CN102351731B - Acetaminophen refining mother liquid recycling device and recycling method - Google Patents
Acetaminophen refining mother liquid recycling device and recycling method Download PDFInfo
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- CN102351731B CN102351731B CN2011102369905A CN201110236990A CN102351731B CN 102351731 B CN102351731 B CN 102351731B CN 2011102369905 A CN2011102369905 A CN 2011102369905A CN 201110236990 A CN201110236990 A CN 201110236990A CN 102351731 B CN102351731 B CN 102351731B
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Abstract
The invention provides an acetaminophen refining mother liquid recycling device and recycling method. The invention is characterized in that the acetaminophen refining mother liquid recycling device comprises a mother liquid injection device, an adsorption-desorption device, a compressed gas injection device, a desorption acid injection device and an eluent recycling device, wherein the mother liquid injection device provides mother liquid with acetaminophen; the adsorption-desorption device performs adsorption and desorption on the acetaminophen in the mother liquid which is injected by the mother liquid injection device in a first direction; the compressed gas injection device injects compressed gas in the adsorption-desorption device to blow the adsorbed mother liquid in the adsorption-desorption device out of the adsorption-desorption device; the desorption acid injection device injects a desorption acid in the adsorption-desorption device in a second direction; and the eluent recycling device is communicated with the adsorption-desorption device to recycle the desorbed eluent. By utilizing the recycling device, the recycling cost of acetaminophen can be reduced, energy can be saved, the recycling quality of acetaminophen can be increased and the benefit can be increased.
Description
Technical field
The present invention relates to a kind of paracetamol treatment facility and treatment process, particularly a kind of acetaminophen refining mother liquid recycling device and recovery and treatment method.
Background technology
As a kind of bulk drug, often must just can obtain quality through refining art breading in water through the synthetic paracetamol crude product obtained of various approach and meet the product that pharmacopeia requires.This treating process is generally to utilize paracetamol large principle of difference in solubility in hot water and cold water, the paracetamol crude product is dissolved in hot water, after utilizing activated carbon decolorizing and removing by filter gac, separate out the paracetamol crystallization by filtrate is in addition cooling, more after filtration, the washing crystallization, dry and obtain the paracetamol finished product.
In this treating process, produce a large amount of mother liquor (filtration go out the mother liquor after the paracetamol crystallization), contain some paracetamol in this mother liquor, must reclaim to guarantee the raising of productive rate, this external treating process is in order to stop the side reaction that in paracetamol, the residual micro-p-aminophenol had causes, in above-mentioned refined liquid after removing by filter gac, need to add a certain amount of sulphite kind antioxidant to receive as bisulfite, pyrosulphite is received, SODIUM HYDROSULPHITE is received etc., this also causes in above-mentioned mother liquor containing some inorganic salts such as sulfurous acid (hydrogen) salt with by sulfurous acid (hydrogen > sulfuric acid<hydrogen of generating of salt oxidation) salt.Because these part inorganic salt can make the adsorption effect variation of gac, so the mother liquor after refining can not directly overlap refining for lower batch of crude product.
In order to reclaim part paracetamol contained in mother liquor, usually adopt at present the method for evaporation concentration mother liquid coming.But in the paracetamol so reclaimed owing to containing in mother liquor concentration and evaporation process together concentrated inorganic salt, so second-rate, in order to improve by the quality of the concentrated paracetamol obtained, often need to re-refine and twice or thrice just can reach the pharmacopeia requirement, cause thus cost recovery high, and the paracetamol saltiness reclaimed is high, second-rate, and mother liquor is concentrated and refining process need consume a large amount of heat energy, so current removal process has increased the consumption of the energy.
Summary of the invention
The object of the present invention is to provide a kind of amino phenol refinement mother liquor recycling equipment and recovery and treatment method, it can reduce energy consumption and the cost that reclaims paracetamol.
Another object of the present invention is to provide a kind of amino phenol refinement mother liquor recycling equipment and recovery and treatment method, it can improve quality and benefit that paracetamol reclaims.
