CN108912198A - A kind of preparation method and system of high yield wood sterol - Google Patents
A kind of preparation method and system of high yield wood sterol Download PDFInfo
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- CN108912198A CN108912198A CN201810646355.6A CN201810646355A CN108912198A CN 108912198 A CN108912198 A CN 108912198A CN 201810646355 A CN201810646355 A CN 201810646355A CN 108912198 A CN108912198 A CN 108912198A
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- sterol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
Abstract
The invention discloses the preparation methods and system of a kind of high yield wood sterol, including, raw materials recovery, lower layer's solution is taken to keep the temperature 4~6h at 120~160 DEG C, obtain sterol ester admixture, the sterol ester admixture is subjected to short-path distillation, fatty acid and concentration sterol ester is isolated, the concentration sterol ester is mixed with the tall oil pitch.We invents the preparation method and system of the high yield wood sterol of offer, and the wooden sterol yield is high.
Description
Technical field
The invention belongs to phytosterol preparation technical fields, and in particular to a kind of preparation method of high yield wood sterol and be
System.
Background technique
When pine to be sliced to and used sodium hydroxide and vulcanized sodium pressure cooking, wood cell film and intracellular resin acid and
Aliphatic ester in timber is all hydrolyzed to be saponified into sodium salt and soluble in water, and lignin and alkali, which act on, also becomes soluble matter, without
Molten cellulose is separated into paper pulp to get by-product spent pulping liquor is arrived.By spent pulping liquor stratification, lower layer's black liquor mainly contains
Lignin, float on upper layer mainly fatty acid sodium soap and resin acid soda soap, scrape upper layer floating object to get thick Bristol soap (also referred to as
Crude sulfate soap).The active constituent content of thick Bristol soap is too low, contains large quantity of moisture, contains lignin simultaneously, is made with thick Bristol soap
For the raw material for extracting tall oil, thick Carvedilol is soaped and is washed, acidification and essence set layering, and upper layer is crude tall oil, and middle layer is mainly
Lignin, lower layer are the inorganic salts etc. of water, separate upper layer substance and obtain crude tall oil.Tall oil is mainly used for soap, varnish, oil
Paint, ink, lubricant, the oil of intermetallic composite coating, disinfectant or adhesive etc., main component is fatty acid and rosin acid, is belonged to
Mixture.
In the food industry, phytosterol is as an effective component for reducing cholesterol in food additives, safety
Property obtained the approval of American-European multiple countries, in recent years there are also research confirm, phytosterol in addition to do norcholesterol ingredient it
It is also used as food antioxidant outside.The country starts late to phytosterol research, is applied to mainly in medicine and day
With fields such as chemical industry, and the application study in field of food is seldom, and there has been no the functional food of addition phytosterol in the market.
The industrialized production of domestic phytosterol there is product yields very low, difficult solvent recovery, solvent-oil ratio be big,
The too deep disadvantage of sterol preparation color.
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.
In view of the extremely low insurmountable technological gap of yield in the preparation method of above-mentioned and/or existing high yield wood sterol,
Propose the present invention.
Therefore, the one of purpose of the present invention is to solve deficiency in the prior art, provides a kind of high yield wood sterol
Preparation method.
In order to solve the above technical problems, the present invention provides following technical solutions：A kind of preparation side of high yield wood sterol
Method, including, tall oil pitch and caustic soda water according to mass volume ratio are 1g by the preparation of wooden sterol：The ratio of 4~10ml mixes,
After reacting at a certain temperature, aqueous citric acid solution is added and stirs to pH of mixed to neutrality, stands, it is molten that mixed liquor is divided into upper layer
Liquid and lower layer's solution, take the upper solution to be distilled, and obtain sterol concentrate；The sterol concentrate is dissolved in methanol
And/or butanone, it crystallizes, filtering, collection obtains the wooden sterol crude product, obtains the wooden sterol product after melt pelletization；Raw materials recovery,
It takes lower layer's solution to keep the temperature 4~6h at 120~160 DEG C, obtains sterol ester admixture, the sterol ester admixture is carried out
Short-path distillation isolates fatty acid and concentration sterol ester, the concentration sterol ester is mixed with the tall oil pitch.
