CN107418724A - A kind of method for separating unsaturated fat acid blend in soybean oil residue aliphatic acid - Google Patents
A kind of method for separating unsaturated fat acid blend in soybean oil residue aliphatic acid Download PDFInfo
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- CN107418724A CN107418724A CN201710257595.2A CN201710257595A CN107418724A CN 107418724 A CN107418724 A CN 107418724A CN 201710257595 A CN201710257595 A CN 201710257595A CN 107418724 A CN107418724 A CN 107418724A
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- temperature
- filtrate
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- soybean oil
- crystallization
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/006—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
- C11B3/16—Refining fats or fatty oils by mechanical means
-
- 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
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0075—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils by differences of melting or solidifying points
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention provides a kind of method for separating unsaturated fat acid blend in soybean oil residue aliphatic acid；Make solvent and soybean oil residue aliphatic acid miscible, clear transparent solutions are formed after heating；Then among solution being poured into cooling reactor, stirring, decrease temperature crystalline, centrifugal filtration at a temperature of 8~10 DEG C are opened；The filtrate obtained after filtering is according to certain falling temperature gradient, crystallize, filter at lower temperatures, repeat step until last low temperature crystallization temperature 2 DEG C~7 DEG C, filtrate crystallize at such a temperature, filter after obtained filtrate pour into desolvation among rectification under vacuum kettle, dry gas stripping further removes dissolvent residual, obtains unsaturated acids product of the unrighted acid total content 94%~98%.Soybean oil residue aliphatic acid is separated using the method for the low temperature crystallization of solvent, the rotten of raw material will not be caused, it is simple to operate, waste water is not produced, solvent is repeatable to be utilized, and product yield is higher.
Description
Technical field
The present invention relates to a kind of chemical products separation and purification technical field, insatiable hunger in more particularly to a kind of separation soybean oil residue
With the method and flow of fatty acid mixt.
Background technology
Palmitic acid (15%~20%), stearic acid (2%~5%), oleic acid (25% are mainly contained in soybean oil residue aliphatic acid
~30%), several materials with higher economic value such as linoleic acid (45%~50%) and leukotrienes (1%~5%).Wherein
Palmitic acid and stearic acid are used equally for the raw material as daily chemical products such as production soap, detergent in daily chemical industry, and palmitic acid is also
Surfactant, emulsifying agent and wetting agent available for production environment-friendly type etc.；Linoleic acid, leukotrienes are essential fatty acids,
Both material human bodies all can not be synthesized voluntarily, it is necessary to be absorbed from food；Alpha-linolenic acid is the precursor for synthesizing DHA, EPA, is sought
Foster value is very high.The unrighted acids such as oleic acid, linoleic acid, leukotrienes can be also used for the cosmetics of super quality, Premium detergents, height
The production of shelves coating and high-grade paint.If these materials can be separated, its economic value will be greatly improved.
At present, the separating technology of aliphatic acid mainly has rectification under vacuum method, urea adduct method, silver ion complexation, low temperature knot
Crystallization, molecular distillation, supercritical extract, biological enzyme several method.The advantages of rectification under vacuum separates is that technological process is simple,
Equipment investment is low, and product color is good, purity is high, and shortcoming is influenceed greatly by operating condition, and operation at high temperature easily causes temperature-sensitive
Property material deterioration, is generally used to fractionation of fatty acid formicester；Urea adduct method is often used to separating saturated fatty acid and unsaturated lipid
Fat acid, technological process is simple, raw material will not be caused to go bad, but urea-containing waste water, Er Qieshou can be produced in this technical process
Rate is relatively low；The advantages of the crystallizing process under low temperature of solvent is simple to operate, cost of equipment is low, solvent is cheap and easy to get and under cryogenic
Unrighted acid is unlikely to deteriorate, and shortcoming is that solvent-oil ratio is big, and it is big to separate cold consumption during polyunsaturated fatty acid；Remaining several side
Method is currently limited to laboratory stage, industrialization is deposited due to the problems such as production cycle is long, equipment investment is high, treating capacity is small be present
In difficulty.
