CN101544557A - Coupling rectification system and application thereof in purifying EPA, DPA, and DHA in seal oil - Google Patents
Coupling rectification system and application thereof in purifying EPA, DPA, and DHA in seal oil Download PDFInfo
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Abstract
The invention relates to a coupling rectification system and application thereof in purifying EPA, DPA, and DHA in seal oil. A material is sent into a raw material storage tank of a novel coupling type rectification system for storage first, and a material stream is sent into a wiped film evaporator through a pump; the raw material is distilled and divided into a light phase and a heavy phase under the action of the rotation of a scraper, the heavy phase returns to the storage tank, and a material flow is introduced from the storage tank after the circulation for multiple times; and the light-phase material enters a rectifying tower, a gas-phase stream and a liquid-phase stream in the rectifying tower are repeatedly evaporated and condensed, finally a high-purity light phase is extracted from a tower top, partial heavy phase is condensed into a liquid phase when passing a partial condenser, the liquid phase refluxes into the rectifying tower, and a gas phase part is finally condensed into a light phase with extremely high purity. The coupling rectification system is applied to the purification of the EPA, the DPA and the DHA in the seal oil, a heavy phase of the seal oil purified by second-stage molecular distillation is connected with the coupling rectification system to obtain a purified EPA, DPA and DHA mixture, and the total concentration of effective components of an obtained product is improved by more than 10 percent than that of an obtained product when a molecular distillation device is not improved.
Description
Technical field
The present invention relates to the application that coupling rectification system reaches purifying EPA, DPA and DHA in Seal fat.
Background technology
Fur seal is the deep-sea Mammals, lives in the north polar circle with in interior-50 ℃ high and cold waters, is food with famous and precious cod, and subcutaneous have a thick lipid layer, is rich in ω-3 polyene fatty acid in the body.With Canada's northern pollution-free marine site sea dog fat is the Seal fat that raw material extracts, wherein contain three kinds of important ω-3 polyene fatty acid: EPA (timnodonic acid), DPA (clupanodonic acid) and DHA (docosahexenoic acid), these three kinds of total fatty acid contents are more than 18%.Medical circle is verified through years of researches, and these three kinds of lipid acid have multiple unique biological active to human body: EPA has the blood circulation of improvement, vessel softening, adjustment blood fat, brings high blood pressure down and blood sugar and anti-inflammatory action; DHA and DPA have the nutrition brain, promote fetus and children's brain development, vision protection, adjusting immunity and antitumous effect that wherein DHA is known as " DHA (docosahexaenoic acid) " again.In the recent period people find again the three kinds of ω-3 polyene fatty acids enrichment in the seal oil is concentrated to total content 25% when above, and seal oil will have treatment and prophylactic effect to some diseases: treat and prophylactic effect as type ii diabetes, fatty liver and prostatitis are had.
Therefore, with highly purified polyunsaturated fatty acid, particularly EPA, DPA and DHA in the commercial run enrichment Seal fat of simple, low cost and mass-producing, become the emphasis and the development trend of research.The at present industrial extracting method that extensively adopts mainly is that esterification process, urea adduct method and molecular distillation are sent out method, and the above two extraction yields are low, easily environment produced pollution; Molecular distillation technique makes liquid separate under the temperature far below its boiling point under high vacuum condition, be suitable for enrichment as thermo-sensitivity in the Seal fat and readily oxidizable substance, but the ubiquity separation efficiency is not high and the bigger situation of energy consumption, often needs multiple-grade molecular distillation just can reach higher degree.
Application number 200410080428.8 discloses a kind of method of extracting Seal fat, now with natural Seal fat esterification, use the multistage purifying of molecular distillation then, when extracting high purity ω-3 type unsaturated fatty acids, remove Seal fat special fishy smell, its physical behavior is greatly improved.But there is the big and higher shortcoming of energy consumption of solvent load in this method.
Application number 200610154614.0 discloses a kind of esterification process that do not use, directly use the technology of molecular distillation purification enrichment unsaturated fatty acids, at feed rate is 20～100ml/min, when vaporization temperature is 290～330 ℃, need not esterification and can obtain the higher Seal fat heavy phase that is rich in ω-3 type unsaturated fatty acids of content.
