CN109289235A - Device, ascorbic method for crystallising for evaporative crystallization - Google Patents
Device, ascorbic method for crystallising for evaporative crystallization Download PDFInfo
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- CN109289235A CN109289235A CN201811291596.XA CN201811291596A CN109289235A CN 109289235 A CN109289235 A CN 109289235A CN 201811291596 A CN201811291596 A CN 201811291596A CN 109289235 A CN109289235 A CN 109289235A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
Abstract
The present invention provides a kind of device for evaporative crystallization, the device for being used for evaporative crystallization includes container for evaporation, crystallisation vessel, the device for evaporative crystallization further includes first circulation unit and second circulation unit, the first circulation unit include sequentially connected first be in charge of, first circulation pump, first circulation inlet pipe；The second circulation unit include described sequentially connected second be in charge of, second circulation pump, heater and second circulation inlet pipe, the first circulation inlet pipe and second circulation inlet pipe are connected in the container for evaporation.The present invention also provides a kind of ascorbic method for crystallising.This method is provided with additional first circulation circuit, and the first fine grain is imported container for evaporation as nucleus again, and growth obtains bigger the second particle and induction and obtains the second particle more and more evenly.
Description
Technical field
The present invention relates to chemical technology improvement areas, more particularly to a kind of device and vitamin C for evaporative crystallization
Method for crystallising.
Background technique
Vitamin C is one of vitamin needed by human, is clinically mainly used for vitamin C deficiency, is also used extensively
Make food, feed addictive, the huge market demand.
Chinese invention patent CN101397286B discloses a kind of ascorbic continuous crystallisation process, and this method is by ion
Vitamin C aqueous solution after exchange is pumped into first order crystallizer and carries out vacuum evaporating crystalization, then will be in first order crystallizer
The vitamin C evaporation concentrated solution of generation is continuously introduced into second level crystallizer and carries out vacuum cooled crystallization, after solid-liquor separation, carries out
Continuous discharge obtains crude product vitamin C crystal after washing brilliant, centrifugation；After the purified water dissolution of crude product vitamin C, it is pumped by filtering
Third level crystallizer realizes fine work vitamin C continuous crystallization, after solid-liquor separation, carries out continuous discharge after washing brilliant, centrifugation and obtains
To fine work vitamin C crystal.The method process is complicated, although the neat crystal grain of coarse, uniform crystal form can be obtained, brilliant
Grain size can not be controlled.
Summary of the invention
In view of the above-mentioned problems, the present invention provides and a kind of can directly obtain that high-purity, crystal grain are uniformly regular and size is controllable
Ascorbic method for crystallising, and the device for evaporative crystallization.
The present invention provides a kind of device for evaporative crystallization comprising:
Container for evaporation, for the container for evaporation for evaporating solvent, diversion pipe is arranged in the bottom of the container for evaporation, described
Boil-off gas outlet is additionally provided at the top of container for evaporation；
Crystallisation vessel, for the crystallisation vessel for crystallizing, the crystallisation vessel is located at the lower section of the container for evaporation, described
Diversion pipe extends in the crystallisation vessel, and is connected with crystallisation vessel, and the bottom of the crystallisation vessel is equipped with magma discharge port；
Wherein,
The side wall of the crystallisation vessel is connected with recycle stock outlet pipe, and the recycle stock outlet pipe is branched into first and is in charge of and
Two are in charge of；
The device for evaporative crystallization further includes first circulation unit and second circulation unit, the first circulation list
Member include described first be in charge of, first circulation pump, first circulation inlet pipe, described first is in charge of and first circulation pump connects；Institute
First circulation inlet pipe is stated with first end and second end, first end and the first circulation of the first circulation inlet pipe pump phase
Even, the second end of the first circulation inlet pipe is connected in the container for evaporation；
The second circulation unit include described second be in charge of, second circulation pump, heater and second circulation inlet pipe, it is described
Second is in charge of and successively connect with second circulation pump, heater, and the second circulation inlet pipe is described with third end and the 4th end
The third end of second circulation inlet pipe is connected with the heater, and the 4th end of the second circulation inlet pipe is connected in the evaporation and holds
Device；
The device for evaporative crystallization further includes material liquid inlet pipe, which is connected to this and second is in charge of,
And for material liquid to be pumped to the heater by second circulation.
The present invention also provides a kind of ascorbic method for crystallising comprising following steps:
(1) the above-mentioned device for evaporative crystallization is provided；
(2) material liquid is persistently injected to the material liquid inlet pipe, wherein ascorbic mass fraction is in the material liquid
10%~45%, the temperature of the material liquid is 25 DEG C~80 DEG C；
(3) evaporate: the material liquid is in charge of via second, second circulation pump, heater, second circulation inlet pipe and into institute
The vacuum degree stated container for evaporation, and control the container for evaporation is 0.09MPa~0.097MPa, and the solvent in the material liquid steams
Hair, obtains evaporation process liquid；
(4) crystallize: the evaporation process liquid enters crystallisation vessel through the diversion pipe, is tied in the crystallisation vessel
Crystalline substance obtains crystalline particle and mother liquor；
(5) it shunts: when the whole height of the crystalline particle and mother liquor reaches or is more than the recycle stock outlet pipe, institute
It states fine grain particle and mother liquor enters the recycle stock outlet pipe, and bifurcated, wherein the mother liquor bifurcated is the first mother liquor and second
Mother liquor, the fine grain particle bifurcated are the first fine grain and the second fine grain, and first fine grain and the first mother liquor flow into first and be in charge of,
Second fine grain and the second mother liquor flow into second and are in charge of, and first particle falls to the bottom of crystallisation vessel；
(6) the second fine grain and the second mother liquor that inflow described second is in charge of will continue to carry out the crystallization i.e. step in next period
(3) evaporation, step (4) crystallization and step (5) shunt；
(7) flow into described first the first fine grain for being in charge of and the first mother liquor pumped by the first circulation, first circulation into
Pipe enters the container for evaporation, and continues crystallization i.e. step (3) evaporation, step (4) crystallization and step in next period
(5) it shunts, wherein first fine grain induces to obtain biggish second particle of partial size and is settled down to crystallisation vessel as nucleus
Bottom；
(8) magma containing first particle and the second particle is exported via magma discharge port, obtains vitamin C
Finished product.
