CN108084016A - A kind of high-purity linoleic preparation method - Google Patents
A kind of high-purity linoleic preparation method Download PDFInfo
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- CN108084016A CN108084016A CN201711424018.4A CN201711424018A CN108084016A CN 108084016 A CN108084016 A CN 108084016A CN 201711424018 A CN201711424018 A CN 201711424018A CN 108084016 A CN108084016 A CN 108084016A
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- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- 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
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- 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
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Abstract
The invention discloses a kind of high-purity linoleic preparation methods, comprise the following steps：S1, fatty acid mixed and highly basic are dissolved in the mixed solution of low-carbon alcohols water, heating, back flow reaction keeps the temperature crystallization after once cooling down, once filters, crystallization will be kept the temperature after first-time filtrate reducing temperature twice, secondary suction filtration adds in excessive strong acid into secondary filtrate, is distilled to recover low-carbon alcohols water, yellow oil is obtained, neutrality is washed to and obtains linoleic acid crude product；The linoleic acid crude product obtained in S2, vacuum distillation step S1, Fractional Collections fraction is to get high-purity linoleic acid.The present invention prepares high-purity linoleic acid by using metal crystallization rectification under vacuum technique, economic and environment-friendly process avoids a large amount of using urea；The preparation method of the present invention is of low cost using natural plant grease as raw material, simple for process controllable, required equipment is simple, and production efficiency is high, and is easy to mass produce, obtained linoleic acid product peroxide value is low, of light color, content is high, has the stronger market competitiveness, has a extensive future.
Description
Technical field
The present invention relates to natural unrighted acid extractive technique field, more particularly, to a kind of high-purity linoleic
Preparation method.
Background technology
Linoleic acid is one kind in functional polyunsaturated fatty acid, plays an important role of to reduce serum cholesterol level, take the photograph
Enter a large amount of linoleic acid has the effect of apparent to the patient of high triglyceride.China's pharmacopeia is still using ethyl linoleate pill, drops
Drug as diseases such as prevention and treatment hypertension, atherosclerosis, angina pectoris and coronary heart disease.Linoleic acid helps to drop
Low serum cholesterol and the formation for inhibiting arterial thrombus, therefore in the angiocardiopathies such as prevention of arterial atherosis and myocardial infarction
Aspect has good action.
Linoleic acid is the necessary aliphatic acid being identified earliest, is present in most greases of people's daily consumption, can
To say that linoleic acid is resource functional polyunsaturated fatty acid the most sufficient.Wherein, cottonseed oil, soybean oil, the sesame oil Central Asia
The content of oleic acid is up to 40-50%, and the content of sunflower oil and maize germ oil Linoleic acid is close to 70%, safflower seed oil and Portugal
The content of grape seed oil Linoleic acid is about 80%.
Although linoleic acid sources are extensive, since it contains there are two carbon-carbon double bond, easily oxidative deformation, make its separation pure
Change technology is most important, and currently used isolation and purification method has urea adduct method, adsorption method of separation, lipase concentration method, super
Supercritical fluid extraction method and molecular distillation etc..Wherein, urea adduct method can generate a large amount of solid waste, and be difficult to handle；
Adsorption method of separation is of high cost, efficiency is low；Lipase concentration method and supercritical fluid extraction are difficult to accomplish high-purity, and molecular distillation
Method is suitable only for linoleic decoloration and deperoxidation value.
In conclusion in linoleic preparation, how using cheap raw material, isolation and purification method is reduced to Asia
Oleic acid product stability influences, and it is to prepare high-purity linoleic acid at present urgently to solve to realize high product yield, purity and production efficiency
Key issue certainly.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of high-purity linoleic preparation methods.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of high-purity linoleic preparation method, comprises the following steps：
S1, fatty acid mixed and highly basic are dissolved in the mixed solution of low-carbon alcohols-water, heated, back flow reaction once cools down
After keep the temperature crystallization, once filter, crystallization will be kept the temperature after first-time filtrate reducing temperature twice, secondary suction filtration was added in into secondary filtrate
Strong acid is measured, low-carbon alcohols-water is distilled to recover, obtains yellow oil, be washed to neutrality and obtain linoleic acid crude product, wherein, it is described
Low-carbon alcohols are the one or more in methanol, ethyl alcohol, n-butanol and isobutanol；
The linoleic acid crude product obtained in S2, vacuum distillation step S1, Fractional Collections fraction is to get high-purity linoleic acid.
