CN108771881B - Method and system for low-residue multistage steam stripping of vitamin E byproduct fatty acid solvent - Google Patents
Method and system for low-residue multistage steam stripping of vitamin E byproduct fatty acid solvent Download PDFInfo
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- CN108771881B CN108771881B CN201810646351.8A CN201810646351A CN108771881B CN 108771881 B CN108771881 B CN 108771881B CN 201810646351 A CN201810646351 A CN 201810646351A CN 108771881 B CN108771881 B CN 108771881B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/38—Steam distillation
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Abstract
The invention discloses a method and a system for low-residue multistage steam stripping of a vitamin E byproduct fatty acid solvent, which comprises the steps of distilling deodorized distillate from which sterol is removed to respectively obtain distillate and residual liquid; and carrying out multistage steam stripping on the distillate, and evaporating the solvent to obtain a vitamin E product. The method for multistage stripping of vitamin E by-product fatty acid solvent with low residue provided by the invention has the advantages of extremely low residue capacity, low labor intensity, low environmental pollution, easy reaction control and high 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 low-residue multistage steam stripping method for a vitamin E byproduct fatty acid solvent 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 residual capacity (more than 5000ppm), 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 the title of the invention of this 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 blank in the existing multi-stage stripping process of vitamin E by-product fatty acid solvent with low residue.
Accordingly, it is an object of the present invention to overcome the deficiencies in the prior art by providing a low residue multi-stage stripping process for vitamin E byproduct fatty acid solvent.
In order to solve the technical problems, the invention provides the following technical scheme: a low-residue multi-stage steam stripping method of a vitamin E byproduct fatty acid solvent comprises the steps of dissolving deodorized distillate of vegetable oil in an acetone-methanol mixed solvent, controlling the temperature to be 30-40 ℃, then slowly cooling to-5 ℃ within 4-6 h, keeping the temperature for 20-24 h, filtering, centrifuging, washing and drying filtrate to obtain deodorized distillate with sterol removed; distilling the deodorized distillate without sterol to respectively obtain distillate and residual liquid; and carrying out multistage steam stripping on the distillate, and evaporating the solvent to obtain a vitamin E product.
As a preferred embodiment of the method for the multi-stage stripping of vitamin E by-product fatty acid solvent with low residue, the method of the invention comprises: the distillation is carried out 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 the multi-stage stripping of vitamin E by-product fatty acid solvent with low residue, the method of the invention comprises: the centrifugation is carried out for 30-40 min at 5000-7000 rpm.
As a preferred embodiment of the method for the multi-stage stripping of vitamin E by-product fatty acid solvent with low residue, the method of the invention comprises: the vegetable oil deodorized distillate comprises corn oil deodorized distillate or soybean oil deodorized distillate.
As a preferred embodiment of the method for the multi-stage stripping of vitamin E by-product fatty acid solvent with low residue, the method of the invention comprises: 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 crystallization-filtration integrated system comprising: the steam power unit comprises evaporation equipment, a steam conveying pipeline and a flow dividing device, and the flow dividing device 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 units 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, and the other end of the conveying units is connected to the interior 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 opening 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 supply passage comprises a first air supply flow path, a second air supply flow path and a third air supply flow path, the first air supply flow path is connected to the first compressed air inlet, the second air supply flow path is connected to the filtrate collecting pipeline, and the third air supply 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 deodorized distillate dissolved in the acetone-methanol mixed solvent into the heat dissipation equipment together, allowing the acetone-methanol mixed solvent to enter the interior of the filtering equipment through the raw material liquid input pipeline after low-temperature crystallization of the heat dissipation equipment, discharging a solid phase obtained by filtering through the filtering equipment from the solid phase outlet, and discharging an obtained liquid phase from the liquid phase outlet.
The invention has the following beneficial effects:
the method and the system for the multistage steam stripping of the vitamin E byproduct fatty acid solvent with low residue provided by the invention have the advantages of extremely low residue capacity, low labor intensity, low environmental pollution, easy reaction control, and high purity and recovery rate of the vitamin E.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a schematic diagram of the overall system distribution in the embodiments 1 to 4 of the present invention.
FIG. 2 is a flow chart of the operation of the refrigeration system according to embodiments 1-4 of the present invention.
FIG. 3 is a schematic diagram of the distribution of the filtration unit system in the 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 comprehensible, embodiments accompanied with examples 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, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the 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 centrifugation of 50VE and sterols comprising:
1t of the deodorized distillate of the soybean oil is dissolved in 5000L of acetone-methanol mixed solvent (the volume ratio of acetone to methanol is 1.5:1), and the mixed solution is injected 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 40 ℃, 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 carried out for 30min at 6000 rpm.
Distilling the deodorized distillate without sterol at the distillation temperature of 230 ℃, the feeding temperature of 90 ℃ and the rotation speed of 120r/min to respectively obtain distillate and residual liquid; and carrying out multi-stage steam stripping on the distillate, and then evaporating the solvent to obtain the vitamin E product.
It was determined that the vitamin E product of example 1 was 49.9%, the recovery was 81.2%, and the residual capacity was 71 ppm.
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 realize the cooling and crystallization 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 heat sink 301 in the second heat exchange unit 300 is cooled and refrigerated by the "refrigeration system" which can be directly used as the end equipment of the refrigeration container. 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 dissipation device 301, and the heat dissipation device 301 is respectively connected with the first heat exchange unit 200 and the steam absorption unit 400; 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, which are respectively a refrigerant and an absorbent, are contained in the boiler or the steam generator, 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 refrigerant to form high-temperature and high-pressure steam, and is externally connected with a steam conveying pipeline 102, the tail end of the steam conveying pipeline 102 is connected to a flow dividing device 103, and the flow dividing device 103 is used for dividing the steam conveyed from the steam conveying pipeline 102 and distributing the steam to a plurality of groups of branch pipelines of the conveying unit 500.
The first heat exchange unit 200 is used for absorbing 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 therein, 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 expands and vaporizes, 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 circulation 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 circulation 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 sequentially connected through a 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 joint of the first delivery pipe 501 and the second delivery pipe 502 has a heat dissipation pipe 205, which has the 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 absorbing device 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 in a butt joint mode, and the other end of the first conveying pipeline 202 extends to the upper portion of the cooling device 204. The first transfer line 202 is provided with an infusion pump, and transfers the endothermic water in the endothermic device 201 to the cooling device 204 through the infusion pump. 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, rapid cooling is facilitated, and finally 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, thereby forming a circulation loop. The cooling apparatus 204 in the present invention is a cooling tower.
Similarly, a cold water pipe is further disposed inside the absorption device 401, two ends of the cold water pipe penetrate through the absorption device 401 and are respectively connected with the second conveying pipeline 404 and the second liquid return pipeline 405 in an external mode, and the second conveying pipeline 404 and the second liquid return pipeline 405 are both connected with the (another) cooling device 204. Wherein one end of the second conveying pipeline 404 is connected with 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 via the infusion pump. Preferably, the end head of the second conveying pipeline 404 is provided with a spray header, so that water is atomized from the spray header, thereby being more beneficial to rapid cooling, and finally the cooled water mist falls into the cooling device 204 and flows back to 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 apparatus 101 heats the mixed solution inside, and the refrigerant with a lower boiling point is directly evaporated due to the difference in boiling point, and is vaporized into high-temperature and high-pressure vapor, and enters the first conveying line 501 from the vapor conveying line 102 through the flow dividing apparatus 103. At the same time, there is another process, namely: the concentration of the absorbent solution in the evaporation apparatus 101 becomes higher and higher 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 delivery pipe 501 is delivered into the heat dissipation pipe 205. Since the heat dissipation pipeline 205 is located in the cold water of the heat sink 201, the cold water absorbs the 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 sink 201 gradually rises due to heat absorption, and the first conveying pipeline 202 can introduce the heat-absorbed and temperature-raised water into the cooling device 204 for cooling, and the cold water is returned to the heat sink 201 through the first liquid return pipeline 203 again to take part in work, so that a cycle is formed.
The refrigerant after being cooled and liquefied flows to the heat absorption circuit 302 through the second transfer circuit 502, and the heat absorption circuit 302 is located in the heat sink 301. Because the second delivery pipe 502 is provided with the throttling device 600, the low-temperature high-pressure liquid refrigerant is decompressed by the throttling device 600 and enters the heat absorption pipe 302, and then is rapidly expanded, vaporized and absorbed heat, so as to form low-temperature steam. Because the heat absorption pipeline 302 is located in the heat dissipation device 301, the ambient temperature in the heat dissipation device 301 is greatly reduced, thereby achieving the purpose of cooling.
Finally, the low-temperature vapor enters the third conveying pipeline 503 from the heat absorbing pipeline 302, 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 device 401 decreases, and the absorbent solution is sent to the inside of the evaporation device 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 device 401 is cooled by the circulation loop of the second delivery 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 are described by three sets of pipelines temporarily, but the scope of the present invention is not affected), each set is transmitted by branching through the branching device 103, and each set of pipelines is arranged side by side, one section of each set is connected to the branching device 103, and the other end is connected to the inside of the absorbing device 401.
Specifically, if the conveying unit 500 is divided into three paths, the three paths can be respectively set as a path a and a 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, when the valves of the other two paths are closed, the pressure of steam in the pipeline is increased, and at the moment, the pressure reducing valve on the opened path can be adjusted to perform pressure reduction treatment, so that the refrigeration effect and the refrigeration space in the heat dissipation device 301 are controlled. Therefore, in the present invention, a user can freely open a pipeline according to actual requirements, adjust the corresponding pressure reducing valve to control the refrigeration effect, and control the temperature in the heat sink 301 by adjusting the evaporation efficiency of the evaporation device 101 (the temperature value can be monitored by a thermometer disposed on the heat sink 301).
An important "filtration system" also included in the crystallization-filtration combination system 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 device 701, a gas 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 outside to promote normal 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 radiating apparatus 301, the following is the corresponding: the heat sink 301 has a first inlet 301a, a second inlet 301b, a second compressed air inlet 301c, and a first outlet 301 d.
The raw material liquid input pipeline 703 has one end connected to the first outlet port 301d of the heat sink 301 and the other end connected to the raw material liquid inlet 701a, and is capable of transporting the crystallization 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 filter apparatus 701 from the liquid phase outlet 701 d. Specifically, the inside of the filter apparatus 701 is provided with a filter assembly 701e for directly performing solid-liquid separation. The filter assembly 701e is in end-to-end contact with the inner port of the liquid phase outlet 701d and is communicated with the filtrate output line 704 through the liquid phase outlet 701d, so that the liquid phase filtered by the filter assembly 701e can be discharged from the liquid phase outlet 701d and discharged through the filtrate output line 704.
It should be noted here that: the filter assembly 701e of the present invention includes a filter media 701e-1 and a header 701 e-2. The liquid collecting pipes 701e-2 are directly butted with the inner opening ends of the liquid phase outlets 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 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, considering that the temperature of the filtering device 701 may rise during operation, 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 of the filtration stroke of the filter apparatus 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 crystallization 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 liquid 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, enabling 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 the positive blowing process); third, 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, air can be blown back from the filtrate collecting line 705 to the filter media 701e-1, so that part of the solid phase attached to the outer surface of the filter media 701e-1 will be blown off by the reverse air flow and fall to the solid phase outlet 701c (this is a back blowing process).
After the above-mentioned one completion process, the solid phase portion in the crystallization mixed solution gradually accumulates and falls on the solid phase outlet 701c, and is finally discharged uniformly. In summary, when the acetone-methanol mixed solvent and the vegetable oil deodorized distillate dissolved therein are injected into the heat dissipating equipment 301, the acetone-methanol mixed solvent enters the inside of the filtering equipment 701 through the raw material liquid input pipeline 703 after being cooled and crystallized by the heat dissipating equipment 301, the solid phase obtained by filtering by the filtering equipment 701 is discharged from the solid phase outlet 701c, and the obtained liquid phase is discharged from the liquid phase outlet 701 d.
Further, in order to avoid waste of resources and ensure the purity of the filtration, a liquid return pipe set 706 may be provided, and the liquid return pipe set 706 includes a first liquid return pipe 706a and a second liquid return 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 element 701e still contains a part of solid phase, the return liquid can be collected again by the return liquid pipe set 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 gas source flow path 702a and the third gas 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 gas 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 collecting pipeline 705 can be selectively opened or not opened according to the situation (the filtrate collecting pipeline 705 is closed when the filtering effect is poor, and the filtrate collecting pipeline 705 is opened when the filtering effect is good);
when the back flushing process is required, the stop valves of the first gas source flow path 702a and the third gas source flow path 702c may be closed, the stop valves of 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 of the second gas source flow path 702b and the filtrate output line 704 may be opened.
Example 2
Dissolving 1t soybean oil deodorized distillate into 6000L 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 24 hr, filtering, centrifuging filtrate, washing, and oven drying to obtain deodorized distillate without sterol, centrifuging at 7000rpm for 35 min;
distilling the deodorized distillate without sterol at distillation temperature of 230 deg.C, feeding temperature of 80 deg.C and rotation speed of 120r/min to obtain distillate and residue liquid respectively; and carrying out multi-stage steam stripping on the distillate, and then evaporating the solvent to obtain the vitamin E product.
The vitamin E product content of example 2 was found to be 51.4%, the recovery was 82.3%, and the residual capacity was 82 ppm.
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 3
Dissolving 1t corn oil deodorized distillate in 5500L acetone-methanol mixed solvent (the volume ratio of acetone to methanol is 2:1), controlling the temperature to 40 ℃, then slowly cooling to-5 ℃ within 6h, keeping for 20h, then filtering, taking filtrate, centrifugally washing and drying to obtain sterol-removed deodorized distillate, and 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 carrying out multi-stage steam stripping on the distillate, and then evaporating the solvent to obtain the vitamin E product.
The vitamin E product content of example 3 was found to be 50.3%, the recovery was 84.1%, and the residual capacity was 83 ppm.
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 corn oil deodorized distillate in 5500L acetone-methanol mixed solvent (volume ratio of acetone to methanol is 1.5:1), controlling temperature at 35 deg.C, slowly cooling to-5 deg.C within 4 hr, maintaining for 20 hr, filtering, centrifuging, washing, and oven drying to obtain deodorized distillate with sterol removed, centrifuging at 6000rpm for 30 min;
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 carrying out multi-stage steam stripping on the distillate, and then evaporating the solvent to obtain the vitamin E product.
It was determined that the vitamin E product of example 4 was 51.1% in yield 84.2% and 77ppm residual capacity.
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.
It is worth mentioning that in the experiment, the invention of 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 sterol is ensured, the purity of vitamin E extraction is further improved, and simultaneously, the invention can help the steam stripping link to remove the solvent residue of fatty acid.
Therefore, the method for multistage stripping of the vitamin E by-product fatty acid solvent with low residue provided by the invention has the advantages of extremely low residue capacity, low labor intensity, low environmental pollution, easy reaction control, and high purity and recovery rate of the vitamin E.
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 has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on 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 (7)
1. A method for multi-stage steam stripping of vitamin E by-product fatty acid solvent with low residue is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
dissolving the deodorized distillate of the vegetable oil in an acetone-methanol mixed solvent, carrying out low-temperature crystallization treatment, controlling the temperature to be 30-40 ℃, then slowly cooling to-5 ℃ within 4-6 h, keeping the temperature for 20-24 h, filtering, centrifuging, washing and drying the filtrate to obtain deodorized distillate with sterol removed;
distilling the deodorized distillate without sterol to respectively obtain distillate and residual liquid; carrying out multi-stage steam stripping on the distillate, and evaporating the solvent to obtain a vitamin E product;
the low temperature crystallization treatment is completed by 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 exchanger comprises a first heat exchange unit (200) and a second heat exchange unit (200), wherein the first heat exchange unit (200) 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 the number of the first and second groups,
a steam absorption unit (400) comprising an absorption apparatus (401), and the absorption apparatus (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 pipeline (205) is located inside the heat sink (201), and the heat absorption pipeline (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 each pipeline is connected to the flow dividing equipment (103), and the other end of each pipeline is connected to the inside of the absorption equipment (401);
the acetone-methanol mixed solvent and the plant oil deodorized distillate dissolved in the acetone-methanol mixed solvent are injected into the heat dissipation equipment (301) together, the acetone-methanol mixed solvent enters the interior of the filtering equipment (701) through a raw material liquid input pipeline (703) after being crystallized at low temperature of the heat dissipation equipment (301), a solid phase obtained by filtering through the filtering equipment (701) is discharged from a solid phase outlet (701 c), and an obtained liquid phase is discharged from a liquid phase outlet (701 d).
2. The vitamin E by-product fatty acid solvent low residue multi-stage stripping process of claim 1, wherein: the distillation is carried out 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.
3. The vitamin E by-product fatty acid solvent low residue multi-stage stripping process of claim 1, wherein: the centrifugation is carried out for 30-40 min at 5000-7000 rpm.
4. The vitamin E by-product fatty acid solvent low residue multi-stage stripping process of claim 1, wherein: the vegetable oil deodorized distillate comprises corn oil deodorized distillate or soybean oil deodorized distillate.
5. The vitamin E by-product fatty acid solvent low residue multi-stage stripping process of claim 1, 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.
6. The vitamin E by-product fatty acid solvent low residue multi-stage stripping process of claim 1, wherein: the crystallization-filtration combination system further comprises a crystallization-filtration unit,
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 (701 a), a first compressed air inlet (701 b), a solid phase outlet (701 c) 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 is connected with the raw material liquid inlet (701 a), and the raw material liquid input pipeline can transmit the crystallization mixed solution from the interior of the heat dissipation device (301) to the interior of the filtering device (701); the filtrate outlet line (704) is connected to the liquid phase outlet (701 d) and is capable of discharging the filtrate from the inside of the filtration apparatus (701) from the liquid phase outlet (701 d).
7. The vitamin E by-product fatty acid solvent low residue multi-stage stripping process of claim 6, wherein: a filtering component (701 e) is arranged inside the filtering device (701), the filtering component (701 e) is in butt joint with the inner opening end of the liquid phase outlet (701 d), 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 (701 d) one by one and are at least provided with one group, and the outer ends of the filtrate output pipelines (704) are all connected to a filtrate collecting pipeline (705) in a centralized manner;
the air source channel (702) comprises a first air source flow path (702 a), a second air source flow path (702 b) and a third air source flow path (702 c), the first air source flow path (702 a) is connected to the first compressed air inlet (701 b), the second air source flow path (702 b) is connected to the filtrate collecting pipeline (705), and the third air source flow path (702 c) is connected to the inside of the heat dissipation device (301); the air supply passage (702) is externally connected to an air supply and provides compressed air to the first air supply flow path (702 a), the second air supply flow path (702 b), and the third air supply flow path (702 c).
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Denomination of invention: The Method and System of Multistage Stripping with Low Residue of Fatty Acid Solvent as the By product of Vitamin E Effective date of registration: 20221201 Granted publication date: 20210316 Pledgee: Jiangsu Taixing Rural Commercial Bank Co.,Ltd. Suzhong Sub branch Pledgor: JIANGSU CONAT BIOLOGICAL PRODUCTS Co.,Ltd. Registration number: Y2022980024522 |
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