CN113336803A - Method for removing monosaccharide and disaccharide from acarbose and acarbose purification method - Google Patents
Method for removing monosaccharide and disaccharide from acarbose and acarbose purification method Download PDFInfo
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- CN113336803A CN113336803A CN202110620664.8A CN202110620664A CN113336803A CN 113336803 A CN113336803 A CN 113336803A CN 202110620664 A CN202110620664 A CN 202110620664A CN 113336803 A CN113336803 A CN 113336803A
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- XUFXOAAUWZOOIT-SXARVLRPSA-N (2R,3R,4R,5S,6R)-5-[[(2R,3R,4R,5S,6R)-5-[[(2R,3R,4S,5S,6R)-3,4-dihydroxy-6-methyl-5-[[(1S,4R,5S,6S)-4,5,6-trihydroxy-3-(hydroxymethyl)-1-cyclohex-2-enyl]amino]-2-oxanyl]oxy]-3,4-dihydroxy-6-(hydroxymethyl)-2-oxanyl]oxy]-6-(hydroxymethyl)oxane-2,3,4-triol Chemical compound O([C@H]1O[C@H](CO)[C@H]([C@@H]([C@H]1O)O)O[C@H]1O[C@@H]([C@H]([C@H](O)[C@H]1O)N[C@@H]1[C@@H]([C@@H](O)[C@H](O)C(CO)=C1)O)C)[C@@H]1[C@@H](CO)O[C@@H](O)[C@H](O)[C@H]1O XUFXOAAUWZOOIT-SXARVLRPSA-N 0.000 title claims abstract description 79
- 229960002632 acarbose Drugs 0.000 title claims abstract description 79
- XUFXOAAUWZOOIT-UHFFFAOYSA-N acarviostatin I01 Natural products OC1C(O)C(NC2C(C(O)C(O)C(CO)=C2)O)C(C)OC1OC(C(C1O)O)C(CO)OC1OC1C(CO)OC(O)C(O)C1O XUFXOAAUWZOOIT-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 38
- 150000002772 monosaccharides Chemical class 0.000 title claims abstract description 29
- 150000002016 disaccharides Chemical class 0.000 title claims abstract description 26
- 238000000746 purification Methods 0.000 title claims abstract description 19
- 239000011347 resin Substances 0.000 claims description 130
- 229920005989 resin Polymers 0.000 claims description 130
- 239000002253 acid Substances 0.000 claims description 57
- 239000003513 alkali Substances 0.000 claims description 43
- 238000005406 washing Methods 0.000 claims description 43
- 230000008929 regeneration Effects 0.000 claims description 40
- 238000011069 regeneration method Methods 0.000 claims description 40
- 239000007788 liquid Substances 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000004458 analytical method Methods 0.000 claims description 28
- 238000011001 backwashing Methods 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000005342 ion exchange Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 125000002091 cationic group Chemical group 0.000 claims description 12
- 150000001768 cations Chemical class 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 7
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 230000002441 reversible effect Effects 0.000 claims description 5
- 238000011033 desalting Methods 0.000 claims description 4
- 238000000855 fermentation Methods 0.000 claims description 4
- 230000004151 fermentation Effects 0.000 claims description 4
- 239000003337 fertilizer Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000004587 chromatography analysis Methods 0.000 claims 1
- 239000003480 eluent Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 21
- 238000004904 shortening Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- 102000004169 proteins and genes Human genes 0.000 description 8
- 108090000623 proteins and genes Proteins 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 7
- 238000011010 flushing procedure Methods 0.000 description 6
- 238000013375 chromatographic separation Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000010612 desalination reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 241001262617 Japonica Species 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a method for removing monosaccharide and disaccharide from acarbose and an acarbose purification method, belonging to the technical field of removing monosaccharide and disaccharide. The method for removing monosaccharide and disaccharide from acarbose and the acarbose purification method have the advantages of reducing production cost, simplifying production method, shortening production period and having high product yield and purity.
