CN204400884U - 1,5-pentamethylene diamine continuously purification device - Google Patents
1,5-pentamethylene diamine continuously purification device Download PDFInfo
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- CN204400884U CN204400884U CN201420811335.7U CN201420811335U CN204400884U CN 204400884 U CN204400884 U CN 204400884U CN 201420811335 U CN201420811335 U CN 201420811335U CN 204400884 U CN204400884 U CN 204400884U
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Abstract
The utility model provides a kind of 1,5-pentamethylene diamine continuously purification device, wherein said purifying plant (100) at least comprises flasher (2), for flash distillation 1, the mixture of 5-pentamethylene diamine solution and high boiling solvent obtains containing the gaseous mixture of 1,5-pentamethylene diamine and water vapour and containing the first parting liquid of salt and high boiling solvent; Leach unit (3), be connected with described flasher (2), in the first parting liquid for outflow from described flasher (2), leach high boiling solvent; With rectifying tower (4), be connected with described flasher (2), for the mixture containing pentamethylene diamine and water vapour that rectifying flashes off from described flasher (2).Continuously purification device of the present utility model, effectively can reduce production cost and promote evaporation purification efficiency, enhancing productivity, reduce production cost, obtain the pentamethylene diamine that purity is higher.
Description
Technical field
The utility model relates to purification techniques field, espespecially by the purification of obtained 1, the 5-pentamethylene diamine of biological process.
Background technology
The main application of 1,5-pentamethylene diamine comprises superpolymer preparation, organic synthesis intermediate, epoxy curing agent, also for biological study.Wherein, synthetic nylon polymkeric substance is 1, an important application of 5-pentamethylene diamine, from 1,5-pentamethylene diamine sets out, can the nylon product nylon 54,510,512 etc. of synthetic nylon 56,5T or full bio-based, these products can be applied in the many aspects of the daily productive lifes such as electronic apparatus, mechanical means, trolley part.The index such as color, performance of quality on final polymkeric substance as 1, the 5-pentamethylene diamine of polymerization single polymerization monomer itself has vital impact.Usual biological process is produced 1,5-pentamethylene diamine and is referred to and produce 1,5-pentamethylene diamine through fermentation direct production or Methionin through decarboxylase decarboxylation, is then separated from the fermented liquid containing 1,5-pentamethylene diamine salt or enzyme reaction solution and obtains target product.But current Biological preparation 1,5-pentamethylene diamine is in the starting stage at home and abroad, less to the preparation research of the finished product of 1,5-pentamethylene diamine, carries out being separated to 1,5-pentamethylene diamine crude product, purifying, the device of rectifying and system also rarely have report.Due to 1,5-pentamethylene diamine has certain corrodibility, its fermentation broth contents is complicated, wherein a large amount of organic/inorganic impurity can be contained, its separating difficulty is very large, therefore production method and the production unit of other chemical of abstraction and purification in prior art is directly applied mechanically, not only can not obtain good separation and purification effect, also comparatively large to the damage of equipment, can not 1 be met, the requirement of 5-pentamethylene diamine purifying, thus causing production efficiency low, production cost is high, and product purity does not reach high request, seriously constrain the application of 1,5-pentamethylene diamine in nylon production and other field.
In existing separation and evaporation technology design, from stock liquid, evaporate chemical generally adopt intermittent type method of evaporation, this method can not realize the continuous operation produced, product can be caused in process of production to waste, also detrimentally affect can be caused to the stability of product quality simultaneously, therefore more evaporation 1 can not be met, the requirement of 5-pentamethylene diamine, evaporation 1 can be caused, during 5-pentamethylene diamine, production efficiency is lower, production cost is higher, 1, 5-pentamethylene diamine purity does not reach requirement yet, and in production 1, a large amount of salt can be produced in 5-pentamethylene diamine process, to the damage comparatively large equipment well damage of equipment, maintenance cost is higher, therefore actual production is unsuitable for, need to develop the equipment that matches with technique and carry out penta 1, the separation and purification of 5-diamines.
Utility model content
In order to solve the problem, the utility model provides a kind of to containing 1, the stock liquid of 5-pentamethylene diamine salt carries out consecutive evaporation and purifies 1, the device of 5-pentamethylene diamine, this device high efficiency separation can go out 1,5-pentamethylene diamine, and avoids the impact of a large amount of salt of separating out in stock liquid, its reasonable in design, production efficiency are high, production cost is lower, and quality product can meet production requirement.
