CN105967998A - Preparation method of linoleic acid with purity of 99% - Google Patents
Preparation method of linoleic acid with purity of 99% Download PDFInfo
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- CN105967998A CN105967998A CN201610292995.2A CN201610292995A CN105967998A CN 105967998 A CN105967998 A CN 105967998A CN 201610292995 A CN201610292995 A CN 201610292995A CN 105967998 A CN105967998 A CN 105967998A
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- linoleic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- 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
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of linoleic acid with purity of 99%. The preparation method utilizes a urea coating-freezing crystallization-molecular distillation combined technology and comprises putting linoleic acid with purity of 80%, urea and anhydrous ethanol into a urea coating reactor according to a mass ratio, carrying out heating stirring and backflow, adding the mixture into a crystallization tank, carrying out crystallization, carrying out cooling and separation, carrying out filtration to obtain a liquid phase, carrying out recrystallization on the liquid phase in the crystallization tank, separating a liquid, injecting the liquid into a mixed liquid storage tank, evaporating the mixed liquid, recovering ethanol, carrying out water washing in a heavy phase recovery tank, discharging water so that purified crude linoleic acid is obtained, pumping the crude linoleic acid into a molecular distillation system, carrying out refinement, collecting a light phase which is linoleic acid, treating solid urea calthrates and recovering aliphatic acid. The product linoleic acid has content of 99% and a product yield of 20% or more. The preparation method is suitable for industrial production and fills in gaps of domestic 99% linoleic acid industrial production.
Description
Technical field
The present invention relates to the linoleic preparation method of purity 99%.
Background technology
Linoleic acid has reduction blood fat, vessel softening, reduces blood pressure, promotes microcirculatory effect, can prevent or reduce the heart
The sickness rate of angiopathy, particularly to hypertension, hyperlipidemia, angina pectoris, coronary heart disease, atherosclerosis, senile obesity
Deng preventing and treating extremely advantageous, the deposition preventing human serum cholesterol in blood vessel wall can be played, have the good reputation of " blood vessel street cleaner ",
There is the health-care effect preventing and treating atherosclerosis and cardiovascular disease.
The most linoleic content, 50～about 80%, is mainly taked the methods such as fractional distillation, distillation, is also taked
Urea bag solvent method, but linoleic content is at most about 90%.
Application No. 201310626940.7 provides the preparation method of a kind of conjugated linoleic acid, and the method includes Asia oil
Acid esters is under the pKa organic base catalytic more than 11, and conjugate linoleate is prepared in reaction, it is also possible to further by conjugated linoleic acid
Ester and glycerol or derivatives thereof carry out ester exchange reaction, prepare conjugated linoleic acid glyceride, although utilize the method to prepare
The content of the fatty acid of the conjugated linoleic acid product obtained meets relevant provisions of laws and regulations, but linoleic content is not
High.
Application No. 201510088971.0 discloses the production technology of a kind of conjugated linoleic acid, comprises the following steps: (1)
Refining reaction；(2) conjugative reaction；(3) saponification；(4) acidification reaction；(5) concentrate；(6) molecular distillation, step is many,
After the linoleic acid content that obtains the highest, the highest to the condition required for some steps.
The linoleic content of existing market is typically about 60%, and high 90%, content is substantially sky at 99% linoleic acid
In vain, industrialized production 99% linoleic acid there is presently no report. and mainly linoleic acid is unsaturated fatty acid, and oxidation stability is poor,
The present invention mainly provides a kind of linoleic acid industrially producing 99% purity and preparation method, and this product is at food, food additive
Add agent, medicine is widely used, specifically take urea bag-freezing and crystallizing-molecular distillation group technology, select suitable former auxiliary material
Material, designed, designed equipment, under special process conditions, the linoleic acid of industrialized production 99%.
Summary of the invention
The purpose of the present invention can be achieved through the following technical solutions:
The linoleic acid of purity 99%, is prepared from by 80% linoleic acid, carbamide and dehydrated alcohol, 80% affiliated linoleic acid: carbamide:
The mass ratio 1～1.5:5～5.5:10～11 of dehydrated alcohol carries out linoleic purification.
Its compound method is:
80% linoleic acid, carbamide and dehydrated alcohol are put in mass ratio in urea bag still, be stirred and heated to 80～85 DEG C, backflow 2
～3 hours, squeeze in crystallizer and crystallize, material temperature is dropped to-5～-10 DEG C, material is separated, by liquid phase-5～-
10 DEG C are repeated to crystallize 2～3 times at crystallizer, each crystallization time 48 hours, are finally recovered out liquid and squeeze into mixing liquid storage
Tank, mixed liquor is evaporated (100～110 DEG C), reclaims ethanol, and heavy phase collecting tank washes, thick for after purifying after discharging water
Linoleic acid.Thick linoleic acid pumps into molecular distillation system, refines, and light phase is 99% linoleic acid.Solid phase urea bag thing processes,
Reclaim fatty acid.
The beneficial effects of the present invention is: the present invention takes urea bag-freezing and crystallizing-molecular distillation group technology, used by set
Standby simple, easily reclaim during with ethanol as solvent, be easily isolated the material of different component in this experiment with freezing and crystallizing, use
Molecular distillation technique, to linoleic good stability, whole Period Process is comparatively short, simple to operate, and in final products obtained therefrom
Linoleic content 99%, product yield more than 20%, can industrialized production, fill up the sky of domestic 99% linoleic acid industrialized production
In vain.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below in conjunction with
Detailed description of the invention, is expanded on further the present invention.
