CN106833908A - A kind of preparation method of height unsaturation linseed oil fatty acid - Google Patents
A kind of preparation method of height unsaturation linseed oil fatty acid Download PDFInfo
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- CN106833908A CN106833908A CN201710117160.8A CN201710117160A CN106833908A CN 106833908 A CN106833908 A CN 106833908A CN 201710117160 A CN201710117160 A CN 201710117160A CN 106833908 A CN106833908 A CN 106833908A
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- Prior art keywords
- linseed oil
- fatty acid
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- unsaturation
- acid
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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
- 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
- C11C1/08—Refining
- C11C1/10—Refining by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- 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
-
- 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
- C11C1/08—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of preparation method of height unsaturation linseed oil fatty acid, it is related to technical field of agricultural product process.The method includes：Linseed oil soap stock is added and is acidified in kettle, agitating heating；Linseed oil soap stock after stirring and heating is acidified；Linseed oil soap stock after acidifying wash and obtains upper strata acidifying grease；Upper strata acidifying grease is passed through into dewatering pan to be dehydrated, upper strata croude fatty acids are obtained；Upper strata croude fatty acids are passed through into hydrolysis tower to be hydrolyzed, the croude fatty acids being layered；Croude fatty acids after layering are passed through dehydrating tower dehydration degassing, the aliphatic acid after dehydration degassing is obtained；The aliphatic acid being dehydrated after degassing is carried out into rectifying and sloughs plant asphalt；Aliphatic acid after rectifying is passed through after stripper carries out desolventing technology, the unsaturated linseed oil fatty acid of finished product height is obtained.Linseed oil fatty acid lighter color prepared by the present invention, containing iodine number is high, yield is high, improve the quality and range of application of linseed oil fatty acid.
Description
Technical field
The present invention relates to technical field of agricultural product process, a kind of height unsaturation linseed oil fatty acid is more particularly related to
Preparation method.
Background technology
Oil seed flax, also known as flax, is one of big oil crops of China five, is mainly distributed on the ground such as Inner Mongol, Shanxi, Hebei,
Annual production is in ten thousand tons of 30-40.Linseed oil be rich in alpha-linolenic acid, content more than 45%, unsaturated fatty acid content 85% with
On, it is described as " deep sea fish oil of land ".In recent years, with the concern of people's green health food, linseed oil is used as one
The nutrition grease for planting degree of unsaturation high is just received more and more attention, and increasing enterprise throws oneself into the processing of linseed oil
And deep processing ranks.Therefore, the accessory substance of linseed oil processing, as soap stock, deodorization distillate and deep-processing process are produced
The yield of the slightly lower linseed oil of linolenic acid content is increasing, and the recycling of accessory substance is directly connected to the economy of processing enterprise
Benefit.
Linseed oil is good drying grease, can form high resilience and firm film, the object of protective covering lid.Flax
Fatty acid oil also with drying property more more preferable than linseed oil, therefore can manufacture perfumed soap, soap in addition to the performance with linseed oil
Deng articles for washing and senior paint, coating and ink.With the development of daily use chemicals and coating and ink industry, market is to high-quality
The demand of linseed oil fatty acid is growing.
However, it is also fewer currently for the research that linseed oil accessory substance prepares linseed oil fatty acid, more have no correlation
Industrialization report.Large oil fatty acid preparation technology hydrolysis at present needs condition of high voltage, and distillation process needs are general in high temperature
More than 240 DEG C, unrighted acid quality is necessarily affected.Research and development economically and reasonably prepare meet relevant industries will
The degree of unsaturation linseed oil fatty acid high of the high-quality asked turns into a problem in the urgent need to address at present.
The content of the invention
The present invention provides a kind of preparation method of height unsaturation linseed oil fatty acid, solves conventional fat acid preparation side
Method product quality is low, high energy consumption, wastewater discharge big, high temperature rectifying unsaturation leukotrienes is susceptible to thermal oxide, thermal polymerization etc.
The rotten problem of reaction.