A kind of preferred embodiment of preparation method as high yield wood sterol of the present invention, wherein：The citric acid water
The mass fraction of solution is 20~25%.
A kind of preferred embodiment of preparation method as high yield wood sterol of the present invention, wherein：The distillation, into
Material rate is 3~4mL/min.
A kind of preferred embodiment of preparation method as high yield wood sterol of the present invention, wherein：The melt pelletization,
Its process temperature is 160~180 DEG C.
A kind of preferred embodiment of preparation method as high yield wood sterol of the present invention, wherein：It is described in certain temperature
The lower reaction of degree, is 3~6h of reaction at 130~160 DEG C.
A kind of preferred embodiment of preparation method as high yield wood sterol of the present invention, wherein：The caustic soda
The mass fraction of NaOH is 12~15% in water.
A kind of preferred embodiment of preparation method as high yield wood sterol of the present invention, wherein：The vapo(u)rizing temperature
It is 85~90 DEG C, preheating temperature is 65~70 DEG C, and condensation temperature is 5~8 DEG C, and vacuum degree is 30~40Pa, knifing rotating speed 300
~350r/min.
Another object of the present invention is to solve deficiency in the prior art, provides a kind of preparation system of high yield wood sterol
System makes product yield height, is easy to solvent recovery.
In order to solve the above technical problems, the present invention provides following technical solutions：A kind of preparation system of high yield wood sterol
System, including, 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.
A kind of preferred embodiment of preparation system as high yield wood sterol of the present invention, wherein：The high yield wood
The preparation system of sterol further includes being stirred to react unit, and the upper end for being stirred to react unit has feed inlet, and lower end is provided with
Discharge port, the external discharging supply pipe road of discharge port, the discharging supply pipe road is connected to standing unit；Stand unit, packet
Include liquid flowing tube, the lower end of the liquid flowing tube protrudes into the inside for standing unit and can adjust height, the liquid flowing tube it is upper
External clear liquid transfer pipeline is held, the clear liquid transfer pipeline is also connected with distillation unit；And filter element, including filter and set
Standby, air supply channel, material liquid intake line and filtrate output tube road are provided with material liquid import, first on the filter plant
Compressed air inlet, solid-phase outlet and liquid-phase outlet；One end of the material liquid intake line is connect with the heat dissipation equipment, separately
One end is connect with the material liquid import, can be transmitted to the crystallized mixed solution inside the heat dissipation equipment described
The inside of filter plant；The filtrate output tube road is connect with the liquid-phase outlet, can will be in the filter plant
Filtrate is discharged from the liquid-phase outlet.
A kind of preferred embodiment of preparation system as high yield wood sterol of the present invention, wherein：The filter plant
Be internally provided with filter assemblies, the filter assemblies are docked with the internal orifice end of the liquid-phase outlet, and are gone out by the liquid phase
Mouth is formed with the filtrate output tube road and is connected to；The filtrate output tube road and the liquid-phase outlet correspond, and at least set
It is equipped 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
One 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
Import, the second gas source flow path are connected to the filtrate manifold trunk road, and the third gas source flow path is connected to the heat dissipation
Inside equipment；The air supply channel external gas source, and to the first gas source flow path, the second gas source flow path and third gas source flow path
Compressed air is provided；The distillation unit distills heat dissipation equipment described in resulting sterol concentrate and organic solvent mixed injection
It is interior, pass through the material liquid intake line after the crystallisation by cooling of the heat dissipation equipment and enters inside the filter plant,
It filters resulting solid phase by the filter plant to be discharged from the solid-phase outlet, resulting liquid phase is arranged from the liquid-phase outlet
Out.
Beneficial effect possessed by the present invention：
We invents the preparation method and system of the high yield wood sterol of offer, so that the wooden sterol yield is high, purity pole
Height, color is bright, and reaction is mild efficient, and the advantage high with low operation temperature, separative efficiency.