To achieve these goals, the invention provides a kind of acetaminophen refining mother liquid recycling device, this recycling equipment comprises: the mother liquor fastener driving device provides the mother liquor that contains paracetamol; Adsorption and analysis device, in the mother liquor that described mother liquor fastener driving device is squeezed into along first direction, contained paracetamol is adsorbed and is resolved; The pressurized gas fastener driving device, blow out described adsorption and analysis device to squeezing into pressurized gas in described adsorption and analysis device with the mother liquor by after absorption in described adsorption and analysis device; Resolve and use sour fastener driving device, will resolve with acid and squeeze into described adsorption and analysis device along second direction; And the elutriant retrieving arrangement, be communicated with described adsorption and analysis device and reclaim after resolving the elutriant obtained.
In foregoing invention, preferably: described adsorption and analysis device comprises one or more resin tower, in each resin tower, is respectively arranged with polymeric adsorbent,
In foregoing invention, preferably: when described adsorption and analysis device comprises a plurality of resin tower, described a plurality of resin tower is set up in parallel, when a part of resin tower of described a plurality of resin towers is accepted mother liquor that described mother liquor fastener driving device transports, described parsing is squeezed into acid for described parsing with sour fastener driving device to the remaining resin tower of described a plurality of resin towers, each described resin tower can only accept at one time parsing that mother liquor that described mother liquor fastener driving device transports and described parsing transport with sour fastener driving device with sour the two one of.
In foregoing invention, preferably: described first direction is to adsorb direction from the top of described adsorption and analysis device towards the following current of bottom, and described second direction is to resolve direction from the bottom of described adsorption and analysis device towards the adverse current at top.
In foregoing invention, preferably: described polymeric adsorbent is LS-200 macromolecules adsorption resin.
In foregoing invention, preferably also comprise: the scavenging solution fastener driving device, to squeezing into scavenging solution in described adsorption and analysis device, the remnants in described adsorption and analysis device are resolved with acid and carry out drip washing; And cleaning fluid recovery, reclaim described adsorption and analysis device is carried out to the scavenging solution after drip washing.
In foregoing invention, preferably: described cleaning fluid recovery comprises according to the acid concentration height and reclaims respectively at least two scavenging solution withdrawers that described adsorption and analysis device carried out to the scavenging solution after drip washing.
In foregoing invention, preferably: described elutriant retrieving arrangement comprises at least two elutriant withdrawers that elutriant reclaimed according to the concentration height segmentation of paracetamol in described elutriant.
In foregoing invention, preferably: described elutriant retrieving arrangement is positioned at the different ends of described adsorption and analysis device from Link Port and the described parsing of described adsorption and analysis device with the Link Port of sour fastener driving device and described adsorption and analysis device.
In addition, the present invention also provides a kind of acetaminophen refined mother liquid recovery and treatment method, this recovery and treatment method comprises: the mother liquor that will contain paracetamol along first direction is squeezed into adsorption and analysis device, described mother liquor is carried out the following current adsorption step of following current absorption in described adsorption and analysis device; Squeeze into pressurized gas in described adsorption and analysis device, with the mother liquor by having carried out mother liquor after described following current absorption in described adsorption and analysis device and blow out described adsorption and analysis device, blow out step; To resolve with acid and squeeze into described adsorption and analysis device along second direction, to carry out the adverse current analyzing step of adverse current parsing; And the elutriant recycling step that reclaims after adverse current is resolved the elutriant obtained.
In foregoing invention, preferably: described adsorption and analysis device comprises one or more resin tower, in each resin tower, is respectively arranged with polymeric adsorbent.
In foregoing invention, preferably: when described adsorption and analysis device comprises described a plurality of resin tower, described a plurality of resin tower is set up in parallel, and when a part of resin tower of described a plurality of resin towers carries out described following current adsorption step, the remaining resin tower of described a plurality of resin towers carries out described adverse current analyzing step.
In foregoing invention, preferably: described first direction is to adsorb direction from the top of described adsorption and analysis device towards the following current of bottom, and described second direction is to resolve direction from the bottom of described adsorption and analysis device towards the adverse current at top.
In foregoing invention, preferably: described polymeric adsorbent is LS-200 macromolecules adsorption resin.
In foregoing invention, preferably: after described elutriant recycling step, also comprise:
Remnants in described adsorption and analysis device are resolved to the scavenging solution that carries out drip washing with acid squeeze into step to squeezing into scavenging solution in described adsorption and analysis device; And
Described adsorption and analysis device is carried out to the scavenging solution recycling step that the scavenging solution after drip washing reclaims respectively according to the acid concentration height.