The content of the invention
The purpose of the present invention, it is to propose a kind of effect separation soybean oil residue fat that is good, pollution-free, being adapted to industrialized production
The method in unrighted acid in fat acid, and provide the process route of the method.
To realize the purpose of the present invention, plan uses following technical scheme：
A kind of method for separating unsaturated fat acid blend in soybean oil residue aliphatic acid；Its step is as follows：
(1) make solvent and soybean oil residue aliphatic acid miscible, clear transparent solutions are formed after heating；
(2) among and then by solution pouring into cooling reactor, stirring, the decrease temperature crystalline under certain temperature in the kettle are opened；
(3) when there is Precipitation in solution, and after the temperature of feed liquid remains unchanged in kettle, feed liquid is filtrated to get filter
Liquid and precipitation solid, because filtrate may newly produce precipitation in filter process, therefore obtained filtrate need to be heated to newly producing
Precipitation be wholly absent；
(4) filtrate that step (3) obtains pours into low temperature crystallization among cooling reactor again, and crystallization temperature now is than last
The temperature of low temperature crystallization is low 4~5 DEG C, opens stirring；After solution separates out precipitation under temperature, the operation of repeat step (3)
Process, obtain new filtrate；
(5) repeat step (4) operates, the crystallization carried out under Different hypothermia stage by stage multiple to filtrate, filter operation, until
The temperature of last low temperature crystallization after -2 DEG C~-7 DEG C, filtrate are filtered according to step (3) at such a temperature, fall by obtained filtrate
Enter desolvation among rectification under vacuum kettle, dry gas stripping further removes dissolvent residual, obtains unrighted acid and always contain
Measure the unsaturated acids product 94%~98%.
Each low temperature crystallization stage is obtained into precipitation consolute, solvent is then added and dissolves to form settled solution, 8~10
Press filtration is carried out under conditions of DEG C, filtrate when next lock out operation, add step (2) start low temperature crystallization before material solution it
In.After precipitation drying after press filtration, solid product of the saturated fatty acid total content more than 90% is obtained.
The solvent is n-hexane, methanol or ethanol.Solvent is with soybean oil residue aliphatic acid according to mass ratio 1.5:1~2.5:
1 feeding.Precipitation is with solvent quality than 1:0.7~1:2.
The present invention compared with the prior art the characteristics of：Use the method separation soybean oil residue fat of the low temperature crystallization of solvent
Acid, the rotten of raw material will not be caused, and simple to operate, treating capacity is big, during will not produce waste water, solvent can repeat profit
With product yield is higher；Using the operation of fraction gradient decrease temperature crystalline, with the mode phase directly disposably crystallized at a temperature of certain
Than greatly reducing solvent load, and crystallization operation will not produce excessive precipitation every time, reduce the difficulty of filtering；Consider
To the reprocessing problem of caused precipitation in each step, a part of product can be reclaimed, improve the total recovery of product, and
Obtain the higher saturated fat acid product of purity
Brief description of the drawings
Fig. 1：Present invention process flow chart.