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 a kind of one of embodiments of the preparation method of high yield wood sterol comprising：
It according to mass volume ratio is 1g by tall oil pitch and caustic soda water：The ratio of 5ml is anti-from the injection stirring of feed inlet 701
It answers in unit 700, and be thoroughly mixed uniformly by being stirred to react unit 700, adjusts the folder for being stirred to react unit 700
Temperature in covering, so that 22% aqueous citric acid solution is added and stirs to mixed after tall oil pitch and caustic soda water react 6h at 140 DEG C
Liquid pH is closed to neutrality, obtains reaction mixture.The reaction mixture is discharged from discharge port 702, and passes through discharging conveying
Pipeline 703, which is input to, to be stood in unit 800, and stewing process is carried out.Standing unit 800 in the present invention can use settling tank,
It is sealed shell of tank, and top is inserted with liquid flowing tube 801, and liquid flowing tube 801 can adjust vertical height and extract and stand inside unit 800
Liquid.The above-mentioned reaction mixture stood in unit 800 that is input to was allowed to stand for after a period of time, reaction mixture point
At upper solution and lower layer's solution, upper solution, and the clear liquid external by 801 upper end of liquid flowing tube are extracted by liquid flowing tube 801
Extracted upper solution is delivered in distillation unit 900 by transfer pipeline 802 distills.Distillation unit 900 is distiller,
Needing to control feed rate in distillation process is 3mL/min, and vapo(u)rizing temperature is 85 DEG C, and preheating temperature is 70 DEG C, condensation temperature 6
DEG C, vacuum degree 35Pa, knifing rotating speed 300r/min finally obtain sterol concentrate.
Sterol concentrate is dissolved in the mixed liquor of methanol and butanone, and this mixed solution is injected into heat dissipation equipment
Crystallisation by cooling is carried out in 301, obtains crystallized mixed solution (including the solid-phase component of liquid phase and precipitation in crystallized mixed solution).So
Crystallized mixed solution is transmitted to filter element 1000 afterwards and is filtered processing, that is, collects and obtains the wooden sterol crude product.By the wooden steroid
Alcohol crude product obtains the wooden sterol product at 170 DEG C after melt pelletization.
It takes lower layer's solution after standing to keep the temperature 5h at 150 DEG C, obtains sterol ester admixture, sterol ester admixture is carried out
Short-path distillation isolates fatty acid and concentration sterol ester, and concentration sterol ester is mixed with tall oil pitch raw material, can regard raw material
Continue on for the preparation of the wooden sterol.
The measurement of the color of the wooden sterol product uses GB/22460-2008《The measurement of animal and plant fat Lovibond color》In
Certain methods carry out.According to the depth of the wooden sterol color, Huang value Y takes 55 and 35, glass cell 25.4mm sulculus and
133.4mm large trough.
The R value for measuring product in embodiment 1 is 3.2, purity 95.6%, yield 82.6%.
It should be noted that：The system that " preparation method of the wooden sterol in high yield " in the above process passes through the wooden sterol in high yield
Standby system is completed, and as shown in figures 1-4, the preparation system of the high yield wood sterol includes：Steam powered units 100, first
Heat exchange unit 200, vapor absorption unit 400, supply unit 500, throttle device 600, is stirred to react second heat exchange unit 300
Unit 700, standing unit 800, distillation unit 900 and filter element 1000 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 unit 700 that is stirred to react in the present invention can be using the function of agitator tank realization stirring and reaction vessel；
Settling tank can be used by standing unit 800, be sealed shell of tank；Distillation unit 900 can use distiller；Filter element 1000
To enable to a set of " filtration system " that is 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).
Than that described above, the preparation system of the high yield wood sterol further includes being stirred to react unit 700, standing unit
800, distillation unit 900 and filter element 1000.
Wherein, unit 700 is stirred to react using agitator tank, and the upper end has feed inlet 701, as entering for dispensing material
Mouthful, lower end is provided with discharge port 702, the outlet as discharge.The external discharging supply pipe road 703 of discharge port 702, discharging conveying
Pipeline 703, which is connected to, stands unit 800, and it is single that the material being stirred to react inside unit 700 or solution can be sent to standing
Member 800.
It stands unit 800 and uses settling tank, be sealed shell of tank.Standing unit 800 includes liquid flowing tube 801, liquid flowing tube 801
Lower end from stand unit 800 top vertical insertion stand unit 800 inside, and can extract stand unit 800 inside
Liquid.In the present invention, its adjustable height of liquid flowing tube 801 to control the vertical height and position of its lower end, therefore can guarantee
The supernatant liquid stood in unit 800 can be extracted.The upper end of liquid flowing tube 801 is circumscribed with clear liquid transfer pipeline 802, clear liquid conveying
Pipeline 802 is also connected to distillation unit 900, and therefore, clear liquid transfer pipeline 802 (can pass through drawing liquid pump) for 801 institute of liquid flowing tube
The liquid of extraction is delivered in distillation unit 900, and sediment can be discharged from lower mouth.
