CN106753753A - The extraction process of fatty acid mixed in a kind of vegetable oil residue - Google Patents
The extraction process of fatty acid mixed in a kind of vegetable oil residue Download PDFInfo
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- CN106753753A CN106753753A CN201611193689.XA CN201611193689A CN106753753A CN 106753753 A CN106753753 A CN 106753753A CN 201611193689 A CN201611193689 A CN 201611193689A CN 106753753 A CN106753753 A CN 106753753A
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- Prior art keywords
- vegetable oil
- oil residue
- fatty acid
- acid mixed
- extraction process
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Classifications
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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
-
- 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
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
- C11C1/025—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by saponification and release of fatty acids
-
- 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
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
- C11C1/04—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis
- C11C1/045—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis using enzymes or microorganisms, living or dead
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- Life Sciences & Earth Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention proposes a kind of extraction process of fatty acid mixed in vegetable oil residue, including pretreatment, saponification, acidolysis, washing, dehydration and vacuum distillation step.Process is simple, beneficial to operation, recovery rate is high, and impurity is few, beneficial to preservation, while the comprehensive utilization value of vegetable oil residue is greatly improved, with application and promotion prospect well.
Description
Technical field
The present invention relates to technical field of oil chemical industry, the extraction work of fatty acid mixed in more particularly to a kind of vegetable oil residue
Skill.
Background technology
Many vegetable oil crude oils, such as soybean oil, rapeseed oil, sunflower oil, corn oil, peanut oil, containing many impurity,
Making the transparency of vegetable oil reduces, and produces flocculent deposit, and bin stability is deteriorated, and 280 DEG C of heat runs are unqualified etc..It is removal
These impurity, while not making vegetable oil aroma fades again, oil-fat plant is mostly using the method staticly settled with cold filtration
Vegetable oil is refined, vegetable oil staticly settles gained accessory substance i.e. vegetable oil residue.In vegetable oil residue, except containing neutral oil,
There are solid impurity, protein, wax, moisture and micro constitutent outside free fatty.
With flourishing for oil chemical industry, the comprehensive development and utilization problem of grease is increasingly taken seriously.At present,
For vegetable oil residue, there is part neutral grease to be recovered, separately there are many small towns chemical plant to be used to vegetable oil residue manufacture " clay fertilizer
Soap ", in addition, the nutritious material such as remaining about 30% neutral grease and free fatty is taken as waste material
Treatment, causes the significant wastage of plant component, and from from the aspect of the deep processing of vegetable oil residue, it is not obtained and makes full use of,
Value-added content of product is very low;Oily factory influences environment and production also because vegetable oil residue can not be processed in time simultaneously.
Aliphatic acid in vegetable oil residue generally has hard fatty acids, oleic acid, linoleic acid etc..It is used directly for painting industry
Make solvent, it can also be used to prepare the chemical fields such as laundry soap, synthetic detergent, cosmetics, lubricating additive and plastic additive.It is mixed
Closing aliphatic acid can also obtain various one pack systems by separation, as application value industrial chemicals higher.
How to be extracted from vegetable oil residue and reclaim fatty acid mixed, improve the level of comprehensive utilization and oil foot of vegetable fat
Added value, is that current grease deep processing enterprise needs attention and the problem for considering.
The content of the invention
The main object of the present invention is, in order to solve the above problems, to propose that a kind of process is simple, recovery rate are high, easy to spread
Vegetable oil residue in fatty acid mixed extraction process.
