CN108912089B - 50VE and sterol centrifugal separation method and crystallization and filtration combined system thereof - Google Patents
50VE and sterol centrifugal separation method and crystallization and filtration combined system thereof Download PDFInfo
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- CN108912089B CN108912089B CN201810646332.5A CN201810646332A CN108912089B CN 108912089 B CN108912089 B CN 108912089B CN 201810646332 A CN201810646332 A CN 201810646332A CN 108912089 B CN108912089 B CN 108912089B
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- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
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Abstract
The invention discloses a centrifugal separation method of 50VE and sterol and a crystallization and filtration combined system thereof, which comprises the steps of dissolving deodorized distillate of vegetable oil in an acetone-methanol mixed solvent, crystallizing at low temperature, filtering, centrifuging filtrate, washing and drying to obtain deodorized distillate with sterol removed. The centrifugal separation method of 50VE and sterol provided by the invention of the invention is low in labor intensity, low in environmental pollution, easy to control reaction, and high in purity and recovery rate of vitamin E.
Description
Technical Field
The invention belongs to the technical field of vitamin E preparation, and particularly relates to a centrifugal separation method of 50VE and sterol and a crystallization and filtration combined system thereof.
Background
The distillate of deodorized vegetable oil is a mixture of fractions obtained during deodorization of vegetable oil. The food mainly contains a large amount of free fatty acid, vitamin E, glyceride and other components.
Vitamin E is a fat-soluble vitamin whose hydrolysate is tocopherol, one of the most important antioxidants. Is dissolved in organic solvents such as fat, ethanol and the like, is insoluble in water, is stable to heat and acid, is unstable to alkali, is sensitive to oxygen and is insensitive to heat, but the activity of vitamin E is obviously reduced during frying. The tocopherol can promote the secretion of sex hormone, so that the vitality and the quantity of sperms of the male are increased; increase female estrogen concentration, improve fertility, prevent abortion, and can be used for preventing and treating male infertility, burn, cold injury, capillary hemorrhage, climacteric syndrome, and skin care. Recently, vitamin E has been found to inhibit the lipid peroxidation in the lens of the eye, dilate peripheral blood vessels, improve blood circulation and prevent the occurrence and development of myopia. The phenolic hydroxyl on the benzene ring of the vitamin E is acetylated, and the ester is hydrolyzed into the phenolic hydroxyl which is then used as tocopherol.
The process unit for producing the vitamin E in China has more operations, high labor intensity, serious environmental pollution, difficult reaction control, low recovery rate and low purity of the vitamin E.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and title of the application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above and/or the technical blanks in the existing methods for centrifugal separation of 50VE and sterols.
Accordingly, it is an object of the present invention to overcome the deficiencies of the prior art by providing a method for centrifugation of 50VE and sterols.
In order to solve the technical problems, the invention provides the following technical scheme: a method for centrifugal separation of 50VE and sterol comprises dissolving deodorized distillate of vegetable oil in acetone-methanol mixed solvent, crystallizing at low temperature, filtering, centrifuging the filtrate, washing, and oven drying to obtain deodorized distillate with sterol removed; distilling the deodorized distillate without sterol to respectively obtain distillate and residual liquid; and (3) evaporating the solvent from the distillate to obtain a vitamin E product.
As a preferred embodiment of the method for centrifugal separation of 50VE and sterol according to the present invention, wherein: and distilling under the conditions that the distillation temperature is 220-230 ℃, the feeding temperature is 80-90 ℃, and the rotating speed is 120-180 r/min.
As a preferred embodiment of the method for centrifugal separation of 50VE and sterol according to the present invention, wherein: and the centrifugation is carried out for 30-40 min at 5000-7000 rpm.
As a preferred embodiment of the method for centrifugal separation of 50VE and sterol according to the present invention, wherein: the deodorized distillate of vegetable oil comprises deodorized distillate of corn oil or deodorized distillate of soybean oil.
As a preferred embodiment of the method for centrifugal separation of 50VE and sterol according to the present invention, wherein: and the low-temperature crystallization is carried out by controlling the temperature to be 30-40 ℃, then slowly cooling to-5 ℃ within 4-6 hours, and keeping for 20-24 hours.
As a preferred embodiment of the method for centrifugal separation of 50VE and sterol according to the present invention, wherein: the volume ratio of acetone to methanol in the acetone-methanol mixed solvent is 1-2: 1, and the usage amount of the mixed solvent is 5-6 ml/g of deodorized distillate of vegetable oil.
It is another object of the present invention to address the deficiencies of the prior art and to provide a crystallization and filtration integrated system that is capable of refrigeration, crystallization and filtration.