In high yield further include a part and parcel in the preparation system of the wooden sterol it is filter element 1000, can also determines
The purity of fixed wood sterol.In the present invention, filter element 1000, including filter plant 1001, air supply channel 1002, material liquid are defeated
Enter pipeline 1003 and filtrate output tube road 1004.Filter plant 1001 therein is for being filtered processing；Air supply channel 1002
Apply pressure for the external world, promotes being normally carried out for filtering；Material liquid intake line 1003 is the input channel of feed liquid to be separated；
Filtrate output tube road 1004 is the liquid phase output channel after being separated by solid-liquid separation.
Wherein, material liquid import 1001a, the first compressed air inlet 1001b, solid phase are provided on filter plant 1001 to go out
Mouth 1001c and liquid-phase outlet 1001d.Since filter element 1000 receives the crystallized mixed solution in heat dissipation equipment 301, because
This is corresponding：There is the first charging interface 301a, the second charging interface 301b, the second compressed air inlet on heat dissipation equipment 301
The discharging of 301c and first interface 301d.
First discharging interface 301d of one end of material liquid intake line 1003 and heat dissipation equipment 301 connect, the other end and
Crystallized mixed solution inside heat dissipation equipment 301 can be transmitted to filter plant by material liquid import 1001a connection
1001 inside.
Filtrate output tube road 1004 is connect with liquid-phase outlet 1001d, can filtrate in inherent filtration in future equipment 1001 from
Liquid-phase outlet 1001d discharge.Specifically, filter plant 1001 is internally provided with filter assemblies 1001e, it is used to directly carry out
It is separated by solid-liquid separation.Filter assemblies 1001e is docked with the internal orifice end of liquid-phase outlet 1001d, and defeated by liquid-phase outlet 1001d and filtrate
Pipeline 1004 forms connection out, and therefore, the liquid phase filtered by filter assemblies 1001e can be discharged from liquid-phase outlet 1001d, and
It is discharged by filtrate output tube road 1004.
Herein it should be noted that：Filter assemblies 1001e in the present invention includes filter medium 1001e-1 and collector tube
1001e-2.Collector tube 1001e-2 is directly docked with the internal orifice end of liquid-phase outlet 1001d, forms connection, every collector tube
1001e-2 is upper can be connected with multiple filter medium 1001e-1 simultaneously, and the filtrate that each filter medium is obtained by filtration is collected
Onto collector tube 1001e-2.In addition, it can be seen from the above, every collector tube 1001e-2 and liquid-phase outlet 1001d, filtrate output tube
1004 three of road corresponds, and at least provided with one group (settable multiple groups), the outer end on each filtrate output tube road 1004 is equal
Filtrate is connected in Unified Set to collect on pipeline 1005.
In addition, it is contemplated that filter plant 1001 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 of collet can be set in the periphery of filter plant 1001
It is respectively arranged with the external cold water water inlet of cold water water inlet interface 1001f and cold water water outlet mouthpiece 1001g, cold water water inlet interface 1001f
Pipe 1001f-1, and it is passed through into collet the cold water for cooling.And the external cold water outlet pipe of cold water water outlet mouthpiece 1001g
1001g-1, for above-mentioned be passed through cold water to be discharged.Therefore, cold water inlet 1001f-1 and cold water outlet pipe 1001g-1
Cold water cooling effect can guarantee that the crystallization being precipitated will not be again dissolved in solution.
The filter run power resources of filter plant 1001 are in air supply channel 1002.Air supply channel 1002 includes the first gas source
Flow path 1002a, the second gas source flow path 1002b and third gas source flow path 1002c, wherein the first gas source flow path 1002a is connected to
One compressed air inlet 1001b, the second gas source flow path 1002b are connected to filtrate and collect on pipeline 1005, third gas source flow path
1002c is connected on the second compressed air inlet 301c, and is communicated to inside heat dissipation equipment 301.1002 external gas of air supply channel
Source processor, and compression sky is provided to the first gas source flow path 1002a, the second gas source flow path 1002b and third gas source flow path 1002c
Gas.