The device for evaporative crystallization has the advantage that
Due to the multiply active force (fluid force come from container for evaporation, by discharging bring active force, by first
Circulating pump, second circulation pump bring active force) effect under so that in crystallisation vessel crystal solution be in turbulence state, can effectively keep away
Exempt from the generation of crystal reunion, so that it is controllable that crystalline particle size is precipitated；Meanwhile turbulence state has more promoted point of big small crystals
From, and under the action of first circulation pump, second circulation pump, so that fine grain particle therein circulation imported into heater and evaporation
In container.The first fine grain that circulation is importing directly into container for evaporation can be used as the nucleus of next period recrystallization, so that subsequent the
Two particles are faster precipitated, and form the second particle of size more evenly.
Described second is in charge of middle setting heater, can give material liquid or the second mother liquor heat that second circulation unit is transported
Amount, and promotes its evaporation section solvent in container for evaporation, be more advantageous to material liquid or the second mother liquor the crystallisation vessel into
Row crystallization.The device, which can be realized, is formed continuously vitamin C finished product, and crystalline rate is higher, is applicable to industrialized production.
Further, when being additionally provided with rectification clasfficiator in the crystallisation vessel, which can comb crystallisation vessel
Chaotic Flow Field Distribution in (when without rectification clasfficiator), so that the liquid stream operation length below rectification clasfficiator reaches unanimity,
Each stock liquid flowing speed reaches unanimity, and keeps Flow Field Distribution regular, promotes the precipitation of crystalline particle more evenly.Meanwhile rectification point
Current difference is formd with below rectification clasfficiator in grade device channel, due to the powerless lasting entrainment of the low flow velocity below rectification clasfficiator
Biggish first particle, so that biggish first particle occurs during the low flow velocity fluid carry-over being rectified below clasfficiator
Precipitating, and be rectified the fine grain particle that liquid stream below clasfficiator is entrained to rectification clasfficiator passage proximate, then it can be rectified classification
In device channel high flow rate liquid stream entrainment, and recycle imported into heater reheat dissolution and circulation imported into evaporation hold
Nucleus is used as in device.Whole process can reach screening, separation knot by adjusting size ratio above and below the percent opening in channel and channel
The effect of brilliant particle, so that finally obtaining partial size more uniform and controllable the first particle and the second particle.
The ascorbic method for crystallising has the advantage that
Material liquid is crystallized, C-Crystals particle is obtained, by dividing fine grain particle wherein included
Stream, and the first fine grain is directly imported into container for evaporation again and enters crystallisation vessel with evaporation process liquid, as next period
The nucleus of crystallization, the final nucleus slowly grows up to obtain the second particle of target sizes, and induces more second particles faster
Precipitation.That is this method is provided with additional first circulation circuit, and the first fine grain is imported container for evaporation as nucleus again,
Finally obtain the second more uniform particle of more and size distribution.This method crystallization yield reaches 90% or more, HPLC purity
It is 99% or more, products obtained therefrom crystal face is smooth, good fluidity, even particle size, and 90% or more size of microcrystal is distributed in 40
Between -100 mesh of mesh.
Further, when being equipped with rectification clasfficiator in the crystallisation vessel, which can comb crystallisation vessel
Chaotic Flow Field Distribution in (when without rectification clasfficiator), so that the liquid stream operation length below rectification clasfficiator reaches unanimity,
Each stock liquid flowing speed reaches unanimity, and keeps Flow Field Distribution regular, promotes the precipitation of crystalline particle more evenly.Meanwhile rectification point
Current difference is formd with below rectification clasfficiator in grade device channel, due to the powerless lasting entrainment of the low flow velocity below rectification clasfficiator
Biggish first particle, so that biggish first particle occurs during the low flow velocity fluid carry-over being rectified below clasfficiator
Precipitating, and be rectified the fine grain particle that liquid stream below clasfficiator is entrained to rectification clasfficiator passage proximate, then it can be rectified classification
In device channel high flow rate liquid stream entrainment, and recycle imported into heater reheat dissolution and circulation imported into evaporation hold
Nucleus is used as in device.Whole process can reach screening, separation knot by adjusting size ratio above and below the percent opening in channel and channel
The effect of brilliant particle, so that finally obtaining the more uniform and controllable product of partial size.
Further, pass through the evaporation rate of solvent and the ratio of the charging rate of the material liquid in the setting material liquid
Value is 0.4~0.8 and the ratio of the charging rate of the discharging speed and material liquid of the magma is 0.1~0.9, with
The degree of supersaturation for maintaining mother liquor, may make that crystallization process is continuous.
Further, by setting the ratio of the flow of the first-class stock and the flow of the second stock as 1:100
~10:1, can be obtained the uniform product of particle size, and this method can also carry out large-scale industrial production.
Detailed description of the invention
Fig. 1 is the structure and flow diagram of the device for evaporative crystallization of the embodiment of the present invention 1.
Fig. 2 is the structure and flow diagram of the device for evaporative crystallization of the embodiment of the present invention 2.