In order to solve the technical problems, the invention provides the following technical scheme: the integrated crystallization and filtration system comprising: the steam power unit comprises evaporation equipment, a steam conveying pipeline and shunt equipment, and the shunt equipment is connected with the evaporation equipment through the steam conveying pipeline; the first heat exchange unit comprises a heat absorption device, and the heat absorption device is connected with the cooling device through a first conveying pipeline and a first liquid return pipeline respectively to form a circulating loop; the second heat exchange unit comprises heat dissipation equipment, and the heat dissipation equipment is respectively connected with the first heat exchange unit and the steam absorption unit; the steam absorption unit comprises absorption equipment, and the absorption equipment is connected with the steam power unit through a first circulation pipeline and a second circulation pipeline respectively; a cold water pipe is further arranged inside the absorption equipment, and two ends of the cold water pipe penetrate out of the absorption equipment and are respectively externally connected with a second conveying pipeline and a second liquid return pipeline; the second conveying pipeline and the second liquid return pipeline are both connected with the cooling equipment; the flow dividing equipment, the first heat exchange unit, the second heat exchange unit and the steam absorption unit are connected in sequence through the conveying unit, and the conveying unit comprises a first conveying pipeline, a second conveying pipeline and a third conveying pipeline; the flow dividing equipment is connected with the first heat exchange unit through the first conveying pipeline, the first heat exchange unit is connected with the second heat exchange unit through the second conveying pipeline, and the second heat exchange unit is connected with the steam absorption unit through the third conveying pipeline; and the second conveying pipeline is provided with throttling equipment; a heat dissipation pipeline is arranged at the joint of the first conveying pipeline and the second conveying pipeline, and a heat absorption pipeline is arranged at the joint of the second conveying pipeline and the third conveying pipeline; the heat dissipation pipeline is positioned inside the heat absorption device, and the heat absorption pipeline is positioned inside the heat dissipation device; the conveying unit is at least provided with two groups, each pipeline is arranged side by side, one section of the conveying unit is connected to the flow dividing equipment, and the other end of the conveying unit is connected to the inside of the absorption equipment.
As a preferable embodiment of the crystallization-filtration combination system of the present invention, wherein: the crystallization and filtration combined system also comprises a filtration unit, wherein the filtration unit comprises filtration equipment, an air source channel, a raw material liquid input pipeline and a filtrate output pipeline, and the filtration equipment is provided with a raw material liquid inlet, a first compressed air inlet, a solid phase outlet and a liquid phase outlet; one end of the raw material liquid input pipeline is connected with the heat dissipation equipment, the other end of the raw material liquid input pipeline is connected with the raw material liquid inlet, and the raw material liquid input pipeline can transmit the crystallization mixed solution from the interior of the heat dissipation equipment to the interior of the filtering equipment; the filtrate output pipeline is connected with the liquid phase outlet and can discharge the filtrate from the filtering equipment from the liquid phase outlet.
As a preferable embodiment of the crystallization-filtration combination system of the present invention, wherein: a filter assembly is arranged in the filter equipment, is butted with the inner port end of the liquid phase outlet and is communicated with the filtrate output pipeline through the liquid phase outlet; the filtrate output pipelines correspond to the liquid phase outlets one by one and are at least provided with one group, and the outer ends of the filtrate output pipelines are all connected to a filtrate collecting pipeline in a centralized manner; the air source channel comprises a first air source flow path, a second air source flow path and a third air source flow path, the first air source flow path is connected to the first compressed air inlet, the second air source flow path is connected to the filtrate collecting pipeline, and the third air source flow path is connected to the interior of the heat dissipation device; the air source channel is externally connected with an air source and provides compressed air for the first air source flow path, the second air source flow path and the third air source flow path.
As a preferable embodiment of the crystallization-filtration combination system of the present invention, wherein: and injecting the acetone-methanol mixed solvent and the plant oil deodorizer distillate dissolved in the acetone-methanol mixed solvent into the heat dissipation equipment, performing low-temperature crystallization on the heat dissipation equipment, then allowing the acetone-methanol mixed solvent to enter the filtering equipment through the raw material liquid input pipeline, discharging a solid phase obtained by filtering the acetone-methanol mixed solvent through the filtering equipment from the solid phase outlet, and discharging a liquid phase obtained by filtering the acetone-methanol mixed solvent from the liquid phase outlet.
The invention has the following beneficial effects:
the centrifugal separation method for 50VE and sterol and the crystallization and filtration combined system thereof provided by the invention have the advantages of low labor intensity, low environmental pollution, easiness in reaction control and high purity and recovery rate of vitamin E.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor. Wherein:
FIG. 1 is a schematic diagram of the distribution of the whole system in embodiments 1 to 4 of the present invention.
FIG. 2 is a flow chart illustrating the operation of the refrigeration system according to embodiments 1 to 4 of the present invention.
FIG. 3 is a schematic diagram of the distribution of the filtration unit system in embodiments 1 to 4 of the present invention.
FIG. 4 is a schematic structural diagram of a filtering apparatus according to embodiments 1 to 4 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying specific embodiments of the present invention are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein, and it will be appreciated by those skilled in the art that the present invention may be practiced without departing from the spirit and scope of the present invention and that the present invention is not limited by the specific embodiments disclosed below.