Therefore, the course of work of filter plant 1001 includes following three step：One, open third gas source flow path 1002c, to dissipate
It is passed through air inside hot equipment 301, due to the effect of air pressure, so that the crystallized mixed solution inside heat dissipation equipment 301 is extruded
And it is discharged that the first discharging interface 301d, entering from material liquid import 1001a 1001 inside of filter plant, (this fill process can also be with
It is realized by infusion pump)；Two, open the first gas source flow path 1002a, to filter plant 1001 inside be passed through air so that filtering
Air pressure enhancing in equipment 1001, liquid phase part compression enter in collector tube 1001e-2 from filter medium 1001e-1, completed
Filter, and be finally discharged to filtrate from filtrate output tube road 1004 and collect in pipeline 1005 (this, which is positive, blows over journey)；Three, third is closed
Gas source flow path 1002c and the first gas source flow path 1002a, and the second gas source flow path 1002b is opened, air can be collected from filtrate
Pipeline 1005 reversely blows to filter medium 1001e-1, thus part is attached to the solid phase on the outer surface filter medium 1001e-1
Air-flow can be reversed to blow off, fall to solid-phase outlet 1001c (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
1001c is exported, discharge is finally unified.To sum up, distillation unit 900 distills resulting sterol concentrate and organic solvent mixed injection
In heat dissipation equipment 301, pass through material liquid intake line 1003 after the crystallisation by cooling of heat dissipation equipment 301 into filter plant
Inside 1001, resulting solid phase is filtered by filter plant 1001 and is discharged from solid-phase outlet 1001c, resulting liquid phase goes out from liquid phase
Mouth 1001d discharge.
Further, to avoid the wasting of resources, guarantee the purity of filtering, liquid back pipe group 1006, described time liquid can be set
Pipe group 1006 includes the first liquid back pipe 1006a and the second liquid back pipe 1006b.Wherein, one end of the first liquid back pipe 1006a is connected to
On the liquid return hole 1001h of filter plant 1001 (overflow channel of 1001 lower end of filter plant setting), the other end is connected to second
It feeds on interface 301b；One end of second liquid back pipe 1006b is connected to filtrate and collects on pipeline 1005, the other end and first time liquid
Pipe 1006a is connected to together on the second charging interface 301b.Therefore, when in the filtrate obtained using only filter assemblies 1001e
When still including partial solid phase, liquid can be carried out back by liquid back pipe group 1006 and collected again, filtered, move in circles again.
Such as Fig. 3,4, it should be noted that：When need just blown over journey when, can open the first gas source flow path 1002a,
Shut-off valve on third gas source flow path 1002c, opens simultaneously material liquid intake line 1003, filtrate output tube road 1004 and filtrate
Collect the shut-off valve on pipeline 1005, and closes the shut-off valve in the second gas source flow path 1002b and liquid back pipe group 1006；
When carrying out back liquid and collecting again, the first gas source flow path 1002a, third gas source flow path 1002c can be opened
On shut-off valve, open simultaneously the cut-off in material liquid intake line 1003, filtrate output tube road 1004 and liquid back pipe group 1006
Valve, and close the shut-off valve on the second gas source flow path 1002b, wherein filtrate collects the shut-off valve on pipeline 1005 can basis
Situation selection open or do not open (when poor filtration effect close filtrate collect pipeline 1005, filter effect it is good when open filtrate
Collect pipeline 1005)；
When needing to carry out blowback process, can close on the first gas source flow path 1002a, third gas source flow path 1002c
Shut-off valve, simultaneously closes off material liquid intake line 1003, filtrate collects pipeline 1005, the shut-off valve in liquid back pipe group 1006, and
Open the shut-off valve on the second gas source flow path 1002b and filtrate output tube road 1004.