Embodiment
The present invention is described in further details below in conjunction with the accompanying drawings：
As shown in Figure 1：
Step (1)：Make solvent (n-hexane, methanol or ethanol) with soybean oil residue aliphatic acid according to solvent and raw material matter first
Measure ratio 1.5:1~2.5:1 ratio, it is miscible and be heated to 30~40 DEG C formation clear transparent solutions；
Step (2)：Then among this solution being poured into cooling reactor, stirring is opened, first in 8 DEG C~10 DEG C of temperature in the kettle
Lower decrease temperature crystalline；
Step (3)：, will when there is a large amount of Precipitations in solution, and after the temperature of feed liquid remains unchanged substantially in kettle
Feed liquid centrifuges among pouring into centrifuge, obtains filtrate and precipitation solid, and it is complete that obtained filtrate is heated into new caused precipitation
Melt；
Step (4)：Filtrate after fusing pours into low temperature crystallization among cooling reactor again, and crystallization temperature now is than last
The temperature of low temperature crystallization is low 4~5 DEG C, pays attention to still opening stirring in crystallization process.When solution separates out precipitation under the temperature
Afterwards, the operating process of repeat step (3), obtains new filtrate；
Step (5)：Repeat step (4) is operated, and crystallization, the filtering repeatedly carried out to the filtrate under Different hypothermia stage by stage is grasped
Make, until last time, when the temperature of low temperature crystallization is at -2 DEG C~-7 DEG C, filtrate filters it according to step (3) at such a temperature
Afterwards, the filtrate obtained is no longer in next cold stage low temperature crystallization；
Step (6)：The filtrate that step (5) finally obtains is poured into desolvation among rectification under vacuum kettle, and then with dry
Pathogenic dryness body stripping, further removes dissolvent residual, and the unsaturated acids for obtaining unrighted acid total content 94%~98% produces
Product；
Step (7)：Each stage obtains precipitating miscible to one piece, and then according to precipitation, (now used is molten with solvent
Agent should be consistent with solvent when dissolving raw material at the beginning) mass ratio 1:0.7~1:2 ratio adds solvent, and heating makes its dissolving,
Press filtration is carried out to it under conditions of 8~10 DEG C, the fluid storage that press filtration is obtained, step is added when next lock out operation
Suddenly among the material solution before (2) beginning low temperature crystallization；
The press filtration precipitation that step (7) obtains is put among 40 DEG C of baking ovens and dried by step (8), obtains content more than 90%
Saturated fat acid blend solid product.
Embodiment 1：
Using n-hexane as solvent, specific experiment step is as follows for the separation process of this embodiment：
(1) it is 1200g n-hexanes and 800g soybean oil residues aliphatic acid (unsaturated fatty acid content 73.54%) is miscible simultaneously
40 DEG C of formation clear transparent solutions are heated to, among this solution then is positioned over into cooling reactor, stirring are opened, in 8 DEG C of kettle
At a temperature of decrease temperature crystalline；
(2) when there are a large amount of Precipitations in solution, and after the temperature of feed liquid remains unchanged substantially in kettle, feed liquid is fallen
Enter and centrifuge among small-sized link-suspended basket centrifuge, the filtrate for centrifuging to obtain again low-grade fever to 20 DEG C make it is wherein new caused by precipitation melt
Change, then by feed liquid again down among cooling reactor；
(3) operating process of repeat step (1) and step (2), the low temperature crystallization at 4 DEG C, 0 DEG C, -4 DEG C, is finally obtained respectively
To the filtrate containing product；
(4) obtained filtrate is evaporated under reduced pressure among rectification under vacuum kettle, the solvent steamed remains among being put in holding vessel
Next time uses, and the crude product in distillation still is dried by a simple gas stripping tower and further removes solvent, finally
To 456g, the product that unrighted acid total content is 98.4%, main component therein is oleic acid and linoleic acid, and acquisition is somebody's turn to do
The yield of unrighted acid mix product is 71%；
(5) precipitation that obtains in each decrease temperature crystalline stage is mixed to one piece, then according to precipitation：Solvent quality is than 1:0.75
Ratio adds n-hexane solvent, and heating makes its dissolving, carries out press filtration to it under conditions of 8 DEG C, the liquid that press filtration obtains is placed in
In holding vessel, separated again among 8 DEG C of cooling reactors of addition until separation process next time.Remaining solid is content after press filtration
The solid mixture of saturated fatty acid more than 90%.
Embodiment 2：
Using ethanol as solvent, specific experiment step is as follows for the separation process of this embodiment：
(1) by 1200g ethanol and 800g soybean oil residues aliphatic acid (unsaturated fatty acid content 73.54%) it is miscible and add
Heat among this solution then is positioned over into cooling reactor, opens stirring to 40 DEG C of formation clear transparent solutions, warm in 10 DEG C of kettle
The lower decrease temperature crystalline of degree；
(2) when there are a large amount of Precipitations in solution, and after the temperature of feed liquid remains unchanged substantially in kettle, feed liquid is fallen
Enter and centrifuge among small-sized link-suspended basket centrifuge, the filtrate for centrifuging to obtain again low-grade fever to 20 DEG C make it is wherein new caused by precipitation melt
Change, then by feed liquid again down among cooling reactor；
(3) operating process of repeat step (1) and step (2), the low temperature crystallization at 4 DEG C, 0 DEG C, -5 DEG C, is finally obtained respectively
To the filtrate containing product；
(4) filtrate that step (3) obtains is evaporated under reduced pressure among rectification under vacuum kettle, and the solvent steamed is put among holding vessel
Remain next use, the crude product in distillation still is by a simple gas stripping tower drying and further removes solvent, most
463g is obtained afterwards, the product that unrighted acid total content is 94.8%, the main component of the product is oleic acid and linoleic acid, no
The yield of saturated fatty acid is 73%.