Description
Technical Field
The invention belongs to the technical field of removal of monosaccharide and disaccharide, and particularly relates to a method for removing monosaccharide and disaccharide from acarbose and an acarbose purification method.
Background
After the acarbose fermentation liquor is subjected to plate-frame filtration and resin desalination and neutralization, the feed liquid also contains a large amount of impurities such as protein, monosaccharide and disaccharide. A large amount of protein and monosaccharide exist in the acarbose liquid, and the existence of the protein and the monosaccharide can influence the purity of the acarbose finished product at the later stage. What traditional acarbose industry was used is traditional three tower fixed bed technique, and this equipment area is big, and the resin utilization ratio is low, and the consumption of resin, regent and water is big, and the waste water volume is big, and acid-base loss is big, product quality unstability scheduling problem and step complex operation, economic benefits is poor.
The traditional fixed bed technology has the disadvantages of complicated links, more operation, low yield and production disadvantage. In order to improve the acarbose yield and reduce the misoperation of human factors, the invention provides a separation method for continuously separating and exchanging acarbose to remove monosaccharide and disaccharide and a purification method for acarbose.
Disclosure of Invention
The invention aims to provide a method for removing monosaccharide and disaccharide from acarbose and an acarbose purification method, which reduce the production cost, simplify the production method, shorten the production period and have high product yield and purity.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for removing the monosaccharide and the disaccharide from the acarbose provided by the invention adopts the continuous ion exchange device filled with the cationic resin, and realizes the removal of the monosaccharide and the disaccharide from the acarbose through the continuous ion exchange device.
Preferably, the continuous ion exchange device comprises at least 30 resin columns, each resin column is filled with cation resin, the continuous ion exchange device is sequentially divided into a feeding area, a material ejecting processing area, a backwashing purification area, an analysis area, a first acid washing area, a backwashing area, an alkali regeneration area, an alkali washing area, an acid regeneration area and a second acid washing area from right to left, acarbose analytic liquid in the analysis area is collected, the feeding area comprises a first stage to a third stage which are sequentially connected in series from left to right, each stage comprises at least 3 resin columns which are connected in parallel, acarbose neutralizing liquid enters from the first stage of the feeding area in a forward feeding mode, the material ejecting processing area comprises at least two resin columns which are connected in series, liquid discharged from the material ejecting processing area enters the third stage of the feeding area in a backwashing mode, the purification area comprises one resin column, liquid is fed in a reverse feeding mode, the liquid is acarbose analytic liquid, the analysis area comprises a first stage to a second stage which are sequentially connected in series from left to right, each stage comprises at least 3 resin columns which are connected in series, acid liquid enters from the first stage of the analysis zone in a forward feeding mode, the second stage effluent liquid of the analysis zone is acarbose analysis liquid, the first acid washing zone comprises one resin column, water enters in a forward feeding mode, the effluent liquid of the first acid washing zone and the first stage effluent liquid of the analysis zone are mixed and then enter the second stage of the analysis zone, the backwashing zone comprises one resin column and water enters in a reverse feeding mode, the alkali regeneration zone comprises at least two resin columns which are connected in series, alkali enters in a forward feeding mode, the alkali washing zone comprises at least three resin columns which are connected in series, water enters in a forward feeding mode, the effluent liquid of the alkali washing zone and the effluent liquid of the first resin column of the alkali regeneration zone are mixed and then enter the second resin column of the alkali regeneration zone, the acid regeneration zone comprises at least three resin columns which are connected in series, acid enters in a forward feeding mode, the second acid washing zone comprises at least two resin columns which are connected in series, and (3) adopting a forward feeding mode to feed water, mixing the effluent of the second acid washing area with the effluent of the first resin column of the acid regeneration area, and then feeding the mixture into the second resin column of the acid regeneration area.
Preferably, an intermediate tank is arranged between the second stage and the third stage of the feeding area, and the second stage effluent of the feeding area and the effluent of the material ejection processing area enter the third stage of the feeding area after transferring.