For transforming the low and huge shortcoming of energy consumption of molecular distillation separation efficiency, occurred comprising increasing the equipment of cycle index, but owing to do not combine with rectifying tower equipment, separation efficiency is generally not high in addition to raise the efficiency.Application number 93211495.4 discloses a kind of outstanding taper centrifugal molecular still, the taper centrifugal reel is vertically rotation on top cover, thereby obtain bigger evaporation area and condensation area, and prevent that the mist back-mixing that occurs that splashes from causing separation efficiency to descend, thereby obtain higher distillation efficiency.But still there is the low shortcoming of separation efficiency in this method.
Application number 200410037167.1 discloses a kind of internal recycle falling film type molecular distillation equipment, by the bottom feed liquid is sucked by propeller pump, in vacuum chamber, become membranaceous dispersion to take away, after concentrating, the condensing surface condensation is back to the bottom, thereby repeatedly circulate up to the qualified multiple-grade molecular distillation of having realized, overcome the low shortcoming of original molecule distillation efficiency.
Application number 200620126549.5 openly can a kind of biofuel knockout tower, and packing layer is all arranged up and down after the charging of middle part, partly guarantees tower still heavy phase quality by separating coking in the reboiler of bottom.
Can see, aforementioned patent uses molecular distillation to carry out enrichment Seal fat ω-3 type unsaturated fatty acids acid glyceride mostly, because the separation efficiency of molecular distillation is not high, the content of EPA, DPA and DHA can be very not high among the heavy phase of employing plural serial stage molecular distillation enrichment in time, single flash separates and to be mixed with part EPA, DPA and DHA in causing gently mutually in addition, makes this part not to be enriched to heavy phase and is wasted.
Summary of the invention
On the basis that character of timnodonic acid (EPA) glyceryl ester, clupanodonic acid (DPA) glyceryl ester and docosahexenoic acid (DHA) glyceryl ester and preparation method thereof is fully understood, we have proposed the present invention through a large amount of exploration and tests.The operational path that pass through to use the polyunsaturated fatty acid in the novel appts extraction Seal fat that this paper proposes, have extraction yield height, environmental pollution little, be easy to the industrial continuous production characteristics, development prospect is good.Studied multiple-grade molecular distillation and novel coupling rectification system coupling technology for this reason and extracted polyunsaturated fatty acid processing method in the Seal fat, with the vapor-phase chromatography quantitative assay lipid acid of product form and relative content.
Technical scheme of the present invention is as follows:
The present invention proposes a kind of coupling rectification system, comprises raw material storage tank, luwa evaporator and rectifying tower; Material is at first sent into novel coupling type distillation system raw material storage tank 1 and is stored, and enters luwa evaporator 2 by pumping material stream 6; Raw material is divided into the weight two-phase under the turning effort of scraper plate 4, heavy phase 5 is returned storage tank 1, and circulation repeatedly back is derived logistics 7 from storage tank, is high purity heavy phase enriched material; Light phase materials 8 enters rectifying tower 3, vapor phase stream thigh 10 in the rectifying tower and liquid phase stream thigh 9 are vaporized and condensation repeatedly, finally extract highly purified light phase 12 out from cat head, the part heavy phase is condensed into stream thigh 11 during by fractional distillating tube 13, backflow enters rectifying tower 3, is the light phase of extreme high purity after the final condensation of gas phase 14 parts.
This coupling rectification system can use in the purification of heat-sensitive material; The light enrichment in rectifying column of recycle feed, in the cat head extraction than light constituent; Heavy constituent can be taken out after separation meets the requirements of degree at storage tank, have reached the purpose of separating the weight component.
The purification of coupling rectification system of the present invention EPA, DPA and DHA in Seal fat is used, and connects manifold type distillation system, the EPA that obtains purifying, DPA and DHA mixture after the Seal fat heavy phase that the two-stage molecular distillation is purified.