(5) precipitation that obtains in each decrease temperature crystalline stage is mixed to one piece, then according to precipitation：Solvent quality is than 1：1.5
Ratio adds alcohol solvent, and heating makes its dissolving, carries out press filtration to it under conditions of 10 DEG C, the liquid that press filtration obtains is placed in storage
Deposit in tank, separated again among 10 DEG C of cooling reactors of addition until separation process next time.Remaining solid is content after press filtration
The solid mixture of saturated fatty acid more than 91%.
Embodiment 3：
Using methanol as solvent, specific experiment step is as follows for the separation process of this embodiment：
(1) by 1600g methanol and 800g soybean oil residues aliphatic acid (unsaturated fatty acid content 73.54%) it is miscible and add
Heat among this solution then is positioned over into cooling reactor, opens stirring to 40 DEG C of formation clear transparent solutions, warm in 9 DEG C of kettle
The lower decrease temperature crystalline of degree；
(2) when there are a large amount of Precipitations in solution, and after the temperature of feed liquid remains unchanged substantially in kettle, feed liquid is fallen
Enter and centrifuge among small-sized link-suspended basket centrifuge, the filtrate for centrifuging to obtain again low-grade fever to 20 DEG C make it is wherein new caused by precipitation melt
Change, then by feed liquid again down among cooling reactor；
(3) operating process of repeat step (1) and step (2), the low temperature crystallization at 5 DEG C, 0 DEG C, -4 DEG C, is finally obtained respectively
To the filtrate containing product；
(4) filtrate that step (3) obtains is evaporated under reduced pressure among rectification under vacuum kettle, and the solvent steamed is put among holding vessel
Remain next use, the crude product in distillation still is by a simple gas stripping tower drying and further removes solvent, most
430g is obtained afterwards, the product that unrighted acid total content is 96.7%, the main component of product is oleic acid and linoleic acid, insatiable hunger
Yield with aliphatic acid is 67%.
(5) precipitation that obtains in each decrease temperature crystalline stage is mixed to one piece, then according to precipitation：Solvent quality is than 1：2 ratio
Example adds methanol solvate, and heating makes its dissolving, carries out press filtration to it under conditions of 10 DEG C, the liquid that press filtration obtains is placed in storage
In tank, separated again among 9 DEG C of cooling reactors of addition until separation process next time.Remaining solid is that content exists after press filtration
The solid mixture of more than 91% saturated fatty acid.
Insatiable hunger in a kind of segmentation decrease temperature crystalline separation soybean oil residue aliphatic acid using solvent that the present invention is disclosed and proposed
With the method for aliphatic acid, those skilled in the art can be by using for reference present disclosure, and the appropriate links such as condition route that change are realized, to the greatest extent
The method and technology of preparing of the pipe present invention is described by preferred embodiment, and person skilled can substantially not take off
Methods and techniques described herein route is modified or reconfigured from present invention, spirit and scope, to realize
Final technology of preparing.In particular, all similar replacements and change be for a person skilled in the art
It will be apparent that they are considered as being included in spiritual, scope and content of the invention.
