CN109289234A - For the device of evaporative crystallization, the method for crystallising of vitamin B6 - Google Patents

For the device of evaporative crystallization, the method for crystallising of vitamin B6 Download PDF

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Publication number
CN109289234A
CN109289234A CN201811289985.9A CN201811289985A CN109289234A CN 109289234 A CN109289234 A CN 109289234A CN 201811289985 A CN201811289985 A CN 201811289985A CN 109289234 A CN109289234 A CN 109289234A
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evaporation
circulation
particle
container
material liquid
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CN109289234B (en
Inventor
刘金龙
鲁国彬
陈卫勇
李浩然
黄顺礼
沈自强
李俊豪
刘晓庆
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Shandong Xin He Cheng Jing Hua Technology Co Ltd
SHANDONG XINHECHENG PHARMACEUTICAL CO Ltd
Zhejiang NHU Co Ltd
Shandong Xinhecheng Fine Chemical Technology Co Ltd
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Shandong Xin He Cheng Jing Hua Technology Co Ltd
SHANDONG XINHECHENG PHARMACEUTICAL CO Ltd
Zhejiang NHU Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0031Evaporation of components of the mixture to be separated by heating
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D213/00Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/60Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom 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
    • C07D213/62Oxygen or sulfur atoms
    • C07D213/63One oxygen atom
    • C07D213/65One oxygen atom attached in position 3 or 5
    • C07D213/66One oxygen atom attached in position 3 or 5 having in position 3 an oxygen atom and in each of the positions 4 and 5 a carbon atom bound to an oxygen, sulphur, or nitrogen atom, e.g. pyridoxal
    • C07D213/672-Methyl-3-hydroxy-4,5-bis(hydroxy-methyl)pyridine, i.e. pyridoxine

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Peptides Or Proteins (AREA)

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 method for crystallising of vitamin B6.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

For the device of evaporative crystallization, the method for crystallising of vitamin B6
Technical field
The present invention relates to chemical technology improvement areas, more particularly to a kind of device and vitamin B6 for evaporative crystallization Method for crystallising.
Background technique
Vitamin B6 is one of vitamin needed by human, is clinically mainly used for pyridoxine deficiency, also extensive As food, feed addictive, the huge market demand.
Currently, vitamin B6 crystallization mainly uses following several method:
A) usual way (Chinese Journal of Pharmaceuticals, 2004,35 (1): 1-2) are as follows: be dissolved in vitamin B6 crude product pure Change water, active carbon decoloring is added, filtrate is concentrated afterwards twice, cooling crystallization obtains crystallizing for the first time.Then first time is crystallized It is re-dissolved in water, active carbon decoloring is added, after carrying out third time decoloration, filtrate, crystallisation by cooling is concentrated, filtration drying obtains product.It is logical Product poor crystal form, the particle for crossing technique preparation are larger, and 40 mesh percent of pass are less than 40%, it is necessary to pulverization process.And it is smashed Product crystal is irregular, poor fluidity, is difficult to meet client's needs.
B) Chinese invention application CN102295598A discloses a kind of method for crystallising of vitamin B6, and this method first will 100g vitamin B6 crude product is dissolved in water, and 300~600mL ethyl alcohol is added into filtrate after active carbon decoloring, and crystallization filters, filter Cake ethanol washing, dry product.According to this although little particle, even-grained crystal can be obtained in method, but crystallizes using big The ethyl alcohol of amount, the industrial ethyl alcohol that recycles is at high cost, is not suitable for industrialized production.
C) Chinese invention application CN104710352A discloses a kind of method for crystallising of vitamin B6, specifically: dimension is given birth to Plain B6 crude product is dissolved in water, and after being decolourized, filtrate is concentrated, and concentrate is heated to 50~100 DEG C of dissolved clarifications, then by the concentration of the dissolved clarification Drop enters in 0-40 DEG C of vitamin B6 fine work saturated aqueous solution, and stirring and crystallizing obtains product.This method although can be obtained particle compared with Small, good fluidity crystal, but the concentrate of heat is instilled in cold saturated solution, due to temperature decrease, the growth of crystal The increase for not catching up with degree of supersaturation causes degree of supersaturation in solution to accumulate, and nucleus generation is excessive too fast, so that crystal package is miscellaneous Matter influences crystal quality.On the other hand, this method crystallizes the fine work that must all consume crude product amount 10~50% every time, and purification is total Yield is low (crystallization yield is lower than 60% after counting the fine work of consumption in), and economic cost is high.