Embodiment 1:
By 80% linoleic acid 120 kg, 636 kilograms of carbamide, dehydrated alcohol 1272 kilograms puts in urea bag still, agitating heating 80～
85 DEG C are refluxed 2.5 hours, pump in crystallizer, and cooling-5～-10 DEG C of crystallizations are filtered and separated liquid phase, pump into crystallizer cooling-5
～-10 DEG C of crystallizations, filtering and separate, liquid phase presses this technique Crystallization Separation, and solid phase is recovered as mixed acid, and isolated liquid phase is steamed
Beaming back receipts ethanol, heavy phase carries out washing to obtain thick linoleic acid, and thick linoleic acid enters molecular distillation system and refines, obtains finished product 99%
Linoleic acid 27.2 kilograms, products obtained therefrom yield 22.67%, each component of gained and content and each component and the comparison of content in raw material
As shown in table 1:
Table 1
Embodiment 2:
By 80% linoleic acid 120 kg, 660 kilograms of carbamide, dehydrated alcohol 1272 kilograms puts in urea bag still, agitating heating 80～
85 DEG C are refluxed 2.5 hours, pump in crystallizer, and cooling-5～-10 DEG C of crystallizations are filtered and separated liquid phase, originally enter crystallizer cooling-5
～-10 DEG C of crystallizations, filtering and separate, liquid phase presses this technique Crystallization Separation, and solid phase is recovered as mixed acid, and isolated liquid phase is steamed
Beaming back receipts ethanol, heavy phase carries out washing to obtain thick linoleic acid, and thick linoleic acid enters molecular distillation system and refines, obtains finished product 99%
Linoleic acid 25.1 kilograms, products obtained therefrom yield 20.91%, each component of gained and content and each component and the comparison of content in raw material
As shown in table 2:
Table 2
Embodiment 3:
By 80% linoleic acid 120 kg, 600 kilograms of carbamide, dehydrated alcohol 1272 kilograms puts in urea bag still, agitating heating 80～
85 DEG C are refluxed 2.5 hours, pump in crystallizer, and cooling-5～-10 DEG C is filtered and separated liquid phase, originally enter crystallizer cooling-5～-
10 DEG C, filtering and separate, liquid phase presses this technique Crystallization Separation, and solid phase is recovered as mixed acid, and isolated liquid phase is evaporated reclaiming
Ethanol, heavy phase carries out washing to obtain thick linoleic acid, and thick linoleic acid enters molecular distillation system and refines, obtains finished product 99% linoleic acid
28.5 kilograms, products obtained therefrom yield 23.75%, each component of gained and content and each component and comparison such as table 3 institute of content in raw material
Show:
Table 3
Obviously the present invention implements and is not subject to the restrictions described above, as long as have employed method design and the technical side of the present invention
The improvement of the various unsubstantialities that case is carried out, or the most improved design by the present invention and technical scheme directly apply to other
Close, all within protection scope of the present invention.
Claims (4)
1. the linoleic preparation method of purity 99%, it is characterised in that: the method takes urea bag-freezing and crystallizing-molecular distillation
Group technology, puts in urea bag still in mass ratio by 80% linoleic acid, carbamide and dehydrated alcohol, heated and stirred, backflow, squeezes into knot
Brilliant tank crystallizes, material cooling is separated, filters and separate liquid phase, liquid phase is repeated crystallization at crystallizer, is finally recovered out
Liquid squeezes into mixing wet tank, and mixed liquor is evaporated, and reclaims ethanol, and heavy phase collecting tank is washed, for purifying after discharging water
After thick linoleic acid, thick linoleic acid pumps into molecular distillation system, refines, light phase for linoleic acid, at solid phase urea bag thing
Reason, reclaims fatty acid.
The linoleic preparation method of purity 99% the most according to claim 1, it is characterised in that: described 80% linoleic acid, carbamide
It is 1～1.5:5～5.5:10～11 in mass ratio with dehydrated alcohol.
The linoleic preparation method of purity 99% the most according to claim 1, it is characterised in that: described inclusion reaction temperature 80
～85 DEG C, reflux 2～3 hours.
The linoleic preparation method of purity 99% the most according to claim 1, it is characterised in that: described crystallization in crystallizer
Time, repeat to crystallize 2～3 times, each crystallization time 48 hours at-5～-10 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610292995.2A CN105967998A (en) | 2016-05-06 | 2016-05-06 | Preparation method of linoleic acid with purity of 99% |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610292995.2A CN105967998A (en) | 2016-05-06 | 2016-05-06 | Preparation method of linoleic acid with purity of 99% |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110499216A (en) * | 2019-08-29 | 2019-11-26 | 安徽省瑞芬得油脂深加工有限公司 | The linoleic preparation method of high-purity |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4776984A (en) * | 1984-10-10 | 1988-10-11 | Nestec S. A. | Process for the enrichment with Δ6 fatty acids of a mixture of fatty acids |
| CN101455399A (en) * | 2008-12-31 | 2009-06-17 | 西藏自治区高原生物研究所 | Linoleate preparation method using highland barley bran oil |
-
2016
- 2016-05-06 CN CN201610292995.2A patent/CN105967998A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4776984A (en) * | 1984-10-10 | 1988-10-11 | Nestec S. A. | Process for the enrichment with Δ6 fatty acids of a mixture of fatty acids |
| CN101455399A (en) * | 2008-12-31 | 2009-06-17 | 西藏自治区高原生物研究所 | Linoleate preparation method using highland barley bran oil |
Non-Patent Citations (1)
| Title |
|---|
| 孙磊等: "亚油酸及共轭亚油酸异构体纯化技术优化", 《中国油脂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110499216A (en) * | 2019-08-29 | 2019-11-26 | 安徽省瑞芬得油脂深加工有限公司 | The linoleic preparation method of high-purity |
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