The present invention proposes a kind of extraction process of fatty acid mixed in vegetable oil residue, comprises the following steps:
S10, pretreatment:A certain amount of vegetable oil residue is taken for raw material, under vacuum in 45-55 DEG C of insulation dehydrations extremely
Water content is less than 5%;Food grade decolorising agent is added, addition is 3%-the 5% of vegetable oil residue quality, in 40-50 DEG C of insulations
Under the conditions of stir 30-40min and decolourized to faint yellow;Wherein, the vacuum is not less than 0.09MPa;
S20, saponification:The vegetable oil residue of step of learning from else's experience S10 dehydration and decolorizations is added in reactor, adds the hydrogen that concentration is 30%
Sodium hydroxide solution makes system pH value reach 10-11, keeps ventilation to boil 3-4h, until generating the saponified of smooth colloidal;
Wherein, sodium hydroxide solution addition is 8%-the 10% of vegetable oil residue quality;
S30, acidolysis:In being 20% sulfuric acid solution by the saponified addition concentration, keep ventilation to boil 1-2h, treat
Solution system stops reaction when producing substantially layering, insulation bleeds off lower floor's acid solution after standing 40-60min, removes upper strata and slightly mixes
Close aliphatic acid standby;Wherein, sulphuric acid is 10%-the 15% of saponified quality;
S40, washing:Will during the thick fatty acid mixed adds deionized water, ventilation is boiled and agitator treating 30-
40min, stratification of then stopping the supple of gas or steam, discards water layer, repeats three times;Until the pH value of the water layer stops water when being 6-7
Wash;
S50, dehydration, vacuum distillation:Above-mentioned thick fatty acid mixed after washing is put into the container with heating coil
In, ventilation 3-4h of heating, 50-60 DEG C of keeping temperature, then stratification, is heated to 90 DEG C, afterwards after bleeding off lower floor's moisture
It is transferred in distillation still, keeps vacuum in 0.08-0.09MPa, 250-270 DEG C of temperature in the kettle, 75-90 DEG C of condensed water temperature,
Collect product cut and be fatty acid mixed.
Preferably, vegetable oil residue described in step S10 is soybean oil, rapeseed oil, sunflower oil, corn oil, peanut oil oil
One or more in pin.
Preferably, the food grade decolorising agent is edible grade hydrogen peroxide, atlapulgite, activated carbon, ClO2In one kind.
Preferably, the food grade decolorising agent is edible grade hydrogen peroxide.
Present invention process, fatty acid mixed recovery rate is high in vegetable oil residue, and impurity is few, beneficial to preservation, country is met comprehensively
The requirement of food hygiene.Method process is simple in itself, beneficial to operation, obvious economic addition value increases, and greatly improves vegetable oil
The comprehensive utilization value of pin, with application and promotion prospect well.
Specific embodiment
It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, the present invention is not intended to limit
Scope.
The present invention proposes a kind of extraction process of fatty acid mixed in vegetable oil residue, and it comprises the following steps:
S10, pretreatment:A certain amount of vegetable oil residue is taken for raw material, under vacuum in 45-55 DEG C of insulation dehydrations extremely
Water content is less than 5%;Food grade decolorising agent is added, addition is 3%-the 5% of vegetable oil residue quality, in 40-50 DEG C of insulations
Under the conditions of stir 30-40min and decolourized to faint yellow;Wherein, the vacuum is not less than 0.09MPa;
Preferably, vegetable oil residue described in this step is soybean oil, rapeseed oil, sunflower oil, corn oil, peanut oil residuals
In one or more.
Preferably, in the present embodiment, the food grade decolorising agent is edible grade hydrogen peroxide, can be converted under heat-retaining condition
It is water, other materials is not introduced.In other embodiments, the food grade decolorising agent can for atlapulgite, activated carbon,
ClO2Deng.And for the ease of decolourizing, described vegetable oil residue is first dehydrated in 45-55 DEG C of insulations under vacuum before decolouring
It is not more than 5% to water content.
In some other implementation method, decolorization process optional step.If the color of vegetable oil residue raw material is than shallower,
In yellowish or slightly yellow, then decolorization process can be omitted, and only carry out dewater treatment.
S20, saponification:The vegetable oil residue of step of learning from else's experience S10 dehydration and decolorizations is added in reactor, adds the hydrogen that concentration is 30%
Sodium hydroxide solution regulation system pH value is 10-11, keeps ventilation to boil 3-4h, until generating the saponified of smooth colloidal;
Wherein, sodium hydroxide solution addition is 8%-the 10% of vegetable oil residue quality;
Vegetable fat is influenceed in extracting, refining production by many objective, human factors so that oil foot is constituted very
Complexity, containing many impurity, fat composition constituent content cannot Accurate Determining.Only according to the chemical property of aliphatic acid, first carry out
Saponification, generates the saponified of smooth colloidal and is separated from former vegetable oil residue, then by follow-up acidolysis, by saponification
Thing, the neutral oil therein etc. that adulterates become aliphatic acid, are then peeled off out.