During the purification of coupling rectification system EPA, DPA and DHA in Seal fat is used, improve for the technology one that reaches before our the Seal fat heavy phase that the two-stage molecular distillation is purified of better effect, actual conditions is as follows:
1) the pre-degasification process of Seal fat: Seal fat enters in the pre-degassing vessel separation of oxygenated decomposition components and utmost point light constituent through the input speed of fresh feed pump with 5.0-20.0kg/h;
2) one-level molecular distillation: will go up step degassing component and be sent in the one-level molecular still, and under 170-220 ℃, the condition of system pressure 0.001-0.01mbar, knifing spinner velocity 150-250rpm, carry out the one-level molecular distillation, and collect heavy constituent with corresponding speed;
3) secondary molecular distillation: will go up the step heavy constituent and be sent in the secondary molecular still with corresponding speed, under 280-320 ℃, the condition of system pressure 0.001-0.01mbar, knifing spinner velocity 150-250rpm, carry out the secondary molecular distillation, collect the heavy constituent under the corresponding conditions, in order to novel coupling rectification system charging;
4) the manifold type distillation system separates: gained heavy constituent in the step 3) are sent among the storage tank; When system pressure reaches 0.001-0.01mbar, the scraper evaporator scraper velocity reaches under the condition of 150-300rpm and separates; Reach at the wiped film vaporization actuator temperature and to start fresh feed pump under the 170-320 ℃ of condition and enter in the luwa evaporator with the input speed of 5.0-20.0kg/h, take out light constituent at the rectifying tower cat head simultaneously, this part mostly is the glycerin fatty acid ester of carbon number 14～16; Through the continuous circulation separation and purification of 1-4h, take out the Seal fat heavy phase that the interior heavy constituent of storage tank are high purity 3A lipid acid.
Novel coupling type distillation system of the present invention has overcome two shortcomings that the molecular distillation separation efficiency is low and rectifying tower equipment tower still is heated for a long time.Native system uses luwa evaporator that raw material is carried out flash distillation, makes it be divided into the weight two-phase.Wherein light phase steam is sent into the rectifying king-post, in the inner-tower filling material layer, form concentration gradient by the rectifying effect, take out the less light constituent of content at cat head, the then enrichment at the bottom of tower of part that content is more makes in the backflow luwa evaporator that light heavy constituent in are mutually reclaimed.Heavy phase is then mixed mutually by pumping and raw material makes heavy constituent constantly cycle through scraped film evaporator, constantly steams light constituent and makes heavy constituent enrichment in storage tank.
This seminar and domestic other researchists once attempt to use the secondary molecular distillation equipment to carry out the enrichment of EPA, DPA and DHA in the Seal fat, do not obtain than pure EPA, DPA and DHA mixture, therefore the subsequent disposal of research molecular distillation purified product on its basis seems particularly important.
The equipment of novel coupling rectification system constitutes and can be divided into: luwa evaporator, rectifying tower section, vacuum system and the storage tank recycle system, its setting drawing is seen accompanying drawing one.Wherein rectifying section can or be a stuffing rectification column for plate distillation column.This equipment is a kind of systematized brand-new equipment, is the blank of previous patent, and this specialized designs is used for the separation and purification of heat-sensitive substance.Experiment shows, this device can be divided into the animal-plant oil that comprises the Seal fat glycerin fatty acid ester based on the heavy phase of growing carbochain and be that 14,16,18 fatty acid glycerine fat are main light phase with carbon number, thereby realizes the enrichment of heavy phase.
The production method of high purity timnodonic acid of the present invention (EPA) glyceryl ester, clupanodonic acid (DPA) glyceryl ester and docosahexenoic acid (DHA) glyceride mixture, combining with novel coupling rectification system by the rectifying of secondary molecule obtains.DPA content is brought up to 99.6% by 4.3% of stock oil, and DHA brings up to more than 99.3% by 9.1%, and EPA brings up to by 6.8%.