In foregoing invention, preferably: described elutriant recycling step is reclaimed elutriant according to the concentration height segmentation of paracetamol in described elutriant.
In foregoing invention, preferably: the elutriant on described adsorption and analysis device reclaims the sour mouthful difference end that is positioned at described adsorption and analysis device of squeezing into for parsing of mouth and described adsorption and analysis device.
Compare the method that adopts the evaporation concentration mother liquid coming in background technology, the present invention is by adopting adsorption and analysis device and corresponding treatment process, reduce energy consumption and the cost recovery of paracetamol, improved recovery quality and the benefit of paracetamol.
The accompanying drawing explanation
Fig. 1 is the formation schematic diagram of acetaminophen refining mother liquid recycling device of the present invention;
Fig. 2 is the configuration schematic diagram of resin tower and resin in adsorption and analysis device;
Fig. 3 is the circular treatment work sesame figure of the following current absorption of macromolecules adsorption resin and adverse current desorb;
The color atlas of the mother liquor material that Fig. 4 obtains by traditional evaporation concentration mother liquor method before being;
Fig. 5 is the color atlas according to the leading portion elutriant obtained after adsorption and analysis device absorption parsing of the present invention;
Fig. 6 is prior art and the application's contrasting colour spectrogram.
Wherein, description of reference numerals is as follows:
1 adsorption and analysis device; 2 scavenging solution fastener driving devices; 3 mother liquor fastener driving devices;
4 pressurized gas fastener driving devices; 5 elutriant retrieving arrangements; 6 cleaning fluid recovery;
The sour fastener driving device of 7 parsing; 8 waste disposal plants; 11 dividing plates with holes;
12 quartz sands; 13 polymeric adsorbents; The 3a strainer;
The 3b pump; 3c mother liquor pond; 5a leading portion elutriant withdrawer;
5b back segment elutriant withdrawer; 6a the first scavenging solution withdrawer;
6b the second scavenging solution withdrawer; 6c the 3rd scavenging solution withdrawer;
The 7a pump; 7b resolves and uses sour pond; 38,39,40,48,49,50 valves;
The 1111# resin tower; The 1212# resin tower.
Embodiment
Below in conjunction with accompanying drawing, illustrate according to acetaminophen refining mother liquid recycling device of the present invention and recovery and treatment method.
Fig. 1 illustrates the formation schematic diagram of acetaminophen refining mother liquid recycling device of the present invention.
As shown in Figure 1, acetaminophen refining mother liquid recycling device of the present invention comprises: mother liquor fastener driving device 3 provides the mother liquor that contains paracetamol; Adsorption and analysis device 1, in the mother liquor that mother liquor fastener driving device 3 is squeezed into along first direction, contained paracetamol is adsorbed and is resolved; Pressurized gas fastener driving device 4, blow out adsorption and analysis device 1 to squeezing into pressurized gas in adsorption and analysis device 1 with the mother liquor by after absorption in adsorption and analysis device 1; Resolve with sour fastener driving device 7, will resolve with acid and squeeze into adsorption and analysis device 1 along second direction; And elutriant retrieving arrangement 5, be communicated with adsorption and analysis device 1 and reclaim and resolve the rear elutriant obtained.
In acetaminophen refining mother liquid recycling device according to the present invention, preferably, also comprise: waste disposal plant 8 is received from the mother liquor after the absorption that adsorption and analysis device 1 blows out, to carry out subsequent disposal and discharge.
In the acetaminophen refining mother liquid recycling device according to invention, preferably, described first direction is contrary with described second direction; Further preferably, described first direction is top-down following current absorption direction, described second direction is that adverse current is from bottom to top resolved direction, wherein " on " be that the upper surface of adsorption and analysis device 1 is top, D score is the i.e. bottom, lower surface of adsorption and analysis device 1.
Adsorption and analysis device 1 by 1 or be set up in parallel two even many resin towers (being also adsorption column) form, dispose polymeric adsorbent (referring to Fig. 2) in each resin tower.
