CN107057852A - A kind of preparation method of unrighted acid tea oil - Google Patents

A kind of preparation method of unrighted acid tea oil Download PDF

Info

Publication number
CN107057852A
CN107057852A CN201710502895.2A CN201710502895A CN107057852A CN 107057852 A CN107057852 A CN 107057852A CN 201710502895 A CN201710502895 A CN 201710502895A CN 107057852 A CN107057852 A CN 107057852A
Authority
CN
China
Prior art keywords
tea oil
time
standby
reaction
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710502895.2A
Other languages
Chinese (zh)
Other versions
CN107057852B (en
Inventor
管天球
管敏
管晖
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201710502895.2A priority Critical patent/CN107057852B/en
Publication of CN107057852A publication Critical patent/CN107057852A/en
Application granted granted Critical
Publication of CN107057852B publication Critical patent/CN107057852B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04—Working-up
    • 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
    • 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/04—Refining fats or fatty oils by chemical reaction with acids
    • 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
    • C11B3/10—Refining fats or fatty oils by adsorption
    • 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
    • C11B3/12—Refining fats or fatty oils by distillation
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
    • C11C3/003—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fatty acids with alcohols

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Fats And Perfumes (AREA)

Abstract

A kind of preparation method of unrighted acid tea oil disclosed by the invention, is related to vegetable oil processing technique field, its preparation technology is as follows：(1), just processing：1., decolourize for the first time；2., second of decolouring；3., wash for the first time；(2), it is esterified:1., esterification；2., neutralize for the first time；3., distill；4., extract for the first time；(3), urea is complexed：1., complex reaction；2., filter；3., second of washing；(4), esterification reconstruction:1., interesterification reacts；2., removal of impurities；3., second of neutralization；4., second of extraction；(5), precision processing：1., concentrate；2., cool down；3., refined filtration.The features such as with can effectively remove in tea oil contained saturated fatty acid, and then produce the tea oil without saturated fatty acid, it can be not only used for preparing unrighted acid tea oil, it can also be used to prepare other unrighted acid vegetable oil.