The utility model provides a kind of pentamethylene diamine continuously purification device 100 on the one hand, at least comprise: flasher 2, mixture for flash distillation 1,5-pentamethylene diamine solution and high boiling solvent obtains containing the gaseous mixture of 1,5-pentamethylene diamine and water vapour and containing the first parting liquid of salt and high boiling solvent; Leach unit 3, be connected with described flasher 2, in the first parting liquid for outflow from described flasher 2, leach high boiling solvent; With rectifying tower 4, be connected with described flasher 2, for the mixture containing 1,5-pentamethylene diamine and water vapour that rectifying flashes off from described flasher 2.
According to a kind of embodiment of the present utility model, 1,5-described pentamethylene diamine continuously purification device 100, also comprises: adjustment tank 1, comprise 1,5-pentamethylene diamine stock liquid opening for feed 11, alkali lye feeding mouth 12 and alkali tune materials feeding mouth 13, for alkalizing, 1,5-pentamethylene diamine stock liquid forms 1,5-pentamethylene diamine solution is for alkalizing 1,5-pentamethylene diamine stock liquid forms 1,5-pentamethylene diamine solution, and the discharge port of described adjustment tank 1 is connected with the opening for feed of described flasher 2; High boiling solvent storage tank 14, is connected with the opening for feed of described flasher 2, for storing high boiling solvent; Withdrawing can 7, is connected with the described unit 3 that leaches, for leaching the high boiling solvent that unit 3 leaches described in reclaiming; With holding tank 8, be connected with described rectifying tower 4, for collecting described rectifying tower 4 rectifying 1,5-pentamethylene diamine out.
According to another kind of embodiment of the present utility model, described 1,5-pentamethylene diamine continuously purification device 100, also comprise and be connected to described flasher 2 and the described setting tank 5 leached between unit 3, obtain the second parting liquid of high boiling solvent and saliferous for separating of isolated described first parting liquid of described flasher 2.
According to another kind of embodiment of the present utility model, 1,5-pentamethylene diamine continuously purification device 100, the high boiling solvent discharge port 53 of wherein said setting tank 5 is connected with the opening for feed 21 of described flasher, and the high boiling solvent that described setting tank 5 is separated enters described flasher 2 from described setting tank 5.
According to another kind of embodiment of the present utility model, 1,5-pentamethylene diamine continuously purification device 100, also comprise be connected to described setting tank 5 and described leach between unit 3 except salt pump 52, described in being sent into by the second parting liquid of described saliferous, leach unit 3.
According to another kind of embodiment of the present utility model, described 1,5-pentamethylene diamine continuously purification device 100, also comprise the heating unit 6 be connected between described setting tank 5 discharge port and described flasher 2 opening for feed, for heating the high boiling solvent in described high boiling solvent storage tank 4, described heating unit 6 discharge port is connected with described flasher 2 opening for feed, described heating unit 6 opening for feed is connected with the high boiling solvent discharge port of described high boiling solvent storage tank 4 and described setting tank 5 respectively, and described heating unit 6 is well heater or interchanger.
According to another kind of embodiment of the present utility model, 1,5-described pentamethylene diamine continuously purification device 100, wherein said flasher 2 is the flasher of single flasher or multiple parallel connection.
According to another kind of embodiment of the present utility model, 1,5-described pentamethylene diamine continuously purification device 100, the wherein said unit 3 that leaches is for whizzer or plate-and-frame filter press.
According to another kind of embodiment of the present utility model, 1,5-described pentamethylene diamine continuously purification device 100, wherein said 1, in the gaseous mixture of 5-pentamethylene diamine and water vapour containing weight percent not higher than 10% described high boiling solvent, preferably not higher than 5%, more preferably no higher than 3%.
According to the utility model relates to 1,5-pentamethylene diamine continuously purification device, this continuously purification device by flasher to 1,5-pentamethylene diamine stock liquid carries out continuous print flash evapn, and removes the solid salt of separating out in flasher in time, can effectively avoid a large amount of solid salt to evaporating 1, the impact of 5-pentamethylene diamine, and the rectifying tower by being connected, 1, the 5-pentamethylene diamine rectifying liquid be further purified can be obtained; By leaching the recycle and reuse of unit to high boiling solvent, effectively can reduce production cost and promoting evaporation purification efficiency, enhancing productivity, reduce production cost, finally can obtain 1, the 5-pentamethylene diamine that purity is higher.