Furthermore, the references herein to "one embodiment" or "an embodiment" refer to a particular feature, structure, or characteristic that may be included in at least one implementation of the present invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
This example provides one embodiment of a method for centrifugal separation of 50VE and sterols comprising:
dissolving 1t of the corn oil deodorized distillate into 6000L of acetone-methanol mixed solvent (the volume ratio of acetone to methanol is 2:1), and injecting the mixed solution into the heat dissipation equipment 301 of the second heat exchange unit 300 for low-temperature crystallization treatment. In the low-temperature crystallization process, the initial temperature in the heat dissipation device 301 needs to be controlled to be 35 ℃, then the temperature is slowly reduced to-5 ℃ within 4 hours, and the temperature is kept for 24 hours, so as to obtain a crystallization mixed solution. And then transmitting the crystal mixed solution in the heat dissipation equipment 301 to a filtering unit 700 for filtering, taking filtrate, centrifuging, washing and drying to obtain deodorized distillate without sterol, wherein the centrifugation is performed for 30min at 5000 rpm.
Distilling the deodorized distillate without sterol at distillation temperature of 220 deg.C, feeding temperature of 80 deg.C and rotation speed of 180r/min to obtain distillate and residue liquid respectively; and (3) evaporating the solvent from the distillate to obtain a vitamin E product.
The vitamin E product content of example 1 was found to be 49.9% with a recovery of 81.2%.
It should be noted that: in the above process, the "50 VE and sterol centrifugal separation method" is completed by a crystallization and filtration combined system, as shown in fig. 1 to 4, the crystallization and filtration combined system includes: the system comprises a steam power unit 100, a first heat exchange unit 200, a second heat exchange unit 300, a steam absorption unit 400, a conveying unit 500, a throttling device 600, a filtering unit 700 and the like.
The steam power unit 100, the first heat exchange unit 200, the second heat exchange unit 300, the steam absorption unit 400, the conveying unit 500 and the throttling device 600 jointly implement the cooling and crystallizing process, so that the local functional system formed by the steam power unit 100, the first heat exchange unit 200, the second heat exchange unit 300, the steam absorption unit 400, the conveying unit 500 and the throttling device 600 can be defined as a refrigeration system. The cooling equipment 301 in the second heat exchange unit 300 is cooled and refrigerated by the end equipment which can be directly used as a refrigeration container in the refrigeration system. Further, the filter unit 700 in the present invention is a set of "filter system" capable of solid-liquid separation.
Based on the above, specifically:
the steam power unit 100 comprises an evaporation device 101, a steam conveying pipeline 102 and a flow dividing device 103, wherein the flow dividing device 103 is connected with the evaporation device 101 through the steam conveying pipeline 102; the first heat exchange unit 200 comprises a heat sink 201, and the heat sink 201 is connected with a cooling device 204 through a first conveying pipeline 202 and a first liquid return pipeline 203 respectively to form a circulation loop; the second heat exchange unit 300 comprises a heat sink 301, and the heat sink 301 is connected to the first heat exchange unit 200 and the vapor absorption unit 400 respectively; and, the steam absorption unit 400 includes an absorption device 401, and the absorption device 401 is connected to the steam power unit 100 through a first circulation line 402 and a second circulation line 403, respectively.
The steam power unit 100 is used, among other things, to generate and deliver steam. In the present invention, the evaporation apparatus 101 may be a boiler or a steam generator, and two mixed solutions with different boiling points are contained in the boiler or the steam generator, wherein the two mixed solutions are respectively a refrigerant and an absorbent, and the two mixed solutions can be mutually soluble, and the boiling point of the refrigerant is lower than that of the absorbent. The evaporation device 101 is used for heating and releasing the refrigerant to form high-temperature and high-pressure steam, and is externally connected with the steam conveying pipeline 102, the tail end of the steam conveying pipeline 102 is connected to the flow dividing device 103, and the flow dividing device 103 is used for dividing the steam transmitted from the steam conveying pipeline 102 and distributing the steam to the multiple sets of branch pipelines of the conveying unit 500.
The first heat exchange unit 200 is configured to absorb heat from the conveying unit 500, so that the high-temperature and high-pressure steam releases heat to form a low-temperature and high-pressure liquid state. The heat sink 201 is a container filled with cold water, and can absorb heat to cool the steam through the cold water.
The second heat exchange unit 300 is used for cooling and refrigerating, and is disposed between the first heat exchange unit 200 and the vapor absorption unit 400, and the low-temperature high-pressure liquid refrigerant from the first heat exchange unit 200 is decompressed by the throttling device 600 and then rapidly expanded and vaporized, and absorbs a large amount of heat in the heat dissipation device 301, thereby achieving the purpose of cooling and refrigerating. The throttle device 600 in the present invention may employ a throttle valve.