Fatty acid metal salts method come separated, is satisfied using different fatty acid metal salts different solubility in organic solvent
It is smaller than unrighted acid with the solubility of the metal salt of aliphatic acid in organic solvent, identical carbon chain lengths it is single unsaturated
The solubility of the metal salt of aliphatic acid in organic solvent is smaller than polyunsaturated fatty acid；Rectification under vacuum technology is that basis does not have to
The method that the difference of aliphatic acid boiling point under vacuum carrys out separation and Extraction polyunsaturated fatty acid；Both approaches, which are combined, to be made
With effectively the Separation of Fatty Acids of different carbon chain, different saturation can be opened.
In the above-mentioned technical solutions, in step S1, the rate of temperature fall once to cool down is 1-3 DEG C/min, and 0~20
DEG C heat preservation 1-10h, preferably keep the temperature 2-3h；The rate of temperature fall of the reducing temperature twice is 1-3 DEG C/min, and in -15~-5 DEG C of guarantors
Warm 1-10h, preferably keeps the temperature 2-3h.
Using once feeding intake, the palmitic acid and stearic acid of the method for crystallization twice, for the first time main removal saturation, second
It is mainly used to separate oleic acid and linoleic acid, in this way, solvent can be saved, while can also saves the time, so as to accomplish economic height
Effect.
Preferably, in the above-mentioned technical solutions, in step S1, the reaction temperature is 50-75 DEG C, reaction time 10-
80min。
At this temperature and under mixing time, the alkali of addition can be just dissolved in alcohol solution without causing insatiable hunger
With the Quick Oxidation of aliphatic acid.
Preferably, in the above-mentioned technical solutions, in step S1, the highly basic for sodium hydroxide, potassium hydroxide, sodium ethoxide and
The mass ratio of one or more in lithium hydroxide, the highly basic and fatty acid mixed is 0.1-2:1；The low-carbon alcohols and water
Mass ratio is 6-9.5:1, it is preferably 8.5-9:1.
The one or more selected in sodium hydroxide, potassium hydroxide, sodium ethoxide and lithium hydroxide are added in as highly basic reacts,
Limit the mass ratio of highly basic and fatty acid mixed and low-carbon alcohol and water simultaneously, be consider cost of material, separating effect and
Product purity selection made.
Preferably, in the above-mentioned technical solutions, in step S1, the strong acid is one kind in hydrochloric acid, sulfuric acid and nitric acid, excellent
Elect hydrochloric acid as.
It selects a kind of as strong acid in hydrochloric acid, sulfuric acid and nitric acid, is to be able to more rapidly more thoroughly with being formed
Soap reactant salt, formed free fatty, and then select hydrochloric acid be because hydrochloric acid there is no oxidisability, unrighted acid will not be made
Oxidation, wherein, the price of hydrochloric acid is relatively cheap.
In the above-mentioned technical solutions, in step S2, vacuum degree is controlled in the vacuum distillation as 0.1-200Pa, and is collected
160-200 DEG C of fraction；Preferably, vacuum degree is controlled in the vacuum distillation as 10-50Pa, and collects 172-185 DEG C and evaporate
Point.
Vacuum degree is lower, and aliphatic acid rectification temperature is lower, but vacuum degree is lower tightened up to equipment requirement, equipment into
It is originally higher, multistage vacuum pump is selected herein, and aliphatic acid rectification temperature is 160-200 DEG C, greatly reduces the high temperature of aliphatic acid
Denaturalization phenomenon, and relatively good can open linoleic acid and other Separation of Fatty Acids.