Fig. 3 is structural schematic diagram of the Fig. 2 for the rectification clasfficiator in the device of evaporative crystallization.
Wherein, 1, material liquid inlet pipe；2a, first are in charge of；2b, second are in charge of；3, second circulation pumps；4, heater；5,
Two circulation inlet pipes；6, container for evaporation；7, diversion pipe；8, crystallisation vessel；9, demister is defoamed；10, boil-off gas exports；11, it puts down
Weighing apparatus pipe；12, recycle stock outlet pipe；13, first circulation pumps；14, first circulation inlet pipe；15, magma discharge port；16, centrifuge；
17, clasfficiator is rectified；18, channel.
Specific embodiment
The technical solution in embodiment of the present invention will be clearly and completely described below, it is clear that described reality
The mode of applying is only some embodiments of the invention, rather than whole embodiments.Based on the embodiment in the present invention,
All other embodiment obtained by those of ordinary skill in the art without making creative efforts belongs to this
Invent the range of protection.
Referring to Fig. 1, the embodiment of the present invention 1 provides a kind of device for evaporative crystallization.It is described for evaporative crystallization
Device includes container for evaporation 6, crystallisation vessel 8, and crystallisation vessel 8 is located at the lower section of container for evaporation 6, and container for evaporation 6 is used for solvent
Evaporation, crystallisation vessel 8 is for crystallizing, and the top of container for evaporation 6 is provided with boil-off gas outlet 10, and the bottom of container for evaporation 6 is set
Diversion pipe 7 is set, diversion pipe 7 extends in crystallisation vessel 8, and is connected with crystallisation vessel 8, and the side wall of crystallisation vessel 8 is connected with circulation
Material outlet pipe 12, recycle stock outlet pipe 12, which is branched into first, to be in charge of 2a and second and is in charge of 2b.
Described for evaporative crystallization further includes first circulation unit and second circulation unit, and first circulation unit includes the
One is in charge of 2a, first circulation pumps 13, first circulation inlet pipe 14, and first, which is in charge of 2a and first circulation, pumps 13 and connect, first circulation into
Pipe 14 has first end and second end, and the first end of first circulation inlet pipe 14 is connected with first circulation pump 13, first circulation inlet pipe
14 second end is connected in container for evaporation 6.
Second circulation unit includes described second being in charge of 2b, second circulation pump 3, heater 4 and second circulation inlet pipe 5, the
Two, which are in charge of 2b, successively connect with second circulation pump 3, heater 4, and second circulation inlet pipe 5 has third end and the 4th end, and second follows
The third end of ring inlet pipe 5 is connected with the heater 4, and the 4th end of second circulation inlet pipe 5 is connected in container for evaporation 6.
The device for evaporative crystallization further includes material liquid inlet pipe 1, and material liquid inlet pipe 1 is connected to this and second is in charge of
2b, and for being given material liquid by second circulation pump 3 to heater 4.
There are two circulation loops with except container for evaporation 6 for the crystallisation vessel 8.(corresponding first follows first circulation loop
Ring element) are as follows: crystallisation vessel 8, recycle stock outlet pipe 12, first are in charge of 2a, first circulation pump 13, first circulation inlet pipe 14, steam
Send out container 6；Second circulation loop (corresponding second circulation unit) are as follows: crystallisation vessel 8, recycle stock outlet pipe 12, second are in charge of
2b, second circulation pump 3, heater 4, second circulation inlet pipe 5, container for evaporation 6.Wherein, second is in charge of 2b and also takes on and raw material
Liquid inlet pipe 1 connects, and material liquid is continuously introduced into the effect in second circulation circuit.
The first circulation circuit be used for by crystallisation vessel 8 partial mother liquid (being defined as the first mother liquor) and crystallization obtain
Part fine grain particle (being defined as the first fine grain) be directed directly to container for evaporation 6, which can be used as the knot in next period
Jingjing core, to can induce to obtain crystalline particle more evenly.It should be noted that first fine grain can continue to grow up to obtain more
The second particle greatly and more evenly, meanwhile, the first fine grain, which reenters crystallisation vessel 8 also, can induce more second particles orderly
Ground is formed, that is to say, that the effect in the first circulation circuit is divided into two aspects: first is that making the second more granulated
At；Second is that fine grain particle is made to be grown to uniform second particle.
The second circulation circuit is used for another part mother liquor (being defined as the second mother liquor) in crystallisation vessel 8 and crystallizes
Obtained another part fine grain particle (being defined as the second fine grain) enters container for evaporation 6, solvent evaporation by the effect of heater 4
Afterwards, the crystallization in next period is carried out into crystallisation vessel 8.
The material liquid or that the container for evaporation 6 flowed into typically without additional heating by the second circulation inlet pipe 5
Two mother liquors are after the heating by heater 4, and temperature can rise, and therefore, material liquid or the second mother liquor can be described
The solvent of part is evaporated in container for evaporation 6.In order to avoid the product of part is walked in the foam entrainment generated in solvent evaporation process,
Yield losses are caused, defoaming demister 9 is equipped at boil-off gas outlet 10 in the inside of container for evaporation 6, defoams demister 9
It can be mesh structure or other types of defoaming demister.
The side wall of the container for evaporation 6 and the side wall of crystallisation vessel 8 are additionally provided with balance pipe 11, and the connection of balance pipe 11 is steamed
Send out container 6 and crystallisation vessel 8.
The bottom of the crystallisation vessel 8 is equipped with magma discharge port 15.