Specifically, in the present invention the unsaturated linseed oil fatty acid of height preparation method, comprise the following steps：
Step 1：Linseed oil soap stock is added and is acidified in kettle, be stirred and heated to 90-100 DEG C；
Step 2：To stirring and adding the concentrated sulfuric acid in linseed oil soap stock after heating, it is acidified；
Step 3：To adding sodium chloride solution to be washed in the linseed oil soap stock after acidifying, rehydration of laying equal stress on is washed 2-3 times, its
In, the addition of sodium chloride solution is the 10-20% of linseed oil soap stock weight, and lower floor's moisture is discharged after washing, obtains upper strata acid
Carburetion fat；
Step 4：Upper strata acidifying grease is passed through into dewatering pan to be dehydrated, upper strata croude fatty acids are obtained；
Step:5：Upper strata croude fatty acids are passed through into hydrolysis tower to be hydrolyzed, the croude fatty acids being layered are water-soluble with glycerine
Liquid；
Step 6：Croude fatty acids after layering are passed through dehydrating tower dehydration degassing, the aliphatic acid after dehydration degassing is obtained；
Step 7：The aliphatic acid being dehydrated after degassing is carried out into rectifying and sloughs plant asphalt；
Step 8：Aliphatic acid after rectifying is passed through after stripper carries out desolventing technology, the unsaturated flax of finished product height is obtained
Fatty acid oil.
Preferably, in step 2, concentrated sulfuric acid concentration is 98%, and concentrated sulfuric acid addition is the 5-10% of linseed oil soap stock weight,
Acidificatoin time is 0.5-2h.
Preferably, in step 3, the mass fraction of sodium chloride solution is 5-10%, and the temperature of sodium chloride solution is 90-95
℃。
Preferably, in step 4, dehydration temperaturre is 95-105 DEG C, and dewatering vacuum degree is 0.085-0.09MPa.
Preferably, in step 5, hydrolysis temperature is 180-220 DEG C, and hydrolysis pressure is 1.4-2.5Mpa, and hydrolysis time is 6-
10h。
Preferably, in step 6, dehydration degassing temperature is 100-105 DEG C, and dehydration devolatilization vacuum degree is 0.085-0.09MPa.
Preferably, in step 7, rectification temperature is 180-200 DEG C, and rectifying vacuum is 400-500Pa.
Preferably, in step 8, bleaching temperature is 180-200 DEG C, and decolouring vacuum is 500-700Pa, during decolouring, directly
Steam intake is the 0.1-0.5% of linseed oil soap stock weight.
Beneficial effects of the present invention are：
The preparation method of the unsaturated linseed oil fatty acid of height is using acidifying, Central Asia hydrolysis, rectifying and air lift in the present invention
The techniques such as decolouring, prepare the high-quality linseed oil fatty acid for meeting relevant industries requirement, and it is low that there is the method versatility to consume energy,
The small advantage of wastewater displacement, at the same the linseed oil fatty acid lighter color for preparing, containing iodine number is high, yield is high, be not susceptible to thermal oxide,
The reaction such as thermal polymerization is rotten, improves the quality and range of application of linseed oil fatty acid.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the process chart of height unsaturation linseed oil fatty acid provided in an embodiment of the present invention；
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
With reference to Fig. 1, the preparation method of the height unsaturation linseed oil fatty acid that the embodiment of the present invention 1 is provided, including it is following
Step：
Step 1：The linseed oil soap stock of 500kg is added and is acidified in kettle, be stirred and heated to 90 DEG C；
Step 2：To stirring and being slowly added to the concentrated sulfuric acid that concentration is 98% in linseed oil soap stock after heating, it is acidified
1h, wherein, concentrated sulfuric acid addition is the 5% of linseed oil soap stock weight, and during acidifying, pH value is 3；
Step 3：Keeping temperature is constant, is 90 DEG C to temperature is added in the linseed oil soap stock after acidifying, and mass fraction is 5%