Accompanying drawing explanation
Describe its example embodiment in detail by referring to accompanying drawing, above-mentioned and further feature of the present utility model and advantage will become more obvious.
Fig. 1 is 1,5-pentamethylene diamine continuously purification device structural representation of the present utility model.
Wherein, description of reference numerals is as follows:
1 adjustment tank, 11 pentamethylene diamine stock liquid opening for feeds, 12 alkali lye opening for feeds, 13 alkali tune materials mouths, 14 high boiling solvent storage tanks, 2 flashers, 21 flasher opening for feeds, 3 leach unit, 4 rectifying tower, 5 setting tanks, 51 pumps, 52 pumps, 53 high boiling solvent discharge ports, 6 heating units, 7 withdrawing cans, 8 holding tanks
Embodiment
In the utility model, " pentamethylene diamine stock liquid " refers to that composition contains the solution of 1,5-pentamethylene diamine salt and non-volatile organic/inorganic impurity.Wherein 1,5-pentamethylene diamine salt is the salt that 1,5-pentamethylene diamine and one or more acid are formed, and one or more acid can be one in organic acid and mineral acid or mixture.Such as, mineral acid includes, but not limited to hydrochloric acid, sulfuric acid, carbonic acid, phosphoric acid.Such as, organic acid includes, but not limited to thapsic acid, hexanodioic acid, acetic acid.Non-volatile inorganic impurity comprises one or more inorganic salt.Non-volatile organic impurity comprises by the carbohydrate fermented or enzymatic conversion process is introduced, protein, pigment and other organism remaining.Pentamethylene diamine stock liquid can be the initial fermented liquid containing 1,5-pentamethylene diamine salt or enzymatic conversion liquid, also can be through except thalline, decolouring, pretreated fermented liquid or the enzymatic conversion liquid containing 1,5-pentamethylene diamine salt such as concentrated.
" pentamethylene diamine " mentioned in the utility model all refers to " 1,5-pentamethylene diamine ".
continuously purification device
Pentamethylene diamine continuously purification device shown in Fig. 1, adds the pentamethylene diamine stock liquid of alkali lye and high boiling solvent for purifying continuously, comprises adjustment tank 1, flasher 2, leaches unit 3 and rectifying tower 4.Adjustment tank 1 is connected with the opening for feed 21 of flasher 2 respectively with high boiling solvent storage tank 14, the pentamethylene diamine stock liquid of alkalization and high boiling solvent are sent into flasher 2, and flash distillation obtains the gaseous mixture containing pentamethylene diamine and water vapour and contains the first parting liquid of salt and high boiling solvent.Mixture containing pentamethylene diamine and water vapour is admitted to rectifying tower 4 and purifies further, and the first parting liquid enters and leaches unit 3 and leach high boiling solvent to recycle.Leach unit 3 to circulate with flasher 2 and be connected (not shown), namely leach unit 3 discharge port and be connected with the opening for feed of flasher 2, the high boiling solvent leached is delivered in flasher 2 and recycles.Leach unit 3 also not circulate with flasher 2 and be connected, and use other device, such as withdrawing can 7 collects the high boiling solvent that leaches to recycle.
Adjustment tank 1 is for the pentamethylene diamine stock liquid that alkalizes.The pH value that pentamethylene diamine stock liquid, alkali lye enter Mixed adjustment mixed solution in adjustment tank 1 respectively by pentamethylene diamine stock liquid opening for feed 11 and alkali lye opening for feed 12 is more than or equal to 12, if pH is less than 12 add the pH value of alkali tune materials adjustment mixed solution to being more than or equal to 12 by alkali tune materials mouth 13.