To sum up, vitamin B6 crystallization production mostly uses andnon-continuous operation manner greatly at present, as evaporative crystallization, crystallisation by cooling and Dilution crystallization etc., device requirement amount is more, investment is big, production efficiency is low, and crystal particle diameter is difficult to control, and must crush through pulverization process Crystal poor fluidity afterwards, it is easy to reunite, it is unable to reach processing request.There is also product qualities between different batches for periodic crystallisation operation The big problem of difference.
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 The method for crystallising of vitamin B6, and the device for evaporative crystallization.
The present invention provides a kind of device for evaporative crystallization for 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 method for crystallising of vitamin B6 comprising following steps:
(1) the above-mentioned device for evaporative crystallization is provided;
(2) persistently inject material liquid to the material liquid inlet pipe, wherein in the material liquid vitamin B6 mass fraction It is 10%~50%, the temperature of the material liquid is 20 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 0.08MPa~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, wherein the crystalline particle includes that biggish first particle of partial size and partial size are lesser thin Brilliant 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, 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 B6 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 B6 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 method for crystallising of the vitamin B6 has the advantage that
Material liquid is crystallized, vitamin B6 crystalline 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.This method is provided with additional first circulation circuit, and the first fine grain is imported container for evaporation as nucleus, most again The second more uniform particle of more and size distribution is obtained eventually.This method crystallization yield reaches 85% or more, HPLC purity 99.8% or more, products obtained therefrom crystal face is smooth, good fluidity, even particle size, 40 99% or more mesh percent of pass.
Further, when being equipped with rectification clasfficiator in the crystallisation vessel, which can comb crystallisation vessel (no When with rectification clasfficiator) in chaotic Flow Field Distribution 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 rectifying clasfficiator In channel with rectification clasfficiator below form current difference, due to rectification clasfficiator below low flow velocity powerlessly persistently carry secretly it is larger Crystalline particle, so that biggish first particle precipitates during the low flow velocity fluid carry-over being rectified below clasfficiator, And be rectified the fine grain particle that liquid stream below clasfficiator is entrained to rectification clasfficiator passage proximate, then it can be rectified clasfficiator channel The liquid stream of interior high flow rate is carried secretly, and is recycled to imported into heater and reheated dissolution and circulation imported into container for evaporation and makees For nucleus.Whole process can reach screening, separation crystalline particle by adjusting size ratio above and below the percent opening in channel and channel Effect 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 0.1~0.9 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 also carries out large-scale industrial production.
Detailed description of the invention
Fig. 1 is the apparatus structure and flow diagram for evaporative crystallization of the embodiment of the present invention 1.
Fig. 2 is the apparatus structure and flow diagram 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, the fine grain particle of the part can be used as next week The crystallization nucleus of phase, to can induce to obtain crystalline particle more evenly.It should be noted that first fine grain can continue to grow up Bigger and the second particle more evenly is obtained, meanwhile, the first fine grain reenters crystallisation vessel 8 also and can induce second more Grain is formed in an orderly manner, that is to say, that the effect in the first circulation circuit is divided into two aspects: first is that making more second Particle is formed;Second is that the first fine grain 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 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 method for crystallising of vitamin B6.The method for crystallising the following steps are included:
(1) device for being used for evaporative crystallization is provided;
(2) persistently inject material liquid to the material liquid inlet pipe 1, wherein in the material liquid vitamin B6 mass fraction It is 10%~50%, the temperature of the material liquid is 20 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 0.08MPa~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 When, fine grain particle and mother liquor in the crystalline particle enter the recycle stock outlet pipe 12, and bifurcated, wherein the mother liquor Bifurcated be the first mother liquor and the second mother liquor, the fine grain particle bifurcated be the first fine grain and the second fine grain, first fine grain and First mother liquor flows into first and is in charge of 2a, and second fine grain and the second mother liquor flow into second and be in charge of 2b, the first particle sedimentation In 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 B6 finished product.