Sodium chloride solution washed, the addition of sodium chloride solution is the 10% of linseed oil soap stock weight, and rehydration of laying equal stress on is washed 3 times,
Lower floor's moisture is discharged after washing, upper strata acidifying grease is obtained；
Step 4：Upper strata acidifying grease is passed through into dewatering pan to be dehydrated, dehydration temperaturre is 105 DEG C, and dewatering vacuum degree is
0.085Mpa, obtains upper strata croude fatty acids；
Step:5：Upper strata croude fatty acids are passed through into hydrolysis tower to be hydrolyzed, hydrolysis temperature is 220 DEG C, hydrolysis pressure is
1.55Mpa, hydrolysis time is 6h, the croude fatty acids and glycerine water solution being layered；
Step 6：Croude fatty acids after layering are passed through dehydrating tower dehydration degassing, dehydration degassing temperature is 100 DEG C, and dehydration is de-
Gas vacuum is 0.09Mpa, obtains the aliphatic acid after dehydration degassing；
Step 7：The aliphatic acid being dehydrated after degassing is carried out into rectifying and sloughs plant asphalt, rectification temperature is 190 DEG C, and rectifying is true
Reciprocal of duty cycle is 500Pa；
Step 8：Aliphatic acid after rectifying is passed through into stripper carries out desolventing technology, and bleaching temperature is 180 DEG C, decolouring vacuum
It is 700Pa to spend, and during decolouring, live (open) steam intake is the 0.1% of linseed oil soap stock weight, after desolventing technology, obtains finished product high
The unsaturated linseed oil fatty acid of degree.
After measured, the height unsaturation linseed oil fatty acid for being prepared in embodiment 1, aliphatic acid yield is 91.3%, color and luster
It is 2#, iodine value is 192.
Embodiment 2
The preparation method of the height unsaturation linseed oil fatty acid that the embodiment of the present invention 2 is provided, comprises the following steps：
Step 1：The linseed oil soap stock of 500kg is added and is acidified in kettle, be stirred and heated to 95 DEG C；
Step 2：To stirring and being slowly added to the concentrated sulfuric acid that concentration is 98% in linseed oil soap stock after heating, it is acidified
2h, wherein, concentrated sulfuric acid addition is the 8% of linseed oil soap stock weight, and during acidifying, pH value is 4；
Step 3：Keeping temperature is constant, is 90 DEG C to temperature is added in the linseed oil soap stock after acidifying, and mass fraction is 8%
Sodium chloride solution washed, the addition of sodium chloride solution is the 15% of linseed oil soap stock weight, and rehydration of laying equal stress on is washed 3 times,
Lower floor's moisture is discharged after washing, upper strata acidifying grease is obtained；
Step 4：Upper strata acidifying grease is passed through into dewatering pan to be dehydrated, dehydration temperaturre is 100 DEG C, and dewatering vacuum degree is
0.085Mpa, obtains upper strata croude fatty acids；
Step:5：Upper strata croude fatty acids are passed through into hydrolysis tower to be hydrolyzed, hydrolysis temperature is 210 DEG C, hydrolysis pressure is
2.5Mpa, hydrolysis time is 8h, the croude fatty acids and glycerine water solution being layered；
Step 6：Croude fatty acids after layering are passed through dehydrating tower dehydration degassing, dehydration degassing temperature is 100 DEG C, and dehydration is de-
Gas vacuum is 0.09Mpa, obtains the aliphatic acid after dehydration degassing；
Step 7：The aliphatic acid being dehydrated after degassing is carried out into rectifying and sloughs plant asphalt, rectification temperature is 180 DEG C, and rectifying is true
Reciprocal of duty cycle is 400Pa；
Step 8：Aliphatic acid after rectifying is passed through into stripper carries out desolventing technology, and bleaching temperature is 190 DEG C, decolouring vacuum
It is 500Pa to spend, and during decolouring, live (open) steam intake is the 0.2% of linseed oil crude oil weight, after desolventing technology, obtains finished product high
The unsaturated linseed oil fatty acid of degree.
After measured, the height unsaturation linseed oil fatty acid for being prepared in embodiment 2, aliphatic acid yield is 92.4%, color and luster
It is 2#, iodine value is 191.