In the above-mentioned technical solutions, in step S2, the adsorption refining to distillation fraction is further included, is specially：Distillation is evaporated
Divide and filtered with adsorbent mixing, vacuum stirring to obtain the final product.
Suitable adsorbent is selected to refine linoleic acid, can effectively adsorb the lipid mistake generated in above-mentioned technique
Oxide and oxidation product reduce the colourity of aliphatic acid, improve its quality.
Preferably, in the above-mentioned technical solutions, in step S2, the adsorbent for atlapulgite, activated carbon, diatomite,
The mass ratio of one or more in bleaching clay, bentonite and attapulgite, the adsorbent and distillation fraction is 0.01-0.04:
1；Temperature, time and the vacuum degree of the vacuum stirring are respectively 30-80 DEG C, 10-100min and -0.05~-0.2Mpa, preferably
Ground, temperature, time and the vacuum degree of the vacuum stirring are respectively 40-60 DEG C, 30-50min and -0.08~-0.1Mpa.
It selects one or more as suction in atlapulgite, activated carbon, diatomite, bleaching clay, bentonite and attapulgite
Attached dose, and above-mentioned absorbing process is selected, harmful substance can be effectively adsorbed, and effectively can prevent grease from existing under vacuum
It is contacted in subtractive process with oxygen, further ensures that the adsorption effect of adsorbent.
In the above-mentioned technical solutions, in step S1, further include and vegetable oil is used to prepare fatty acid mixed for raw material hydrolysis, institute
Vegetable oil is stated as one kind in sunflower oil, corn oil, cottonseed oil and safflower oil.
Selection crude vegetal is raw material, derives from a wealth of sources, can stablize the supply of material, in addition natural oil is safer.
Preferably, in the above-mentioned technical solutions, in step S1, the hydrolysis is specially using alkali catalyzed hydrolysis technique：It will
Vegetable oil is stirred at reflux with the aqueous slkali that concentration is 0.2-30wt% at 60-90 DEG C, is reacted 3-8h, is added in 4-10mol/L's
Inorganic acid solution, until the water layer pH value after layering is 3-4, water washed reservoir is up to fatty acid mixed；Preferably, the alkali is hydrogen
One or more in lithia, sodium hydroxide, potassium hydroxide and sodium ethoxide.
Using alkali catalyzed hydrolysis technique, soap first is obtained with the saponification of highly basic and grease, is then acidified again
To free fatty, the method is more thorough with respect to acid hydrolytic reaction, compared with the enzyme hydrolysis time is short, at low cost, convenient post-treatment.
Advantages of the present invention：
(1) present invention prepares high-purity linoleic acid by using metal crystallization-rectification under vacuum technique, and process avoids a large amount of
It is economic and environment-friendly using urea；
(2) preparation method of the invention is using the extensive natural plant grease in source as raw material, low raw-material cost, technique mistake
Journey is simply controllable, and required equipment is simple, and production efficiency is high, and is easy to mass produce, obtained linoleic acid product peroxidating
It is worth that low, of light color, content is high, there is the stronger market competitiveness, can be widely applied to chemical industry, food, cosmetics and drug
Field.
Description of the drawings
Fig. 1 is the gas chromatographic analysis collection of illustrative plates of the safflower seed oil fatty acid mixed of the embodiment of the present invention 1；
Fig. 2 be the embodiment of the present invention 1 using safflower seed oil as raw metal salt crystallization after gas chromatographic analysis collection of illustrative plates；
Fig. 3 is the gas chromatographic analysis for high-purity linoleic acid finished product that the embodiment of the present invention 1 is prepared by raw material of safflower seed oil
Collection of illustrative plates；
Fig. 4 is the gas chromatographic analysis collection of illustrative plates of the sunflower oil fatty acid mixed of the embodiment of the present invention 2.