Description

A kind of preparation method of unrighted acid tea oil
Technical field
The present invention relates to vegetable oil processing technique field, particularly a kind of preparation method of unrighted acid tea oil.
Background technology
Aliphatic acid needed by human is divided into saturated fatty acid, monounsaturated fatty acids (predominantly oleic acid) and how unsaturated fat Fat acid, excessive saturated fatty acid is the arch-criminal of human body diseases, if its content has exceeded 12%, will be produced in human body Raw fat generation, and then trigger the serious cardiovascular and cerebrovascular diseases such as hypertension, high fat of blood, artery sclerosis.Monounsaturated fatty acids It is a kind of safe fats acid, it is highly beneficial to people body-centered, brain, lung, blood vessel.The monounsaturated fatty acids (oleic acid) contained in edible oil More, its nutritive value is higher.
Camellia seed oil (being commonly called as tea oil) also known as Wild camellia seed oil, camellia oil, are pure natural senior woody edible oils, and it is unsaturated Content of fatty acid is up to 85% or so.Under normal circumstances, after camellia seed oil is processed by refining (or even non-refined crude oil), That is edible, still.Still containing 12% or so saturated fatty acid in tea oil, after eating, cardiovascular and cerebrovascular disease is suffered to those The crowd of disease, can still bring harmful effect.
A kind of disclosed " the unrighted acid in sunflower oil of Chinese patent (number of patent application is 201310601243.6) Extracting method ", comprise the following steps that：First, sunflower oil raw material is prepared, it is desirable to which it is taken the photograph using preceding needs not higher than five Refrigerated in the environment of family name's degree；Then sodium hydroxide solution of the mass fraction more than 90 percent with three times volume is carried out Mixing；It is positioned over immediately in hydrogen environment；Squeezing, concentration；Freezing is put into after separation of solid and liquid；Temperature control, three circular press, i.e., Can.The freezing environment refers to that temperature is not higher than subzero ten degrees Celsius of condition；The beneficial effect of the invention is：Extracted not Saturated fatty acid, stability is very high, and purity is also high, and the invigoration effect for natural is obvious.
Another Chinese patent (number of patent application is 201410187831.4) is disclosed, and " one kind extracts high-purity from soybean oil The method of unrighted acid ", step is as follows：(1) preparation of unrighted acid is mixed：Using soybean oil as raw material, add big 3~6% Al of soya-bean oil weight2O3- MgO catalyst, its reaction temperature is 150~200 DEG C, makes fatty acid glycerine in soybean oil Ester and water reaction generation fatty acid mixed crude product, then pass through and catalyst is recovered by filtration obtains fatty acid mixed filtrate；(2) it is high-purity The preparation of unrighted acid：The oleate of pentaerythrite four of filtrate weight 5~15% is added into fatty acid mixed filtrate, is risen 5-15 DEG C is cooled to after temperature to 60 DEG C of uniform dissolutions, crystallizes, filter, filtrate is high pure unsaturated fatty acid；The invented technology is walked Rapid simple, reaction condition is gentle, and reaction temperature is low, in the Al of selection2O3The lower soybean oil hydrolysis of-MgO solid acid alkali catalytics agent effect Fully, unrighted acid of the catabolite Jing Guo low temperature crystallization activity high-purity, filtrate can be used with repetitive cycling, not produced Extra production waste water.
Also Chinese patent (number of patent application is 201310221671.6) is disclosed " a kind of from the oily mixing-in fat of Snakegourd Fruit seed The method of enriching and purifying polyunsaturated fatty acid in acid ", using the oily fatty acid mixed of Snakegourd Fruit seed as raw material, using urea adduct method pair Polyunsaturated fatty acid (PUFA) in fatty acid mixed carries out enriching and purifying.The purification process comprises the following steps：Prepare urine Element-methanol solution → fatty acid mixed-urea-methyl alcohol mixed liquor → inclusion → suction filtration is separated → collects filtrate → extraction organic phase → washing → drying → is concentrated under reduced pressure → PUFA products.
" a kind of Jatropha curcus grease how unsaturated also disclosed in Chinese patent (number of patent application is 201010278686.2) The isolated method of aliphatic acid ", croude fatty acids, urea and methanol obtain urea inclusion by dissolving by heating, freezing, being separated by filtration And filtrate, the obtained sticky solid formation petroleum ether extraction of filtrate decompression distillation, extraction phase vacuum distillation is light through what is be enriched with Yellow fat acid, the method included stage by stage using precooling-freezing during PUFAs is isolated, first at 0.5~-5 DEG C before freezing Lower precooling 1h, then freezes 2h at 0.5~-30 DEG C again；PUFAs purity is in the faint yellow aliphatic acid being enriched with 69.38~100%, PUFAs yield are 9.63~54.51%.Described urea inclusion reclaims urine therein by processing Element and aliphatic acid, the urea of recovery participate in inclusion reaction again.