The production method of high purity timnodonic acid of the present invention (EPA) glyceryl ester, clupanodonic acid (DPA) glyceryl ester and docosahexenoic acid (DHA) glyceryl ester has the following advantages:
1, Seal fat is before entering novel coupling rectification system, earlier to its distillation that outgased in advance with two fractions.The one, guaranteed dissolved gas or the discharge as far as possible before entering novel coupling Distallation systm of highly volatile component in the Seal fat; Thereby avoided the defective of separating out, destroying the system vacuum degree, produce spittle phenomenon, stain condensing surface, shorten the work-ing life of vacuum pump hurried in the gas from liquid under the high vacuum; The 2nd, by the secondary molecular distillation Seal fat was purified in advance before entering novel coupling Distallation systm earlier, make the finished product purity improve more than 10% than the product purity of directly using novel coupling rectification system.
2, the present invention uses pure physical separation method, do not introduce any impurity atom, do not change the natural sweet three ester proterties of effective constituent in the Seal fat, and first product effective constituent total concn is brought up to more than 40%, improve more than 10% than the simple molecular distillation apparatus product purity of using, products obtained therefrom more can be given full play to the biological activity to human body, and various diseases is had better therapeutic.
3, by using novel coupling rectification system, the purity of EPA, DPA and DHA is improved, also can obtains purified relatively light constituent by the enrichment of rectifying tower part.This makes this equipment not only be applicable to the separation and purification of heavy phase, also goes for the extraction enrichment of light constituent in the raw material.
Description of drawings
Fig. 1: novel coupling rectification equipment;
Among the figure: 1 is raw material storage tank; 2 is scraper evaporator; 3 are rectifying tower main body (form can be plate distillation column or stuffing rectification column); 4 is rotor segment; 5 for flowing out the heavy phase of scraper evaporator; 6 for entering the material of scraper evaporator; 7 are the heavy constituent product; 8 steam light phase for scraper evaporator; 9 is the rectifying tower withdrawing fluid; 10 is rectifying tower rising steam; 11 is the light phase of condensing reflux; 12 for going out the light phase steam of tower; 13 is fractional distillating tube; 14 is light phase product.
Fig. 2: Seal fat raw material gas chromatogram;
Fig. 3: novel coupling rectification equipment steams the gas chromatogram of light phase;
Fig. 4: novel coupling rectification equipment flows out the gas chromatogram of heavy phase.
Embodiment
Below be the specific embodiment of the present invention, described embodiment is for further describing the present invention, rather than restriction the present invention.
[embodiment 1]
Novel coupling rectification system as herein described makes the separation and purification of its suitable thermo-sensitivity animal-plant oil by the form of transforming rectifying device.The material system of novel distillation equipment is following trend: material is at first sent into novel coupling type distillation system raw material storage tank 1 and is stored by the heavy phase that pre-degassing vessel, two-stage molecular distillation storage tank obtain, and enters luwa evaporator 2 by pumping material stream 6.Raw material is divided into the weight two-phase under the turning effort of scraper plate 4, heavy phase 5 is returned storage tank 1, and circulation repeatedly back is derived logistics 7 from storage tank, is high purity heavy phase enriched material; Light phase materials 8 enters rectifying tower 3, vapor phase stream thigh 10 in the rectifying tower and liquid phase stream thigh 9 are vaporized and condensation repeatedly, finally extract highly purified light phase 12 out from cat head, the part heavy phase is condensed into stream thigh 11 during by fractional distillating tube 13, backflow enters rectifying tower 1, is the light phase of extreme high purity after the final condensation of gas phase 14 parts.
The present invention adopts equipment as shown in Figure 1.The scraper evaporator evaporation area is 0.01m
2Rectifying column internal diameter 30cm is board-like or filler king-post, can be according to the different needs adjustment, and theoretical plate number of the present invention is 6～12.
[embodiment 2]
Use novel coupling rectification equipment and extract secondary molecular distillation Seal fat 3A lipid acid (its moiety accompanying drawing 2) later, comprise the steps:
Gained heavy constituent in the secondary molecular distillation are sent among the novel coupling type distillation system storage tank.When system pressure reaches 0.01mbar, the scraper evaporator scraper velocity reaches under the condition of 150rpm and separates.The following fresh feed pump that starts that reaches 170 ℃ of conditions at the wiped film vaporization actuator temperature enters in the luwa evaporator with the input speed of 5.0kg/h, take out light constituent (its moiety accompanying drawing 3) at the rectifying tower cat head simultaneously, this part mostly is the glycerin fatty acid ester of carbon number 14～16.Through the continuous circulation separation and purification of 1h, take out the Seal fat heavy phase (its moiety accompanying drawing 4) that the interior heavy constituent of storage tank are high purity 3A lipid acid.