Referring to Fig. 2, the embodiment of the present invention 2 provides a kind of device for evaporative crystallization.This is used for the dress of evaporative crystallization
Set it is essentially identical with the structure of the device for evaporative crystallization of embodiment 1, difference be: rectification is set in crystallisation vessel 8
Clasfficiator 17.Referring to Fig. 3, the rectification clasfficiator 17 includes multiple channels 18.It is described rectification clasfficiator 17 effect be
To crystalline particle more evenly.
The size of the lower end in the channel 18 is greater than the size of the upper end in the channel 18, and there are two sides for this purpose of design
Face: (1) generation of particle " back-mixing " phenomenon is prevented；(2) possibility of the blocking of channel 18 is avoided.The shaft section in the channel 18 can
Think but is not limited to trapezoidal, bowl-type, water-drop-shaped.
The ratio of the size of the upper end in the size of the lower end in the channel 18 and the channel 18 is 1.1:1~10:1, excellent
Choosing, the ratio of the size of the upper end in the size of the lower end in the channel 18 and the channel 18 is 1.5:1~5:1.
The size of the upper end in the channel 18 is 3 millimeters~100 millimeters, preferably 5 millimeters~50 millimeters.
The percent opening in multiple channels 18 is (that is, the sum of the area of upper end in channel accounts for the upper table of the rectification clasfficiator
The percentage of the area in face) it is 5%~50%, preferably 10%~30%.
The device for evaporative crystallization has the advantage that
The container for evaporation 6 is used to evaporate solvent in material liquid, and crystallisation vessel 8 is for crystallizing, by by recycle stock
Outlet pipe 12, which is branched into first, to be in charge of 2a and second and is in charge of 2b, and first is in charge of 2a for material liquid to be crystallized to the first fine grain weight to be formed
It is newly directed in container for evaporation 6, which can be used as the nucleus of next Periodical crystallization, so that growth obtains the second particle and lures
More and the second particle more evenly is led to be formed；Described second is in charge of setting heater 4 in 2b, can give material liquid or second
Mother liquor heat, and solvent portion is evaporated in container for evaporation 6, is more advantageous to material liquid or the second mother liquor in the crystallisation vessel 8
It is crystallized.
The present invention also provides a kind of ascorbic method for crystallising.The method for crystallising the following steps are included:
(1) device for being used for evaporative crystallization is provided；
(2) material liquid is persistently injected to the material liquid inlet pipe 1, wherein ascorbic mass fraction in the material liquid
It is 10%~45%, the temperature of the material liquid is 25 DEG C~80 DEG C；
(3) evaporate: the material liquid via second be in charge of 2b, second circulation pump 3, heater 4, second circulation inlet pipe 5 and
Into the container for evaporation 6, and the vacuum degree of the container for evaporation is controlled for 0.09MPa~0.097MPa, in the material liquid
Solvent evaporation, obtain evaporation process liquid；
(4) crystallize: the evaporation process liquid through the diversion pipe 7 enter crystallisation vessel 8, in the crystallisation vessel 8 into
Row crystallization, obtains crystalline particle and mother liquor, wherein the crystalline particle includes that biggish first particle of partial size and partial size are smaller
Fine grain particle；
(5) it shunts: when the whole height of the crystalline particle and mother liquor reaches or is more than the recycle stock outlet pipe 12,
The fine grain particle and mother liquor enter the recycle stock outlet pipe 12, and bifurcated, wherein the mother liquor bifurcated be the first mother liquor and
Second mother liquor, the fine grain particle bifurcated are the first fine grain and the second fine grain, and first fine grain and the first mother liquor flow into first
It is in charge of 2a, second fine grain and the second mother liquor flow into second and be in charge of 2b, and first particle falls to the bottom of crystallisation vessel；
(6) the second fine grain of 2b and the second mother liquor are in charge of in inflow described second will continue to carry out the crystallization in next period and walks
Suddenly (3) evaporation, step (4) crystallization and step (5) shunt；
(7) the first fine grain of 2a is in charge of in inflow described first and the first mother liquor is followed by first circulation pump 13, first
Ring inlet pipe 14 enter the container for evaporation 6, and continue next period crystallization i.e. step (3) evaporation, step (4) crystallization with
And step (5) shunts, wherein first fine grain induces to obtain biggish second particle of partial size as nucleus and is settled down to knot
The bottom of brilliant container；
(8) magma containing first particle and the second particle is exported via magma discharge port 15, obtains dimension life
Plain C finished product.
Wherein, it is preferred that ascorbic mass fraction is 15%~30% in step (2) described material liquid, the raw material
The temperature of liquid is 30 DEG C~70 DEG C.
Step (2) is exported crystalline substance by magma discharge port 15 by the material liquid inlet pipe 1 injection material liquid to step (8) for the first time
The time of slurry is 0.5 hour~6 hours.The ratio of the charging rate of evaporation rate of solvent and the material liquid in the material liquid
Value is 0.4~0.8, preferably 0.5~0.7.This is because need to inject more material liquid when crystallization for the first time,
So as to have enough vitamin Cs in the crystallisation vessel 8, to reach suitable degree of supersaturation and residence time.Export magma
Opportunity, can be according to the solid content of the crystal grain (including first particle and the second particle) in the crystallisation vessel 8
To determine.Such as when solid content be greater than 42% when, openable magma discharge port 15 and discharge.Certainly, in subsequent process,
By the lasting injection material liquid of the material liquid inlet pipe 1, can magma discharge port 15 it is lasting obtain magma.
The summation of first fine grain and the first mother liquor is defined as first-class stock, by the total of the second fine grain and the second mother liquor
Be defined as second stock.In the case where the total amount of mother liquor and fine grain particle is certain in the case where fine grain even particle distribution,
It is believed that the ratio of the first fine grain and the second fine grain is equal to the ratio of the flow of the first-class stock and the flow of the second stock
Example.In the present invention, the ratio by controlling the flow of the first-class stock and the flow of the second stock is 1:100~10:
1, it can control the shared ratio of first fine grain, and then control loop returns to the ratio of the nucleus in the container for evaporation 6.