The content of the invention
The technical problems to be solved by the invention are to provide the saturated fatty acid contained by a kind of can effectively remove in tea oil, And then produce the preparation method of the tea oil without saturated fatty acid.
In order to solve the above technical problems, the technical solution used in the present invention is the preparation of invention unrighted acid tea oil Method, its preparation technology is as follows：
(1), just processing：
1., decolourize for the first time：First the silica decoloration sand of 80-120 mesh is fitted into container, it is container height to load height 60-70%, then, raw material tea oil is pumped into by the top of container, allows raw material tea oil to be flowed downward naturally along silica decoloration sand, is received Collect the first time decolouring tea oil of outflow, it is standby；
2., second of decolouring：Particle diameter is fitted into container for 0.1-0.25cm activated carbon again, loads height to hold The 40-50% of device height, then, first time decolouring tea oil is pumped into by the top of container, makes first time decolouring tea oil edge active Charcoal flows downward naturally, collects second of decolouring tea oil of outflow, standby；
3., wash for the first time：
It is the second that 9-10, volumetric concentration are 25-38% that second of decolouring tea oil, which is put into, and accounts for 3-5 times of its weight, pH value In alcohol solution, the stir process 50-70min at 60-70 DEG C, then stand, be layered, filter, oil reservoir is collected, obtains washing for the first time Tea oil is washed, it is standby；
(2), it is esterified:
1., esterification：By first time washing tea oil with accounting for its weight 15-26% absolute ethyl alcohol and accounting for its weight 0.6- 1.5% caustic alcohol is mixed and stirred for, until oil/alkanol interface disappearance (under normal circumstances, its reaction time is 35-75min), Mixing tea oil must be esterified, it is standby；
2., neutralize for the first time：
By the C of equimolar amounts1~C4Organic acid is added in esterification mixing tea oil, carries out closing reaction in first time, middle to close anti- It is 30-50min between seasonable, reaction temperature is 40-48 DEG C, obtains first time neutralization reaction mixing tea oil, standby；
3., distill：
In temperature it is 50-70 DEG C, under the conditions of pressure is 5-10KPa by first time neutralization reaction mixing tea oil, distillation to nothing Ethanol state, reclaims absolute ethyl alcohol and remaining distillation tea oil, standby；
4., extract for the first time：
Using organic solvent as extractant, residue distillation tea oil is extracted at normal temperatures, the consumption of extractant is 1-2 times of residue distillation tea oil weight, is extracted 3 times, combining extraction liquid；Then, it is 45-65 DEG C, pressure in temperature by extract To be concentrated into no extractant residual under 5-10KPa, concentrate is obtained, then concentrate in refrigerating chamber refrigerated into 5-6h (temperature is usually 4-10 DEG C), then filter, obtain the first time extraction mixing containing saturated fat acid alkyl ester and unsaturated fat acid alkyl ester Thing, it is standby；
(3), urea is complexed：
1., complex reaction：Added into first time extraction mixture and account for its weight 10-18% urea, account for its weight 30- 38%th, volumetric concentration is 80-90% ethanol solution, mixes, urea is then heated in 60-70 DEG C of water-bath completely molten Solution, then complex reaction 12-18h is carried out at room temperature, complex compound is obtained, it is standby；
2., filter：Complex compound is filtered by vacuum through fast grade filter paper, the knot of urea-saturated fat acid complex therein is removed Brilliant complex compound, collects filtered fluid, standby；
3., second of washing：Filtered fluid is put into the warm water that 2-4 times of weight, temperature are 60-70 DEG C, at insulated and stirred Manage 1-2.5h, stand, layering, it is to be cooled arrive room temperature when, collect oil reservoir, obtain second of washing tea oil, it is standby；
(4), esterification reconstruction:
1., interesterification reacts：According to mole 3：1 ratio, will second of washing tea oil and glyceryl triacetate one The caustic alcohol for mixing and adding and account for second of washing tea oil weight 0.5-1.0% is acted, interesterification reaction is carried out, treats mutual ester Change after the completion of reaction, obtain esterification reaction mixture, it is standby；
2., removal of impurities：Added into esterification reaction mixture at the warm water for accounting for 1-3 times, 40-50 DEG C of its weight, constant temperature stirring 20-30min is managed, static, layering, filtering remove the fatty acid alkyl esters produced in interesterification course of reaction, collect upper strata Reactant of esterification, it is standby；