[embodiment 3]
The integrated optimization process of novel coupling rectification equipment and secondary molecular distillation of using is extracted highly purified Seal fat 3A lipid acid, and the concrete operations parameter is as follows:
1) the pre-degasification process of Seal fat: Seal fat enters in the pre-degassing vessel through the input speed of fresh feed pump with 20.0kg/h, and separation of oxygenated decomposition components and utmost point light constituent play the provide protection to vacuum pump.
2) one-level molecular distillation: will go up step degassing component and be sent in the one-level molecular still, and under 220 ℃, the condition of system pressure 0.001mbar, knifing spinner velocity 250rpm, carry out the one-level molecular distillation, and collect heavy constituent with corresponding speed;
3) secondary molecular distillation: will go up the step heavy constituent and be sent in the secondary molecular still, and under 320 ℃, the condition of system pressure 0.001mbar, knifing spinner velocity 250rpm, carry out the secondary molecular distillation, and collect heavy constituent with corresponding speed.
4) the novel coupling type distillation system separates: gained heavy constituent in the step 3) are sent among the storage tank.When system pressure reaches 0.001mbar, the scraper evaporator scraper velocity reaches under the condition of 300rpm and separates.Reach at the wiped film vaporization actuator temperature and to start fresh feed pump under 320 ℃ of conditions and enter in the luwa evaporator with the input speed of 20.0kg/h, take out light constituent at the rectifying tower cat head simultaneously, this part mostly is the glycerin fatty acid ester of carbon number 14～16.Through the continuous circulation separation and purification of 4h, take out the Seal fat heavy phase that the interior heavy constituent of storage tank are high purity 3A lipid acid.
[embodiment 4]
Basic technology is with embodiment 3, and the concrete operations parameter is as follows:
1) the pre-degasification process of Seal fat: Seal fat enters in the pre-degassing vessel through the input speed of fresh feed pump with group 10.0kg/h, and separation of oxygenated decomposition components and utmost point light constituent play the provide protection to vacuum pump.
2) one-level molecular distillation: will go up step degassing component and be sent in the one-level molecular still, and under 200 ℃, the condition of system pressure 0.005mbar, knifing spinner velocity 200rpm, carry out the one-level molecular distillation, and collect heavy constituent with corresponding speed;
3) secondary molecular distillation: will go up the step heavy constituent and be sent in the secondary molecular still with corresponding speed, under 300 ℃, the condition of system pressure 0.005mbar, knifing spinner velocity 200rpm, carry out the secondary molecular distillation, collect the cut under the corresponding conditions, promptly obtain functional seal oil.
4) the novel coupling type distillation system separates: gained heavy constituent in the step 3) are sent among the storage tank.When system pressure reaches 0.001mbar, the scraper evaporator scraper velocity reaches under the condition of 300rpm and separates.Reach at the wiped film vaporization actuator temperature and to start fresh feed pump under 250 ℃ of conditions and enter in the luwa evaporator with the input speed of 10.0kg/h, take out light constituent at the rectifying tower cat head simultaneously, this part mostly is the glycerin fatty acid ester of carbon number 14～16.Through the continuous circulation separation and purification of 4h, take out the Seal fat heavy phase that the interior heavy constituent of storage tank are high purity 3A lipid acid.