Wherein, the mass fraction of vitamin B6 is preferably 20%~35% in step (2) described material liquid, the material liquid Temperature be 40 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 1 hour~8 hours.The ratio of the charging rate of evaporation rate of solvent and the material liquid in the material liquid It is 0.1~0.9, preferably 0.35~0.75.This is because need to inject more material liquid when crystallization for the first time, So as to have enough vitamin B6s 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 53% 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 50 DEG C~70 DEG C.
During step (3) are evaporated, the vacuum degree of the container for evaporation 6 is preferably 0.085MPa~0.097MPa.
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 fine grain Particle and mother liquor are by rectifying clasfficiator 17 into the recycle stock outlet pipe 12.It is described rectification clasfficiator 17 effect be, So that fine grain particle enters recycle stock outlet pipe 12, and biggish first particle of particle still remains in the crystallisation vessel 8, most Realize that product particle is uniform eventually.It is appreciated that the bottom of the crystallisation vessel 8 can be set to conical region, in order to realize crystalline substance Body gradation 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) Time be 1 hour~8 hours.After first time exports magma by magma discharge port 15, the solvent in the material liquid steams The ratio of hair speed and the charging rate of the material liquid is turned down.By the original of the discharging speed of the magma of step (8) and step (2) The ratio of the charging rate of feed liquid is adjusted to 0.1~0.9.Residence time of material can evaporated crystallization device stable state according to the present invention Material total amount when operation is calculated divided by discharging speed.When preferably, in order to maintain suitable degree of supersaturation and stop Between, thus guarantee the even particle size distribution of final crystal grain, the discharging speed of the magma of step (8) and the raw material of step (2) The ratio of the charging rate of liquid is 0.25~0.65.
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 method for crystallising of the vitamin B6 has the advantage that
Material liquid is crystallized, vitamin B6 crystalline 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.
It will be further described below by method for crystallising of the embodiment to vitamin B6 of the present invention.
Vitamin B6 crude product purity range in the present embodiment selects between 98%-99%.
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 B6 crude product that HPLC purity is 98% is dissolved with water, is decolourized, that mass percent is obtained by filtration is dense The material liquid for the vitamin B6 that degree is 23%, temperature are 40 DEG C.
(2) heater 4 are pumped into the material liquid of vitamin B6 from material liquid inlet pipe 1, via 3 conveying of second circulation pump To heater 4, the temperature of material liquid is increased to 55 DEG C.Material liquid after heating, which continuously flows into evaporation with the speed of 220kg/h, to be held Device 6.
(3) vacuum degree for controlling container for evaporation 6 is 0.095MPa, reaches boiling-like after so that material liquid is entered container for evaporation 6 State, water evaporation rate maintain 141kg/h, and solvent largely evaporates, 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 141kg/h, second circulation pump 3 flow controls in 1200kg/h, and the flow control of first circulation pump 13 is in 318kg/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 55%, 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 79kg/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 220kg/h, first circulation pump In 294kg/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 vitamin B6 crystalline particle of white after drying, and HPLC purity is 99.96% with charging Meter, crystallization yield 89.10%, wherein 40 mesh percent of pass 100% of vitamin B6 crystalline particle, 60 mesh percent of pass 60%, 100 mesh percent of pass 4% meet CP2015, EP8.0, USP33 requirement.
Embodiment 2
The present embodiment using as shown in Figure 2 for evaporative crystallization device carry out crystallization operation, specifically according to the following steps into Row: (1) by HPLC purity be 98% vitamin B6 crude product dissolved with water, decolourized, mass percent concentration be obtained by filtration be The material liquid of 23% vitamin B6, temperature are 40 DEG C.