Embodiment 2
It according to mass volume ratio is 1g by tall oil pitch and caustic soda water：The ratio of 7ml mixes, and reacts 3h at 160 DEG C
Afterwards, 22% aqueous citric acid solution is added to stir to pH of mixed to neutrality, stands, mixed liquor is divided into upper solution and lower layer is molten
Liquid takes upper solution to be distilled, feed rate 4mL/min, and vapo(u)rizing temperature is 85 DEG C, and preheating temperature is 70 DEG C, condensation temperature
Degree obtains sterol concentrate for 5 DEG C, vacuum degree 30Pa, knifing rotating speed 350r/min；Sterol concentrate is dissolved in methanol
It with the mixed liquor of butanone, crystallizes, filtering, collection obtains the wooden sterol crude product, and the wooden sterol is obtained after 170 DEG C of melt pelletizations and is produced
Product；
It takes lower layer's solution after standing to keep the temperature 4h at 130 DEG C, obtains sterol ester admixture, sterol ester admixture is carried out
Short-path distillation isolates fatty acid and concentration sterol ester, and concentration sterol ester is mixed with tall oil pitch raw material, can regard raw material
Continue on for the preparation of the wooden sterol.
The measurement of the color of the wooden sterol product uses GB/22460-2008《The measurement of animal and plant fat Lovibond color》In
Certain methods carry out.According to the depth of the wooden sterol color, Huang value Y takes 55 and 35, glass cell 25.4mm sulculus and
133.4mm large trough.
The R value for measuring product in embodiment 2 is 3.4, purity 95.7%, yield 83.6%.
The above process of the present embodiment was prepared using the preparation system of high yield wood sterol described in embodiment 1
Journey is as shown in figures 1-4.
Embodiment 3
It according to mass volume ratio is 1g by tall oil pitch and caustic soda water：The ratio of 6ml mixes, and reacts 6h at 150 DEG C
Afterwards, 23% aqueous citric acid solution is added to stir to pH of mixed to neutrality, stands, mixed liquor is divided into upper solution and lower layer is molten
Liquid takes upper solution to be distilled, feed rate 3mL/min, and vapo(u)rizing temperature is 85 DEG C, and preheating temperature is 70 DEG C, condensation temperature
Degree obtains sterol concentrate for 6 DEG C, vacuum degree 40Pa, knifing rotating speed 350r/min；Sterol concentrate is dissolved in methanol
It with the mixed liquor of butanone, crystallizes, filtering, collection obtains the wooden sterol crude product, and the wooden sterol is obtained after 170 DEG C of melt pelletizations and is produced
Product；
It takes lower layer's solution after standing to keep the temperature 5h at 140 DEG C, obtains sterol ester admixture, sterol ester admixture is carried out
Short-path distillation isolates fatty acid and concentration sterol ester, and concentration sterol ester is mixed with tall oil pitch raw material, can regard raw material
Continue on for the preparation of the wooden sterol.
The measurement of the color of the wooden sterol product uses GB/22460-2008《The measurement of animal and plant fat Lovibond color》In
Certain methods carry out.According to the depth of the wooden sterol color, Huang value Y takes 55 and 35, glass cell 25.4mm sulculus and
133.4mm large trough.
The R value for measuring product in embodiment 3 is 3.2, purity 96.5%, yield 84.3%.
The above process of the present embodiment was prepared using the preparation system of high yield wood sterol described in embodiment 1
Journey is as shown in figures 1-4.
Embodiment 4
It according to mass volume ratio is 1g by tall oil pitch and caustic soda water：The ratio of 5ml mixes, and reacts 4h at 150 DEG C
Afterwards, 24% aqueous citric acid solution is added to stir to pH of mixed to neutrality, stands, mixed liquor is divided into upper solution and lower layer is molten
Liquid takes upper solution to be distilled, feed rate 3mL/min, and vapo(u)rizing temperature is 85 DEG C, and preheating temperature is 70 DEG C, condensation temperature
Degree obtains sterol concentrate for 8 DEG C, vacuum degree 40Pa, knifing rotating speed 300r/min；Sterol concentrate is dissolved in methanol
It with the mixed liquor of butanone, crystallizes, filtering, collection obtains the wooden sterol crude product, and the wooden sterol is obtained after 180 DEG C of melt pelletizations and is produced
Product；
It takes lower layer's solution after standing to keep the temperature 4h at 160 DEG C, obtains sterol ester admixture, sterol ester admixture is carried out
Short-path distillation isolates fatty acid and concentration sterol ester, and concentration sterol ester is mixed with tall oil pitch raw material, can regard raw material
Continue on for the preparation of the wooden sterol.