Below with adsorption and analysis device 1, by two resin towers that are set up in parallel, be configured to its working order of example explanation:
The first state: wherein one (below be called the First resin tower) is communicated with, successively carries out the following current absorption of first direction and the adverse current parsing work of second direction (being that an independent resin tower just can form a set of independently recycling and processing device) with the mother liquor fastener driving device 3 of front and the parsing of back successively with sour fastener driving device 7, another (below be called second resin tower) " leaving unused " is for standby, at the First resin tower because of the reasons such as maintenance used time again, enable second, make like this production line turn round all the time, make mother liquor can process all the time.The benefit one that adopts following current absorption, adverse current to resolve is for handled easily, but advantages of good adsorption effect during following current absorption can be dissolved paracetamol because resolving with acid when adverse current is resolved to greatest extent, and the parsing effect also can be better.
The following current absorption of first direction is exactly that mother liquor is adsorbed resin absorption by the paracetamol polymeric adsorbent and mother liquor from top to bottom from the top of resin tower; The adverse current parsing of second direction refers to resolve with acid and by the polymeric adsorbent absorption, the paracetamol adsorbed in polymeric adsorbent is resolved and taken away from bottom to top from the bottom of resin tower.
The second state: mother liquor fastener driving device 3 is first squeezed into mother liquor the First resin tower, carry out the following current absorption of first direction in the first resin tower, when absorption completes, stop squeezing into mother liquor to the first resin tower, then utilize to resolve with sour fastener driving device 7 and will resolve with acid and squeeze into the First resin tower and carry out the adverse current parsing of second direction, meanwhile, mother liquor fastener driving device 3 is squeezed into second resin tower by mother liquor, carry out the following current absorption of first direction in second resin tower, complete following current absorption work Deng second resin tower, the First resin tower also completes adverse current and resolves, during cleaning, just make the First resin tower enter the following current adsorption process of first direction again, second resin tower enters the adverse current resolving of second direction, so move in circles to improve treatment capacity and equipment efficiency of usage.
In a word, each resin tower can and be resolved with mother liquor fastener driving device 3 and is together in series work and can become separately a cover system with sour fastener driving device 7, is adsorbed and resolves.Be set up in parallel two or many resin towers and can make resin tower operate at full capacity, to meet and to produce to greatest extent, increase the treatment capacity of mother liquor, reduce processing cost.Although a plurality of resin towers can carry out following current absorption simultaneously, and then carry out the adverse current parsing simultaneously, but preferably making embodiment is a part of resin tower of a plurality of resin towers while accepting mother liquor that the mother liquor fastener driving device transports, resolves with sour fastener driving device and squeezes into and resolve with sour to the remaining resin tower of a plurality of resin towers.
But, no matter any working order, each described resin tower can only accept the mother liquor that the mother liquor fastener driving device transports at one time and resolve the parsing that transports with sour fastener driving device with sour the two one of, can not accept the two simultaneously.
Reach requirement in the mother liquor amount of squeezing into resin tower, stop the input after, pressurized gas fastener driving device 4 imports pressurized gas in resin tower, the mother liquor that will carry out after resin absorption blows out from resin tower, and the mother liquor blown out is squeezed into waste disposal plant 8 by pipeline and processed.
Blow off after mother liquor to utilize to resolve with sour fastener driving device 7 and will resolve with sour and squeeze into resin tower with the direction of squeezing into opposite direction with mother liquor, carry out the parsing work of resin tower institute adsorbent, obtain the elutriant that the Determination of Acetaminophen height does not wait, and reclaimed by elutriant retrieving arrangement 5.This elutriant retrieving arrangement 5 can be reclaimed elutriant according to the concentration height segmentation of paracetamol in elutriant.The elutriant concentration of general leading portion is higher, and the concentration of back segment is lower.After the leading portion elutriant that concentration is higher reclaims, for the production of batching, the back segment elutriant that concentration is lower collects cover for resolve (such as acid for the parsing as next time) next time.
After the parsing work of resin tower completes, in order to carry out following current absorption again, preferably the remnants acid in resin tower is controlled, the mode that imports the slow drip washing resin tower of cleaning liquid in generally adopting from top to resin tower reaches the absorption operation remaining sour requirement.For this reason, in paracetamol mother liquor recycling equipment, can also comprise the scavenging solution fastener driving device 2 that cleaning liquid is squeezed into to adsorption and analysis device, adsorption and analysis device carried out to drip washing; With the cleaning fluid recovery 6 that is connected with adsorption and analysis device, the scavenging solution after described adsorption and analysis device drip washing is just reclaimed respectively according to acid concentration.