Specific embodiment
Specific embodiment below in conjunction with the accompanying drawings is described in further detail the specific embodiment of the present invention.Following reality
Example is applied for illustrating the present invention, but is not limited to protection scope of the present invention.
Raw materials and reagents used in the embodiment of the present invention is commercially available production commonly used in the art unless otherwise specified
Product, the method used in the embodiment of the present invention, is conventional method in the art unless otherwise specified, and the present invention is implemented
" yield " described in example is mass percent.
Embodiment 1
An embodiment of the present invention provides a kind of high-purity linoleic preparation methods, comprise the following steps：
S1,200kg safflower seed oils are added in after 60kg sodium hydroxides and 800kg water are sufficiently stirred dissolving, is stirred at 85 DEG C
Reflux is mixed, after reaction solution completely clarification, when clock reaction 4 is small, the hydrochloric acid solution of 6mol/L is slowly added into reaction solution, directly
To reaction liquid layer, lower aqueous layer pH value is 4, and water layer is released using separatory funnel, and oil reservoir is washed with warm water repeatedly up to neutral,
And 5% anhydrous sodium sulfate heating stirring is added in colourless to oil reservoir, fatty acid mixed 185kg is obtained, its Central Asia is learnt in detection
Oleic acid content is 80.68%；The sodium hydroxide of 19.28kg is dissolved in the methanol-water solution of 740kg (W/W=90：10),
The fatty acid mixed of above-mentioned 185kg is added in, 50 DEG C of progress back flow reaction 30min are then stirred and heated to, with 1.5 DEG C/min's
Rate of temperature fall be once cooled to 10 DEG C heat preservation 2 it is small when, once filter, first-time filtrate continued to squeeze into reducing temperature twice in crystallization tank
To -8 DEG C, when heat preservation crystallization 3 is small, secondary suction filtration, the hydrochloric acid of addition 6mol/L, recycling design, by what is obtained into secondary filtrate
Oil temperature water washing adds in a small amount of desiccant dryness and obtains linoleic acid 98kg, wherein linoleic acid content is learnt in detection to neutrality
95.95%；
S2, the linoleic acid obtained in step S1 is put into rectifying still, controls vacuum degree as 20Pa, rectification temperature control
For 165-195 DEG C, 165-170 DEG C, 172-185 DEG C and 185-195 DEG C of fraction is collected respectively, will be collected at 172-185 DEG C
Fraction stirred evenly with 2.2kg activated carbons, 50 DEG C of vacuum stirring 30min obtain linoleic acid finished product 69kg, detection is learnt wherein
Linoleic acid content is 99.35%, color be colourless, peroxide value 0.35, acid value 197, anisidine value 1.0.
Fig. 1, Fig. 2 and Fig. 3 are respectively after the safflower seed oil fatty acid mixed of the embodiment of the present invention 1, metal salt crystallization and make
The gas chromatographic analysis collection of illustrative plates of standby high-purity linoleic acid finished product.
From figure 1 it appears that the aliphatic acid in safflower seed oil is palmitic acid, stearic acid, oleic acid and linoleic mixing
Object, wherein, linoleic acid is main matter, and its content is up to more than 80%, is conducive to linoleic purifying；It can be with from Fig. 2
Find out, by solvent crystallization twice, major impurity has been efficiently removed, and linoleic acid content is increased to from 80.68%
95.95%；From figure 3, it can be seen that rectifying can be very good the impurity of removal height boiling, content is increased to more than 99%.