The vapor absorption unit 400 is used for refrigerant recovery and cycle refrigeration, and its absorption device 401 is connected to the vapor power unit 100 through a first circulation line 402 and a second circulation line 403. The first circulation pipeline 402 is a connecting pipeline between the bottom of the evaporation apparatus 101 and the absorption apparatus 401, and the solution in the evaporation apparatus 101 is transported to the inside of the absorption apparatus 401 through the first circulation pipeline 402 for absorbing the vaporized refrigerant. Meanwhile, the second recycling line 403 returns the solution in the absorption apparatus 401 to the evaporation apparatus 101 again, and the power is transferred by the pump 403a on the second recycling line 403.
Further, the flow dividing device 103, the first heat exchange unit 200, the second heat exchange unit 300 and the steam absorption unit 400 are connected in sequence through the conveying unit 500, and the conveying unit 500 includes a first conveying pipeline 501, a second conveying pipeline 502 and a third conveying pipeline 503. The flow dividing device 103 is connected with the first heat exchange unit 200 through a first conveying pipeline 501, the first heat exchange unit 200 is connected with the second heat exchange unit 300 through a second conveying pipeline 502, the second heat exchange unit 300 is connected with the steam absorption unit 400 through a third conveying pipeline 503, and the second conveying pipeline 502 is provided with a throttling device 600.
Further, the connection between the first delivery pipe 501 and the second delivery pipe 502 has a heat dissipation pipe 205, which has a function of a condenser. The junction of the second delivery line 502 and the third delivery line 503 has a heat absorption line 302, which functions as an evaporator. The heat dissipation pipe 205 is located inside the heat sink 201, and the heat absorption pipe 302 is located inside the heat sink 301.
In the present invention, the heat sink 201 is connected to the cooling device 204 through the first transfer line 202 and the first return line 203, respectively, to form a circulation circuit. As can be seen from the above, the heat sink 201 contains water, and the wall of the heat sink 201 has a water inlet and a water outlet. The water outlet of the first conveying pipeline 202 is connected to the first conveying pipeline 202, and the other end of the first conveying pipeline 202 extends to the upper part of the cooling device 204. The first conveying pipeline 202 is provided with an infusion pump, and the infusion pump conveys the heat absorption water in the heat absorption device 201 to the cooling device 204. Preferably, a spray header is arranged at the end head of the first conveying pipeline 202, so that water is atomized from the spray header, and rapid cooling is facilitated, and finally, the cooled water mist falls into the cooling device 204 and flows back into the heat sink 201 through the first liquid return pipeline 203 via the water inlet of the heat sink 201, so as to form a circulation loop. The cooling apparatus 204 in the present invention is a cooling tower.
The same as that, the inside of the absorption device 401 is further provided with a cold water pipe, two ends of the cold water pipe penetrate through the absorption device 401 and are respectively connected with a second conveying pipeline 404 and a second liquid return pipeline 405, and the second conveying pipeline 404 and the second liquid return pipeline 405 are both connected with the (another) cooling device 204. One end of the second conveying pipeline 404 is connected to the cold water pipe in the absorption device 401, and the other end extends to the upper part of the (another) cooling device 204. The second transfer line 404 is provided with an infusion pump, and transfers the endothermic water in the absorption device 401 to the (another) cooling device 204 through the infusion pump. Preferably, a spray header is arranged at the end head of the second conveying pipeline 404, so that water is atomized from the spray header, and rapid cooling is facilitated, and finally, the cooled water mist falls into the cooling device 204 and flows back into the absorption device 401 through the second liquid return pipeline 405.
In the present invention, the operation flow of the refrigeration system is as follows:
first, the evaporation device 101 heats the mixed solution therein, and the refrigerant with a lower boiling point directly evaporates due to a difference in boiling point, vaporizes into high-temperature and high-pressure vapor, and enters the first conveying line 501 from the vapor conveying line 102 through the flow dividing device 103. Meanwhile, another process is also accompanied, namely: the absorbent solution in the evaporation apparatus 101 becomes higher in concentration due to vaporization of the refrigerant, and enters the absorption apparatus 401 from the first circulation line 402.
The high-temperature and high-pressure steam introduced into the first transfer line 501 is transferred to the heat dissipation line 205. Since the heat dissipation pipeline 205 is located in the cold water of the heat sink 201, the cold water absorbs heat of the high-temperature and high-pressure steam in the heat dissipation pipeline 205, so that the steam is cooled and liquefied, and a low-temperature and high-pressure liquid refrigerant is formed. Meanwhile, the temperature of the cold water in the heat absorption device 201 gradually rises due to heat absorption, and the first conveying pipeline 202 can introduce the heat-absorbed and temperature-increased water into the cooling device 204 for cooling, and the cold water is returned to the heat absorption device 201 through the first liquid return pipeline 203 again to take part in work, so that a cycle is formed.