(2) heater 4 are pumped into the material liquid of vitamin B6 from material liquid inlet pipe 1, via 3 conveying of second circulation pump To heater 4, the temperature of material liquid is increased to 55 DEG C.Material liquid after heating, which continuously flows into evaporation with the speed of 220kg/h, to be held Device 6.The diameter of the upper end in channel 18 is 30 millimeters, and the diameter of the lower end in channel 18 is with the diameter ratio value of the upper end in channel 18 2:1, the percent opening in the channel are 20%.
(3) vacuum degree for controlling container for evaporation 6 is 0.095MPa, reaches boiling-like after so that material liquid is entered container for evaporation 6 State, water evaporation rate maintain 141kg/h, and solvent largely evaporates, 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 141kg/h, for the flow control of second circulation pump 3 in 1200kg/h, the flow control of first circulation pump 13 is described in 318kg/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 55%, 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 79kg/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 220kg/h, first circulation pump 13 Flow control in 294kg/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 obtain after drying white vitamin B6 crystalline particle, HPLC purity be 99.93%, with into Doses meter, crystallization yield 88.70%, wherein 40 mesh percent of pass 100% of vitamin B6 crystalline particle, 60 mesh percent of pass 44%, 100 mesh percent of pass 0.2% meet CP2015, EP8.0, USP33 requirement.
Embodiment 3
On the basis of embodiment 2, the flow velocity of step (3) first circulation pump 13 is set as 423kg/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 392kg/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 vitamin B6 crystalline particle of white after drying, and HPLC purity is 99.90%, with inlet amount Meter, crystallization yield 89.03%, wherein 40 mesh percent of pass 100% of vitamin B6 crystalline particle, 60 mesh percent of pass 80%, 100 mesh percent of pass 8%.
Embodiment 4
On the basis of embodiment 2, the flow velocity of step (3) first circulation pump 13 is set as 212kg/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 196kg/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 vitamin B6 crystalline particle of white after drying, and HPLC purity is 99.95%, with inlet amount Meter, crystallization yield 89.00%, wherein 40 mesh percent of pass 99.5% of vitamin B6 crystalline particle, 60 mesh percent of pass 50%, 100 mesh percent of pass 0.5%.
Embodiment 5
On the basis of embodiment 2, the flow velocity of step (3) first circulation pump 13 is set as 53kg/h, the first-class stock Flow and the ratio control of flow of the second stock be 0.05, step (4) taper decanting zone solid content reaches 54%, step Suddenly the flow control of (5) first circulation pump 13 is in 49kg/h, the flow of the first-class stock and the flow of the second stock Ratio control is 0.05;Remaining condition is the same as embodiment 2.Gained filter cake obtains the vitamin B6 crystallization of white after drying Grain, HPLC purity is 99.88%, to feed meter, crystallization yield 86.60%, wherein 40 mesh of vitamin B6 crystalline particle Percent of pass 100%, 60 mesh percent of pass 83%, 100 mesh percent of pass 14%.
Embodiment 6
On the basis of embodiment 2, the flow velocity of step (3) first circulation pump 13 is set as 1059kg/h, it is described first-class The ratio control of the flow of the flow and second stock of stock is 1, and step (4) taper decanting zone solid content reaches 53%, step Suddenly the flow control of (5) first circulation pump 13 is in 980kg/h, the flow of the first-class stock and the flow of the second stock Ratio control is 1;Remaining condition is the same as embodiment 2.Gained filter cake obtains the vitamin B6 crystalline particle of white after drying, HPLC purity is 99.85%, to feed meter, crystallization yield 85.50%, wherein 40 mesh of vitamin B6 crystalline particle are logical Cross rate 100%, 60 mesh percent of pass 84%, 100 mesh percent of pass 16%.
Embodiment 7
The present embodiment using as shown in Figure 2 for evaporative crystallization device carry out crystallization operation, specifically according to the following steps into Row:
(1) the vitamin B6 crude product that HPLC purity is 98% is dissolved with water, is decolourized, that mass percent is obtained by filtration is dense The material liquid for the vitamin B6 that degree is 30%, temperature are 60 DEG C.