Preferably, the running period of the continuous ion exchange device is 2880s, the cation resin filling amount of each resin column is 300-500ml, the treatment amount of each cation resin is 7-10L/h, and the cation resin is PT151 resin.
Preferably, the feeding speed of the feeding area is 120-160ml/min, the feeding speed of the top material treatment area is 5-10ml/min, the feeding speed of the backwashing purification area is 8-10ml/min, the feeding speed of the analysis area is 25-30ml/min, the feeding speed of the first acid washing area is 5-10ml/min, the feeding speed of the backwashing area is 20-40ml/min, the feeding speed of the alkali regeneration area is 20-40ml/min, the feeding speed of the alkali washing area is 30-50ml/min, the feeding speed of the acid regeneration area is 20-40ml/min, and the feeding speed of the second acid washing area is 30-50 ml/min.
Preferably, the pH of the effluent of the first resin column of the second acid washing zone is more than 6 and the conductivity is less than 100 us/cm.
Preferably, the pH of the first resin column effluent from the acid regeneration zone is < 2.
Preferably, the effluent of the first resin column in the alkali regeneration zone has a pH of more than 13 and a conductivity of less than 50 us/cm.
Preferably, the acid used in the desorption zone is 0.05-0.15mol/L hydrochloric acid, and the acid used in the acid regeneration zone is 1-2mol/L hydrochloric acid.
Preferably, the alkali used in the alkali regeneration zone is 1-2mol/L sodium hydroxide.
The invention also provides a method for purifying acarbose, which comprises the following steps: s1: filtering the acarbose fermentation liquor by using a plate-and-frame filter, collecting filter residues as a fertilizer, and performing S2: performing resin desalting treatment on the filtrate obtained by filtering in the step S1, wherein the step S3: and (3) carrying out monosaccharide-disaccharide removal treatment on the acarbose neutralized liquid obtained after the resin desalination treatment in the step S2 by adopting the acarbose monosaccharide-disaccharide removal method, wherein S4: and (4) performing chromatographic separation on the acarbose analysis solution obtained after the treatment of the step S3, wherein the chromatographic separation is performed in S5: concentrating the eluate obtained after the treatment in the step S4, and S6: and (4) carrying out spray drying or freeze drying on the concentrated solution obtained after the treatment of the step S5 to obtain the acarbose.
The invention has the beneficial effects that:
1. integrates the procedures, simplifies the production method, reduces the production cost, improves the production efficiency, shortens the production period and has high product yield and purity.
2. On the premise that the system operates with the feeding amount of 120-; compared with the prior fixed bed, the resin consumption can be saved by more than 90 percent, the unit consumption can be realized according to the unit feeding amount, the unit water consumption can be saved by 30 percent, the unit consumption of acid can be saved by 60 percent, the unit consumption of alkali can be saved by 50 percent, and the wastewater discharge can be reduced by nearly 45 percent.
3. And errors caused by manual operation are reduced.
4. Continuously running and continuously discharging.
Drawings
FIG. 1 is a schematic view of the structure of a continuous ion exchange apparatus of the present invention.
FIG. 2 is a flow chart of the purification process of acarbose according to the invention.
Detailed Description
The invention will now be further described with reference to the accompanying drawings and detailed description.
Those not described in detail in this specification are within the skill of the art. In the description of the present invention, it is to be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
As shown in fig. 1, in the method for removing monosaccharides and disaccharides by acarbose provided in this example, a continuous ion exchange device filled with cationic resin is used, and the removal of monosaccharides and disaccharides by acarbose is achieved by the continuous ion exchange device.
In this embodiment, the continuous ion exchange device includes 30 resin columns, each resin column is filled with cation resin, the continuous ion exchange device is divided into a feeding area, a material ejection processing area, a backwashing purification area, an analysis area, a first acid washing area, a backwashing area, an alkali regeneration area, an alkali washing area, an acid regeneration area, and a second acid washing area from right to left in sequence, and acarbose analysis liquid in the analysis area is collected.