The measurement of the color of the wooden sterol product uses GB/22460-2008《The measurement of animal and plant fat Lovibond color》In
Certain methods carry out.According to the depth of the wooden sterol color, Huang value Y takes 55 and 35, glass cell 25.4mm sulculus and
133.4mm large trough.
The R value for measuring product in embodiment 4 is 3.3, purity 96.4%, yield 82.6%.
The above process of the present embodiment was prepared using the preparation system of high yield wood sterol described in embodiment 1
Journey is as shown in figures 1-4.
It is noted that discovery vapo(u)rizing temperature is low during the experiment, sterol yield is low, and vapo(u)rizing temperature is excessively high, sterol
Yield can also reduce, and manufactured product viscosity can be made to increase, color burn.
In addition, charging rate is slow, raw material is longer in the residence time of evaporation evaporating surface, will lead to the wooden sterol yield decline and
Purity is not high, the reason is that the probability that component reaches cryosurface becomes larger, charging increases to 2mL~4mL/min, yield and purity meeting
It greatly improves, if further speeding up, raw material components have not enough time to be sufficiently heated evaporation, cause non-target components that can not reach
Cryosurface and flow directly into target components collector, cause purity to decline.
Also, it was found that, knifing rotating speed is with charging rate, there are synergistic effects, only when charging rate be 3~
4ml/min, when knifing speed is 300~350r/min, the purity and yield of the wooden sterol just can be very high, this also with individually measure
The result that unitary variant is tested is different.From the point of view of analysis, this is because the two conditions have synergistic effect, in this value range
It inside can control the formation of evaporating surface uniform liquid film, and can guarantee that the thickness of liquid film reduces, so that the heat transfer in evaporation process
More complete with mass transfer, the non-target components in material is evaporated also more abundant, and purity and yield significantly improve.Reaction condition
It is excessive or too small, it is also possible to will lead to knifing rotor and generate eccentric vibrating, make material liquid film on evaporating surface under distributing homogeneity
Drop.
The brown materials that protein degradation generates in the wooden sterol can further deepen the color of the wooden sterol.In traditional handicraft,
With the influence of reaction process high temperature and other conditions, the phytosterol often prepared can color intensification.And we invents
It finds in an experiment, in the preparation process of the wooden sterol, due to the particularity of the wooden sterols, is by the control of melt pelletization temperature
160~180 DEG C, the control of saponification temperature is 130~150 DEG C, can efficiently control the generation of chromophore free state, thus
Darkening for the wooden sterol is effectively controlled, guarantees the Color Quality of product.
It can be seen that we invents the preparation method and system of the high yield wood sterol of offer, the wooden sterol yield is high, pure
Spend high, color is bright, and reaction is mild efficient, and the advantage high with low operation temperature, separative efficiency.
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. a kind of preparation method of high yield wood sterol, it is characterised in that：Including,
Tall oil pitch and caustic soda water according to mass volume ratio are 1g by the preparation of wooden sterol：The ratio of 4~10ml mixes, one
Determine after being reacted at temperature, aqueous citric acid solution be added and stirs to pH of mixed to neutrality, stands, mixed liquor be divided into upper solution and
Lower layer's solution takes the upper solution to be distilled, and obtains sterol concentrate；By the sterol concentrate be dissolved in methanol and/
Or butanone, it crystallizes, filtering, collection obtains the wooden sterol crude product, obtains the wooden sterol product after melt pelletization；
Raw materials recovery takes lower layer's solution to keep the temperature 4~6h at 120~160 DEG C, obtains sterol ester admixture, by the steroid
Alcohol ester blends carry out short-path distillation, fatty acid and concentration sterol ester are isolated, by the concentration sterol ester and the tall oil
Pitch mixing.
2. the preparation method of the wooden sterol of high yield according to claim 1, it is characterised in that：The matter of the aqueous citric acid solution
Measuring score is 20~25%.
3. the preparation method of the wooden sterol of high yield according to claim 1, it is characterised in that：The distillation, feed rate
For 3~4mL/min.