Embodiment 2
An embodiment of the present invention provides a kind of high-purity linoleic preparation methods, comprise the following steps：
S1,200kg sunflower oils are added in after 60kg sodium hydroxides and 800kg water to be sufficiently stirred to dissolving, is stirred at 85 DEG C
Reflux, when clock reaction 4 is small after reaction solution completely clarification.The hydrochloric acid solution of 6mol/L is slowly added into reaction solution, until
Reaction liquid layer, lower aqueous layer pH value are 4, and separatory funnel releases water layer, and oil reservoir is washed with warm water repeatedly until neutral, and oil reservoir adds
Enter 5% anhydrous sodium sulfate heating stirring to colourless, obtain fatty acid mixed 180kg, content 65.31%；By 10.34kg's
Sodium hydroxide is dissolved in the ethanol-water solution of 720kg (W/W=90：10) fatty acid mixed of processing, is walked in addition, then
Be stirred and heated to 50 DEG C of progress saponification back flow reaction 30min, slow cooling to 8 DEG C of heat preservations 2 it is small when, filter, filtrate continues to squeeze into
Continue to be cooled to -12 DEG C, when heat preservation crystallization 4 is small in crystallization tank, filter, the hydrochloric acid of a small amount of 6mol/L in filtrate, recycling design,
Obtained oil temperature water washing adds in a small amount of desiccant dryness and obtains linoleic acid 85kg, content 94.74% to neutrality；
S2, the linoleic acid obtained in step S1 is put into rectifying still, vacuum degree control is in 15pa or so, rectification temperature
Control collects second fraction at 175 DEG C or so, weight 69kg, color to be faint yellow, linoleic acid that rectifying is obtained with
The atlapulgite of 3.5kg stirs evenly, and 60 DEG C of vacuum stirring 30min obtain linoleic acid finished product 62kg, content ＞ 99%, face
Color be colourless, peroxide value 0.2, acid value 196, anisidine value 1.5.
Fig. 4 is the gas chromatographic analysis collection of illustrative plates of the sunflower oil fatty acid mixed of the embodiment of the present invention 2.It can from figure
Going out, the aliphatic acid composition of sunflower oil is similar to safflower seed oil, but content is different, and sunflower oil linoleic acid content is low, and
Major impurity oleic acid content is higher, this requires separation purifying technique tightened up, it is necessary to which controlling of production process is more careful.
Comparative example 1
Comparative example 1 of the present invention provides a kind of high-purity linoleic preparation method, comprises the following steps：
S1,5kg safflower seed oils are added in after 1.5kg sodium hydroxides and 20kg water are sufficiently stirred dissolving, is stirred at 85 DEG C
After reaction solution completely clarification, when clock reaction 4 is small, the hydrochloric acid solution of 6mol/L is slowly added into reaction solution for reflux, until
Reaction liquid layer, lower aqueous layer pH value are 4, and water layer is released using separatory funnel, and oil reservoir is washed with warm water repeatedly up to neutral, and
5% anhydrous sodium sulfate heating stirring is added in colourless to oil reservoir, obtains fatty acid mixed 4.5kg, its Central Asia oil is learnt in detection
Acid content is 81%；
S2, the above-mentioned safflower seed oil fatty acid mixeds of 1000g is taken to carry out urea clathrate processing respectively, urine bag ratio is respectively
Fatty acid mixed：Urea：Alcohol=1:1.5:4.5、1:2:5.5、1:2.5:7.5、1:3:8.1, wherein the temperature control of urine bag is 10
DEG C, the urine bag time is 12h, is filtered, and collects filtrate, deals and purity, peroxidating are surveyed after linoleic acid is handled with activated carbon adsorption
Value, anisidine value, test result are as shown in table 1 below.
The linoleic product analysis result of different urine bag ratios in 1 comparative example 1 of the present invention of table
Can be seen that the linoleic acid content obtained with the method for urea clathrate from the result in table 1 is up to 98%, and
The peroxide value and anisidine value of linoleic acid product are higher, and fatty acid quality is relatively low.