Preferably, the ratio of the flow of the flow of the first-class stock and the second stock is 1:10~4:5.
Step (3) evaporate during, the material liquid or flow into described second be in charge of 2b the second mother liquor passing through
It crosses after the heater 4, temperature is increased to 30 DEG C~90 DEG C.Preferably, the material liquid or inflow described second are in charge of
For the second mother liquor of 2b after by the heater 4, temperature is increased to 40 DEG C~70 DEG C.
During step (5) shunt, rectification clasfficiator 17 can be equipped in the crystallisation vessel 8.When crystalline particle and
When the whole height of mother liquor reaches or is connected in the position of the crystallisation vessel 8 more than the recycle stock outlet pipe 12, the crystallization
Fine grain particle and mother liquor in particle enter the recycle stock outlet pipe 12 by rectification clasfficiator 17.The rectification clasfficiator 17
Effect be that so that fine grain particle enters recycle stock outlet pipe 12, and biggish first particle of particle still remains in the knot
It is final to realize that product cut size is uniform in brilliant container 8.It is appreciated that the bottom of the crystallisation vessel 8 can be set to conical region,
In order to realize crystal grain classification and relatively easily discharging.
Step (2) injects material liquid by the material liquid inlet pipe and exports magma for the first time by magma discharge port to step (8)
Material time be 1 hour~8 hours.After first time exports magma by magma discharge port 15, in the material liquid
Evaporation rate of solvent and the ratio of the charging rate of the material liquid are turned down.By the discharging speed and step of the magma of step (8)
(2) ratio of the charging rate of material liquid is adjusted to 0.1~0.9.Residence time of material can evaporative crystallization according to the present invention
Material total amount when device steady-state operation is calculated divided by discharging speed.Preferably, in order to maintain suitable degree of supersaturation
And the residence time, thus guarantee the even particle size distribution of final crystal grain, the discharging speed and step of the magma of step (8)
(2) ratio of the charging rate of material liquid is 0.3~0.6.
After step (8), the magma containing first particle and the second particle is led via magma discharge port 15
After out, filter cake is obtained by centrifugation by centrifuge 16 and centrifugation is mother liquid obtained, and the mother liquid obtained recycling of the centrifugation is recycled
To material liquid inlet pipe 1.
The ascorbic method for crystallising has the advantage that
Material liquid is crystallized, C-Crystals particle is obtained, by dividing fine grain particle wherein included
Stream, and the first fine grain is directly imported into container for evaporation 6 again and enters crystallisation vessel 8 with evaporation process liquid, as next week
The nucleus of phase crystallization, the final nucleus slowly grow up to obtain the second more uniform particle of more and crystal grain.
Ascorbic method for crystallising of the present invention will be further described by embodiment below.
Vitamin C crude product purity range in the present embodiment selects between 90%-95%.
Data and effect do not limit the practical ranges of the technology of the present invention in the embodiment of the present invention.
Embodiment 1
The present embodiment using as shown in Figure 1 for evaporative crystallization device carry out crystallization operation, specifically according to the following steps into
Row:
(1) the vitamin C crude product that HPLC purity is 94% is dissolved with water, is decolourized, that mass percent is obtained by filtration is dense
The ascorbic material liquid that degree is 20%, temperature are 40 DEG C.
(2) heater 4 are pumped into ascorbic material liquid from material liquid inlet pipe 1, are delivered to via second circulation pump 3
Heater 4, the temperature of material liquid are increased to 55 DEG C.Material liquid after heating continuously flows into container for evaporation with the speed of 200kg/h
6。
(3) vacuum degree for controlling container for evaporation 6 is 0.095MPa, and boiling is rapidly reached after so that material liquid is entered container for evaporation 6
State is risen, water evaporation rate maintains 140kg/h, and solvent largely volatilizees, and concentrate enters crystallisation vessel 8 through diversion pipe 7.When
Liquid level reaches recycle stock outlet pipe 12 and is able to achieve when circulating in crystallisation vessel 8, reduces the charging rate of material liquid extremely
140kg/h, second circulation pump 3 flow controls in 1000kg/h, and the flow control of first circulation pump 13 is in 258kg/h, and described the
0.3, maintenance is stablized 3 hours for the ratio control of the flow of the flow of first-class stock and the second stock.
(4) when the bottom pyramidal decanting zone solid content of crystallisation vessel 8 reaches 57%, the bottom magma of crystallisation vessel 8 is opened
The valve of discharge port 15, the magma in crystallisation vessel 8 is entered in continuous centrifugal machine 16 with the flow velocity of 60kg/h to be filtered, and filter cake is used
Continuous discharge after technique water washing, filtrated stock is concentrated, is recycled to material liquid inlet pipe 1 after decolorization.
(5) after the magma in crystallisation vessel 8 starts discharging, the charging rate of material liquid is adjusted to 200kg/h, first circulation pump
In 240kg/h, the ratio of the flow of the flow of the first-class stock and the second stock is controlled 0.3 13 flow control.
(6) gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.6% with inlet amount
Meter, crystallization yield 91%, wherein 40 mesh percent of pass 100% of C-Crystals particle, 60 mesh percent of pass 59%, 100 mesh
Percent of pass 8% meets CP2015, EP8.0, USP33 requirement.
Embodiment 2
Device used by the ascorbic method for crystallising that the embodiment uses for evaporative crystallization is shown in Fig. 2
Device for evaporative crystallization.