The alkali lye of alkalization pentamethylene diamine stock liquid can be include but not limited in alkaline metal oxide/hydroxide, alkaline earth metal oxide/oxyhydroxide and corresponding basic salt (such as sodium phosphate, potassiumphosphate, sodium carbonate, salt of wormwood etc.) one or more.When alkali joins pentamethylene diamine salt brine solution composition, can disposable input also can repeatedly drop into.If drop into multiple alkali, drop into again after first alkali can being mixed into mixture, also can add often kind of alkali respectively.One or more highly basic and one or more weak base can be comprised in alkali mixture.Highly basic and weak base mixture include but not limited to, the mixture of sodium phosphate and sodium hydroxide, and the mixture of sodium carbonate, sodium hydroxide and potassium hydroxide.Highly basic mixture can be the mixture of one or more highly basic.Alkali mixture includes but not limited to, the mixture of sodium hydroxide and potassium hydroxide.Alkali can add with the form of solid and/or solution (as the aqueous solution).The usage quantity of alkali, as long as substantially all can be converted into pentamethylene diamine by the pentamethylene diamine salt in stock liquid.Alkali can add in pentamethylene diamine stock liquid at any suitable temperature, as long as pentamethylene diamine salt energy conversion energy pentamethylene diamine at such a temperature.
Alkali tune materials can be above-mentioned solid alkali and/or alkaline solution, can be that the alkali identical from alkali lye also can be different.
High boiling solvent can be comprise any polar solvent, one or more in non-polar solvent, and boiling point is higher than the boiling point of pentamethylene diamine, and such as boiling point is more than 185 degree.In flasher 2, the usage ratio of high boiling solvent and pentamethylene diamine stock liquid does not limit.High boiling solvent should not react under evaporation/distillation condition, and does not affect the quality of pentamethylene diamine.The solvent do not reacted refer in evaporation/still-process weight percent be less than 2% high boiling solvent and pentamethylene diamine react.High boiling solvent includes but not limited to, alkane, chloroparaffin, benzene derivative, alcohol, ether, amine, ester, in nitrile one or more.Such as, suitable chloroparaffin includes, but not limited to the C that chlorine atomic component replaces hydrogen atom
nalkane, n=12,13,14,15,16,17,18,19,20, (preferably, 1-chlorododecane, the 1-chlorine tetradecane, and composition).Such as, suitable benzene derivative includes, but not limited to one or more alkyl C
n, benzene (preferably, dodecylbenzene, Tetradecylbenzene, toluene dichloride, and composition), biphenyl and composition thereof after the chloro deriveding group replacement of n=11,12,13,14,15, or 16 or abovementioned alkyl.Such as, suitable alcohol includes, but not limited to C
nalkyl alcohol, n=8,9,10,11,12,13,14,15,16,17,18,19, or 20 (preferably, 1-octanol, lauryl alcohol, tetradecyl alcohol, glycerine, and composition).Such as, suitable ether includes, but not limited to phenyl ether.Such as, suitable amine includes, but not limited to C
nalkylamine, C
nalkyl polyamine, c=10,11,12,13,14,15,16,17,18,19, or 20 (preferably, hexanediamine, decamethylene diamines, and composition).Such as, suitable ester includes, but not limited to diethyl succinate, diethylene adipate, and composition.Such as, suitable nitrile includes, but not limited to succinonitrile, adiponitrile, and composition.
Flasher 2 can be an independent flasher, also can be several flashers in parallel, and the flasher 2 shown in Fig. 1 is the flasher arranged separately.Leaching unit 3 can be whizzer or plate-and-frame filter press, or other equipment for separating liquid from solid, and the unit that leaches shown in Fig. 1 is whizzer.Rectifying tower 4 can be any can the rectifying tower of rectifying pentamethylene diamine, the pentamethylene diamine of purifying from rectifying tower 4 can be stored into holding tank 8.
Pentamethylene diamine continuously purification device can also comprise the setting tank 5 being connected to flasher 2 and leaching between unit 3, for the first parting liquid that initial gross separation is discharged from flasher 2, by settlement separate go out high boiling solvent and the second parting liquid containing salt and high boiling solvent.The high boiling solvent discharge port 53 of setting tank 11 is connected with the opening for feed 21 of flasher 2, and high boiling solvent separation obtained is sent in flasher 2 and recycled.The second parting liquid separated in setting tank 5 enters and leaches unit 3.