3., second of neutralization：By the C of equimolar amounts1~C4Organic acid is added in reactant of esterification, is carried out in second Reaction is closed, the middle conjunction reaction time is 30-50min, and reaction temperature is 40-48 DEG C, obtains second of neutralization reactant, standby；
4., second of extraction：
The organic solvent of identical weight is added into second of neutralization reactant and second of neutralization reactant weight 10- is accounted for 25%th, volumetric concentration is stir process 10-20min under 50-55% ethanol solution, normal temperature, stands, after after its layering, collects Organic solvent layer, obtains second of extract, standby；
(5), precision processing：
1., concentrate：Second of extract is put into falling film condenser, it is dense in the case where 70-80 DEG C of temperature, pressure are 3-5KPa Organic solvent-free residual is reduced to, concentrate is obtained, it is standby；
2., cool down:Concentrate is transferred in freezer, the cooling treatment 5-8h at -15 DEG C to -10 DEG C, filters, must cool down Liquid, it is standby；
3., refined filtration：By the filtering of the coolant ultra-filtration membrane device that via hole diameter is 20-30nm in the case where pressure is 1.5-2.5MPa, Filtering fluid is collected, unrighted acid tea oil is produced.
In the first time decolorization process, the flow control that raw material tea oil flows downward naturally along silica decoloration sand is 5- 6L/min。
In second of decolorization process, the flow control that first time decolouring tea oil flows downward naturally along activated carbon is 12-18L/min。
In the first time washing step, stir speed (S.S.) control is 500-800r/min.
In the first time washing step, the pH value of ethanol water be 9-10 be use weight concentration for 1% hydrogen Sodium hydroxide solution or weight concentration are 2.5% sodium carbonate liquor regulation.
In the complex reaction of the complex reaction step 12-18h, preceding 4-7h is stirred, and stir speed (S.S.) is 100-200r/min, it is follow-up to put processing for nature is quiet.
In second of washing step, stir speed (S.S.) control is 50-80r/min.
C in the first time neutralization procedure and second of neutralization procedure1~C4Organic acid is acetic acid or propionic acid.
Organic solvent used is n-hexane, butane, No. six solvents in the first time extraction and second of extraction step One kind in oil.
The preparation method of the unrighted acid tea oil of the present invention, is after decolouring and washing, by esterification, to make knot The saturated fatty acid and unrighted acid closed in same triglyceride molecules is separated from each other, so as to produce saturated fatty acid The mixture of Arrcostab and unsaturated fat acid alkyl ester；Further through the urea complex compound fractional crystallization of fatty acid alkyl esters, thoroughly Remove contained saturated fat acid alkyl ester；Again by with the interesterification of unsaturated fat acid alkyl ester and glyceryl triacetate Reconstruction of triglyceride, thus, saturated fatty acid contained in tea oil is effectively removes, so as to produce without saturated fat Sour tea oil, i.e.,：Unrighted acid tea oil.Especially by twice decolourize, twice washing, twice neutralize, extract twice, then add Upper concentration, cooling and refined filtration, greatly reduce the content of saturated fatty acid in finished product, and significantly improve unsaturated in finished product The content of aliphatic acid.
Detection is factually tested, the composition composition of tea oil is as follows before and after treatment：
After preparation method processing it can be seen from upper table data by the present invention, contained saturation in the tea oil of gained Aliphatic acid is seldom, and the content of unrighted acid is significantly improved, so that, further increase application The health-care efficacy for the unrighted acid tea oil that the preparation method of the present invention is processed.
Embodiment
With reference to embodiments, the present invention is further illustrated.Following explanation is but this hair in the way of enumerating Bright protection domain is not limited thereto.
The preparation method of the unrighted acid tea oil of the present embodiment, its preparation technology is as follows：
(1), just processing：
1., decolourize for the first time：First the silica decoloration sand of 100 mesh is fitted into container, it is container height to load height 65%, then, raw material tea oil is pumped into by the top of container, allows raw material tea oil to be flowed downward naturally along silica decoloration sand, flow The first time decolouring tea oil flowed out for 5.5L/min, collection is controlled, it is standby；
2., second of decolouring：Particle diameter is fitted into container for 0.15cm activated carbon again, loads height high for container Degree 45%, then, first time decolouring tea oil is pumped into by the top of container, allow first time decolouring tea oil along activated carbon naturally to Lower flowing, flow control is 15L/min, collects second of decolouring tea oil of outflow, standby；