During the concrete operations of this step, first by through the vegetable oil residue of dehydration and decolorization add reactor in, according to saponification number add
The NaOH of respective amount, naoh concentration 30% or so, boil 3-4 hours by then ventilation, keep system PH 10-
Between 11, sample acidified acid number of surveying is taken when reaching 180, you can stop saponification.When operating simultaneously, it should be noted that in control reactor
Can not be overflow pot, and cold water defervescence can be added if necessary.
S30, acidolysis:In being 20% sulfuric acid solution by the saponified addition concentration, keep ventilation to boil 1-2h, treat
Solution system stops reaction when producing substantially layering, insulation bleeds off lower floor's acid solution after standing 40-60min, removes upper strata and slightly mixes
Close aliphatic acid standby;Wherein, sulphuric acid is 10%-the 15% of saponified quality;
Principle:In water, dissociation and form hydrogen ion and show acidity in molecule to aliphatic acid there is. But belong to weak acid, it can generate salt, such as RCOOH+NaOH → RCOONa+H with alkaline matter2O, this is
Most common saponification.This soap, aliphatic acid can be separated out after through dilute sulfuric acid acidification again.Meanwhile, former plant
Neutral oil in oil foot also can under the action of an acid be hydrolyzed to aliphatic acid, here it is we carry out acid to vegetable oil residue aborning
Change the principle foundation for the treatment of.
S40, washing:Will during the thick fatty acid mixed adds deionized water, ventilation is boiled and agitator treating 30-
40min, stratification of then stopping the supple of gas or steam, discards water layer, repeats three times;Until the pH value of the water layer stops water when being 6-7
Wash;
S50, dehydration, vacuum distillation:Above-mentioned thick fatty acid mixed after washing is put into the container with heating coil
In, ventilation 3-4h of heating, 50-60 DEG C of keeping temperature, then stratification, is heated to 90 DEG C, afterwards after bleeding off lower floor's moisture
It is transferred in distillation still, keeps vacuum in 0.08-0.09MPa, 250-270 DEG C of temperature in the kettle, 75-90 DEG C of condensed water temperature,
Collect product cut and be fatty acid mixed.
Croude fatty acids after washing should first carry out dewater treatment before it is distilled, to prevent bumping after kettle from overflowing pot.
The principle of vacuum distillation is:Boiling point is higher at ambient pressure for aliphatic acid, up to 300 DEG C, heat-sensitive materials is belonged to again, in higher pressure
Distillation can will cause fatty acid part to decompose under power, generation acid anhydrides, ketone, hydrocarbon, short carbon chain aliphatic acid etc..Meanwhile, unsaturated fat
There is polymerization in acid also part, generate polymerized fatty acid, oxyacid, lactone, alcohol, hydrocarbon and other products, so as to reduce product
Quality, reduces yield.Therefore, during practical operation, using forming certain vacuum, aliphatic acid in vacuum distillation, i.e. distillation still
Negative pressure state is in, boiling point reduction, so as to first distill, is separated with other materials in croude fatty acids.The aliphatic acid of vaporization
Aliphatic acid by forming liquid after condensation, difficult volatile component is periodically or continuously discharged from distillation still.
It should be noted that:Before distillation still charging, steam pressure, vacuum, pipeline, heating working of a furnace etc. should be also checked, made
Meet regulation requirement.During charging vacuum should in more than 0.087MPa, inlet amount 1/2-2/3 in the kettle at, temperature in the kettle reaches
Can enter after 200 DEG C and run well;Boiling situation in observation kettle is should be noted that during distillation, when distillate reaches the 30% of inlet amount
When one 40%, charging should be supplemented.Aliphatic acid flow below device to be condensed is significantly reduced, and can be considered distillation still slagging.This
When can open slag pumping system, drain water, slag pipe afterbody valve recoil, when temperature in the kettle be less than 280 DEG C when
Slagging.