Comparative example 2
Comparative example 2 of the present invention provides a kind of high-purity linoleic preparation method, comprises the following steps：
S1,2.5kg safflower seed oils are added in after 0.75kg sodium hydroxides and 10kg water are sufficiently stirred dissolving, is stirred at 85 DEG C
Reflux is mixed, after reaction solution completely clarification, when clock reaction 4 is small, the hydrochloric acid solution of 6mol/L is slowly added into reaction solution, directly
To reaction liquid layer, lower aqueous layer pH value is 4, and water layer is released using separatory funnel, and oil reservoir is washed with warm water repeatedly up to neutral,
And 5% anhydrous sodium sulfate heating stirring is added in colourless to oil reservoir, fatty acid mixed 2.35kg is obtained, its Central Asia is learnt in detection
Oleic acid content is 80.15%；The sodium hydroxide of 13.28kg is dissolved in the methanol-water solution of 740kg (W/W=90：10),
The fatty acid mixed of above-mentioned 185kg is added in, 45 DEG C of progress back flow reaction 30min are then stirred and heated to, with the drop of 3 DEG C/min
Warm rate be once cooled to 10 DEG C of heat preservations 2 it is small when, filter, the hydrochloric acid of 6mol/L, recycling design, the oil that will be obtained added in filtrate
Warm water is washed to neutrality, is added in a small amount of desiccant dryness and is obtained linoleic acid 1.5kg, wherein linoleic acid content 93.69% is learnt in detection；
S2, the linoleic acid obtained in step S1 is put into rectifying still, controls vacuum degree as 250Pa, rectification temperature control
185-250 DEG C is made as, 3 fractions of Fractional Collections stir the fraction being collected at 193-215 DEG C and 0.02kg activated carbons equal
Even, 50 DEG C of vacuum stirring 30min obtain linoleic acid finished product 0.75kg, and detection learns that wherein linoleic acid content is 97.7%, color
To be colourless, peroxide value 0.33, acid value 198, anisidine value 1.2.
The result of comparison comparative example 2 and embodiment 1 can be seen that fatty acid metal salts employed in embodiment 1 twice
Segmentation filters crystallization and use obtained linoleic acid content control after a crystallization more preferably than 2 kinds of comparative example, and wherein fat
The vacuum degree of sour rectifying is affected to its rectification effect.
The present invention prepares high-purity linoleic acid by using metal crystallization-rectification under vacuum technique, the linoleic acid which obtains
Purity is high, and quality is good, and monomelic impurities are controlled, and meets biological medicine ingredient requirement；The preparation method of the present invention is to derive from a wealth of sources
Natural plant grease for raw material, low raw-material cost, technical process is simply controllable, and required equipment is simple, and production efficiency is high, and
It is easy to mass produce, obtained linoleic acid product peroxide value is low, of light color, content is high, has stronger market competition
Power can be widely applied to chemical industry, food, cosmetics and medicine field.
Finally, it these are only the preferred embodiment of the present invention, be not intended to limit the scope of the present invention.It is all this
Within the spirit and principle of invention, any modifications, equivalent replacements and improvements are made should be included in the protection model of the present invention
Within enclosing.
Claims (10)
1. a kind of high-purity linoleic preparation method, which is characterized in that comprise the following steps：
S1, fatty acid mixed and highly basic are dissolved in the mixed solution of low-carbon alcohols-water, heated, back flow reaction, protected after once cooling down
Warm crystallization, once filters, and crystallization will be kept the temperature after first-time filtrate reducing temperature twice, and secondary suction filtration adds in excessive strong into secondary filtrate
Acid is distilled to recover low-carbon alcohols-water, obtains yellow oil, be washed to neutrality and obtain linoleic acid crude product, wherein, the low-carbon
Alcohol is the one or more in methanol, ethyl alcohol, n-butanol and isobutanol；
The linoleic acid crude product obtained in S2, vacuum distillation step S1, Fractional Collections fraction is to get high-purity linoleic acid.
2. preparation method according to claim 1, which is characterized in that in step S1, the rate of temperature fall once to cool down
For 1-3 DEG C/min, and 1-10h is kept the temperature at 0~20 DEG C, preferably keep the temperature 2-3h；The rate of temperature fall of the reducing temperature twice is 1-3
DEG C/min, and 1-10h is kept the temperature at -15~-5 DEG C, preferably keep the temperature 2-3h.