3., wash for the first time：
The sodium hydroxide solution that the ethanol water for being first 35% by volumetric concentration is 1% with weight concentration adjusts its pH value For 9.5, then, then second of decolouring tea oil put into accounted in the ethanol water that 4 times of its weight, volumetric concentration are 35%, The stir process 60min at 65 DEG C, then stand, be layered, filter, oil reservoir is collected, washing tea oil for the first time is obtained, it is standby；
(2), it is esterified:
1., esterification：By first time washing tea oil with accounting for the absolute ethyl alcohol of its weight 20% and accounting for its weight 1.2% Caustic alcohol (playing catalytic action) is mixed and stirred for, and until oil/alkanol interface disappears, must be esterified mixing tea oil, standby；
2., neutralize for the first time：
The acetic acid of equimolar amounts is added in esterification mixing tea oil, carries out closing reaction, middle conjunction reaction time in first time For 40min, reaction temperature is 45 DEG C, obtains first time neutralization reaction mixing tea oil, standby；
3., distill：
In temperature it is 60 DEG C, under the conditions of pressure is 8KPa by first time neutralization reaction mixing tea oil, distillation is to without ethanol shape State, reclaims absolute ethyl alcohol and remaining distillation tea oil, standby；
4., extract for the first time：
Using n-hexane as extractant, residue distillation tea oil is extracted at normal temperatures, the consumption of extractant is surplus 1.5 times of remaining distillation tea oil weight, extraction 3 is counted, combining extraction liquid；Then, by extract temperature be 55 DEG C, pressure be 8KPa Under be concentrated into no extractant residual, obtain concentrate, then concentrate in refrigerating chamber is refrigerated into 5h (temperature is 5 DEG C), then filter, obtain First time extraction mixture containing saturated fat acid alkyl ester and unsaturated fat acid alkyl ester, it is standby；
(3), urea is complexed：
1., complex reaction：To first time extraction mixture in add account for its weight 15% urea, account for its weight 35%, Volumetric concentration is 85% ethanol solution, mixes, is then heated to urea in 65 DEG C of water-bath and is completely dissolved, then at room temperature Complex reaction 15h is carried out, complex compound is obtained, it is standby；
2., filter：Complex compound is filtered by vacuum through fast grade filter paper, the knot of urea-saturated fat acid complex therein is removed Brilliant complex compound, collects filtered fluid, standby；
3., second of washing：Filtered fluid is put into 3 times of weight, temperature in 65 DEG C of warm water, insulated and stirred is handled 1.8h, stand, layering, it is to be cooled arrive room temperature when, collect oil reservoir, obtain second of washing tea oil, it is standby；
(4), esterification reconstruction:
1., interesterification reacts：According to mole 3：1 ratio, will second of washing tea oil and glyceryl triacetate one The caustic alcohol (playing catalytic action) for mixing and adding and account for second of washing tea oil weight 0.8% is acted, interesterification reaction is carried out, Treat after the completion of interesterification reaction, obtain esterification reaction mixture, it is standby；
2., removal of impurities：Added into esterification reaction mixture and account for 2 times of its weight, 45 DEG C of warm water, constant temperature stir process The reactant of esterification on upper strata is collected in 25min, static, layering, filtering, standby；
3., second of neutralization：The acetic acid of equimolar amounts is added in reactant of esterification, carries out closing reaction in second, The middle conjunction reaction time is 40min, and reaction temperature is 45 DEG C, obtains second of neutralization reactant, standby；
4., second of extraction：
The n-hexane of identical weight is added into second of neutralization reactant and account for second neutralization reactant weight 18%, Volumetric concentration is stir process 15min under 52% ethanol solution, normal temperature, stands, after after its layering, collects n-hexane layer, obtain Second of extract, it is standby；
(5), precision processing：
1., concentrate：Second of extract is put into falling film condenser, is concentrated into the case where 75 DEG C of temperature, pressure are 4KPa Without n-hexane residual, concentrate is obtained, it is standby；
2., cool down:Concentrate is transferred in freezer, the cooling treatment 5-8h at -15 DEG C to -10 DEG C, filters, must cool down Liquid, it is standby；
3., refined filtration：By the filtering of the coolant ultra-filtration membrane device that via hole diameter is 20-30nm in the case where pressure is 1.5-2.5MPa, Filtering fluid is collected, unrighted acid tea oil is produced.
The preparation method of the unrighted acid tea oil of the present invention, can be not only used for preparing unrighted acid tea oil, also may be used For preparing other unrighted acid vegetable oil.