Pentamethylene diamine continuously purification device can also comprise the pump 52 being connected to setting tank 5 and leaching between unit 3, unit 3 is leached for being separated second to send into night, salt and high boiling solvent separate through leaching unit 3 by the second parting liquid, and supernatant fraction is circulated to high boiling solvent storage tank 14 or direct circulation adds flasher 2.High boiling solvent in setting tank 5 is recycled into flasher, and therefore high boiling solvent discharge port position is the position that most of solvent can be made to pump, and usually in the upper middle portion of tank, but specifically will determine according to the ratio precipitated in the first parting liquid; Salt outlet is usually in bottom.
Pentamethylene diamine continuously purification device can also comprise heating unit 6, and heating unit 6 can circulate with flasher 2 and be connected, or circulates successively with flasher 2, setting tank 5 and be connected.Namely the discharge port of heating unit 6 is connected with the opening for feed of flasher, and the opening for feed of heating unit 6 is connected (not shown) with the discharge port of flasher 2; Or the discharge port of heating unit 6 is connected with the opening for feed 21 of flasher 2, the discharge port of flasher 2 is connected with the opening for feed of setting tank 5, and the discharge port of setting tank 5 is connected (as shown in Figure 1) with the opening for feed of heating unit 6.The opening for feed of heating unit 6 connects the discharge port of high boiling solvent storage tank 14 and the high boiling solvent discharge port of setting tank 5 respectively, from flasher 2 or setting tank 5, high boiling solvent out enters heating unit 6, and heating unit 6 heating enters into the high boiling solvent of flasher 2.Heating unit 6 can be well heater or interchanger.
In the process of circulating and evaporating, containing in the gaseous mixture of pentamethylene diamine and water of separating in flasher 2 also contains constant concentration weight percent not higher than 10%, preferably not higher than 5%, more preferably no higher than the high boiling solvent of 3%, holding in liquid of flasher 2 also comprises the pentamethylene diamine that constant concentration weight percent is 1%-10%, preferred 3%-5%.
continuous method of purification
The utility model can be purified pentamethylene diamine continuously by following steps:
Flash steps: as shown in Figure 1, carry out concentrated pretreated pentamethylene diamine stock liquid and alkali lye and enter adjustment tank 1 respectively by pentamethylene diamine stock liquid opening for feed 11 and alkali lye opening for feed 12 by pentamethylene diamine stock liquid or for raising the efficiency and be uniformly mixed, if the pH value of mixed solution is less than 12, so alkali tune materials is joined in adjustment tank 5 by alkali tune materials mouth and regulate the pH value of mixed solution to being more than or equal to 12.
The alkali lye added or alkaline matter can be include but not limited in alkaline metal oxide/hydroxide, alkaline earth metal oxide/oxyhydroxide and corresponding basic salt (such as sodium phosphate, potassiumphosphate, sodium carbonate, salt of wormwood etc.) one or more.When alkali joins pentamethylene diamine salt brine solution composition, can disposable input also can repeatedly drop into.If drop into multiple alkali, drop into again after first alkali can being mixed into mixture, also can add often kind of alkali respectively.One or more highly basic and one or more weak base can be comprised in alkali mixture.Highly basic and weak base mixture include but not limited to, the mixture of sodium phosphate and sodium hydroxide, and sodium carbonate, sodium hydroxide, potassium hydroxide and calcium hydroxide, calcium oxide mixture.Highly basic mixture can be the mixture of one or more highly basic.Alkali mixture includes but not limited to, the mixture of sodium hydroxide and potassium hydroxide.Alkali can add with the form of solid and/or solution (as the aqueous solution).The usage quantity of alkali, as long as substantially all can be converted into pentamethylene diamine by the pentamethylene diamine salt in stock liquid.Alkali can add in pentamethylene diamine stock liquid at any suitable temperature, as long as pentamethylene diamine salt energy conversion energy pentamethylene diamine at such a temperature.
Alkali tune materials can be above-mentioned solid alkali and/or alkaline solution, can be that the alkali identical from alkali lye also can be different.
Mixed solution in adjustment tank 1 and the high boiling solvent of high boiling point storage tank 14 enter flasher 2 by the opening for feed 21 of flasher 2 and carry out flash distillation, and evaporation obtains the gaseous mixture containing pentamethylene diamine and water vapour and contains the first parting liquid of salt and high boiling solvent.