(1) the vitamin C crude product that HPLC purity is 94% is dissolved with water, is decolourized, that mass percent is obtained by filtration is dense
The ascorbic material liquid that degree is 20%, temperature are 40 DEG C.
(2) heater 4 are pumped into ascorbic material liquid from material liquid inlet pipe 1, are delivered to via second circulation pump 3
Heater 4, the temperature of material liquid are increased to 55 DEG C.Material liquid after heating continuously flows into container for evaporation with the speed of 200kg/h
6.The diameter of the upper end in channel 18 is 10 millimeters, and the diameter of the lower end in channel 18 is with the diameter ratio value of the upper end in channel 18
2.7:1, the percent opening in the channel are 20%.
(3) vacuum degree for controlling container for evaporation 6 is 0.095MPa, and boiling is rapidly reached after so that material liquid is entered container for evaporation 6
State is risen, water evaporation rate maintains 140kg/h, and solvent largely volatilizees, and concentrate enters crystallisation vessel 8 through diversion pipe 7.When
Liquid level reaches recycle stock outlet pipe 12 and is able to achieve when circulating in crystallisation vessel 8, reduces the charging rate of material liquid extremely
140kg/h, for the flow control of second circulation pump 3 in 1000kg/h, the flow control of first circulation pump 13 is described in 258kg/h
0.3, maintenance is stablized 3 hours for the ratio control of the flow of the flow of first-class stock and the second stock.
(4) when the bottom pyramidal decanting zone solid content of crystallisation vessel 8 reaches 57%, the valve of bottom magma discharge port 15 is opened
, the magma in crystallisation vessel 8 is entered in continuous centrifugal machine 16 with the flow velocity of 60kg/h to be filtered, after filter cake technique water washing
Continuous discharge, filtrated stock is concentrated, is recycled to material liquid inlet pipe 1 after decolorization.
(5) after the magma in crystallizer starts discharging, material liquid charging rate is adjusted to 200kg/h, first circulation pump 13
Flow control in 240kg/h, the ratio of the flow of the flow of the first-class stock and the second stock is controlled 0.3.
(6) gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.5%, with charging
Meter, crystallization yield 91%, wherein 40 mesh percent of pass 99% of C-Crystals particle, 60 mesh percent of pass 44%, 100
Mesh percent of pass 0.2% meets CP2015, EP8.0, USP33 requirement.
Embodiment 3
On the basis of embodiment 2, by the control of step (3) first circulation pump 13 for 344kg/h, the first-class stock
Flow and the second stock flow ratio control be 0.4, step (5) first circulation pump 13 flow control exist
The ratio control of the flow of 320kg/h, the flow of the first-class stock and the second stock is 0.4；Remaining condition is the same as real
Apply example 2.Gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.3%, to feed meter,
Crystallization yield is 90.5%, wherein 40 mesh percent of pass 100% of vitamin C crystalline particle, 60 mesh percent of pass 81%, 100 mesh
Percent of pass 10%.
Embodiment 4
On the basis of embodiment 2, by the control of step (3) first circulation pump 13 for 172kg/h, the first-class stock
Flow and the second stock flow ratio control be 0.2, step (5) first circulation pump 13 flow control exist
The ratio control of the flow of 160kg/h, the flow of the first-class stock and the second stock is 0.2；Remaining condition is the same as real
Apply example 2.Gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.7%, to feed meter,
Crystallization yield is 91.5%, wherein 40 mesh percent of pass 99.5% of vitamin C crystalline particle, 60 mesh percent of pass 48%, 100 mesh
Percent of pass 2%.
Embodiment 5
On the basis of embodiment 2, by the control of step (3) first circulation pump 13 for 43kg/h, the first-class stock
Flow and the second stock flow ratio control be 0.05, step (5) first circulation pump 13 flow control exist
The ratio control of the flow of 40kg/h, the flow of the first-class stock and the second stock is 0.05；Remaining condition is the same as real
Apply example 2.Gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.8%, to feed meter,
Crystallization yield is 90.9%, wherein 40 mesh percent of pass 100% of vitamin C crystalline particle, 60 mesh percent of pass 82%, 100 mesh
Percent of pass 16%.
Embodiment 6
On the basis of embodiment 2, by the control of step (3) first circulation pump 13 in 860kg/h, the first-class stock
The ratio control of the flow of flow and the second stock is 1, and the flow control of step (5) first circulation pump 13 is in 800kg/
The ratio control of the flow of h, the flow of the first-class stock and the second stock is 1；Remaining condition is the same as embodiment 2.Institute
The C-Crystals particle that filter cake obtains white after drying is obtained, HPLC purity is 99.4%, to feed meter, crystallization yield
It is 91%, wherein 40 mesh percent of pass 100% of C-Crystals particle, 60 mesh percent of pass 84%, 100 mesh percent of pass 17%.
Embodiment 7
Device used by the ascorbic method for crystallising that the embodiment uses for evaporative crystallization is shown in Fig. 2
Device for evaporative crystallization.
(1) the vitamin C crude product that HPLC purity is 94% is dissolved with water, is decolourized, that mass percent is obtained by filtration is dense
The ascorbic material liquid that degree is 20%, temperature are 60 DEG C.
(2) heater 4 are pumped into ascorbic material liquid from material liquid inlet pipe 1, are delivered to via second circulation pump 3
Heater 4, the temperature of material liquid are increased to 66 DEG C.Material liquid after heating continuously flows into container for evaporation with the speed of 250kg/h
6.The diameter of the upper end in channel 18 is 10 millimeters, and the diameter of the lower end in channel 18 is with the diameter ratio value of the upper end in channel 18
2.7:1, the percent opening in the channel are 20%.