It is the mother liquor recovery and treatment method that the present invention utilizes above-mentioned acetaminophen refining mother liquid recycling device to provide the circulating disposal process of a kind of absorption of the following current by polymeric adsorbent and adverse current desorb to form.And according to the mother liquid coming treatment capacity the larger and lower principle of processing cost, can adopt and be set up in parallel the resin tower (being also adsorption column) that two or many internal configuration have polymeric adsorbent.
Below, be described in more detail above-mentioned embodiment of the present invention based on embodiment.
Fig. 3 is the circulating disposal process figure of the following current absorption of macromolecules adsorption resin and adverse current desorb.As the polymeric adsorbent used in the present invention, so long as can complete above-mentioned following current absorption and adverse current, resolve just passablely, be not particularly limited.Take macromolecules adsorption resin (LS-200 macromolecules adsorption resin) at this and carry out the circulating disposal process operation as example.
In the present embodiment, adsorption and analysis device consists of 1# resin tower and 2# resin tower.
With pump 3b after by the paracetamol liquor abstraction and through filter 3a, the suspended substance in mother liquor being filtered out the 3c of mother liquor pond, according to mother liquid flow rate, with the amount of resin in resin tower, become the mode of the relation of certainty ratio to squeeze into 1# resin tower 111 from top to bottom with certain flow velocity, carry out following current based on macromolecules adsorption resin absorption in 1# resin tower 111, now 3 valves of the other end of resin tower 111 (bottom) are all closed (for the valve 38 of sewage disposal, squeeze into and resolve with sour valve 39 and scavenging solution recovery valve 40).Now, the mother liquor fastener driving device 3 of Fig. 1 can comprise pump 3b and mother liquor pond 3c; Certainly mother liquor device 3 also can comprise strainer 3b.
Flow velocity while squeezing into about mother liquor, although can not consider the volume of resin, with any flow velocity, mother liquor is pumped into to 1# resin tower 111, but consider the adsorptive power of working efficiency, resin, amount of resin proportion relation in preferred mother liquor flow velocity and resin tower, this is for following factor: the excessive unit time adsorptive power that can surpass resin of mother liquor flow velocity, mother liquor is not easy fully to contact with resin, can cause adsorption efficiency low, the rate of recovery of paracetamol is low; The mother liquor flow velocity is too small can make mother liquor pump into overlong time because of the unit time adsorptive power far below resin, causes working efficiency to reduce, and has also reduced the mother liquid disposal amount in the unit time.
In mother liquor volumetric flow rate and tower, the proportionlity of resinite accumulated amount, preferably at 0.8: 1～1.1: 1, is more preferably 1: 1, such as the resinite accumulated amount in adsorption tower is 10m
3The time, the flow velocity of mother liquor is 8m preferably
3/ h～11m
3/ h, be more preferably 10m
3/ h.
Mother liquor is squeezed in process, and the paracetamol in mother liquor just is attracted on resin.When the amount of squeezing into mother liquor reaches specified amount, stop to the interior importing mother liquor of 1# resin tower 111.About this specified amount, such as preferred mother liquor volume be the resinite accumulated amount 10-12 doubly, be more preferably 10 times.After stopping importing mother liquor, can standing certain hour, so that mother liquor is fully adsorbed by the resin in resin tower.
Then, utilize pressurized gas fastener driving device 4 (referring to Fig. 1) by pressurized gas (so long as do not react and get final product with mother liquor, such as pressurized air) squeeze into resin tower, the mother liquor that carried out resin absorption in resin tower is blown out, and the mother liquor blown out is driven into waste disposal plant 8 (referring to Fig. 1) by pipeline and is processed rear discharge.
Blow off after mother liquor that will to resolve with acid be dilute acetic acid (the acetic acid degree is approximately more than 45%) such as the collected by-product acid of sour process of adopting of industrial acetic acid or paracetamol acylation reaction; with certain speed, such as with the mother liquor flow velocity the same from (resin tower bottom) and go up (resin tower top) adverse current and squeeze into resin tower and resolved regenerative operation.As shown in Figure 3, via pump 7a, from resolving with suction sour pond 7b, resolve with acid to 1# resin tower 111.At this, the parsing of Fig. 1 can comprise pump 7a and resolve with sour pond 7b with sour fastener driving device 7.