Claims (6)
- A kind of 1. method for separating unsaturated fat acid blend in soybean oil residue aliphatic acid；It is characterized in that step is as follows：(1) make solvent and soybean oil residue aliphatic acid miscible, be heated to 30~40 DEG C of formation clear transparent solutions；(2) among and then by solution pouring into cooling reactor, stirring, the decrease temperature crystalline under 8 DEG C~10 DEG C of temperature in the kettle are opened；(3) when there is Precipitation in solution, and after the temperature of feed liquid remains unchanged in kettle, feed liquid is poured among centrifuge Centrifugation, obtains filtrate and precipitation solid, by obtained filtrate low-grade fever to 20 DEG C make it is wherein new caused by precipitation melt；(4) filtrate after melting pours into low temperature crystallization among cooling reactor again, and crystallization temperature now is than last low temperature crystallization Temperature it is low 4~5 DEG C, open stirring；After solution separates out precipitation under temperature, the operating process of repeat step (3), obtain New filtrate；(5) repeat step (4) operates, the crystallization carried out under Different hypothermia stage by stage multiple to filtrate, filter operation, until last The temperature of low temperature crystallization at -2 DEG C~-7 DEG C, after filtrate is filtered according to step (3) at such a temperature, pour into by obtained filtrate Desolvation among rectification under vacuum kettle, dry gas stripping further remove dissolvent residual, obtain unsaturated fat acid blend.
- 2. the method as described in claim 1, it is characterized in that each crystallization stage obtains precipitating consolute to one piece, then add Solvent, heating make its dissolving, press filtration are carried out under conditions of 8~10 DEG C, and filtrate adds step (2) when next lock out operation Among material solution before beginning low temperature crystallization.
- 3. method as claimed in claim 2, it is characterized in that press filtration precipitation is dried among being put into 40 DEG C of baking ovens, obtain content and exist The solid product of more than 90% saturated fat acid blend.
- 4. the method as described in claim 1, it is characterized in that solvent is n-hexane, methanol or ethanol.
- 5. the method as described in claim 1, it is characterized in that solvent and soybean oil residue aliphatic acid are according to mass ratio 1.5:1~2.5: 1。
- 6. method as claimed in claim 2, it is characterized in that precipitation and solvent quality are than 1:0.7~1:2.
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| CN201710257595.2A CN107418724A (en) | 2017-04-19 | 2017-04-19 | A kind of method for separating unsaturated fat acid blend in soybean oil residue aliphatic acid |
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| CN201710257595.2A CN107418724A (en) | 2017-04-19 | 2017-04-19 | A kind of method for separating unsaturated fat acid blend in soybean oil residue aliphatic acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694943A (en) * | 2020-08-21 | 2021-04-23 | 重庆市帅克食品有限公司 | Low-cholesterol low-saturated-fat hotpot beef tallow and preparation method thereof |
| CN114681996A (en) * | 2020-12-29 | 2022-07-01 | 中国石油化工股份有限公司 | Device and method for preparing diesel antiwear agent by separating saturated fatty acid |
| CN115074184A (en) * | 2022-07-14 | 2022-09-20 | 江苏创新石化有限公司 | Method for preparing diesel antiwear agent by using mixed oleic acid |
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| CN103409224A (en) * | 2013-08-10 | 2013-11-27 | 新疆西部加斯特药业有限公司 | Grease rich in unsaturated fattyacid and preparation method thereof |
| CN105316113A (en) * | 2015-04-21 | 2016-02-10 | 江南大学 | Polyunsaturated fatty acid enriching method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103409224A (en) * | 2013-08-10 | 2013-11-27 | 新疆西部加斯特药业有限公司 | Grease rich in unsaturated fattyacid and preparation method thereof |
| CN105316113A (en) * | 2015-04-21 | 2016-02-10 | 江南大学 | Polyunsaturated fatty acid enriching method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694943A (en) * | 2020-08-21 | 2021-04-23 | 重庆市帅克食品有限公司 | Low-cholesterol low-saturated-fat hotpot beef tallow and preparation method thereof |
| CN114681996A (en) * | 2020-12-29 | 2022-07-01 | 中国石油化工股份有限公司 | Device and method for preparing diesel antiwear agent by separating saturated fatty acid |
| CN114681996B (en) * | 2020-12-29 | 2024-07-02 | 中国石油化工股份有限公司 | Device and method for preparing diesel antiwear agent by separating saturated fatty acid |
| CN115074184A (en) * | 2022-07-14 | 2022-09-20 | 江苏创新石化有限公司 | Method for preparing diesel antiwear agent by using mixed oleic acid |
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