(3) vacuum degree for controlling container for evaporation 6 is 0.09MPa, and boiling is rapidly reached after so that material liquid is entered container for evaporation 6
State, water evaporation rate maintain 150kg/h, and solvent largely volatilizees, and concentrate enters crystallisation vessel 8 through diversion pipe 7.Work as knot
Liquid level reaches recycle stock outlet pipe 12 and is able to achieve when circulating in brilliant container 8, reduces the charging rate of material liquid extremely
150kg/h, for the flow control of second circulation pump 3 in 1300kg/h, the flow control of first circulation pump 13 is described in 230kg/h
0.2, maintenance is stablized 3 hours for the ratio control of the flow of the flow of first-class stock and the second stock.
(4) when the bottom pyramidal decanting zone solid content of crystallisation vessel 8 reaches 42%, the valve of bottom magma discharge port 15 is opened
, the magma in crystallisation vessel 8 is entered in continuous centrifugal machine 16 with the flow velocity of 100kg/h to be filtered, filter cake technique water washing
Continuous discharge afterwards, filtrated stock is concentrated, is recycled to material liquid inlet pipe 1 after decolorization.
(5) after the magma in crystallizer starts discharging, material liquid charging rate is adjusted to 250kg/h, first circulation pump 13
Flow control in 210kg/h, the ratio of the flow of the flow of the first-class stock and the second stock is controlled 0.2.
(6) gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.8%, with charging
Meter, crystallization yield 90.8%, wherein 40 mesh percent of pass 100% of C-Crystals particle, 60 mesh percent of pass 40%,
100 mesh percent of pass 0.3% meet CP2015, EP8.0, USP33 requirement.
Embodiment 8
It is 50 millimeters by the diameter of the upper end in step (2) channel 18 on the basis of embodiment 7, the lower end in channel 18
The diameter ratio value of the upper end in diameter and channel 18 is 1.5:1, and the percent opening in the channel is 20%；Remaining condition is the same as implementation
Example 7.Gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.3%, to feed meter, knot
Brilliant yield is 90.3%, wherein 40 mesh percent of pass 100% of C-Crystals particle, 60 mesh percent of pass 52%, 100 mesh are logical
Cross rate 6%.
Embodiment 9
It is 5 millimeters by the diameter of the upper end in step (2) channel 18 on the basis of embodiment 7, the lower end in channel 18
The diameter ratio value of the upper end in diameter and channel 18 is 5:1, and the percent opening in the channel is 20%；The same embodiment of remaining condition
7.Gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.1%, to feed meter, crystallization
Yield is 90.1%, wherein 40 mesh percent of pass 100% of C-Crystals particle, 60 mesh percent of pass 50%, 100 mesh pass through
Rate 5%.
Embodiment 10
It is 50 millimeters by the diameter of the upper end in step (2) channel 18 on the basis of embodiment 7, the lower end in channel 18
The diameter ratio value of the upper end in diameter and channel 18 is 1.5:1, and the percent opening in the channel is 40%；Remaining condition is the same as implementation
Example 7.Gained filter cake obtains the C-Crystals particle of white after drying, and HPLC purity is 99.4%, to feed meter, knot
Brilliant yield is 90.4%, wherein 40 mesh percent of pass 100% of C-Crystals particle, 60 mesh percent of pass 51%, 100 mesh are logical
Cross rate 8%.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (12)
1. a kind of device for evaporative crystallization comprising:
Container for evaporation, for the container for evaporation for evaporating solvent, diversion pipe, the evaporation is arranged in the bottom of the container for evaporation
Boil-off gas outlet is additionally provided at the top of container；
Crystallisation vessel, for the crystallisation vessel for crystallizing, the crystallisation vessel is located at the lower section of the container for evaporation, the water conservancy diversion
Pipe extends in the crystallisation vessel, and is connected with crystallisation vessel, and the bottom of the crystallisation vessel is equipped with magma discharge port；It is special
Sign is,
The side wall of the crystallisation vessel is connected with recycle stock outlet pipe, and the recycle stock outlet pipe is branched into first and is in charge of and second point
Pipe；
The device for evaporative crystallization further includes first circulation unit and second circulation unit, the first circulation unit packet
Include described first be in charge of, first circulation pump, first circulation inlet pipe, described first is in charge of and first circulation pump connects；Described
One circulation inlet pipe has first end and second end, and the first end of the first circulation inlet pipe is connected with first circulation pump, institute
The second end for stating first circulation inlet pipe is connected in the container for evaporation；
The second circulation unit include described second be in charge of, second circulation pump, heater and second circulation inlet pipe, described second
It to be in charge of and successively connect with second circulation pump, heater, the second circulation inlet pipe is with third end and the 4th end, and described second
The third end of circulation inlet pipe is connected with the heater, and the 4th end of the second circulation inlet pipe is connected in the container for evaporation；
The device for evaporative crystallization further includes material liquid inlet pipe, which is connected to this and second is in charge of, and is used in combination
In material liquid is pumped to the heater by second circulation.
2. being used for the device of evaporative crystallization as described in claim 1, which is characterized in that be additionally provided with rectification in the crystallisation vessel
Clasfficiator, the rectification clasfficiator include multiple channels, the size of the size of the lower end in the channel and the upper end in the channel
Ratio be 1.1:1~10:1.
3. being used for the device of evaporative crystallization as claimed in claim 2, which is characterized in that the size of the upper end in the channel is 3
Millimeter~100 millimeters.
4. as claimed in claim 2 be used for evaporative crystallization device, which is characterized in that the percent opening in the channel be 5%~
50%.
5. being used for the device of evaporative crystallization as described in claim 1, which is characterized in that the inside of the container for evaporation is close to institute
It states boil-off gas exit and is equipped with defoaming demister.
