stopping heating, reactor evaporator overhead condenser does not have condensed fluid to drip down
When, feed liquid separation is carried out, is comprised the concrete steps that：Extract is filtered using 50 μm of high pressure filter membrane or centrifuged by tubular type
Machine, separation of solid and liquid being carried out under centrifuge speed 18000r/min, the liquid obtained after separation is cooled further to 25-40 DEG C,
Stratification, upper strata are ethanol, and middle level is oil, and lower floor is salt deposit, collects oil reservoir, obtain crude oil, crude oil is again by decolourizing, at deodorization
Reason, obtain product oil, recovery rate 82.4%.
Embodiment 3 realizes the present invention using following steps：
（1）The pretreatment of raw material：Cashew kernel is taken, is cleaned, vacuum dehydrating at lower temperature to water content is less than 12%；The vacuum of use is low
Warm drying condition is：50-60 DEG C of drying temperature, drying time 15h；
（2）The crushing of raw material：Dried kernel is refrigerated to -15 DEG C, by air-stream type ultrafine pulverizer, kernel be crushed to
Granularity is 100 μm, crushes temperature control less than 90 DEG C；
（3）Ultrasound-assisted extraction：Kernel after crushing and volumetric concentration are pressed into solid-liquid ratio 1 for 85% ethanol:1 is mixed
Afterwards, the sodium chloride powder of ethanol addition 1% is added, is placed in ultrasonic response kettle, the mixed liquor in reactor is heated,
Carry out ultrasound-assisted extraction；
Wherein, hot water jacket's formula reactor is used in reactor, condenser is set at the top of reactor；Mixing in the reactor
Feed liquid heating is by the hot water heating in chuck, and the temperature of hot water is used with Gradient rate-determining steps in chuck：First by hot water
Temperature control is at 90-100 DEG C, when mixed liquor temperature is up to 70 ± 2 DEG C, hot water temperature is reduced to 80-95 DEG C, by adjusting heat
The size of water inlet, it is 75-90 DEG C to control mixed liquor temperature；
Ultrasound-assisted extraction process, it is 0.1MPa, ultrasonic power 500W to control reacting system pressure in reactor, is extracted
Time 30min；
In step（3）During ultrasound-assisted extraction, when the temperature in reactor reaches the azeotropic point of system, ethanol starts to steam
Hair, steam state ethanol starts to condense in the presence of the condensing unit at the top of reactor, when being back in kettle, controls the cold of condenser
The inflow of water is in 1-3kg/min；
（4）Extract separation of solid and liquid：When extraction terminates, stopping heating, reactor evaporator overhead condenser does not have condensed fluid to drip down
When, feed liquid separation is carried out, is comprised the concrete steps that：Extract is filtered using 50 μm of high pressure filter membrane or centrifuged by tubular type
Machine, separation of solid and liquid being carried out under centrifuge speed 18000r/min, the liquid obtained after separation is cooled further to 25-40 DEG C,
Stratification, upper strata are ethanol, and middle level is oil, and lower floor is salt deposit, collects oil reservoir, obtain crude oil, crude oil is again by decolourizing, at deodorization
Reason, product oil is obtained, extract yield 70.02%.
Claims (6)
- A kind of 1. method of ultrasonic wave-vapour-liquid coexistence state ethanol fluid oil and grease extracting, it is characterised in that：Comprise the following steps：（1）The pretreatment of raw material：The removal of impurities of nut kernel, vacuum dehydrating at lower temperature to water content are less than 12%；（2）The crushing of raw material：Dried kernel is refrigerated to -10 to -20 DEG C, by air-stream type ultrafine pulverizer, by kernel Granularity is crushed to as 100-300 μm, crushes temperature control less than 90 DEG C；（3）Ultrasound-assisted extraction：Kernel after crushing and ethanol are pressed into solid-liquid ratio 1:1-1:After 15 are mixed, chlorination is added Sodium, it is placed in ultrasonic response kettle, the mixed liquor in reactor is heated, carries out ultrasound-assisted extraction；Wherein, hot water jacket's formula reactor is used in the reactor, condenser is set at the top of reactor；In the reactor Mixed liquor heating is by the hot water heating in chuck, and the temperature of hot water is used with Gradient rate-determining steps in chuck：First will Hot water temperature is controlled at 90-100 DEG C, when mixed liquor temperature is up to 70 ± 2 DEG C, is reduced hot water temperature to 80-95 DEG C, is passed through tune The size of hot water inlet is saved, it is 75-90 DEG C to control mixed liquor temperature；The ultrasound-assisted extraction, reacting system pressure is 0.1MPa, ultrasonic power 500W-1000W in reactor, extraction Take time 30-120min；（4）Extract separation of solid and liquid：When extraction terminates, stopping heating, reactor evaporator overhead condenser does not have condensed fluid to drip down When, feed liquid separation is carried out, is comprised the concrete steps that：Extract is filtered using 50 μm of high pressure filter membrane or centrifuged by tubular type Machine, separation of solid and liquid being carried out under centrifuge speed 18000r/min, the liquid obtained after separation is cooled further to 25-40 DEG C, Stratification, upper strata are ethanol, and middle level is oil, and lower floor is salt deposit, collects oil reservoir, obtain crude oil, crude oil is again by decolourizing, at deodorization Reason, obtain product oil.
- 2. according to the method for claim 1, it is characterised in that：The vacuum dehydrating at lower temperature condition is：Drying temperature 50-60 DEG C, drying time 10-15h.
- 3. according to the method for claim 1, it is characterised in that：The volumetric concentration of the ethanol is 80-100%.
- 4. according to the method for claim 1, it is characterised in that：The addition of the sodium chloride is the 1- of ethanol addition 5%。
- 5. according to the method for claim 1, it is characterised in that：In step（3）During ultrasound-assisted extraction, work as reaction Temperature in kettle reaches the azeotropic point of system, and ethanol starts to evaporate, the effect of condensing unit of the steam state ethanol at the top of reactor Under start to condense, when being back in kettle, control the inflow of cold water of condenser in 1-3Kg/min.
- 6. according to the method for claim 1, it is characterised in that：The nut be cashew nut, Queensland nut, tea seed kernel or One or more in grease type nut.
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| CN201710816528.XA CN107446693B (en) | 2017-09-12 | 2017-09-12 | Method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid |
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| CN201710816528.XA CN107446693B (en) | 2017-09-12 | 2017-09-12 | Method for extracting grease by ultrasonic-vapor-liquid coexisting state ethanol fluid |
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| CN107446693B CN107446693B (en) | 2020-08-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113133690A (en) * | 2020-01-17 | 2021-07-20 | 广东美的生活电器制造有限公司 | Food processing apparatus, control method, control device, and storage medium |
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