Embodiment 3
The preparation method of the height unsaturation linseed oil fatty acid that the embodiment of the present invention 3 is provided, comprises the following steps：
Step 1：The linseed oil soap stock of 500kg is added and is acidified in kettle, be stirred and heated to 100 DEG C；
Step 2：To stirring and being slowly added to the concentrated sulfuric acid that concentration is 98% in linseed oil soap stock after heating, it is acidified
0.5h, wherein, concentrated sulfuric acid addition is the 10% of linseed oil soap stock weight, and during acidifying, pH value is 4；
Step 3：Keeping temperature is constant, is 95 DEG C to temperature is added in the linseed oil soap stock after acidifying, and mass fraction is
10% sodium chloride solution is washed, and the addition of sodium chloride solution is the 20% of linseed oil soap stock weight, and rehydration of laying equal stress on washes 2
It is secondary, lower floor's moisture is discharged after washing, obtain upper strata acidifying grease；
Step 4：Upper strata acidifying grease is passed through into dewatering pan to be dehydrated, dehydration temperaturre is 95 DEG C, and dewatering vacuum degree is
0.09Mpa, obtains upper strata croude fatty acids；
Step:5：Upper strata croude fatty acids are passed through into hydrolysis tower to be hydrolyzed, hydrolysis temperature is 180 DEG C, hydrolysis pressure is
1.4Mpa, hydrolysis time is 10h, the croude fatty acids and glycerine water solution being layered；
Step 6：Croude fatty acids after layering are passed through dehydrating tower dehydration degassing, dehydration degassing temperature is 105 DEG C, and dehydration is de-
Gas vacuum is 0.085Mpa, obtains the aliphatic acid after dehydration degassing, and glycerine water solution recycles 3 times and directly carries out outer following afterwards
Ring is concentrated by evaporation and reclaims crude glycerine；
Step 7：The aliphatic acid being dehydrated after degassing is carried out into rectifying and sloughs plant asphalt, rectification temperature is 200 DEG C, and rectifying is true
Reciprocal of duty cycle is 500Pa；
Step 8：Aliphatic acid after rectifying is passed through into stripper carries out desolventing technology, and bleaching temperature is 200 DEG C, decolouring vacuum
It is 700Pa to spend, and during decolouring, live (open) steam intake is the 0.5% of the semi-refined weight of oil of linseed oil, after desolventing technology, is obtained into
The unsaturated linseed oil fatty acid of product height.
After measured, the height unsaturation linseed oil fatty acid for being prepared in embodiment 3, aliphatic acid yield is 91.4%, color and luster
It is 2#, iodine value is 190.
, but those skilled in the art once know basic creation although preferred embodiments of the present invention have been described
Property concept, then can make other change and modification to these embodiments.So, appended claims are intended to be construed to include excellent
Select embodiment and fall into having altered and changing for the scope of the invention.
Obviously, those skilled in the art can carry out various changes and modification without deviating from essence of the invention to the present invention
God and scope.So, if these modifications of the invention and modification belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising these changes and modification.
Claims (8)
1. the preparation method of a kind of height unsaturation linseed oil fatty acid, it is characterised in that comprise the following steps：
Step 1：Linseed oil soap stock is added and is acidified in kettle, be stirred and heated to 90-100 DEG C；
Step 2：To stirring and adding the concentrated sulfuric acid in linseed oil soap stock after heating, it is acidified；
Step 3：To adding sodium chloride solution to be washed in the linseed oil soap stock after acidifying, rehydration of laying equal stress on is washed 2-3 times, wherein,
The addition of sodium chloride solution is the 10-20% of linseed oil soap stock weight, and lower floor's moisture is discharged after washing, obtains upper strata acidification oil
Fat；
Step 4：Upper strata acidifying grease is passed through into dewatering pan to be dehydrated, upper strata croude fatty acids are obtained；
Step:5：Upper strata croude fatty acids are passed through into hydrolysis tower to be hydrolyzed, the croude fatty acids and glycerine water solution being layered；
Step 6：Croude fatty acids after layering are passed through dehydrating tower dehydration degassing, the aliphatic acid after dehydration degassing is obtained；
Step 7：The aliphatic acid being dehydrated after degassing is carried out into rectifying and sloughs plant asphalt；
Step 8：Aliphatic acid after rectifying is passed through after stripper carries out desolventing technology, the unsaturated linolein of finished product height is obtained
Fat acid.