6. being used for the device of evaporative crystallization as described in claim 1, which is characterized in that the side wall of the container for evaporation and institute
The side wall for stating crystallisation vessel is additionally provided with balance pipe, and the balance pipe is connected to the container for evaporation and crystallisation vessel.
7. a kind of ascorbic method for crystallising, which is characterized in that itself the following steps are included:
(1) hair crystallization apparatus as described in any one of claims 1 to 6 is provided；
(2) material liquid is persistently injected to the material liquid inlet pipe, wherein ascorbic mass fraction is 10% in the material liquid
~45%, the temperature of the material liquid is 25 DEG C~80 DEG C；
(3) evaporate: the material liquid is in charge of via second, second circulation pump, heater, second circulation inlet pipe and the entrance steaming
The vacuum degree sent out container, and control the container for evaporation is 0.09MPa~0.097MPa, the solvent evaporation in the material liquid,
Obtain evaporation process liquid；
(4) crystallize: the evaporation process liquid enters crystallisation vessel through the diversion pipe, is crystallized in the crystallisation vessel,
Obtain crystalline particle and mother liquor；
(5) it shunts: described thin when the whole height of the crystalline particle and mother liquor reaches or is more than the recycle stock outlet pipe
Brilliant particle and mother liquor enter the recycle stock outlet pipe, and bifurcated, wherein the mother liquor bifurcated is that the first mother liquor and second are female
Liquid, the fine grain particle bifurcated are the first fine grain and the second fine grain, and first fine grain and the first mother liquor flow into first and be in charge of, institute
It states the second fine grain and the second mother liquor flows into second and is in charge of, first particle falls to the bottom of crystallisation vessel；
(6) the second fine grain and the second mother liquor that inflow described second is in charge of will continue to carry out the crystallization i.e. step (3) in next period
Evaporation, step (4) crystallization and step (5) shunt；
(7) flow into described first the first fine grain for being in charge of and the first mother liquor pumped by the first circulation, first circulation inlet pipe into
Enter the container for evaporation, and continues crystallization i.e. step (3) evaporation, step (4) crystallization and step (5) point in next period
Stream, wherein first fine grain induces to obtain biggish second particle of partial size and is settled down to the bottom of crystallisation vessel as nucleus；
(8) magma containing first particle and the second particle is exported via magma discharge port, obtain vitamin C at
Product.
8. ascorbic method for crystallising as claimed in claim 7, which is characterized in that the solvent in the material liquid evaporates speed
Degree and the ratio of the charging rate of the material liquid are 0.4~0.8, the charging of the discharging speed of the magma and the material liquid
The ratio of speed is 0.1~0.9.
9. ascorbic method for crystallising as claimed in claim 7, which is characterized in that during step (5) shunt, institute
It states and is additionally provided with rectification clasfficiator in crystallisation vessel, when the whole height of crystalline particle and mother liquor reaches or is more than the recycle stock
When outlet pipe is connected in the position of the crystallisation vessel, the fine grain particle and mother liquor are by rectifying clasfficiator into the recycle stock
Outlet pipe.
10. ascorbic method for crystallising as claimed in claim 7, which is characterized in that during step (3) are evaporated, institute
It states material liquid or flows into described second the second mother liquor for being in charge of after by the heater, temperature is increased to 30 DEG C~90
℃。
11. ascorbic method for crystallising as claimed in claim 7, which is characterized in that be in charge of flowing into first in step (5)
First fine grain and the first mother liquor be defined as first-class stock, second fine grain is in charge of in inflow second and the second mother liquor is determined
Justice is second stock, and the ratio of the flow of the flow of the first-class stock and the second stock is 1:100~10:1.
12. ascorbic method for crystallising as claimed in claim 7, which is characterized in that, will be containing described after step (8)
After the magma of first particle and the second particle is exported via magma discharge port, filter cake is obtained by centrifugation and centrifugation gained is female
Liquid, and the mother liquid obtained recycling of the centrifugation is recycled to material liquid inlet pipe.
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| CN109289233A (en) * | 2018-10-31 | 2019-02-01 | 浙江新和成股份有限公司 | For the device of evaporative crystallization, the method for crystallising of methionine |
| CN109453539A (en) * | 2018-10-31 | 2019-03-12 | 浙江新和成股份有限公司 | For the device of evaporative crystallization, the method for crystallising of Sucralose |
| CN109513232A (en) * | 2018-10-31 | 2019-03-26 | 浙江新和成股份有限公司 | For the device of evaporative crystallization, the method for crystallising of ethylmaltol |
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| CN109289234A (en) * | 2018-10-31 | 2019-02-01 | 浙江新和成股份有限公司 | For the device of evaporative crystallization, the method for crystallising of vitamin B6 |
| CN109289233A (en) * | 2018-10-31 | 2019-02-01 | 浙江新和成股份有限公司 | For the device of evaporative crystallization, the method for crystallising of methionine |
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| CN109289233B (en) * | 2018-10-31 | 2020-12-15 | 浙江新和成股份有限公司 | Device for evaporative crystallization and method for crystallizing methionine |
| CN109289234B (en) * | 2018-10-31 | 2020-12-15 | 浙江新和成股份有限公司 | Device for evaporative crystallization and crystallization method of vitamin B6 |
| CN109513232B (en) * | 2018-10-31 | 2020-12-15 | 浙江新和成股份有限公司 | Device for evaporative crystallization and crystallization method of ethyl maltol |
| CN109453539B (en) * | 2018-10-31 | 2020-12-15 | 浙江新和成股份有限公司 | Device for evaporative crystallization and method for crystallizing sucralose |
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