The production process of above-mentioned by-product acid is: during the paracetamol acylation reaction, p-aminophenol and Glacial acetic acid are at high temperature reacted; because reaction is reversible; so need constantly the water in resultant of reaction to be steamed out in reaction process; when steaming, water can take a part of acetic acid out of; in the mixture of this part water and acetic acid, the content of acetic acid is more than 45%, and this process is just named and adopted acid.
In this resolving, resolve by sour volumetric usage such as being 1.0～2.0 times of resinite accumulated amount, preferably 1.5 times.Although parsing from principle, there is no positive connection with amount of resin by the sour speed of squeezing into, and, in general, squeeze into flow velocity slower, the parsing effect is better.But should consider and resolve speed and efficiency and determine that parsing squeezes into speed with acid, therefore, preferably resolve by the amount of resin proportion relation in sour flow velocity and resin tower, such as resolving proportionlity by resinite accumulated amount in sour volumetric flow rate and tower preferably at 0.8: 1～1.1: 1, be more preferably 1: 1.
In order to guarantee to resolve with the reverse resin tower of squeezing into of acid, resolve with sour import and will be arranged on resin tower and squeeze into a mouthful different position from mother liquor, when mother liquor is squeezed into and mouthful is arranged on the resin tower top, parsing is squeezed into mouth with acid and is arranged on place, close bottom in resin tower bottom or side, to guarantee liquid, squeezes into the direction contrary.
Parsing entering with the sour bottom from resin tower is taken away the paracetamol be adsorbed on resin, forms elutriant, by the elutriant retrieving arrangement, is reclaimed.Wherein, the leading portion elutriant that Determination of Acetaminophen is higher (for example front 50% elutriant) is reclaimed by leading portion elutriant withdrawer 5a, with for the production of batching.The back segment elutriant that concentration is lower (for example, after 50% elutriant) is reclaimed by back segment elutriant withdrawer 5b, usings cover for resolve (as acid for parsing next time) next time.Selectively, the elutriant that leading portion elutriant withdrawer 5a and back segment elutriant withdrawer 5b collect is respectively 1/2 of acid for parsing used.At this, the elutriant retrieving arrangement 5 of Fig. 1 can comprise leading portion elutriant withdrawer 5a and back segment elutriant withdrawer 5b.Certainly in actual production, the elutriant withdrawer is not limited to two, can be for one or more
After parse operation completes, utilize scavenging solution fastener driving device 2 (referring to Fig. 1) make tap water (referring to Fig. 3) from top slow drip washing 1# resin tower 111, to reach the front requirement to remaining acid of absorption operation, and the scavenging solution after drip washing is reclaimed by cleaning fluid recovery 6.Selectively, the cleaning fluid recovery 6 of Fig. 1 can comprise three scavenging solution withdrawer 6a, 6b and 6c (as shown in Figure 3), with the concentration according to 1# resin tower 111 being carried out to the scavenging solution after drip washing, scavenging solution is reclaimed, certainly in actual production, the scavenging solution withdrawer is not limited to three, can be one, two or more.Upper moisture three phases in lessivation, first stage is with after water wash, and the concentration of acid is higher, and the scavenging solution that this stage reclaims is collected by the first scavenging solution withdrawer 6a, can be used as diluted acid for selling; Subordinate phase is collected by the second scavenging solution withdrawer 6b with the scavenging solution after water wash, now because sour concentration is not high, and the water of drip washing for the first time when subordinate phase can be used as next cycle resin tower is carried out to drip washing with the scavenging solution after water wash; Phase III is collected by the 3rd scavenging solution withdrawer 6c with the scavenging solution after water wash, now lower because of sour concentration, the water of drip washing for the second time when the phase III can be used as next cycle resin tower is carried out to drip washing with the scavenging solution after water wash, realized recycling of resource.After the phase III, drip washing completed, go out water ph value approximately between 6-7, now can drop into next cycle absorption operation.
The absorption of carrying out based on 2# resin tower 121 is resolved with the working process of above-mentioned 1# resin tower 111 basic identical, just when 1# resin tower 111 carries out following current absorption, 2# resin tower 121 carries out the adverse current parsing, and 1# resin tower 111 is when carrying out the adverse current parsing, and 2# resin tower 121 is carrying out following current absorption.