2. the preparation method of height according to claim 1 unsaturation linseed oil fatty acid, it is characterised in that in step 2,
Concentrated sulfuric acid concentration is 98%, and concentrated sulfuric acid addition is the 5-10% of linseed oil soap stock weight, and acidificatoin time is 0.5-2h.
3. the preparation method of height according to claim 1 unsaturation linseed oil fatty acid, it is characterised in that in step 3,
The mass fraction of sodium chloride solution is 5-10%, and the temperature of sodium chloride solution is 90-95 DEG C.
4. the preparation method of height according to claim 1 unsaturation linseed oil fatty acid, it is characterised in that in step 4,
Dehydration temperaturre is 95-105 DEG C, and dewatering vacuum degree is 0.085-0.09MPa.
5. the preparation method of height according to claim 1 unsaturation linseed oil fatty acid, it is characterised in that in step 5,
Hydrolysis temperature is 180-220 DEG C, and hydrolysis pressure is 1.4-2.5Mpa, and hydrolysis time is 6-10h.
6. the preparation method of height according to claim 1 unsaturation linseed oil fatty acid, it is characterised in that in step 6,
Dehydration degassing temperature is 100-105 DEG C, and dehydration devolatilization vacuum degree is 0.085-0.09MPa.
7. the preparation method of height according to claim 1 unsaturation linseed oil fatty acid, it is characterised in that in step 7,
Rectification temperature is 180-200 DEG C, and rectifying vacuum is 400-500Pa.
8. the preparation method of height according to claim 1 unsaturation linseed oil fatty acid, it is characterised in that in step 8,
Bleaching temperature is 180-200 DEG C, and decolouring vacuum is 500-700Pa, and during decolouring, live (open) steam intake is linseed oil soap stock weight
The 0.1-0.5% of amount.
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Citations (6)
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| CN1276413A (en) * | 1999-06-04 | 2000-12-13 | 淄博市周村北安社会福利油酸厂 | Process for preparing fatty acid by hydrolyzing of plant oil soapstock without catalyst |
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| CN101831356A (en) * | 2010-06-02 | 2010-09-15 | 安徽省瑞芬得油脂深加工有限公司 | Method for preparing linseed oil fatty acid with light color |
| CN101838590A (en) * | 2010-05-25 | 2010-09-22 | 九江力山环保科技有限公司 | Production process of rectified light-colored oleic acid |
| CN102304435A (en) * | 2011-08-04 | 2012-01-04 | 北京印钞有限公司 | Linoleic acid and production technique thereof |
| CN104725217A (en) * | 2015-02-27 | 2015-06-24 | 蓬莱市海洋生物有限公司 | Production process of conjugated linoleic acids |
-
2017
- 2017-03-01 CN CN201710117160.8A patent/CN106833908A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1276413A (en) * | 1999-06-04 | 2000-12-13 | 淄博市周村北安社会福利油酸厂 | Process for preparing fatty acid by hydrolyzing of plant oil soapstock without catalyst |
| CN101462938A (en) * | 2008-12-12 | 2009-06-24 | 中南大学 | Method for preparing mixed fatty acid from hogwash oil and use method of mixed fatty acid |
| CN101838590A (en) * | 2010-05-25 | 2010-09-22 | 九江力山环保科技有限公司 | Production process of rectified light-colored oleic acid |
| CN101831356A (en) * | 2010-06-02 | 2010-09-15 | 安徽省瑞芬得油脂深加工有限公司 | Method for preparing linseed oil fatty acid with light color |
| CN102304435A (en) * | 2011-08-04 | 2012-01-04 | 北京印钞有限公司 | Linoleic acid and production technique thereof |
| CN104725217A (en) * | 2015-02-27 | 2015-06-24 | 蓬莱市海洋生物有限公司 | Production process of conjugated linoleic acids |
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| Title |
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| （加）沙希迪: "《贝雷油脂化学与工艺学：第6版 第5卷 食用油脂产品加工技术》", 30 September 2016, 中国轻工业出版社 * |
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Application publication date: 20170613 |