Embodiment 1:
S10, pretreatment:The peanut oil residuals of 500g are taken for raw material, in 55 DEG C of insulation dehydrations under 0.09MPa vacuum conditions
It is 4% to water content;The edible grade hydrogen peroxides of 25g are added, 35min is stirred under 40 DEG C of heat-retaining conditions and is decolourized to faint yellow;
S20, saponification:Take in the vegetable oil residue 480g addition reactors of above-mentioned dehydration and decolorization, addition 38.4g, concentration are
30% sodium hydroxide solution (now system pH value is 10.5), keeps ventilation to boil 4h, until generating the soap of smooth colloidal
Compound 108g;
S30, acidolysis:Boiled ventilation in the saponified addition 10.8g of above-mentioned 108g, the sulfuric acid solution that concentration is 20%, is kept
Boiling 1.5h, stops reaction when solution system produces substantially layering, and insulation bleeds off lower floor's acid solution after standing 60min, in removal
The thick fatty acid mixed of layer is standby;
S40, washing:By in the thick fatty acid mixed addition deionized water, ventilation is boiled and agitator treating 30min, so
After stop the supple of gas or steam stratification, discard water layer, repeat three times;Until stopping washing when the pH value of the water layer is 6;
S50, dehydration, vacuum distillation:Above-mentioned thick fatty acid mixed after washing is put into the container with heating coil
In, ventilation heating 3h, 60 DEG C of keeping temperature, then stratification, 90 DEG C are heated to after bleeding off lower floor's moisture, and steaming is transferred to afterwards
Evaporate in kettle, keep vacuum in 0.08MPa, 250 DEG C of temperature in the kettle, 90 DEG C of condensed water temperature collects product cut and is mixing fat
Fat acid.
Embodiment 2:
S10, pretreatment:1Kg pecan oils oil foot is taken for raw material, in 45 DEG C of insulation dehydrations under 0.12MPa vacuum conditions
It is 5% to water content;30g food grade atlapulgites are added, 30min is stirred under 50 DEG C of heat-retaining conditions and is decolourized to yellowish
Color;
S20, saponification:Take in the pecan oil oil foot 860g addition reactors of above-mentioned dehydration and decolorization, addition 86g, concentration are
30% sodium hydroxide solution (now system pH value is 11), keeps ventilation to boil 3h, until generating the saponification of smooth colloidal
Thing 268g;
S30, acidolysis:Boiled ventilation in the saponified addition 40.2g of above-mentioned 268g, the sulfuric acid solution that concentration is 20%, is kept
Boiling 2h, stops reaction when solution system produces substantially layering, and insulation bleeds off lower floor's acid solution, removes upper strata after standing 40min
Thick fatty acid mixed is standby;
S40, washing:By in the thick fatty acid mixed addition deionized water, ventilation is boiled and agitator treating 40min, so
After stop the supple of gas or steam stratification, discard water layer, repeat three times;Until stopping washing when the pH value of the water layer is 7;
S50, dehydration, vacuum distillation:Above-mentioned thick fatty acid mixed after washing is put into the container with heating coil
In, ventilation heating 4h, 50 DEG C of keeping temperature, then stratification, 90 DEG C are heated to after bleeding off lower floor's moisture, and steaming is transferred to afterwards
Evaporate in kettle, keep vacuum in 0.09MPa, 270 DEG C of temperature in the kettle, 75 DEG C of condensed water temperature collects product cut and is mixing fat
Fat acid.
Product appearance:The fatty acid mixed that the present invention is prepared is light yellow translucent liquid.Its main component has firmly
Aliphatic acid, oleic acid, linoleic acid etc..