Claims (9)

1. a kind of preparation method of unrighted acid tea oil, it is characterised in that preparation technology is as follows：
(1), just processing：
1., decolourize for the first time：First the silica decoloration sand of 80-120 mesh is fitted into container, loads the 60- that height is container height 70%, then, raw material tea oil is pumped into by the top of container, allows raw material tea oil to be flowed downward naturally along silica decoloration sand, is collected The first time decolouring tea oil of outflow, it is standby；
2., second of decolouring：Particle diameter is fitted into container for 0.1-0.25cm activated carbon again, loads height high for container The 40-50% of degree, then, first time decolouring tea oil is pumped into by the top of container, allow first time decolouring tea oil along activated carbon from So flow downward, collect second of decolouring tea oil of outflow, it is standby；
3., wash for the first time：
It is the ethanol water that 9-10, volumetric concentration are 25-38% that second of decolouring tea oil, which is put into, and accounts for 3-5 times of its weight, pH value In solution, the stir process 50-70min at 60-70 DEG C, then stand, be layered, filter, oil reservoir is collected, washing tea for the first time is obtained Oil, it is standby；
(2), it is esterified:
1., esterification：By first time washing tea oil with accounting for its weight 15-26% absolute ethyl alcohol and accounting for its weight 0.6- 1.5% caustic alcohol is mixed and stirred for, and until oil/alkanol interface disappears, must be esterified mixing tea oil, standby；
2., neutralize for the first time：
By the C of equimolar amounts1~C4Organic acid, which is added to, to be esterified in mixing tea oil, carries out closing reaction in first time, during middle conjunction reaction Between be 30-50min, reaction temperature be 40-48 DEG C, obtain first time neutralization reaction mixing tea oil, it is standby；
3., distill：
In temperature it is 50-70 DEG C, under the conditions of pressure is 5-10KPa by first time neutralization reaction mixing tea oil, distillation is to without ethanol State, reclaims absolute ethyl alcohol and remaining distillation tea oil, standby；
4., extract for the first time：
Using organic solvent as extractant, residue distillation tea oil is extracted at normal temperatures, the consumption of extractant is residue Distill tea oil weight 1-2 times, is extracted 3 times, combining extraction liquid；Then, by extract temperature be 45-65 DEG C, pressure be 5- No extractant residual is concentrated under 10KPa, obtain concentrate, then then concentrate is filtered, must contained in refrigerating chamber refrigeration 5-6h The first time extraction mixture of saturated fat acid alkyl ester and unsaturated fat acid alkyl ester, it is standby；
(3), urea is complexed：
1., complex reaction：Added into first time extraction mixture and account for its weight 10-18% urea, account for its weight 30- 38%th, volumetric concentration is 80-90% ethanol solution, mixes, urea is then heated in 60-70 DEG C of water-bath completely molten Solution, then complex reaction 12-18h is carried out at room temperature, complex compound is obtained, it is standby；
2., filter：Complex compound is filtered by vacuum through fast grade filter paper, the crystallization network of urea-saturated fat acid complex therein is removed Compound, collects filtered fluid, standby；
3., second of washing：Filtered fluid is put into 2-4 times of weight, temperature in 60-70 DEG C of warm water, insulated and stirred handles 1- 2.5h, stand, layering, it is to be cooled arrive room temperature when, collect oil reservoir, obtain second of washing tea oil, it is standby；
(4), esterification reconstruction:
1., interesterification reacts：According to mole 3：1 ratio, second of washing tea oil is mixed together with glyceryl triacetate The caustic alcohol for accounting for second of washing tea oil weight 0.5-1.0% is closed and added, interesterification reaction is carried out, treats that interesterification is anti- After the completion of answering, esterification reaction mixture is obtained, it is standby；
2., removal of impurities：The warm water for accounting for 1-3 times, 40-50 DEG C of its weight, constant temperature stir process 20- are added into esterification reaction mixture 30min, static, layering, filtering, removes the fatty acid alkyl esters produced in interesterification course of reaction, collects the esterification on upper strata Reactant, it is standby；
3., second of neutralization：By the C of equimolar amounts1~C4Organic acid is added in reactant of esterification, carries out closing anti-in second Should, the middle conjunction reaction time is 30-50min, and reaction temperature is 40-48 DEG C, obtains second of neutralization reactant, standby；
4., second of extraction：
The organic solvent of identical weight is added into second of neutralization reactant and second of neutralization reactant weight 10- is accounted for 25%th, volumetric concentration is stir process 10-20min under 50-55% ethanol solution, normal temperature, stands, after after its layering, collects Organic solvent layer, obtains second of extract, standby；
(5), precision processing：
1., concentrate：Second of extract is put into falling film condenser, is concentrated into the case where 70-80 DEG C of temperature, pressure are 3-5KPa Organic solvent-free is remained, and obtains concentrate, standby；
2., cool down:Concentrate is transferred in freezer, the cooling treatment 5-8h at -15 DEG C to -10 DEG C, filters, obtain coolant, It is standby；
3., refined filtration：By the filtering of the coolant ultra-filtration membrane device that via hole diameter is 20-30nm in the case where pressure is 1.5-2.5MPa, collect Fluid is filtered, unrighted acid tea oil is produced.
2. the preparation method of unrighted acid tea oil according to claim 1, it is characterised in that：Decolourized in the first time In step, the flow control that raw material tea oil flows downward naturally along silica decoloration sand is 5-6L/min.
3. the preparation method of unrighted acid tea oil according to claim 1 or claim 2, it is characterised in that：At described second In decolorization process, the flow control that first time decolouring tea oil flows downward naturally along activated carbon is 12-18L/min.
4. the preparation method of unrighted acid tea oil according to claim 3, it is characterised in that：In first time washing In step, stir speed (S.S.) control is 500-800r/min.
5. the preparation method of unrighted acid tea oil according to claim 4, it is characterised in that：In first time washing In step, the pH value of ethanol water is that 9-10 is to use the weight concentration to be for 1% sodium hydroxide solution or weight concentration 2.5% sodium carbonate liquor regulation.
6. the preparation method of unrighted acid tea oil according to claim 5, it is characterised in that：In complex reaction step In rapid 12-18h complex reaction, preceding 4-7h is stirred, and stir speed (S.S.) is 100-200r/min, follow-up to be put for nature is quiet Processing.
7. the preparation method of unrighted acid tea oil according to claim 6, it is characterised in that：Washed at described second In step, stir speed (S.S.) control is 50-80r/min.
8. the preparation method of unrighted acid tea oil according to claim 7, it is characterised in that：The first time neutralizes step C in rapid and second of neutralization procedure1~C4Organic acid is acetic acid or propionic acid.
9. the preparation method of unrighted acid tea oil according to claim 8, it is characterised in that：First time extraction and Organic solvent used is one kind in n-hexane, butane, No. six solvent naphthas in second of extraction step.
CN201710502895.2A 2017-06-27 2017-06-27 Preparation method of unsaturated fatty acid tea oil Active CN107057852B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710502895.2A CN107057852B (en) 2017-06-27 2017-06-27 Preparation method of unsaturated fatty acid tea oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710502895.2A CN107057852B (en) 2017-06-27 2017-06-27 Preparation method of unsaturated fatty acid tea oil