The high boiling solvent added in flasher 2 can be comprise any polar solvent, one or more in non-polar solvent, and boiling point is higher than the boiling point of pentamethylene diamine.High boiling solvent should not react under evaporation/distillation condition, and does not affect the quality of pentamethylene diamine.The solvent do not reacted refer in evaporation/still-process weight percent be less than 2% high boiling solvent and pentamethylene diamine react.High boiling solvent includes but not limited to, alkane, chloroparaffin, benzene derivative, alcohol, ether, amine, ester, in nitrile one or more.Such as, suitable chloroparaffin includes, but not limited to the C that chlorine atomic component replaces hydrogen atom
nalkane, n=12,13,14,15,16,17,18,19,20, (preferably, 1-chlorododecane, the 1-chlorine tetradecane, and composition).Such as, suitable benzene derivative includes, but not limited to one or more alkyl C
n, benzene (preferably, dodecylbenzene, Tetradecylbenzene, toluene dichloride, and composition), biphenyl and composition thereof after the chloro deriveding group replacement of n=11,12,13,14,15, or 16 or abovementioned alkyl.Such as, suitable alcohol includes, but not limited to C
nalkyl alcohol, n=8,9,10,11,12,13,14,15,16,17,18,19, or 20 (preferably, 1-octanol, lauryl alcohol, tetradecyl alcohol, glycerine, and composition).Such as, suitable ether includes, but not limited to phenyl ether.Such as, suitable amine includes, but not limited to C
nalkylamine, C
nalkyl polyamine, c=10,11,12,13,14,15,16,17,18,19, or 20 (preferably, hexanediamine, decamethylene diamines, and composition).Such as, suitable ester includes, but not limited to diethyl succinate, diethylene adipate, and composition.Such as, suitable nitrile includes, but not limited to succinonitrile, adiponitrile, and composition.
In flasher, the temperature and pressure of 2 is any conditions of applicable pentamethylene diamine flash separation, can be but not be defined as, and such as, pressure is-0.09MPa ~ 0MPa, and temperature is 110 ~ 200 degrees Celsius.
Pump 15 can also be connected with adjust between tank 1 and flasher 2, for by the pentamethylene diamine mixed solution feeding flasher 2 containing alkalization according to adjustment tank 1 and flasher 2 relative position.Certainly, if the position of adjustment tank 1 is higher than flasher 2, the mixed solution in adjustment tank 1 just can be made under gravity to flow in flasher 2, therefore between adjustment tank 1 and flasher 2, just need not pump be set.Those skilled in the art can arrange other device of the smooth charging of any guarantee according to the actual needs between adjustment tank 1 and flasher 2, can be but be not limited to, such as pump, throttling valve, sensor.
Rectification step: the mixture containing pentamethylene diamine and water vapour that flasher 2 is evaporated enters rectifying tower 4 rectification and purification further.
Reclaim high boiling solvent step: the first parting liquid of saliferous and high boiling solvent enters and leaches unit 3 (whizzer), after centrifugal, the first parting liquid obtains the second parting liquid of high boiling solvent and saliferous and high boiling solvent, and the high boiling solvent obtained is admitted to flasher 2 and recycles.Or the first parting liquid is introduced into setting tank 5, the first parting liquid is separated into high boiling solvent and the second parting liquid containing salt and high boiling solvent through the sedimentation of setting tank 5; The high boiling solvent that separation obtains is admitted to flasher 2 and recycles; Second parting liquid is sent in whizzer centrifugal except salt pump 52, then the high boiling solvent that centrifuge obtains is circulated to high boiling solvent storage tank 14 or sends into flasher 2 to recycle.
Heating steps: the high boiling solvent of the high boiling solvent flowed out from flasher 2 or setting tank 5 and outflow from high boiling solvent storage tank 14 heats by heating unit 6, then the high boiling solvent after heating is sent into flasher 2.Heating unit 6 can be well heater or interchanger.