Present invention process, fatty acid mixed recovery rate is high in vegetable oil residue, and impurity is few, beneficial to preservation, country is met comprehensively
The requirement of food hygiene.Method process is simple in itself, beneficial to operation, economic value added is high, and the comprehensive of vegetable oil residue is improved energetically
Close value.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (4)
1. in a kind of vegetable oil residue fatty acid mixed extraction process, it is characterised in that comprise the following steps:
S10, pretreatment:A certain amount of vegetable oil residue is taken for raw material, under vacuum in 45-55 DEG C of insulation dehydrations to aqueous
Amount is less than 5%;Food grade decolorising agent is added, addition is 3%-the 5% of vegetable oil residue quality, in 40-50 DEG C of heat-retaining conditions
30-40min of lower stirring is decolourized to faint yellow;Wherein, the vacuum is not less than 0.09MPa;
S20, saponification:The vegetable oil residue of step of learning from else's experience S10 dehydration and decolorizations is added in reactor, adds the hydroxide that concentration is 30%
Sodium solution regulation system pH value is 10-11, keeps ventilation to boil 3-4h, until generating the saponified of smooth colloidal;Wherein,
Sodium hydroxide solution addition is 8%-the 10% of vegetable oil residue quality;
S30, acidolysis:In being 20% sulfuric acid solution by the saponified addition concentration, keep ventilation to boil 1-2h, treat solution
System stops reaction when producing substantially layering, insulation bleeds off lower floor's acid solution after standing 40-60min, removes upper strata and slightly mixes fat
Fat acid is standby;Wherein, sulphuric acid is 10%-the 15% of saponified quality;
S40, washing:By in the thick fatty acid mixed addition deionized water, ventilation is boiled and 30-40min of agitator treating, so
After stop the supple of gas or steam stratification, discard water layer, repeat three times;Until stopping washing when the pH value of the water layer is 6-7;
S50, dehydration, vacuum distillation:Above-mentioned thick fatty acid mixed after washing is put into the container with heating coil, is led to
Gas 3-4h of heating, 50-60 DEG C of keeping temperature, then stratification, 90 DEG C are heated to after bleeding off lower floor's moisture, are transferred to afterwards
In distillation still, keep vacuum in 0.08-0.09MPa, 250-270 DEG C of temperature in the kettle, 75-90 DEG C of condensed water temperature is collected and produced
Product cut is fatty acid mixed.
2. in vegetable oil residue as claimed in claim 1 fatty acid mixed extraction process, it is characterised in that institute in step S10
It is one or more in soybean oil, rapeseed oil, sunflower oil, corn oil, peanut oil residuals to state vegetable oil residue.
3. in vegetable oil residue as claimed in claim 1 fatty acid mixed extraction process, it is characterised in that institute in step S10
It is edible grade hydrogen peroxide, atlapulgite, activated carbon, ClO to state food grade decolorising agent2In one kind.
4. in vegetable oil residue as claimed in claim 3 fatty acid mixed extraction process, it is characterised in that the food grade take off
Toner is edible grade hydrogen peroxide.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107382695A (en) * | 2017-07-25 | 2017-11-24 | 江南大学 | A kind of high-purity erucic acid and preparation method thereof |
CN108753466A (en) * | 2018-05-24 | 2018-11-06 | 华南理工大学 | A kind of tea oil linoleic acid and its preparation method and application |
CN113735897A (en) * | 2021-08-25 | 2021-12-03 | 安徽天凯生物科技有限公司 | Preparation process of phospholipid type DHA |
CN113736568A (en) * | 2021-08-25 | 2021-12-03 | 安徽天凯生物科技有限公司 | Preparation process of water-soluble fatty acid |
-
2016
- 2016-12-21 CN CN201611193689.XA patent/CN106753753A/en not_active Withdrawn
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107382695A (en) * | 2017-07-25 | 2017-11-24 | 江南大学 | A kind of high-purity erucic acid and preparation method thereof |
CN108753466A (en) * | 2018-05-24 | 2018-11-06 | 华南理工大学 | A kind of tea oil linoleic acid and its preparation method and application |
CN108753466B (en) * | 2018-05-24 | 2021-06-08 | 华南理工大学 | Tea oil linoleic acid and preparation method and application thereof |
CN113735897A (en) * | 2021-08-25 | 2021-12-03 | 安徽天凯生物科技有限公司 | Preparation process of phospholipid type DHA |
CN113736568A (en) * | 2021-08-25 | 2021-12-03 | 安徽天凯生物科技有限公司 | Preparation process of water-soluble fatty acid |
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