The cooled and liquefied refrigerant flows to the heat absorption circuit 302 through the second delivery pipe 502, and the heat absorption circuit 302 is located in the heat sink 301. Because the throttling device 600 is arranged on the second conveying pipeline 502, the low-temperature high-pressure liquid refrigerant is decompressed by the throttling device 600 and enters the heat absorption pipeline 302, and then is rapidly expanded, vaporized and absorbed heat to form low-temperature steam. Because the heat absorption circuit 302 is located in the heat dissipation device 301, the ambient temperature in the heat dissipation device 301 is greatly reduced, so as to achieve the purpose of cooling.
Finally, the low-temperature vapor enters the third conveying pipeline 503 from the heat absorbing pipeline 302, and enters the absorption device 401 through the third conveying pipeline 503, and is absorbed by the absorbent solution discharged into the absorption device 401. At this time, the solubility of the absorbent solution in the absorption apparatus 401 decreases, and the absorbent solution is sent to the inside of the evaporation apparatus 101 by the pump 403a on the second circulation line 403, so that the refrigerant and the absorbent are circulated and used. In the process, the temperature in the absorption apparatus 401 is cooled by the circulation loop of the second conveying pipe 404 and the second return pipe 405.
In the present invention, the conveying unit 500 may be provided with at least two sets (although the description of the present invention and the corresponding drawings temporarily illustrate three sets of pipelines, but do not affect the protection scope of the present invention), each set is divided and transmitted by the flow dividing device 103, and each pipeline is arranged side by side, one section of each pipeline is connected to the flow dividing device 103, and the other end of each pipeline is connected to the inside of the absorption device 401.
Specifically, if the conveying unit 500 is divided into three paths, the three paths can be respectively set as path a and path B, and the three paths have the same pipeline specification and are arranged side by side. When all three pipelines are opened, the heat dissipation device 301 can uniformly and efficiently refrigerate. If only one path is opened and the valves of the other two paths are closed, the steam pressure in the pipeline is increased, and the pressure reducing valve on the opened path can be adjusted to reduce the pressure, so that the refrigerating effect and the refrigerating space in the heat dissipation device 301 are controlled. Therefore, in the present invention, a user can arbitrarily open a pipeline according to an actual demand, adjust a corresponding pressure reducing valve to control a refrigeration effect, and control a temperature in the heat dissipation device 301 by adjusting the evaporation efficiency of the evaporation device 101 (a temperature value thereof can be monitored by a thermometer disposed on the heat dissipation device 301).
An important "filtration system" also included in the crystallization-filtration combination is a filtration unit 700, which also enables solid-liquid separation of the crystallized solution. In the present invention, the filtering unit 700 includes a filtering apparatus 701, an air source channel 702, a raw material liquid input pipeline 703 and a filtrate output pipeline 704. The filtering device 701 is used for filtering; the air source channel 702 is used for applying pressure to the outside to promote the normal operation of filtration; the raw material liquid input pipeline 703 is an input pipeline of the material liquid to be separated; the filtrate output pipeline 704 is a liquid phase output pipeline after solid-liquid separation.
The filter 701 is provided with a raw material liquid inlet 701a, a first compressed air inlet 701b, a solid phase outlet 701c, and a liquid phase outlet 701 d. Since the filtering unit 700 receives the crystallization mixture solution from the heat sink 301, the following is applied: the heat sink 301 has a first inlet port 301a, a second inlet port 301b, a second compressed air inlet 301c, and a first outlet port 301 d.
The raw material liquid input pipeline 703 has one end connected to the first discharge port 301d of the heat sink 301 and the other end connected to the raw material liquid inlet 701a, and is capable of transferring the crystal mixture solution from the inside of the heat sink 301 to the inside of the filter apparatus 701.
The filtrate outlet line 704 is connected to the liquid phase outlet 701d, and is capable of discharging the filtrate from the inside of the filtration apparatus 701 through the liquid phase outlet 701 d. Specifically, the inside of the filter device 701 is provided with a filter module 701e for directly performing solid-liquid separation. The filter module 701e is in end-to-end engagement with the inner port of the liquid phase outlet 701d and is in communication with the filtrate output line 704 through the liquid phase outlet 701d, so that the liquid phase filtered by the filter module 701e can be discharged from the liquid phase outlet 701d and through the filtrate output line 704.
It should be noted here that: filter assembly 701e of the present invention includes filter media 701e-1 and header 701 e-2. The liquid collecting pipes 701e-2 are directly butted with the inner opening end of the liquid phase outlet 701d to form communication, a plurality of filter media 701e-1 can be connected to each liquid collecting pipe 701e-2 at the same time, and filtrate obtained by filtering of each filter medium is collected to the liquid collecting pipes 701 e-2. In addition, as can be seen from the above description, each liquid collecting pipe 701e-2 corresponds to the liquid phase outlet 701d and the filtrate output pipeline 704 one by one, and at least one group (or multiple groups) is provided, and the outer ends of the filtrate output pipelines 704 are all connected to the filtrate collecting pipeline 705 in a unified and centralized manner.