Resulting heavy phase of molecular distillation apparatus among raw material Seal fat and the embodiment 2 and embodiment 2-4 products obtained therefrom are carried out the chromatogram content analysis, and wherein the content of EPA, DHA, DPA sees the following form: (unit: weight percent %)
| Percentage composition | The raw material seal oil | Behind the secondary | Embodiment | 2 | Embodiment 3 | |
| EPA | 6.8 | 8.3 | 12.52 | 13.88 | 16.91 | |
| DHA | 9.1 | 11.5 | 19.44 | 21.84 | 23.95 | |
| DPA | 4.3 | 5.5 | 8.87 | 8.66 | 9.62 | |
| Total effective constituent | 20.2 | 25.3 | 40.83 | 44.38 | 48.48 |
The present invention has done a large amount of simultaneous tests, above-mentioned just wherein several examples.The content of EPA, DHA and DPA in the contrast products obtained therefrom illustrates that the improvement effect to conventional molecular distillation apparatus is significant among the present invention, and products obtained therefrom effective constituent total concn improves more than 10% than not improving molecular distillation apparatus products obtained therefrom concentration.
The coupling rectification system that the present invention proposes reaches the application of purifying EPA, DPA and DHA in Seal fat, be described by embodiment, person skilled obviously can be changed or suitably change and combination making method as herein described in not breaking away from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (4)
1. a coupling rectification system comprises raw material storage tank, luwa evaporator and rectifying tower; It is characterized in that material at first sends into novel coupling type distillation system raw material storage tank 1 and store, enter luwa evaporator 2 by pumping material stream 6; Raw material is divided into the weight two-phase under the turning effort of scraper plate 4, heavy phase 5 is returned storage tank 1, and circulation repeatedly back is derived logistics 7 from storage tank, is high purity heavy phase enriched material; Light phase materials 8 enters rectifying tower 3, vapor phase stream thigh 10 in the rectifying tower and liquid phase stream thigh 9 are vaporized and condensation repeatedly, finally extract highly purified light phase 12 out from cat head, the part heavy phase is condensed into stream thigh 11 during by fractional distillating tube 13, backflow enters rectifying tower 3, is the light phase of extreme high purity after the final condensation of gas phase 14 parts.
2. coupling rectification system as claimed in claim 1 is characterized in that this system uses in the purification of heat-sensitive material; The light enrichment in rectifying column of recycle feed, in the cat head extraction than light constituent; Heavy constituent can be taken out after separation meets the requirements of degree at storage tank, have reached the purpose of separating the weight component.
3. the purification of the coupling rectification system of claim 1 EPA, DPA and DHA in Seal fat is used, and it is characterized in that connecting after the Seal fat heavy phase that the two-stage molecular distillation is purified manifold type distillation system, the EPA that obtains purifying, DPA and DHA mixture.
4. application as claimed in claim 3 is characterized in that may further comprise the steps:
1) the pre-degasification process of Seal fat: Seal fat enters in the pre-degassing vessel separation of oxygenated decomposition components and utmost point light constituent through the input speed of fresh feed pump with 5.0-20.0kg/h;
2) one-level molecular distillation: will go up step degassing component and be sent in the one-level molecular still, and under 170-220 ℃, the condition of system pressure 0.001-0.01mbar, knifing spinner velocity 150-250rpm, carry out the one-level molecular distillation, and collect heavy constituent with corresponding speed;
3) secondary molecular distillation: will go up the step heavy constituent and be sent in the secondary molecular still with corresponding speed, under 280-320 ℃, the condition of system pressure 0.001-0.01mbar, knifing spinner velocity 150-250rpm, carry out the secondary molecular distillation, collect the heavy constituent under the corresponding conditions, in order to novel coupling rectification system charging;
4) the manifold type distillation system separates: gained heavy constituent in the step 3) are sent among the storage tank; When system pressure reaches 0.001-0.01mbar, the scraper evaporator scraper velocity reaches under the condition of 150-300rpm and separates; Reach at the wiped film vaporization actuator temperature and to start fresh feed pump under the 170-320 ℃ of condition and enter in the luwa evaporator with the input speed of 5.0-20.0kg/h, take out light constituent at the rectifying tower cat head simultaneously, this part mostly is the glycerin fatty acid ester of carbon number 14～16; Through the continuous circulation separation and purification of 1-4h, take out the Seal fat heavy phase that the interior heavy constituent of storage tank are high purity 3A lipid acid.
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