The feeding area comprises a first stage to a third stage which are sequentially connected in series from left to right, each stage comprises 3 resin columns which are connected in parallel, the first stage (3#, 4#, 5#), the second stage (6#, 7#, 8#), and the third stage (9#, 10#, 11 #). The acarbose neutralization solution enters from the first stage of the feeding area, a positive feeding mode is adopted, namely feeding is carried out from top to bottom, the effluent of the third stage is directly discharged into the wastewater, the feeding speed of the feeding area is 140ml/min, complete adsorption of the cationic resin is required to be ensured, and no acarbose is detected at the tail solution outlet before 11# rotary column.
The material ejection processing areas (1#, 2#) comprise two resin columns connected in series, the feeding speed of the material ejection processing areas is 8ml/min, the condition that no acarbose content exists in the detection liquid of the front outlet of the 1# resin column rotating column needs to be ensured, an intermediate tank is arranged between the second stage and the third stage of the feeding areas, the second stage liquid outlet of the feeding areas and the liquid outlet of the material ejection processing areas enter the third stage of the feeding areas after entering the intermediate tank for transferring, and the 2# outlet is directly discharged into the intermediate tank. Because the resin column of feeding leads to empty column because the feed liquid produces the bubble easily, so set up the material pans, on the one hand conveniently exhausts, and on the other hand guarantees that the cationic resin two-stage adsorbs, makes the acalep japonicas in the feed liquid adsorb on the resin column. Through two resin columns connected in series, the acarbose top washing can be ensured to be clean to the maximum extent while the water consumption for the top material is saved, and the system yield is ensured; and (3) passing the 1# and 2# top water acarbose feed liquid through the intermediate tank, and adding 9#, 10# and 11# again, so that impurities such as monosaccharide and disaccharide remained in the resin column are washed out to the maximum extent while the acarbose yield of the system is ensured.
The backwashing purification area comprises a resin column (No. 30), liquid is fed in a reverse feeding mode, namely from bottom to top, the liquid is acarbose analysis liquid, the feeding speed of the backwashing purification area is 9ml/min, a No. 30 outlet is detected before the column rotation, the concentration of the discharged acarbose is detected, and the product yield is ensured. The product concentration can be effectively improved through backwashing the purification area, the phenomenon that the concentration of the analyzed product is too low is prevented, part of water is recycled, and the utilization efficiency of the water is improved.
The analysis area comprises a first stage (24#, 25#, 26#) to a second stage (27#, 28#, 29#) which are sequentially connected in series from left to right, each stage comprises 3 resin columns which are connected in series, the analysis time of the acarbose is prolonged as much as possible, the acarbose is fully analyzed, the use amount of analysis liquid is reduced, and the production efficiency is increased. 0.1mol/L hydrochloric acid enters from No. 24 in a forward mode, No. 29 effluent is acarbose analysis solution, the feeding speed of an analysis area is 28ml/min, and the acarbose content of the No. 23 resin needs to be detected before conversion to ensure that the acarbose is completely analyzed.
The first acid washing area (23#) comprises a resin column, pure water is fed in a positive mode, 23# effluent and 26# effluent are mixed and then enter the No. 27, and partial acid is recycled in the resolving area to save the use amount of resolving acid. The feed rate to the first pickling section was 8 ml/min.
The backwashing area (22#) comprises a resin column, pure water adopts a water inlet mode (backwashing) of the resin column from bottom to top, the feeding speed of the backwashing area is 30ml/min, the resin needs to be ensured to be completely overturned in the flushing process, impurities remained in the resin are flushed out by a large amount of water, and the water quality of the outlet of the 22#, so that the resin is ensured to be flushed completely. Because the feed liquid contains a large amount of protein, the protein is easy to separate out when meeting acid after the resin is absorbed and analyzed, so that the resin is hardened and the treatment efficiency is low. The backwashing area is arranged to allow the protein to be washed away with water flow from the resin column from bottom to top, so that the cleanliness of the cationic resin of the system is ensured, and the adsorption efficiency of the cationic resin is ensured.