In addition, in consideration of the situation that the temperature of the filtering device 701 may rise during the operation process, which may cause the solid phase that has been crystallized and precipitated to be dissolved in the solution again, a jacket may be disposed on the periphery of the filtering device 701, a cold water inlet port 701f and a cold water outlet port 701g are disposed on two sides of the jacket, respectively, the cold water inlet port 701f is externally connected to the cold water inlet pipe 701f-1, and cold water for reducing the temperature is introduced into the jacket. The cold water outlet port 701g is externally connected with a cold water outlet pipe 701g-1 for discharging the introduced cold water. Therefore, the cooling effect of the cold water inlet pipe 701f-1 and the cold water outlet pipe 701g-1 can ensure that the precipitated crystals are not dissolved in the solution again.
The power for the filtration stroke of the filtration device 701 is derived from the air supply channel 702. The air source channel 702 comprises a first air source flow path 702a, a second air source flow path 702b and a third air source flow path 702c, wherein the first air source flow path 702a is connected to the first compressed air inlet 701b, the second air source flow path 702b is connected to the filtrate collecting pipeline 705, and the third air source flow path 702c is connected to the second compressed air inlet 301c and is communicated to the inside of the heat sink 301. The air supply passage 702 is external to the air supply processor and provides compressed air to the first air supply flow path 702a, the second air supply flow path 702b, and the third air supply flow path 702 c.
Therefore, the operation of the filtering apparatus 701 includes the following three steps: firstly, a third air source flow path 702c is opened, air is introduced into the heat dissipation device 301, and due to the action of air pressure, the crystal mixed solution in the heat dissipation device 301 is extruded to be discharged from the first discharge port 301d and enter the filtering device 701 from the raw material solution inlet 701a (the feeding process can also be realized by an infusion pump); secondly, opening a first air source flow path 702a, introducing air into the filtering device 701 to increase the air pressure in the filtering device 701, allowing the liquid phase part to enter a liquid collecting pipe 701e-2 from a filtering medium 701e-1 under pressure, completing filtration, and finally discharging the liquid phase part from a filtrate output pipeline 704 to a filtrate collecting pipeline 705 (in this case, a positive blowing process); and thirdly, closing the third air source flow path 702c and the first air source flow path 702a, and opening the second air source flow path 702b, so that air can be blown back to the filter medium 701e-1 from the filtrate collecting line 705, and thus part of the solid phase attached to the outer surface of the filter medium 701e-1 can be blown off by the reverse air flow and fall to the solid phase outlet 701c (in this process, a back blowing process).
After the above-mentioned one completion process, the solid phase portion in the crystallization mixed solution gradually accumulates and falls to the solid phase outlet 701c, and is finally discharged in a unified manner. In summary, when the acetone-methanol mixed solvent and the vegetable oil deodorized distillate dissolved therein are injected into the heat radiating device 301, the acetone-methanol mixed solvent is cooled and crystallized in the heat radiating device 301, and then enters the filtering device 701 through the raw material liquid input pipeline 703, the solid phase filtered by the filtering device 701 is discharged from the solid phase outlet 701c, and the liquid phase is discharged from the liquid phase outlet 701 d.
Further, in order to avoid resource waste and ensure the purity of the filtration, a return liquid pipe set 706 may be provided, and the return liquid pipe set 706 includes a first return liquid pipe 706a and a second return liquid pipe 706 b. One end of the first liquid return pipe 706a is connected to a liquid return port 701h of the filtering apparatus 701 (an overflow channel arranged at the lower end of the filtering apparatus 701), and the other end is connected to the second feeding port 301 b; the second liquid return pipe 706b is connected to the filtrate collecting line 705 at one end and is connected to the second feed connection 301b together with the first liquid return pipe 706a at the other end. Therefore, when the filtrate obtained by using only the filter module 701e still contains a part of solid phase, the return liquid can be collected again by the return liquid pipe group 706, filtered again, and circulated.
As shown in fig. 3 and 4, it should be noted that: when the forward blowing process is required, the stop valves on the first air source flow path 702a and the third air source flow path 702c can be opened, the stop valves on the raw material liquid input pipeline 703, the filtrate output pipeline 704 and the filtrate collecting pipeline 705 can be opened, and the stop valves on the second air source flow path 702b and the liquid return pipe group 706 can be closed;
when liquid return is required to be collected again, the stop valves on the first air source flow path 702a and the third air source flow path 702c can be opened, the stop valves on the raw material liquid input pipeline 703, the filtrate output pipeline 704 and the liquid return pipe group 706 can be opened, and the stop valve on the second air source flow path 702b can be closed, wherein the stop valve on the filtrate collection pipeline 705 can be selectively opened or not opened according to the situation (the filtrate collection pipeline 705 is closed when the filtering effect is poor, and the filtrate collection pipeline 705 is opened when the filtering effect is good);
When the back flushing process is required, the stop valves on the first air source flow path 702a and the third air source flow path 702c may be closed, the stop valves on the raw material liquid input line 703, the filtrate collecting line 705 and the liquid return pipe group 706 may be closed, and the stop valves on the second air source flow path 702b and the filtrate output line 704 may be opened.