Publications (2)

Publication Number Publication Date
CN107057852A true CN107057852A (en) 2017-08-18
CN107057852B CN107057852B (en) 2021-01-05

Family

ID=59613370

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710502895.2A Active CN107057852B (en) 2017-06-27 2017-06-27 Preparation method of unsaturated fatty acid tea oil

Country Status (1)

Country Link
CN (1) CN107057852B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109200137A (en) * 2018-10-17 2019-01-15 赣州哈克生物科技有限公司 A kind of tea oil bacteriostatic agent and preparation method thereof
CN109355138A (en) * 2017-10-09 2019-02-19 赣南医学院 A kind of preparation method, product and its application of tea oil polyunsaturated fatty acid
CN110484353A (en) * 2019-08-23 2019-11-22 福建师范大学 A kind of preparation method of water solubility camellia oil
CN112403271A (en) * 2020-10-28 2021-02-26 中海油天津化工研究设计院有限公司 Method for preparing diesel antiwear agent by removing saturated fatty acid through membrane separation
CN113956918A (en) * 2021-11-07 2022-01-21 芷江华兴油业有限公司 Edible vegetable oil and processing method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101472483A (en) * 2006-06-22 2009-07-01 E.S.生物技术有限公司 Edible plant oils from which saturated fatty acids were removed and manufacturing process thereof
CN101768511A (en) * 2010-01-27 2010-07-07 卢玉胜 Low-temperature refining method for tea seed oil and refining adsorbent
CN102028042A (en) * 2010-10-28 2011-04-27 福建省尤溪县沈郎食用油有限公司 Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake
CN103614237A (en) * 2013-12-12 2014-03-05 酉阳县康友粮油有限公司 Rapeseed crude oil refining process
CN104529739A (en) * 2014-12-25 2015-04-22 北京阳光基业药业有限公司 Purification method of unsaturated fatty acid