In the process of circulating and evaporating, containing in the gaseous mixture of pentamethylene diamine and water of separating in flasher also contains constant concentration weight percent not higher than 10%, preferably not higher than 5%, more preferably no higher than the high boiling solvent of 3%, also constant concentration weight percent 1%-10% is comprised, the pentamethylene diamine of preferred 3%-5% in flasher.
control method
The concentration of pentamethylene diamine stock liquid is 2%-15%, and form the pentamethylene diamine solution containing free state pentamethylene diamine by the adjustment adjusting tank 1, be admitted to flasher 2, this pentamethylene diamine solution can heat before entering flasher 2, also can not heat.Temperature and pressure in reasonable set flasher 2 and suitable input speed, make pentamethylene diamine and water fully be evaporated in flasher 2.When continuously purification device brings into operation, what obtain through flasher 2 evaporation enters rectifying tower 4 continuously with the mixture of water vapour be separated containing pentamethylene diamine, the first parting liquid containing salt and high boiling solvent and a small amount of water then flows out from flasher 2, precipitated tank 5 receives gradually, in setting tank 5, first parting liquid starts layering, salt and part high boiling solvent are positioned at (i.e. the second parting liquid bottom setting tank, be generally solidliquid mixture state), other high boiling solvents are then positioned at solution upper strata.This part high boiling solvent can flow out from setting tank 5, and circulation enters flasher 2 and reuses, or enters flasher 2 after heating unit 6 heats.When the second parting liquid of rich salt reaches certain liquid level in setting tank 5, except salt pump 52 starts, by second parting liquid interval or send into whizzer continuously, salt and high boiling solvent separate through whizzer by the second parting liquid, and supernatant fraction is circulated to high boiling solvent storage tank or direct circulation adds flasher 2.Finally, in the product that rectifying obtains from rectifying tower 4, the concentration of pentamethylene diamine is more than 78%, and preferably more than 95%.
embodiment 1
As shown in Figure 1, the continuously purification device of the present embodiment comprises adjustment tank 1, high boiling solvent storage tank 14, flasher 2, leaches unit 3, rectifying tower 4, setting tank 5, heating unit 6, withdrawing can 7, holding tank 8 and pump 15,51,52.In the present embodiment, heating unit 6 is well heater.
Concentration be 9.1% pentamethylene diamine stock liquid by opening for feed 11 enter adjustment tank 1 in, alkali lye such as 50% sodium hydroxide enters the pH value of solution in adjustment adjustment tank 1 in adjustment tank 1 by alkali lye opening for feed 12, detect the pH value of solution in adjustment tank 1, if the pH value of solution does not reach reservation scope in adjustment tank 1, adding the pH of alkali tune materials such as 10% sodium hydroxide adjustment solution to being greater than 13.5 by alkali tune materials entrance 14, then by pump 15, this solution being sent in flasher 2.
The high boiling solvent flowed out from high boiling solvent storage tank 14 enters in well heater, and well heater heats high boiling solvent, after high boiling solvent reaches preset temperature, flows out from well heater, enters in flasher 2.
Adjustment enters the input speed of high boiling solvent and pentamethylene diamine solution in flasher 2, pentamethylene diamine and water are evaporated fully in flasher 2, the vaporization temperature in flasher 2 can be such as about 180 degree, evaporating pressure can be such as-0.09MPa (gauge pressure).Flasher 2 flash separation obtains the gaseous mixture of pentamethylene diamine and water, and contains the first parting liquid of salt and high boiling solvent.
The pentamethylene diamine flashed off and the mixture of water enter rectifying tower 4 rectification and purification further.In the rectifying liquid that rectifying tower 4 flows out, the concentration of pentamethylene diamine is up to 95%.
First parting liquid is admitted to setting tank 5, and in setting tank 5, the first parting liquid sedimentation obtains the second parting liquid that salt and high boiling solvent are contained in the high boiling solvent on upper strata and lower floor.The high boiling solvent on upper strata is admitted in well heater by pump 51, recycles by being admitted to flasher 2 after heater heats to preset temperature.
Heating unit 6 also can be interchanger (not marking in figure), in setting tank 5 reclaim high boiling solvent and high boiling solvent storage tank 14 in high boiling solvent enter from two of interchanger opening for feeds respectively, after carrying out heat exchange, flow out from two discharge ports corresponding with two opening for feeds and together enter flasher.Second parting liquid by pump 52 be admitted to leach in unit 3 such as whizzer centrifugal.
Leach unit 3, such as whizzer, obtain high boiling solvent by centrifugal for the second parting liquid, the centrifugal high boiling solvent obtained can be collected by holding tank 7.