Example 2
Dissolving 1t of corn oil deodorized distillate in 5000L of acetone-methanol mixed solvent (the volume ratio of acetone to methanol is 1.5:1), controlling the temperature to 40 ℃, then slowly cooling to-5 ℃ within 6h, keeping for 22h for low-temperature crystallization treatment, then filtering, taking filtrate, centrifugally washing and drying to obtain sterol-removed deodorized distillate, and centrifuging at 7000rpm for 30 min;
distilling the deodorized distillate without sterol at distillation temperature of 220 deg.C, feeding temperature of 90 deg.C, and rotation speed of 150r/min to obtain distillate and residue liquid respectively; and (3) evaporating the solvent from the distillate to obtain a vitamin E product.
The vitamin E product content of example 2 was found to be 51.2% with a recovery of 82.6%.
In this embodiment, "low-temperature crystallization" and "filtration" in the above process are implemented by using the crystallization and filtration combination system described in embodiment 1, and the working process thereof is shown in fig. 1 to 4.
Example 3
Dissolving 1t soybean oil deodorized distillate in 5500L acetone-methanol mixed solvent (volume ratio of acetone to methanol is 2:1), controlling temperature at 35 deg.C, slowly cooling to-5 deg.C within 5 hr, maintaining for 20 hr for low temperature crystallization treatment, filtering, centrifuging filtrate, washing and drying to obtain deodorized distillate without sterol, centrifuging at 6000rpm for 35 min;
distilling the deodorized distillate without sterol at the distillation temperature of 230 ℃, the feeding temperature of 90 ℃ and the rotation speed of 160r/min to respectively obtain distillate and residual liquid; and (3) evaporating the solvent from the distillate to obtain a vitamin E product.
The vitamin E product content of example 3 was found to be 50.3% with a recovery of 84.1%.
In this embodiment, "low-temperature crystallization" and "filtration" in the above process are implemented by using the crystallization and filtration combination system described in embodiment 1, and the working process is shown in fig. 1 to 4.
Example 4
Dissolving 1t of soybean oil deodorized distillate in 5500L of acetone-methanol mixed solvent (the volume ratio of acetone to methanol is 1.5:1), controlling the temperature to 35 ℃, slowly cooling to-5 ℃ within 5h, keeping for 22h for low-temperature crystallization treatment, filtering, taking filtrate, centrifuging, washing and drying to obtain deodorized distillate without sterol, and centrifuging at 6000rpm for 35 min;
Distilling the deodorized distillate without sterol at distillation temperature of 220 deg.C, feeding temperature of 90 deg.C and rotation speed of 160r/min to obtain distillate and residue liquid respectively; and (3) evaporating the solvent from the distillate to obtain a vitamin E product.
The vitamin E product content of example 4 was found to be 51.1% with a recovery of 84.2%.
In this embodiment, "low-temperature crystallization" and "filtration" in the above process are implemented by using the crystallization and filtration combination system described in embodiment 1, and the working process thereof is shown in fig. 1 to 4.
It is worth mentioning that in the experiment, the invention discovers that the operation of maintaining the second-order temperature during low-temperature crystallization, namely (controlling the temperature to be 30-40 ℃, then slowly cooling to-5 ℃ within 4-6 h, and maintaining for 20-24 h), the two temperature control factors can generate a synergistic effect, so that the high removal of the sterol is ensured, and the purity of the extracted vitamin E is further improved.