The process of carrying out the acetaminophen refined mother liquid recycling due to employing resin tower as above no longer needs to heat concentrated mother liquor and just can reclaim paracetamol, so no longer expend a large amount of energy, therefore, can say that the present invention has reduced the cost recovery of paracetamol, has saved the energy.
The color atlas of the mother liquor material that Fig. 4 obtains by traditional evaporation concentration mother liquor method before being, it detects the corresponding table 1 of data.Fig. 5 is that it detects the corresponding table 2 of data according to the color atlas of the leading portion elutriant obtained after adsorption and analysis device absorption parsing of the present invention, and instrument is Shimadzu LC liquid chromatograph, and detecting is 245nm with wavelength,, sample detection volume 20uL.
The color atlas of the mother liquor material that table 1 obtained by traditional evaporation concentration mother liquor method in the past detects data
The color atlas of the elutriant that table 2 obtains after resolving by resin absorption detects data
With reference to Fig. 4 and Fig. 5 and table 1 and table 2, in two color atlass, the appearance time of paracetamol is about 2.8 minutes.The peak area of paracetamol in Fig. 4 (being content) is 95.185%.The peak area of paracetamol in Fig. 5 (being content) is 99.795%, the high 4-5% that comparative illustration is processed than traditional technology with the material content after the plastic resin treatment mother liquor.
Fig. 6 is the color atlas that the data of Fig. 4 (prior art) and Fig. 5 (the application) are put together and obtained, by contrast, also can find out significantly (please in the corresponding basis of solid line, the corresponding prior art of dotted line), the peak area of the peak area ratio prior art that the application's embodiment obtains is large, illustrates with the quality of material after resin absorption resolver processing paracetamol mother liquor more guaranteed.Be the quality that the present invention has also improved paracetamol, increased benefit.
Claims (8)
1. an acetaminophen refining mother liquid recycling device, is characterized in that, described acetaminophen refining mother liquid recycling device comprises:
The mother liquor fastener driving device, provide the mother liquor that contains paracetamol;
Adsorption and analysis device, in the mother liquor that described mother liquor fastener driving device is squeezed into along first direction, contained paracetamol is adsorbed and is resolved;
The pressurized gas fastener driving device, blow out described adsorption and analysis device to squeezing into pressurized gas in described adsorption and analysis device with the mother liquor by after absorption in described adsorption and analysis device;
Resolve and use sour fastener driving device, will resolve with acid and squeeze into described adsorption and analysis device along second direction; And
The elutriant retrieving arrangement, be communicated with described adsorption and analysis device and reclaim after resolving the elutriant obtained;
Described adsorption and analysis device comprises one or more resin tower, in each resin tower, is respectively arranged with polymeric adsorbent,
When described adsorption and analysis device comprises a plurality of resin tower, described a plurality of resin tower is set up in parallel, when a part of resin tower of described a plurality of resin towers is accepted mother liquor that described mother liquor fastener driving device transports, described parsing is squeezed into acid for described parsing with sour fastener driving device to the remaining resin tower of described a plurality of resin towers
Each described resin tower can only accept at one time parsing that mother liquor that described mother liquor fastener driving device transports and described parsing transport with sour fastener driving device with sour the two one of;
Described first direction is to adsorb direction from the top of described adsorption and analysis device towards the following current of bottom, and described second direction is to resolve direction from the bottom of described adsorption and analysis device towards the adverse current at top, and described polymeric adsorbent is LS-200 macromolecules adsorption resin.
2. acetaminophen refining mother liquid recycling device according to claim 1, is characterized in that, also comprises:
The scavenging solution fastener driving device, resolve with acid and carry out drip washing the remnants in described adsorption and analysis device to squeezing into scavenging solution in described adsorption and analysis device; And
Scavenging solution withdrawer or reclaim respectively at least two scavenging solution withdrawers that described adsorption and analysis device carried out to the scavenging solution after drip washing according to the acid concentration height.
3. acetaminophen refining mother liquid recycling device according to claim 1, is characterized in that,
Described elutriant retrieving arrangement comprises at least two elutriant withdrawers that elutriant reclaimed according to the concentration height segmentation of paracetamol in described elutriant;
Described elutriant retrieving arrangement is positioned at the different ends of described adsorption and analysis device from Link Port and the described parsing of described adsorption and analysis device with the Link Port of sour fastener driving device and described adsorption and analysis device.