According to the pentamethylene diamine continuously purification device that the utility model relates to, this continuously purification device reasonable in design, continuous print flash evapn is carried out to containing pentamethylene diamine mixed solution by flasher 2, and remove the salt of precipitation in time, can effectively avoid a large amount of solid salt on the impact of evaporation pentamethylene diamine, and the rectifying tower 4 by being connected, the pentamethylene diamine rectifying liquid be further purified can be obtained; By setting tank 5 and the recycle and reuse leaching unit 3 pairs of high boiling solvents, effectively can reduce production cost and promote evaporation purification efficiency, this device production efficiency is higher, and production cost is lower, finally can obtain the very high pentamethylene diamine of purity.
Below illustrative embodiments of the present utility model is illustrate and described particularly.Should be appreciated that, the utility model is not limited to disclosed embodiment, and on the contrary, the utility model intention contains the various amendment and equivalent replacement that comprise within the scope of the appended claims.
Claims (8)
1. a pentamethylene diamine continuously purification device (100), is characterized in that, at least comprise:
Flasher (2), the mixture for flash distillation 1,5-pentamethylene diamine solution and high boiling solvent obtains containing the gaseous mixture of 1,5-pentamethylene diamine and water vapour and containing the first parting liquid of salt and high boiling solvent;
Leach unit (3), be connected with described flasher (2), in the first parting liquid for outflow from described flasher (2), leach high boiling solvent; With
Rectifying tower (4), is connected with described flasher (2), for the mixture containing 1,5-pentamethylene diamine and water vapour that rectifying flashes off from described flasher (2).
2. 1,5-pentamethylene diamine continuously purification device (100) according to claim 1, also comprises:
Adjustment tank (1), comprise 1,5-pentamethylene diamine stock liquid opening for feed (11), alkali lye feeding mouth (12) and alkali tune materials feeding mouth (13), for alkalizing 1,5-pentamethylene diamine stock liquid forms 1,5-pentamethylene diamine solution, the discharge port of described adjustment tank (1) is connected with the opening for feed of described flasher (2);
High boiling solvent storage tank (14), is connected with the opening for feed of described flasher (2), for storing high boiling solvent;
Withdrawing can (7), is connected with the described unit (3) that leaches, for leaching the high boiling solvent that unit (3) leaches described in reclaiming; With
Holding tank (8), is connected with described rectifying tower (4), for collecting described rectifying tower (4) rectifying 1,5-pentamethylene diamine out.
3. according to claim 1 and 21,5-pentamethylene diamine continuously purification device (100), also comprise and be connected to described flasher (2) and the described setting tank (5) leached between unit (3), obtain the second parting liquid of high boiling solvent and saliferous for separating of isolated described first parting liquid of described flasher (2).
4. according to claim 31,5-pentamethylene diamine continuously purification device (100), the high boiling solvent discharge port (53) of wherein said setting tank (5) is connected with the opening for feed (21) of described flasher, and the high boiling solvent that described setting tank (5) is separated enters described flasher (2) from described setting tank (5).
5. according to claim 31,5-pentamethylene diamine continuously purification device (100), also comprise be connected to described setting tank (5) and described leach between unit (3) except salt pump (52), described in being sent into by the second parting liquid of described saliferous, leach unit (3).
6. according to claim 31, 5-pentamethylene diamine continuously purification device (100), also comprise the heating unit (6) be connected between described setting tank (5) discharge port and described flasher (2) opening for feed, for heating the high boiling solvent in described high boiling solvent storage tank (4), described heating unit (6) discharge port is connected with described flasher (2) opening for feed, described heating unit (6) opening for feed is connected with the high boiling solvent discharge port of described high boiling solvent storage tank (4) and described setting tank (5) respectively, described heating unit (6) is well heater or interchanger.
7. 1,5-pentamethylene diamine continuously purification device (100) according to claim 1, the flasher that wherein said flasher (2) is single flasher or multiple parallel connection.
8. 1,5-pentamethylene diamine continuously purification device (100) according to claim 1, the wherein said unit (3) that leaches is for whizzer or plate-and-frame filter press.
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| CN107043331A (en) * | 2016-02-06 | 2017-08-15 | 上海凯赛生物技术研发中心有限公司 | The extracting method of one kind 1,5- pentanediamines |
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| CN107043332A (en) * | 2016-02-06 | 2017-08-15 | 上海凯赛生物技术研发中心有限公司 | A kind of extracting method of 1,5- pentanediamines |
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