Therefore, the method for centrifugal separation of 50VE and sterol and the crystallization and filtration combined system thereof provided by the invention have the remarkable advantages of low labor intensity, low environmental pollution, easiness in reaction control, high purity and recovery rate of vitamin E and the like.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (1)
1. A method for centrifugal separation of 50VE and sterol is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
dissolving the deodorized distillate of vegetable oil in acetone-methanol mixed solvent, crystallizing at low temperature, filtering, centrifuging the filtrate, washing, and oven drying to obtain deodorized distillate without sterol;
distilling the deodorized distillate without sterol to respectively obtain distillate and residual liquid; evaporating the distillate to remove the solvent to obtain a vitamin E product;
distilling at the distillation temperature of 220-230 ℃, the feeding temperature of 80-90 ℃ and the rotation speed of 120-180 r/min;
the centrifugation is carried out for 30-40 min at 5000-7000 rpm;
the vegetable oil deodorized distillate comprises corn oil deodorized distillate or soybean oil deodorized distillate;
the low-temperature crystallization is carried out by controlling the temperature to be 30-40 ℃, then slowly cooling to-5 ℃ within 4-6 hours, and keeping for 20-24 hours;
the volume ratio of acetone to methanol in the acetone-methanol mixed solvent is 1-2: 1, and the usage amount of the mixed solvent is 5-6 ml/g of deodorized distillate of vegetable oil;
the low-temperature crystallization adopts a crystallization and filtration combined system which comprises,
the steam power unit (100) comprises an evaporation device (101), a steam conveying pipeline (102) and a flow dividing device (103), wherein the flow dividing device (103) is connected with the evaporation device (101) through the steam conveying pipeline (102);
The heat exchange system comprises a first heat exchange unit (200) and a second heat exchange unit (200), wherein the first heat exchange unit comprises a heat absorption device (201), and the heat absorption device (201) is connected with a cooling device (204) through a first conveying pipeline (202) and a first liquid return pipeline (203) respectively to form a circulation loop;
a second heat exchange unit (300) comprising a heat sink (301), the heat sink (301) being connected to the first heat exchange unit (200) and the vapor absorption unit (400), respectively; and (c) a second step of,
a steam absorption unit (400) comprising an absorption device (401), and the absorption device (401) is connected with the steam power unit (100) through a first circulation line (402) and a second circulation line (403), respectively; a cold water pipe is further arranged inside the absorption equipment (401), and two ends of the cold water pipe penetrate through the absorption equipment (401) and are respectively externally connected with a second conveying pipeline (404) and a second liquid return pipeline (405); the second conveying pipeline (404) and the second liquid return pipeline (405) are connected with the cooling device (204);
the flow dividing device (103), the first heat exchange unit (200), the second heat exchange unit (300) and the steam absorption unit (400) are sequentially connected through a conveying unit (500), and the conveying unit (500) comprises a first conveying pipeline (501), a second conveying pipeline (502) and a third conveying pipeline (503);
The flow dividing device (103) is connected with the first heat exchange unit (200) through the first conveying pipeline (501), the first heat exchange unit (200) is connected with the second heat exchange unit (300) through the second conveying pipeline (502), and the second heat exchange unit (300) is connected with the steam absorption unit (400) through the third conveying pipeline (503); a throttling device (600) is arranged on the second conveying pipeline (502);
a heat dissipation pipeline (205) is arranged at the joint of the first conveying pipeline (501) and the second conveying pipeline (502), and a heat absorption pipeline (302) is arranged at the joint of the second conveying pipeline (502) and the third conveying pipeline (503); -the heat dissipation circuit (205) is located inside the heat sink (201), the heat absorption circuit (302) is located inside the heat dissipation device (301);
the conveying units (500) are at least provided with two groups, pipelines are arranged side by side, one section of the conveying units is connected to the flow dividing equipment (103), and the other end of the conveying units is connected to the inside of the absorption equipment (401);
the filter unit (700) comprises a filter device (701), an air source channel (702), a raw material liquid input pipeline (703) and a filtrate output pipeline (704), wherein the filter device (701) is provided with a raw material liquid inlet (701a), a first compressed air inlet (701b), a solid phase outlet (701c) and a liquid phase outlet (701 d); one end of the raw material liquid input pipeline (703) is connected with the heat dissipation device (301), and the other end of the raw material liquid input pipeline is connected with the raw material liquid inlet (701a), so that the crystallization mixed solution from the interior of the heat dissipation device (301) can be transmitted to the interior of the filtering device (701); the filtrate output line (704) is connected with the liquid phase outlet (701d) and can discharge the filtrate from the inside of the filtering device (701) from the liquid phase outlet (701 d);
A filtering component (701e) is arranged in the filtering device (701), and the filtering component (701e) is butted with the inner opening end of the liquid phase outlet (701d) and is communicated with the filtrate output pipeline (704) through the liquid phase outlet (701 d); the filtrate output pipelines (704) correspond to the liquid phase outlets (701d) one by one, at least one group of filtrate output pipelines is arranged, and the outer ends of the filtrate output pipelines (704) are connected to a filtrate collecting pipeline (705) in a centralized manner;
the air source channel (702) comprises a first air source flow path (702a), a second air source flow path (702b) and a third air source flow path (702c), the first air source flow path (702a) is connected to the first compressed air inlet (701b), the second air source flow path (702b) is connected to the filtrate collecting pipeline (705), and the third air source flow path (702c) is connected to the inside of the heat dissipation device (301); the air source channel (702) is externally connected with an air source and provides compressed air for the first air source flow path (702a), the second air source flow path (702b) and the third air source flow path (702 c);
injecting the acetone-methanol mixed solvent and the vegetable oil deodorizer distillate dissolved therein into the heat dissipation device (301), performing low-temperature crystallization on the heat dissipation device (301), allowing the acetone-methanol mixed solvent to enter the filtering device (701) through the raw material liquid input pipeline (703), discharging a solid phase obtained by filtering through the filtering device (701) from the solid phase outlet (701c), and discharging an obtained liquid phase from the liquid phase outlet (701 d).
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