(2) heater 4 are pumped into the material liquid of vitamin B6 from material liquid inlet pipe 1, via 3 conveying of second circulation pump To heater 4, the temperature of material liquid is increased to 66 DEG C.Material liquid after heating, which continuously flows into evaporation with the speed of 300kg/h, to be held Device 6.The diameter of the upper end in channel 18 is 30 millimeters, and the diameter of the lower end in channel 18 is with the diameter ratio value of the upper end in channel 18 2:1, the percent opening in the channel are 20%.
(3) vacuum degree for controlling container for evaporation 6 is 0.085MPa, reaches boiling-like after so that material liquid is entered container for evaporation 6 State, water evaporation rate maintain 157kg/h, and solvent largely evaporates, 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 157kg/h, for the flow control of second circulation pump 3 in 1500kg/h, the flow control of first circulation pump 13 is described in 268kg/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 54%, 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 143kg/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 300kg/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 0.2.
(6) gained filter cake obtain after drying white vitamin B6 crystalline particle, HPLC purity be 99.96%, with into Doses meter, crystallization yield 88.80%, wherein 40 mesh percent of pass 99% of vitamin B6 crystalline 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 vitamin B6 crystalline particle of white after drying, and HPLC purity is 99.94%, to feed meter, Crystallization yield is 88.40%, wherein 40 mesh percent of pass 99.5% of vitamin B6 crystalline particle, 60 mesh percent of pass 50%, and 100 Mesh percent of pass 5%.
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 vitamin B6 crystalline particle of white after drying, and HPLC purity is 99.96%, to feed meter, knot Brilliant yield is 87.80%, wherein 40 mesh percent of pass 100% of vitamin B6 crystalline particle, 60 mesh percent of pass 54%, 100 mesh are logical Cross rate 3%.
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 vitamin B6 crystalline particle of white after drying, and HPLC purity is 99.89%, to feed meter, Crystallization yield is 88.00%, wherein 40 mesh percent of pass 99.5% of vitamin B6 crystalline particle, 60 mesh percent of pass 49%, and 100 Mesh percent of pass 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 method for crystallising of vitamin B6, which is characterized in that itself the following steps are included:
(1) device as described in any one of claims 1 to 6 for evaporative crystallization is provided;
(2) material liquid is persistently injected to the material liquid inlet pipe, wherein the mass fraction of vitamin B6 is in the material liquid 10%~50%, the temperature of the material liquid is 20 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 0.08MPa~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, Crystalline particle and mother liquor are obtained, wherein the crystalline particle includes biggish first particle of partial size and the lesser fine grain of partial size Grain;
(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 B6 at Product.
8. the method for crystallising of vitamin B6 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 0.1~0.9, the charging of the discharging speed of the magma and the material liquid The ratio of speed is 0.1~0.9.
9. the method for crystallising of vitamin B6 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. the method for crystallising of vitamin B6 as claimed in claim 7, which is characterized in that during step (3) are evaporated, The material liquid flows into described second the second mother liquor for being in charge of after by the heater, temperature be increased to 30 DEG C~ 90℃。
11. the method for crystallising of vitamin B6 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. the method for crystallising of vitamin B6 as claimed in claim 7, which is characterized in that after step (8), will contain State the first particle and the second particle magma exported via magma discharge port after, obtain filter cake and centrifugation gained by centrifugation Mother liquor, and the mother liquid obtained recycling of the centrifugation is recycled to material liquid inlet pipe.
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CN109289235A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 Device, ascorbic method for crystallising for evaporative crystallization
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
CN110627177A (en) * 2019-09-26 2019-12-31 北京朗新明环保科技有限公司 Fluorine removal method for fluorine-containing wastewater and fluidized bed crystallization separator for fluorine removal
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CN109289235A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 Device, ascorbic method for crystallising for evaporative crystallization
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
CN109289235B (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 C
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
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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
CN110627177A (en) * 2019-09-26 2019-12-31 北京朗新明环保科技有限公司 Fluorine removal method for fluorine-containing wastewater and fluidized bed crystallization separator for fluorine removal
CN114377424A (en) * 2022-01-24 2022-04-22 国家能源集团宁夏煤业有限责任公司 Suspension concentration evaporation device

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