4. an acetaminophen refined mother liquid recovery and treatment method, is characterized in that, described acetaminophen refined mother liquid recovery and treatment method comprises:
The mother liquor that will contain paracetamol along first direction is squeezed into adsorption and analysis device, described mother liquor is carried out the following current adsorption step of following current absorption in described adsorption and analysis device;
Squeeze into pressurized gas in described adsorption and analysis device, with the mother liquor by having carried out mother liquor after described following current absorption in described adsorption and analysis device and blow out described adsorption and analysis device, blow out step;
To resolve with acid and squeeze into described adsorption and analysis device along second direction, to carry out the adverse current analyzing step of adverse current parsing; And
Reclaim after adverse current is resolved the elutriant recycling step of the elutriant obtained.
5. acetaminophen refined mother liquid recovery and treatment method according to claim 4, is characterized in that,
Described adsorption and analysis device comprises one or more resin tower, in each resin tower, is respectively arranged with polymeric adsorbent;
When described adsorption and analysis device comprises described a plurality of resin tower, described a plurality of resin towers are set up in parallel, and when a part of resin tower of described a plurality of resin towers carries out described following current adsorption step, the remaining resin tower of described a plurality of resin towers carries out described adverse current analyzing step.
6. acetaminophen refined mother liquid recovery and treatment method according to claim 5, is characterized in that,
Described first direction is to adsorb direction from the top of described adsorption and analysis device towards the following current of bottom, and described second direction is to resolve direction from the bottom of described adsorption and analysis device towards the adverse current at top, and described polymeric adsorbent is LS-200 macromolecules adsorption resin.
7. acetaminophen refined mother liquid recovery and treatment method according to claim 4, is characterized in that,
After described elutriant recycling step, also comprise:
Remnants in described adsorption and analysis device are resolved to the scavenging solution that carries out drip washing with acid squeeze into step to squeezing into scavenging solution in described adsorption and analysis device; And
Described adsorption and analysis device is carried out to the scavenging solution recycling step that the scavenging solution after drip washing reclaims respectively according to the acid concentration height.
8. acetaminophen refined mother liquid recovery and treatment method according to claim 4 is characterized in that:
Described elutriant recycling step is reclaimed elutriant according to the concentration height segmentation of paracetamol in described elutriant;
Elutriant on described adsorption and analysis device reclaims the sour mouthful difference end that is positioned at described adsorption and analysis device of squeezing into for parsing of mouth and described adsorption and analysis device.
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| CN102824758B (en) * | 2012-08-24 | 2015-01-07 | 安徽丰原发酵技术工程研究有限公司 | System and method for separating paracetamol by simulated moving bed chromatography |
| CN102816080A (en) * | 2012-08-24 | 2012-12-12 | 安徽丰原发酵技术工程研究有限公司 | Method of recovering paracetamol from mother solution |
| CN103012186B (en) * | 2012-12-24 | 2015-02-25 | 西安蓝晓科技新材料股份有限公司 | Method for recycling paracetamol from refined mother liquor by using adsorption resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4565890A (en) * | 1983-10-27 | 1986-01-21 | Mallinckrodt, Inc. | Process for the preparation of N-acetyl-P-aminophenol |
| CN101624352A (en) * | 2009-07-30 | 2010-01-13 | 浙江康乐药业股份有限公司 | Method for processing acetaminophen refined mother liquid |
| CN202186952U (en) * | 2011-08-18 | 2012-04-11 | 河北冀衡（集团）药业有限公司 | Acetaminophen refining mother liquid recycling device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4565890A (en) * | 1983-10-27 | 1986-01-21 | Mallinckrodt, Inc. | Process for the preparation of N-acetyl-P-aminophenol |
| CN101624352A (en) * | 2009-07-30 | 2010-01-13 | 浙江康乐药业股份有限公司 | Method for processing acetaminophen refined mother liquid |
| CN202186952U (en) * | 2011-08-18 | 2012-04-11 | 河北冀衡（集团）药业有限公司 | Acetaminophen refining mother liquid recycling device |
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Address after: 053000 No.1, Weiwu street, high tech Zone, Hengshui City, Hebei Province Patentee after: Hebei Jiheng Pharmaceutical Co.,Ltd. Address before: 053000 No.368 Jianshe North Street, Hengshui City, Hebei Province Patentee before: HEBEI JIHENG (Group) PHARMACEUTICAL Co.,Ltd. |