3. preparation method according to claim 1 or 2, which is characterized in that in step S1, the reaction temperature is 50-75
DEG C, reaction time 10-80min.
4. preparation method according to claim 1 or 2, which is characterized in that in step S1, the highly basic for sodium hydroxide,
The mass ratio of one or more in potassium hydroxide, sodium ethoxide and lithium hydroxide, the highly basic and fatty acid mixed is 0.1-2:
1；The mass ratio of the low-carbon alcohols and water is 6-9.5:1, it is preferably 8.5-9:1.
5. preparation method according to claim 1 or 2, which is characterized in that in step S1, the strong acid is hydrochloric acid, sulfuric acid
It is preferably hydrochloric acid with one kind in nitric acid.
6. preparation method according to claim 1, which is characterized in that in step S2, vacuum is controlled in the vacuum distillation
It spends for 0.1-200Pa, and collects 160-200 DEG C of fraction；Preferably, vacuum degree is controlled in the vacuum distillation as 10-50Pa,
And collect 172-185 DEG C of fraction.
7. according to the preparation method described in claim 1-6, which is characterized in that in step S2, further include the suction to distillation fraction
It is attached refined, be specially：By distillation fraction and adsorbent mixing, be stirred under vacuum, filter to obtain the final product.
8. preparation method according to claim 7, which is characterized in that in step S2, the adsorbent is atlapulgite, work
The mass ratio of one or more in property charcoal, diatomite, bleaching clay, bentonite and attapulgite, the adsorbent and distillation fraction
For 0.01-0.04:1；Temperature, time and the vacuum degree of the vacuum stirring are respectively 30-80 DEG C, 10-100min and -0.05
~-0.2Mpa, it is preferable that temperature, time and the vacuum degree of the vacuum stirring are respectively 40-60 DEG C, 30-50min and -0.08
~-0.1Mpa.
9. according to the preparation method described in claim 1-6, which is characterized in that in step S1, further include and use vegetable oil as original
Material hydrolysis prepares fatty acid mixed, and the vegetable oil is one kind in sunflower oil, corn oil, cottonseed oil and safflower oil.
10. preparation method according to claim 9, which is characterized in that in step S1, the hydrolysis is using alkali catalyzed hydrolysis
Technique, specially：Vegetable oil with concentration for the aqueous slkali of 0.2-30wt% at 60-90 DEG C is stirred at reflux, 3-8h is reacted, adds
Enter the inorganic acid solution of 4-10mol/L, until the water layer pH value after layering is 3-4, water washed reservoir is up to fatty acid mixed；It is preferred that
Ground, the alkali are the one or more in lithium hydroxide, sodium hydroxide, potassium hydroxide and sodium ethoxide.
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| CN201711424018.4A CN108084016A (en) | 2017-12-25 | 2017-12-25 | A kind of high-purity linoleic preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110257175A (en) * | 2019-06-20 | 2019-09-20 | 深圳市仙迪化妆品有限公司 | It is a kind of to prepare linoleic method and linoleic application using rose hip oil |
| CN113121332A (en) * | 2021-03-29 | 2021-07-16 | 湖南万象生物科技有限公司 | Method for reducing content of unsaponifiable matters in high-purity oleic acid |
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| WO2016182452A1 (en) * | 2015-05-13 | 2016-11-17 | Epax Norway As | Very long chain polyunsaturated fatty acids from natural oils |
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| CN106590939A (en) * | 2015-10-16 | 2017-04-26 | 浙江医药股份有限公司新昌制药厂 | Method for purification preparation of high content linoleic acid by using vegetable oil as raw material |
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| CN110257175A (en) * | 2019-06-20 | 2019-09-20 | 深圳市仙迪化妆品有限公司 | It is a kind of to prepare linoleic method and linoleic application using rose hip oil |
| CN113121332A (en) * | 2021-03-29 | 2021-07-16 | 湖南万象生物科技有限公司 | Method for reducing content of unsaponifiable matters in high-purity oleic acid |
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