4. the preparation method of the wooden sterol of high yield according to claim 1, it is characterised in that：The melt pelletization, process
Temperature is 160~180 DEG C.
5. the preparation method of the wooden sterol of high yield according to claim 1, it is characterised in that：It is described anti-at a certain temperature
It answers, is 3~6h of reaction at 130~160 DEG C.
6. the preparation method of the wooden sterol of high yield according to claim 1, it is characterised in that：NaOH in the caustic soda water
Mass fraction be 12~15%.
7. the preparation method of the wooden sterol of high yield according to claim 1, it is characterised in that：The vapo(u)rizing temperature is 85~90
DEG C, preheating temperature is 65~70 DEG C, and condensation temperature is 5~8 DEG C, and vacuum degree is 30~40Pa, and knifing rotating speed is 300~350r/
min。
8. a kind of preparation system of high yield wood sterol, 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).
9. the preparation system of high yield wood sterol according to claim 8, it is characterised in that：Further include,
It is stirred to react unit (700), the upper end for being stirred to react unit (700) has feed inlet (701), and lower end is provided with out
Material mouth (702), the external discharging supply pipe road (703) of discharge port (702), the discharging supply pipe road (703) is connected to quiet
Set unit (800)；
It stands unit (800), including the standing unit (800) is protruded into liquid flowing tube (801), the lower end of the liquid flowing tube (801)
Inside and height can be adjusted, the external clear liquid transfer pipeline (802) in the upper end of the liquid flowing tube (801), clear liquid conveying
Pipeline (802) is also connected with distillation unit (900)；And filter element (1000), including filter plant (1001), gas source be logical
Road (1002), material liquid intake line (1003) and filtrate output tube road (1004) are provided on the filter plant (1001)
Material liquid import (1001a), the first compressed air inlet (1001b), solid-phase outlet (1001c) and liquid-phase outlet (1001d)；Institute
The one end for stating material liquid intake line (1003) is connect with the heat dissipation equipment (301), the other end and the material liquid import
(1001a) connection can will be transmitted to the filter plant from the heat dissipation equipment (301) internal crystallized mixed solution
(1001) inside；The filtrate output tube road (1004) connect with the liquid-phase outlet (1001d), can will come from the mistake
The filtrate filtered in equipment (1001) is discharged from the liquid-phase outlet (1001d).
10. the preparation system of high yield wood sterol according to claim 9, it is characterised in that：The filter plant
(1001) be internally provided with filter assemblies (1001e), the filter assemblies (1001e) and the liquid-phase outlet (1001d's)
The docking of internal orifice end, and formed and be connected to the filtrate output tube road (1004) by the liquid-phase outlet (1001d)；The filtrate
Output pipe (1004) and the liquid-phase outlet (1001d) are corresponded, and at least provided with one group, the filtrate output tube road
(1004) outer end, which is concentrated, to be connected to filtrate and collects on pipeline (1005)；
The air supply channel (1002) includes the first gas source flow path (1002a), the second gas source flow path (1002b) and third gas source stream
Road (1002c), the first gas source flow path (1002a) are connected to first compressed air inlet (1001b), second gas
Source stream road (1002b) is connected to the filtrate and collects on pipeline (1005), and the third gas source flow path (1002c) is connected to described
Heat dissipation equipment (301) is internal；Air supply channel (1002) external gas source, and to the first gas source flow path (1002a), second
Gas source flow path (1002b) and third gas source flow path (1002c) provide compressed air；
The distillation unit (900) distills heat dissipation equipment (301) described in resulting sterol concentrate and organic solvent mixed injection
It is interior, the mistake is entered by the material liquid intake line (1003) after the crystallisation by cooling of the heat dissipation equipment (301)
Equipment (1001) inside is filtered, resulting solid phase is filtered by the filter plant (1001) and is arranged from the solid-phase outlet (1001c)
Out, resulting liquid phase is discharged from the liquid-phase outlet (1001d).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111777655A (en) * | 2020-07-27 | 2020-10-16 | 福建省格兰尼生物工程股份有限公司 | Method for extracting wood sterol from tall oil pitch |
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| CN1639184A (en) * | 2002-01-28 | 2005-07-13 | 福布斯梅迪泰克公司 | Process of extracting and purifying phytosterols and phytostanols from tall oil pitch |
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