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08100191A (en) * 1994-09-30 1996-04-16 Nisshin Flour Milling Co Ltd Purification of highly unsaturated fatty acid or ester thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101472483A (en) * 2006-06-22 2009-07-01 E.S.生物技术有限公司 Edible plant oils from which saturated fatty acids were removed and manufacturing process thereof
CN101768511A (en) * 2010-01-27 2010-07-07 卢玉胜 Low-temperature refining method for tea seed oil and refining adsorbent
CN102028042A (en) * 2010-10-28 2011-04-27 福建省尤溪县沈郎食用油有限公司 Method and equipment for preparing tea seed oil from tea seeds and extracting tea polyphenol from byproduct tea seed cake
CN103614237A (en) * 2013-12-12 2014-03-05 酉阳县康友粮油有限公司 Rapeseed crude oil refining process
CN104529739A (en) * 2014-12-25 2015-04-22 北京阳光基业药业有限公司 Purification method of unsaturated fatty acid

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109355138A (en) * 2017-10-09 2019-02-19 赣南医学院 A kind of preparation method, product and its application of tea oil polyunsaturated fatty acid
CN109200137A (en) * 2018-10-17 2019-01-15 赣州哈克生物科技有限公司 A kind of tea oil bacteriostatic agent and preparation method thereof
CN110484353A (en) * 2019-08-23 2019-11-22 福建师范大学 A kind of preparation method of water solubility camellia oil
CN112403271A (en) * 2020-10-28 2021-02-26 中海油天津化工研究设计院有限公司 Method for preparing diesel antiwear agent by removing saturated fatty acid through membrane separation
CN113956918A (en) * 2021-11-07 2022-01-21 芷江华兴油业有限公司 Edible vegetable oil and processing method thereof

Also Published As

Publication number Publication date
CN107057852B (en) 2021-01-05

Similar Documents

Publication Publication Date Title
CN107057852A (en) A kind of preparation method of unrighted acid tea oil
CN106010779B (en) Production method of camellia seed oil with high natural sterol content in plants
CN104277906A (en) Refining process for cold-pressed camellia oil at low temperature
CN101449710B (en) Production technique of hickory oil
CN106221895B (en) A kind of preparation method of high-quality edible camellia oil
CN104611130B (en) A kind of preparation technology rich in oryzanol vitamin E nutrition Rice oil
CN103289816A (en) Tea oil processing method and device special for tea oil processing method
CN107057845A (en) A kind of method of idesia oil extraction purification
CN102311882A (en) Extraction method for unsaturated fatty acid
CN105255587A (en) Low-temperature physical refining method for rapeseed oil with aromatic flavor
CN103881807A (en) Soybean unsaturated fatty acid extraction method
CN106929160A (en) The method of refined plant oil wax
CN104522190A (en) Special peony oil for children
CN105037417B (en) Method for preparing egg yolk lecithin used for injection through aluminum oxide static adsorption impurity removal and low-temperature sediment oil removal
CN107418728A (en) A kind of semicontinuous refining production technology of 58 ton day linseed oil
CN101760300B (en) Evening primrose oil processing method
CN110305732A (en) A kind of method of cold pressing edible oil
CN109232239A (en) A kind of extraction process of shikimic acid
CN102329691B (en) Decolorizing method of rice bran first-grade oil
CN109233999A (en) A kind of preparation method of original fragrant vegetable seed oil
CN108084016A (en) A kind of high-purity linoleic preparation method
CN108546589A (en) A kind of preparation method of the tea oil rich in tea polyphenols
CN107212386B (en) Health food with auxiliary memory improving function and preparation process thereof
CN101796984B (en) Method for supercritical constant-pressure purification of deep sea fish oil
CN104830521A (en) Production method of refined soybean oil

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant