CN108912089A - A kind of method and its crystallization filtering association system of 50VE and sterol centrifuge separation - Google Patents
A kind of method and its crystallization filtering association system of 50VE and sterol centrifuge separation Download PDFInfo
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- CN108912089A CN108912089A CN201810646332.5A CN201810646332A CN108912089A CN 108912089 A CN108912089 A CN 108912089A CN 201810646332 A CN201810646332 A CN 201810646332A CN 108912089 A CN108912089 A CN 108912089A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- 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
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/70—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with two hydrocarbon radicals attached in position 2 and elements other than carbon and hydrogen in position 6
- C07D311/72—3,4-Dihydro derivatives having in position 2 at least one methyl radical and in position 6 one oxygen atom, e.g. tocopherols
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Abstract
The method and its crystallization filtering association system being centrifugated the invention discloses a kind of 50VE and sterol, including, plant oil deodorizing distillate is dissolved in acetone-methanol in the mixed solvent, low temperature crystallization, filtering takes filtrate centrifugation, washing, drying, must remove the deodorization distillate of sterol.The method that we invents the 50VE and sterol centrifuge separation of offer, the method that we invents the 50VE and sterol centrifuge separation of offer, labor intensity is low, and environmental pollution is low, is easy to control reaction, and the purity and the rate of recovery of vitamin E are high.
Description
Technical field
The invention belongs to vitamin E preparation technical fields, and in particular to a kind of method of 50VE and sterol centrifuge separation and
It crystallizes filtering association system.
Background technique
Plant oil deodorizing distillate is the mixture of vegetable oil obtained each fraction in deodorising process.Wherein mainly contain
There are a large amount of free fatty acids, vitamin E, glyceride and other components etc..
Vitamin E is a kind of liposoluble vitamin, and it is one of most important antioxidant that hydrolysate, which is tocopherol,.
It is dissolved in the organic solvents such as fat and ethyl alcohol, it is not soluble in water, heat, acid are stablized, it is unstable to alkali, it is sensitive to oxygen, it is unwise to heat
Sense, but Vitamin E activity is substantially reduced when frying.Tocopherol can promote sex hormone to secrete, and increase man's sperm motility and quantity
Add；Increase woman's female hormone concentration, improve fecundity, prevention of miscarriage, it may also be used for prevention and treatment male sterility, burn,
Frostbite, capillary hemorrhage, climacteric syndrome, beauty etc..Recently it has also been found that vitamin E can inhibit in ocular lens body
Lipid peroxidation reaction, make peripheral vasodilation, improve blood circulation, pre- Anti-myopic eye occurrence and development.On vitamin E phenyl ring
Phenolic hydroxyl group be acetylation, it is tocopherol that ester hydrolysis, which is after phenolic hydroxyl group,.
The process unit operation of domestic production vitamin E is more, and large labor intensity, environmental pollution is serious, and reaction controlling is tired
The purity of difficulty, the rate of recovery and vitamin E is not high.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
The technological gap in method being centrifugated in view of above-mentioned and/or existing 50VE and sterol, proposes the present invention.
Therefore, the one of purpose of the present invention is to solve deficiency in the prior art, provide a kind of 50VE and sterol from
The method of heart separation.
In order to solve the above technical problems, the present invention provides following technical solutions：A kind of 50VE and sterol centrifuge separation
Method, including, plant oil deodorizing distillate is dissolved in acetone-methanol in the mixed solvent, low temperature crystallization, filtering, take filtrate from
The heart, washing, drying must remove the deodorization distillate of sterol；The deodorization distillate of the removal sterol is distilled, respectively
To distillate and residual solution；The distillate is boiled off into solvent, obtains vitamin E product.
As a kind of preferred embodiment for the method that 50VE of the present invention and sterol are centrifugated, wherein：The distillation,
Condition be 220~230 DEG C of vapo(u)rizing temperature, 80~90 DEG C of feeding temperature, 120~180r/min of revolving speed.
As a kind of preferred embodiment for the method that 50VE of the present invention and sterol are centrifugated, wherein：The centrifugation,
It is 30~40min of centrifugation at 5000~7000rpm.
As a kind of preferred embodiment for the method that 50VE of the present invention and sterol are centrifugated, wherein：The vegetable oil
Deodorization distillate includes corn oil deodorization distillate or soybean oil deodorizer distillate.
As a kind of preferred embodiment for the method that 50VE of the present invention and sterol are centrifugated, wherein：The low temperature knot
It is 30~40 DEG C that crystalline substance, which is by temperature control, then extremely -5 DEG C of slow cooling in 4~6h, and holding 20~for 24 hours.
As a kind of preferred embodiment for the method that 50VE of the present invention and sterol are centrifugated, wherein：Acetone-the first
The volume ratio of alcohol in the mixed solvent acetone and methanol is 1~2:1, the dosage of the mixed solvent is that 5~6ml/g is vegetable oil deodorized
Distillate.
Another object of the present invention is to solve deficiency in the prior art, provides a kind of crystallization filtering association system,
It is able to carry out refrigeration, crystallization and filtering.
In order to solve the above technical problems, the present invention provides following technical solutions：Association system is filtered in a kind of crystallization,
It includes：Steam powered units, the steam powered units include evaporation equipment, steam conveying pipeline and shunting device, described
Shunting device is connect by the steam conveying pipeline with the evaporation equipment；First heat exchange unit comprising heat sink, institute
It states heat sink and passes through the first transfer pipeline and the first liquid back pipe road respectively and be attached with cooling equipment, form circulation loop；
Second heat exchange unit comprising heat dissipation equipment, the heat dissipation equipment respectively with first heat exchange unit and vapor absorption list
Member is attached；And vapor absorption unit comprising absorption equipment, and the absorption equipment passes through first circulation pipe respectively
Road and second circulation pipeline are attached with the steam powered units；The inside of the absorption equipment is additionally provided with cold water pipe,
The both ends of the cold water pipe are pierced by the absorption equipment, and external second transfer pipeline and the second liquid back pipe road respectively；Described
Cooling equipment described in two transfer pipelines and the second liquid back pipe Lu Junyu is attached；The shunting device, the first heat exchange unit,
It passes sequentially through supply unit between two heat exchange units and vapor absorption unit to be attached, the supply unit includes first defeated
Send pipeline, the second transfer pipeline and third transfer pipeline；By described between the shunting device and first heat exchange unit
First transfer pipeline is attached, between first heat exchange unit and the second heat exchange unit by second transfer pipeline into
Row connection, is attached between second heat exchange unit and vapor absorption unit by the third transfer pipeline；And it is described
Throttle device is provided on second transfer pipeline；The junction of first transfer pipeline and the second transfer pipeline has heat-dissipating pipe
The junction of road, second transfer pipeline and third transfer pipeline has heat absorption pipeline；The heat dissipation pipeline is located at the suction
Inside hot equipment, the heat absorption pipeline is located inside the heat dissipation equipment；The supply unit is at least provided with two groups, and each pipe
Road is arranged side by side, and one section is connected to the shunting device, and the other end is connected to inside the absorption equipment.
As a kind of preferred embodiment of crystallization filtering association system of the present invention, wherein：The crystallization filtering joint system
System further includes filter element, including filter plant, air supply channel, material liquid intake line and filtrate output tube road, the filtering
Material liquid import, the first compressed air inlet, solid-phase outlet and liquid-phase outlet are provided in equipment；The material liquid intake line
One end connect with the heat dissipation equipment, the other end is connect with the material liquid import, can will come from the heat dissipation equipment
Internal crystallized mixed solution is transmitted to the inside of the filter plant；The filtrate output tube road and the liquid-phase outlet connect
It connects, the filtrate in the filter plant can be discharged from the liquid-phase outlet.
As a kind of preferred embodiment of crystallization filtering association system of the present invention, wherein：The inside of the filter plant
Filter assemblies are provided with, the filter assemblies are docked with the internal orifice end of the liquid-phase outlet, and pass through the liquid-phase outlet and institute
It states filtrate output tube road and forms connection；The filtrate output tube road and the liquid-phase outlet correspond, and at least provided with one
Group, the outer end on the filtrate output tube road, which is concentrated, is connected to filtrate manifold trunk road；The air supply channel includes the first gas source
Flow path, the second gas source flow path and third gas source flow path, the first gas source flow path are connected to first compressed air inlet, institute
It states the second gas source flow path and is connected to the filtrate manifold trunk road, the third gas source flow path is connected in the heat dissipation equipment
Portion；The air supply channel external gas source, and pressure is provided to the first gas source flow path, the second gas source flow path and third gas source flow path
Contracting air.
As a kind of preferred embodiment of crystallization filtering association system of the present invention, wherein：The acetone-methanol is mixed
It solvent and is dissolved in the co-implanted heat dissipation equipment of the plant oil deodorizing distillate therein, is set by the heat dissipation
Entered inside the filter plant by the material liquid intake line again after standby low temperature crystallization, by the filter plant
It filters resulting solid phase to be discharged from the solid-phase outlet, resulting liquid phase is discharged from the liquid-phase outlet.
Beneficial effect possessed by the present invention：
We invents the 50VE of offer and the method for sterol centrifuge separation and its crystallization filtering association system, so that labour is strong
Spend low, environmental pollution is low, is easy to control reaction, and the purity and the rate of recovery of vitamin E are high.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without any creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein：
Fig. 1 is the total system distribution schematic diagram in the 1st~4 embodiment of the invention.
Fig. 2 is the refrigeration system work flow diagram in the 1st~4 embodiment of the invention.
Fig. 3 is the filter element system distribution schematic diagram in the 1st~4 embodiment of the invention.
Fig. 4 is the filter plant structural schematic diagram in the 1st~4 embodiment of the invention.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right combined with specific embodiments below
A specific embodiment of the invention is described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
The present embodiment provides the one of embodiments for a kind of method that 50VE and sterol are centrifugated comprising：
1t corn oil deodorization distillate is dissolved in the 6000L acetone-methanol in the mixed solvent (volume ratio of acetone and methanol
It is 2:1), and this mixed solution is injected and carries out low temperature crystallization processing in the heat dissipation equipment 301 of the second heat exchange unit 300.Herein
During low temperature crystallization, it is 35 DEG C that the present invention, which needs to control the initial temperature in heat dissipation equipment 301, is then slowly dropped in 4h
Temperature is kept to -5 DEG C for 24 hours, to obtain crystallized mixed solution.Then the crystallized mixed solution in heat dissipation equipment 301 is transmitted to
Be filtered in filter element 700, take filtrate centrifuge washing to dry, must remove the deodorization distillate of sterol, centrifugation be
30min is centrifuged under 5000rpm.
It is 220 DEG C that the deodorization distillate of sterol, which will be removed, in vapo(u)rizing temperature, and feeding temperature is 80 DEG C, revolving speed 180r/min
Under conditions of distilled, respectively obtain distillate and residual solution；The distillate is boiled off into solvent, obtains vitamin E product.
The content for measuring vitamin E product in embodiment 1 is 49.9%, the rate of recovery 81.2%.
It should be noted that：" method of 50VE and sterol centrifuge separation " in the above process passes through crystallization filtering joint system
System is completed, and as shown in figures 1-4, the crystallization filtering association system includes：Steam powered units 100, the first heat exchange unit
200, the second heat exchange unit 300, vapor absorption unit 400, supply unit 500, throttle device 600 and filter element 700 etc..
Wherein, steam powered units 100, the first heat exchange unit 200, the second heat exchange unit 300, vapor absorption unit 400,
Supply unit 500 and throttle device 600 realize above-mentioned " crystallisation by cooling " process jointly, therefore the present invention can be by " steam
Power unit 100, the first heat exchange unit 200, the second heat exchange unit 300, vapor absorption unit 400, supply unit 500 and section
The topical functional system that flow device 600 " is constituted is defined as " refrigeration system ".It can be directly as refrigeration in " refrigeration system "
The end-equipment of container is 301 cooling refrigeration of heat dissipation equipment in the second heat exchange unit 300.In addition, the filtering list in the present invention
Member 700 is a set of " filtration system " for enabling to be separated by solid-liquid separation.
Based on above-mentioned, specifically：
Steam powered units 100 include evaporation equipment 101, steam conveying pipeline 102 and shunting device 103, shunting device
103 are connect by steam conveying pipeline 102 with evaporation equipment 101；First heat exchange unit 200 includes heat sink 201, and heat absorption is set
Standby 201 are attached by the first transfer pipeline 202 and the first liquid back pipe road 203 with cooling equipment 204 respectively, and formation is recycled back to
Road；Second heat exchange unit 300 includes heat dissipation equipment 301, and heat dissipation equipment 301 is inhaled with the first heat exchange unit 200 and steam respectively
Unit 400 is received to be attached；And vapor absorption unit 400 includes absorption equipment 401, and absorption equipment 401 is respectively by the
One circulation line 402 and second circulation pipeline 403 are attached with steam powered units 100.
Wherein, steam powered units 100 are for generating and conveying steam.Here " steam " is after refrigerant heats are evaporated
Steam, in the present invention, evaporation equipment 101 can use boiler or steam generator, internal to contain that there are two types of boiling points not
Same mixed solution, respectively refrigerant and absorbent, the two can dissolve each other, and the boiling point of refrigerant is lower than absorbent.And it steams
Hair equipment 101 is for heating and discharging refrigerant, to form the steam of high temperature and pressure, steam-out (SO) transfer pipeline 102, steam
The end of transfer pipeline 102 is connected to shunting device 103, and shunting device 103 is used for the steam for transmitting steam conveying pipeline 102
Branch is carried out, is distributed in the multiple groups bypass line of supply unit 500.
First heat exchange unit 200 is for absorbing the heat from supply unit 500, so that after the steam heat release of high temperature and pressure
Form the liquid condition of cryogenic high pressure.Wherein, heat sink 201 is the container that inside fills cold water, can pass through cold water pair
Steam carries out absorbing and cooling temperature.
Second heat exchange unit 300 is used for cooling refrigeration, is set to the first heat exchange unit 200 and vapor absorption unit 400
Between, it is rapidly swollen after decompression of the liquid refrigerant of the cryogenic high pressure from the first heat exchange unit 200 Jing Guo throttle device 600
Swollen vaporization, and the amount of heat in heat dissipation equipment 301 is absorbed, realize the purpose of cooling refrigeration.Throttle device 600 in the present invention
Throttle valve can be used.
Vapor absorption unit 400 is used for refrigerant-recovery and circularly cooling, and absorption equipment 401 passes through first circulation pipeline
402 and second circulation pipeline 403 be attached with steam powered units 100.Wherein, first circulation pipeline 402 is evaporation equipment
Connecting pipe between 101 bottom and absorption equipment 401, the solution in evaporation equipment 101 are defeated by first circulation pipeline 402
It send to absorption equipment 401, for absorbing the refrigerant of vaporization.Meanwhile second circulation pipeline 403 will be in absorption equipment 401
Solution be recycled in evaporation equipment 101 again, conveying power is carried out real by the pump 403a on second circulation pipeline 403
It is existing.
Further, shunting device 103, the first heat exchange unit 200, the second heat exchange unit 300 and vapor absorption unit
It passes sequentially through supply unit 500 between 400 to be attached, supply unit 500 includes the first transfer pipeline 501, the second delivery pipe
Road 502 and third transfer pipeline 503.Wherein, pass through the first transfer pipeline between shunting device 103 and the first heat exchange unit 200
501 are attached, and are attached between the first heat exchange unit 200 and the second heat exchange unit 300 by the second transfer pipeline 502,
It is attached between second heat exchange unit 300 and vapor absorption unit 400 by third transfer pipeline 503, and the second delivery pipe
Throttle device 600 is provided on road 502.
Further, the junction of the first transfer pipeline 501 and the second transfer pipeline 502 has heat dissipation pipeline 205, tool
There is condenser.The junction of second transfer pipeline 502 and third transfer pipeline 503 has heat absorption pipeline 302, has
The effect of evaporator.Heat dissipation pipeline 205 is located at the inside of heat sink 201, and heat absorption pipeline 302 is located at the interior of heat dissipation equipment 301
Portion.
In addition, in the present invention, heat sink 201 respectively by the first transfer pipeline 202 and the first liquid back pipe road 203 with
Cooling equipment 204 is attached, and forms circulation loop.It can be seen from the above, filling water inside heat sink 201, and heat sink
There are inlet and outlet on 201 tube wall.Its water outlet is docked with the first transfer pipeline 202, the first transfer pipeline
202 other end extends to the top of cooling equipment 204.It is provided with infusion pump on first transfer pipeline 202, and passes through infusion pump
Heat-absorption water in heat sink 201 is delivered to cooling equipment 204.Preferably, the end head of the first transfer pipeline 202 is provided with
Spray head is more advantageous to fast cooling cooling, finally cooling water mist falls into cooling equipment so that water is atomized from spray head
It in 204, and is flowed back into heat sink 201 by the first liquid back pipe road 203 via the water inlet of heat sink 201, formation follows
Loop back path.Cooling equipment 204 in the present invention is cooling tower.
Same, the inside of absorption equipment 401 is additionally provided with cold water pipe, and the both ends of cold water pipe are pierced by absorption equipment
401, external second transfer pipeline 404 and the second liquid back pipe road 405, and the second transfer pipeline 404 and the second liquid back pipe road respectively
405 are attached with (another) cooling equipment 204.Wherein, in one end of the second transfer pipeline 404 and absorption equipment 401
Cold water pipe connection, the other end extends to the top of (another) cooling equipment 204.It is provided on second transfer pipeline 404 defeated
Liquid pump, and the heat-absorption water in absorption equipment 401 is delivered in (another) cooling equipment 204 by infusion pump.Preferably, the
The end head of two transfer pipelines 404 is provided with spray head, so that water is atomized from spray head, is more advantageous to fast cooling cooling,
Finally cooling water mist is fallen into cooling equipment 204, and is flowed back into absorption equipment 401 by the second liquid back pipe road 405.
In the present invention, the workflow of the refrigeration system is as follows：
Firstly, evaporation equipment 101 heats the mixed solution of its inside, due to boiling point difference, mid-boiling point is lower
Refrigerant directly evaporate, be vaporized into the steam of high temperature and pressure, and enter from steam conveying pipeline 102 by shunting device 103
In first transfer pipeline 501.At the same time, also with another process, i.e.,：Due to the vaporization of refrigerant, evaporation equipment 101
The solution concentration of middle absorbent is higher and higher, and enters in absorption equipment 401 from first circulation pipeline 402.
The high temperature and high pressure steam entered in the first transfer pipeline 501 is transported in heat dissipation pipeline 205.Due to heat-dissipating pipe
Road 205 is located in the cold water of heat sink 201, therefore cold water absorbs the heat of 205 high temperature high steam of heat dissipation pipeline, so that
Steam cooling liquefaction, forms the liquid refrigerant of cryogenic high pressure.At the same time, since the cold water in heat sink 201 absorbs heat
It will be gradually warmed up, and the water of heat absorption heating can be introduced into cooling equipment 204 and cool down by the first transfer pipeline 202, again
Cold-water reflux is participated in into work into heat sink 201 by the first liquid back pipe road 203, forms circulation.
Refrigerant after cooled liquefaction is absorbed heat pipeline 302 by the second transfer pipeline 502 flow direction heat absorption pipeline 302
In heat dissipation equipment 301.Due to being provided with throttle device 600 on the second transfer pipeline 502, so that the liquid refrigeration of cryogenic high pressure
Agent expands rapidly after throttle device 600 is depressured and enters absorbing pipe road 302, and vaporization heat absorption forms Low Temperature Steam.By
It is located in heat dissipation equipment 301 in heat absorption pipeline 302, so that the environment temperature considerable decrease in heat dissipation equipment 301, to reach system
Cold purpose.
Finally, Low Temperature Steam from heat absorption pipeline 302 enter third transfer pipeline 503, and by third transfer pipeline 503 into
Enter in absorption equipment 401, the absorbent solution being exhausted into absorption equipment 401 is absorbed.At this point, in absorption equipment 401
Absorbent solution solubility reduces, and is transported to inside evaporation equipment 101 by the pump 403a on second circulation pipeline 403, realizes
The recycling of refrigerant and absorbent.In the process, the temperature in absorption equipment 401 passes through 404 He of the second transfer pipeline
The circulation loop on the second liquid back pipe road 405 cools down.
In the present invention, supply unit 500 can be at least provided with two groups of (specifications and corresponding attached drawing of the invention
In be temporarily illustrated with three groups of pipelines, but do not influence protection scope of the present invention), by shunting device 103 carry out branch biography
It is defeated, and each pipeline is arranged side by side, one section is connected to the shunting device 103, and the other end is connected to the absorption equipment 401
It is internal.
Specifically, can be set to the road A, the road the B road C if tri- tunnel 500 Fen Wei of supply unit, three tunnel pipeline specifications are identical, and
It is arranged side by side.It, can uniform, highly effective refrigeration in heat dissipation equipment 301 when three road pipelines are all opened.If only opening any one
Road, when closing the valve of other two-way, in pipeline steam pressure increase, the pressure reducing valve opened on the way adjustable at this time into
Row reduced pressure treatment, to control the refrigeration effect and refrigeration space in heat dissipation equipment 301.Therefore, in the present invention, user can be with
Pipeline is arbitrarily opened according to actual needs, and is adjusted corresponding pressure reducing valve and carried out the effect of control refrigeration, and adjusting is cooperated to steam
(its temperature value can be by being set to heat dissipation equipment to control the temperature in heat dissipation equipment 301 for the evaporation efficiency of hair equipment 101
Thermometer on 301 is monitored).
Crystallization filtering association system in further include one important " filtration system " be filter element 700, also can be right
Solution after crystallization is separated by solid-liquid separation.In the present invention, filter element 700, including filter plant 701, air supply channel 702,
Material liquid intake line 703 and filtrate output tube road 704.Filter plant 701 therein is for being filtered processing；Air supply channel
702 apply pressure for extraneous, promote being normally carried out for filtering；Material liquid intake line 703 is the input pipe of feed liquid to be separated
Road；Filtrate output tube road 704 is the liquid phase output channel after being separated by solid-liquid separation.
Wherein, material liquid import 701a, the first compressed air inlet 701b, solid-phase outlet are provided on filter plant 701
701c and liquid-phase outlet 701d.Since filter element 700 receives the crystallized mixed solution in heat dissipation equipment 301, phase
It answers：There is the first charging interface 301a, the second charging interface 301b, the second compressed air inlet 301c on heat dissipation equipment 301
With the first discharging interface 301d.
One end of material liquid intake line 703 is connect with the first discharging interface 301d of heat dissipation equipment 301, the other end and original
Crystallized mixed solution inside heat dissipation equipment 301 can be transmitted to filter plant 701 by liquor inlet 701a connection
It is internal.
Filtrate output tube road 704 is connect with liquid-phase outlet 701d, can filtrate in inherent filtration in future equipment 701 from liquid phase
Export 701d discharge.Specifically, filter plant 701 is internally provided with filter assemblies 701e, it is used to directly carry out solid-liquid point
From.Filter assemblies 701e is docked with the internal orifice end of liquid-phase outlet 701d, and passes through liquid-phase outlet 701d and filtrate output tube road 704
Connection is formed, therefore, the liquid phase filtered by filter assemblies 701e can be discharged from liquid-phase outlet 701d, and export by filtrate
Pipeline 704 is discharged.
Herein it should be noted that：Filter assemblies 701e in the present invention includes filter medium 701e-1 and collector tube
701e-2.Collector tube 701e-2 is directly docked with the internal orifice end of liquid-phase outlet 701d, is formed and is connected to, on every collector tube 701e-2
It can be connected with multiple filter medium 701e-1 simultaneously, the filtrate that each filter medium is obtained by filtration is pooled to collector tube
On 701e-2.In addition, it can be seen from the above, every collector tube 701e-2 and liquid-phase outlet 701d, 704 three one of filtrate output tube road
One is corresponding, and at least provided with one group (settable multiple groups), is connected in the equal Unified Set in the outer end on each filtrate output tube road 704
Filtrate is collected on pipeline 705.
In addition, it is contemplated that filter plant 701 is in the process of work, it is understood that there may be temperature recovery causes crystallized analysis
Solid phase out is again dissolved in the situation in solution, therefore collet, the two sides point of collet can be set in the periphery of filter plant 701
It is not provided with cold water water inlet interface 701f and the external cold water inlet of cold water water outlet mouthpiece 701g, cold water water inlet interface 701f
701f-1, and it is passed through into collet the cold water for cooling.And the external cold water outlet pipe 701g-1 of cold water water outlet mouthpiece 701g, it uses
In above-mentioned the be passed through cold water of discharge.Therefore, the cold water cooling effect of cold water inlet 701f-1 and cold water outlet pipe 701g-1
It can guarantee that the crystallization being precipitated will not be again dissolved in solution.
The filter run power resources of filter plant 701 are in air supply channel 702.Air supply channel 702 includes the first gas source stream
Road 702a, the second gas source flow path 702b and third gas source flow path 702c, wherein the first gas source flow path 702a is connected to the first compression
Air intlet 701b, the second gas source flow path 702b are connected to filtrate and collect on pipeline 705, and third gas source flow path 702c is connected to
On two compressed air inlet 301c, and it is communicated to inside heat dissipation equipment 301.702 external gas source processor of air supply channel, and to
One gas source flow path 702a, the second gas source flow path 702b and third gas source flow path 702c provide compressed air.
Therefore, the course of work of filter plant 701 includes following three step：One, third gas source flow path 702c is opened, to heat dissipation
Be passed through air inside equipment 301, due to the effect of air pressure so that the crystallized mixed solution inside heat dissipation equipment 301 be extruded and
The first discharging of discharge interface 301d, entering 701 inside of filter plant from material liquid import 701a, (this fill process can also pass through
Infusion pump is realized)；Two, open the first gas source flow path 702a, to filter plant 701 inside be passed through air so that filter plant 701
Interior air pressure enhancing, liquid phase part compression enter in collector tube 701e-2 from filter medium 701e-1, complete filtering, and finally from
Filtrate output tube road 704 is discharged to filtrate and collects in pipeline 705 (this, which is positive, blows over journey)；Three, third gas source flow path 702c is closed
With the first gas source flow path 702a, and the second gas source flow path 702b is opened, air can be collected into pipeline 705 from filtrate and reversely blown to
Filter medium 701e-1, thus the solid phase being partially attached on the outer surface filter medium 701e-1 can also be reversed air-flow and blow off,
Fall to solid-phase outlet 701c (this is blowback process).
After an above-mentioned complete process, the solid fraction in crystallized mixed solution, which can be built up, falls within solid phase
701c is exported, discharge is finally unified.To sum up, when acetone-methanol mixed solvent and being dissolved in therein vegetable oil deodorized evaporate
Out in the co-implanted heat dissipation equipment 301 of object, pass through material liquid intake line 703 after the crystallisation by cooling of heat dissipation equipment 301
Into inside filter plant 701, resulting solid phase is filtered by filter plant 701 and is discharged from solid-phase outlet 701c, resulting liquid
Mutually it is discharged from liquid-phase outlet 701d.
Further, to avoid the wasting of resources, guarantee the purity of filtering, liquid back pipe group 706, the liquid back pipe can be set
Group 706 includes the first liquid back pipe 706a and the second liquid back pipe 706b.Wherein, one end of the first liquid back pipe 706a is connected to filtering and sets
On standby 701 liquid return hole 701h (overflow channel of 701 lower end of filter plant setting), the other end is connected to the second charging interface
On 301b；One end of second liquid back pipe 706b is connected to filtrate and collects on pipeline 705, and the other end is together with the first liquid back pipe 706a
It is connected on the second charging interface 301b.It therefore, include that part is solid when being used only in the filtrate that filter assemblies 701e is obtained still
Xiang Shi can carry out back liquid by liquid back pipe group 706 and collect again, filter, move in circles again.
Such as Fig. 3,4, it should be noted that：When needing just to be blown over journey, the first gas source flow path 702a, the can be opened
Shut-off valve on three gas source flow path 702c opens simultaneously material liquid intake line 703, filtrate output tube road 704 and filtrate and collects
Shut-off valve on pipeline 705, and close the shut-off valve in the second gas source flow path 702b and liquid back pipe group 706；
When carrying out back liquid and collecting again, can open on the first gas source flow path 702a, third gas source flow path 702c
Shut-off valve, open simultaneously the shut-off valve in material liquid intake line 703, filtrate output tube road 704 and liquid back pipe group 706, and
Close the shut-off valve on the second gas source flow path 702b, wherein filtrate, which collects the shut-off valve on pipeline 705, according to circumstances to be selected
Open or do not open (when poor filtration effect close filtrate collect pipeline 705, filter effect it is good when open filtrate collect pipeline
705)；
When needing to carry out blowback process, cutting on the first gas source flow path 702a, third gas source flow path 702c can be closed
Only valve, simultaneously closes off material liquid intake line 703, filtrate collects pipeline 705, the shut-off valve in liquid back pipe group 706, and opens the
Shut-off valve on two gas source flow path 702b and filtrate output tube road 704.
Embodiment 2
1t corn oil deodorization distillate is dissolved in the 5000L acetone-methanol in the mixed solvent (volume ratio of acetone and methanol
It is 1.5:1) it is 40 DEG C that, temperature, which is controlled, then extremely -5 DEG C of slow cooling in 6h, and keeps 22h to carry out at low temperature crystallization
Reason, is then filtered, and is taken filtrate centrifuge washing to dry, must be removed the deodorization distillate of sterol, centrifugation is centrifuged at 7000rpm
30min；
It is 220 DEG C that the deodorization distillate of sterol, which will be removed, in vapo(u)rizing temperature, and feeding temperature is 90 DEG C, revolving speed 150r/min
Under conditions of distilled, respectively obtain distillate and residual solution；The distillate is boiled off into solvent, obtains vitamin E product.
The content for measuring vitamin E product in embodiment 2 is 51.2%, the rate of recovery 82.6%.
" low temperature crystallization " and " filtering " in the present embodiment above process is using the filtering joint of crystallization described in embodiment 1
System is realized that the course of work is as shown in figures 1-4.
Embodiment 3
1t soybean oil deodorizer distillate is dissolved in the 5500L acetone-methanol in the mixed solvent (volume ratio of acetone and methanol
It is 2:1) it is 35 DEG C that, temperature, which is controlled, then extremely -5 DEG C of slow cooling in 5h, and keeps 20h to carry out low temperature crystallization processing,
Then it filters, takes filtrate centrifuge washing to dry, the deodorization distillate of sterol must be removed, centrifugation is centrifuged at 6000rpm
35min；
It is 230 DEG C that the deodorization distillate of sterol, which will be removed, in vapo(u)rizing temperature, and feeding temperature is 90 DEG C, revolving speed 160r/min
Under conditions of distilled, respectively obtain distillate and residual solution；The distillate is boiled off into solvent, obtains vitamin E product.
The content for measuring vitamin E product in embodiment 3 is 50.3%, the rate of recovery 84.1%.
" low temperature crystallization " and " filtering " in the present embodiment above process is using the filtering joint of crystallization described in embodiment 1
System is realized that the course of work is as shown in figures 1-4.
Embodiment 4
1t soybean oil deodorizer distillate is dissolved in the 5500L acetone-methanol in the mixed solvent (volume ratio of acetone and methanol
It is 1.5:1) it is 35 DEG C that, temperature, which is controlled, then extremely -5 DEG C of slow cooling in 5h, and keeps 22h to carry out at low temperature crystallization
Reason, is then filtered, and is taken filtrate centrifuge washing to dry, must be removed the deodorization distillate of sterol, centrifugation is centrifuged at 6000rpm
35min；
It is 220 DEG C that the deodorization distillate of sterol, which will be removed, in vapo(u)rizing temperature, and feeding temperature is 90 DEG C, revolving speed 160r/min
Under conditions of distilled, respectively obtain distillate and residual solution；The distillate is boiled off into solvent, obtains vitamin E product.
The content for measuring vitamin E product in embodiment 4 is 51.1%, the rate of recovery 84.2%.
" low temperature crystallization " and " filtering " in the present embodiment above process is using the filtering joint of crystallization described in embodiment 1
System is realized that the course of work is as shown in figures 1-4.
It is noted that our invention is found in an experiment, the operation of holding second-order temperature when low temperature crystallization, i.e.,
(controlling temperature is 30~40 DEG C, then extremely -5 DEG C of slow cooling in 4~6h, and holding 20~for 24 hours), the two temperature controls
The factor of system can generate synergistic effect, guarantee the height removing of sterol, and then improve the purity for extracting vitamin E.
It can be seen that we invents the 50VE of offer and the method for sterol centrifuge separation and its crystallization filtering association system,
Low with labor intensity, environmental pollution is low, is easy to control reaction, the remarkable advantages such as the purity of vitamin E and rate of recovery height.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (10)
1. the method for a kind of 50VE and sterol centrifuge separation, it is characterised in that：Including,
Plant oil deodorizing distillate is dissolved in acetone-methanol in the mixed solvent, low temperature crystallization, filtering takes filtrate centrifugation, washes
It washs, dry, the deodorization distillate of sterol must be removed；
The deodorization distillate of the removal sterol is distilled, distillate and residual solution are respectively obtained；The distillate is steamed
Solvent is removed, vitamin E product is obtained.
2. the method for 50VE and sterol centrifuge separation according to claim 1, it is characterised in that：The distillation, condition are
220~230 DEG C of vapo(u)rizing temperature, 80~90 DEG C of feeding temperature, 120~180r/min of revolving speed.
3. the method for 50VE and sterol centrifuge separation according to claim 1, it is characterised in that：The centrifugation, be
30~40min is centrifuged under 5000~7000rpm.
4. the method for 50VE and sterol centrifuge separation according to claim 1, it is characterised in that：It is described vegetable oil deodorized to distillate
Object includes corn oil deodorization distillate or soybean oil deodorizer distillate.
5. the method for 50VE and sterol centrifuge separation according to claim 1, it is characterised in that：The low temperature crystallization is
It is 30~40 DEG C that temperature, which is controlled, then extremely -5 DEG C of slow cooling in 4~6h, and holding 20~for 24 hours.
6. the method for 50VE and sterol centrifuge separation according to claim 1, it is characterised in that：The acetone-methanol mixing
The volume ratio of acetone and methanol is 1~2 in solvent:1, the dosage of the mixed solvent, which is that 5~6ml/g is vegetable oil deodorized, to be distillated
Object.
7. association system is filtered in a kind of crystallization, it is characterised in that：Including,
Steam powered units (100), the steam powered units (100) include evaporation equipment (101), steam conveying pipeline
(102) and shunting device (103), the shunting device (103) pass through the steam conveying pipeline (102) and the evaporation equipment
(101) it connects；
First heat exchange unit (200) comprising heat sink (201), the heat sink (201) pass through the first delivery pipe respectively
Road (202) and the first liquid back pipe road (203) are attached with cooling equipment (204), form circulation loop；
Second heat exchange unit (300) comprising heat dissipation equipment (301), the heat dissipation equipment (301) exchange heat with described first respectively
Unit (200) and vapor absorption unit (400) are attached；And
Vapor absorption unit (400) comprising absorption equipment (401), and the absorption equipment (401) passes through first circulation respectively
Pipeline (402) and second circulation pipeline (403) are attached with the steam powered units (100)；The absorption equipment (401)
Inside be additionally provided with cold water pipe, the both ends of the cold water pipe are pierced by the absorption equipment (401), and respectively it is external second conveying
Pipeline (404) and the second liquid back pipe road (405)；Second transfer pipeline (404) and the second liquid back pipe road (405) with it is described
Cooling equipment (204) are attached；
The shunting device (103), the first heat exchange unit (200), the second heat exchange unit (300) and vapor absorption unit
(400) it passes sequentially through supply unit (500) between to be attached, the supply unit (500) includes the first transfer pipeline
(501), the second transfer pipeline (502) and third transfer pipeline (503)；
It is carried out between the shunting device (103) and first heat exchange unit (200) by first transfer pipeline (501)
Connection, between first heat exchange unit (200) and the second heat exchange unit (300) pass through second transfer pipeline (502) into
Row connection, passes through the third transfer pipeline (503) between second heat exchange unit (300) and vapor absorption unit (400)
It is attached；And throttle device (600) are provided on second transfer pipeline (502)；
The junction of first transfer pipeline (501) and the second transfer pipeline (502) has heat dissipation pipeline (205), and described the
The junction of two transfer pipelines (502) and third transfer pipeline (503) has heat absorption pipeline (302)；The heat dissipation pipeline (205)
Internal positioned at the heat sink (201), it is internal that the heat absorption pipeline (302) is located at the heat dissipation equipment (301)；
The supply unit (500) is at least provided with two groups, and each pipeline is arranged side by side, and one section is connected to the shunting and sets
Standby (103), it is internal that the other end is connected to the absorption equipment (401).
8. association system is filtered in crystallization according to claim 7, it is characterised in that：Further include,
Filter element (700), including filter plant (701), air supply channel (702), material liquid intake line (703) and filtrate are defeated
Pipeline (704) out, be provided on the filter plant (701) material liquid import (701a), the first compressed air inlet (701b),
Solid-phase outlet (701c) and liquid-phase outlet (701d)；One end of the material liquid intake line (703) and the heat dissipation equipment
(301) it connects, the other end is connect with the material liquid import (701a), and it is internal can will to come from the heat dissipation equipment (301)
Crystallized mixed solution be transmitted to the inside of the filter plant (701)；The filtrate output tube road (704) goes out with the liquid phase
The filtrate in the filter plant (701) can be discharged from the liquid-phase outlet (701d) for mouth (701d) connection.
9. association system is filtered in crystallization according to claim 8, it is characterised in that：The inside of the filter plant (701)
It is provided with filter assemblies (701e), the filter assemblies (701e) are docked with the internal orifice end of the liquid-phase outlet (701d), and are led to
The liquid-phase outlet (701d) is crossed to be connected to the filtrate output tube road (704) formation；The filtrate output tube road (704) and institute
Liquid-phase outlet (701d) one-to-one correspondence is stated, and at least provided with one group, the outer end company of concentration of the filtrate output tube road (704)
Filtrate is connected to collect on pipeline (705)；
The air supply channel (702) includes the first gas source flow path (702a), the second gas source flow path (702b) and third gas source flow path
(702c), the first gas source flow path (702a) are connected to first compressed air inlet (701b), the second gas source stream
Road (702b) is connected to the filtrate and collects on pipeline (705), and the third gas source flow path (702c) is connected to the heat dissipation and sets
Standby (301) are internal；Air supply channel (702) external gas source, and to the first gas source flow path (702a), the second gas source flow path
(702b) and third gas source flow path (702c) provide compressed air.
10. association system is filtered in crystallization according to claim 9, it is characterised in that：By the acetone-methanol mixed solvent
And be dissolved in the co-implanted heat dissipation equipment (301) of the plant oil deodorizing distillate therein, by the heat dissipation
Entered in the filter plant (701) by the material liquid intake line (703) again after the low temperature crystallization of equipment (301)
Portion filters resulting solid phase by the filter plant (701) and is discharged from the solid-phase outlet (701c), and resulting liquid phase is from institute
State liquid-phase outlet (701d) discharge.
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| CN108912089B (en) | 2022-07-15 |
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