The alkali regeneration areas (20#, 21#) comprise two resin columns connected in series, and two series modes are adopted, so that the utilization rate of alkali is improved, impurities such as protein and the like polluting the resin are fully reacted with the alkali, and the complete alkali regeneration of the No. 20 before column conversion is ensured. 1.5mol/L sodium hydroxide adopts a forward mode to feed alkali, the feeding speed of an alkali regeneration area is 30ml/min, the pH value of an outlet of a 20# resin column is detected to be more than 13 before the operation, and an outlet of a 21# resin column is directly discharged into waste water to ensure that the resin is completely regenerated. Because a large amount of protein exists in the acarbose feed liquid, the organic matter pollution of the resin can be well removed by using 1.5mol/L sodium hydroxide to regenerate the cationic resin.
The alkali washing area (17#, 18#, 19#) comprises three resin columns connected in series, pure water is fed in a positive feeding mode, the 19# effluent and the 20# effluent are mixed and then enter the 21#, the feeding speed of the alkali washing area is 40ml/min, the outlet conductivity of the 20# resin column needs to be detected before the alkali washing area is changed, the conductivity needs to be less than 50us/cm, and the resin is ensured to be washed cleanly. And a three-string mode is adopted, wherein the water inlet mode is a flushing mode (forward inlet) for water inlet from the upper end of the resin column and water outlet from the lower end of the resin column, so that pollutants and residual alkali liquor flow out of the resin column along with water. The washing process with the multi-stage series connection increases the flowing water turbulence effect of the resin column washing while saving the alkali washing water quantity as much as possible, and increases the washing efficiency.
The acid regeneration zone (14#, 15#, 16#) comprises three resin columns connected in series, 1.5mol/L hydrochloric acid is fed in a forward mode, the feeding speed of the acid regeneration zone is 30ml/min, the pH value of the outlet of the 14# resin column is detected to be less than 2 before the operation, the outlet of the 16# resin column is directly discharged into wastewater, and the complete regeneration of the resin is ensured. The utilization rate of acid is improved by adopting a three-string mode; as a large amount of carbonate exists in the cationic resin pollution, the resin hardening phenomenon caused by resin scaling can be effectively prevented by regenerating the cationic resin by using 1.5mol/L hydrochloric acid.
The second acid washing areas (12#, 13#) comprise two resin columns connected in series, pure water is fed in a positive mode, the feeding speed of the second acid washing areas is 40ml/min, the pH value of an outlet of the 12# resin column is detected to be more than 6 before the second acid washing area is turned, the conductance is less than 100us/cm, the outlet of the 13# is connected to an outlet of the No. 14 to be mixed together and then enters an upper inlet of the No. 15, and on the premise of saving water, the resin is guaranteed to be washed cleanly and completely. The method is mainly used for washing and regenerating residual hydrochloric acid in the complete cation resin, and the residual hydrochloric acid in the resin can influence the effect of adsorbing the acarbon by the resin; two series of processes are adopted for flushing, so that the flushing water quantity can be effectively saved, and the resin flushing effect is ensured.
Wherein the operation period of the continuous ion exchange device is 2880s, the cation resin filling amount of each resin column is 400ml, each cation resin can process 10 liters of acarbose neutralization solution per hour, and the cation resin is PT151 resin.
In the embodiment, the feed liquid is acarbose neutralization liquid with the pH value of 5.5-7, the color is light yellow, and the acarbose titer is 2500-4000 mg/l; on the premise that the system operates with the feeding amount of 120-; compared with the prior fixed bed, the resin consumption can be saved by more than 90 percent, the unit consumption can be realized according to the unit feeding amount, the unit water consumption can be saved by 30 percent, the unit consumption of acid can be saved by 60 percent, the unit consumption of alkali can be saved by 50 percent, and the wastewater discharge can be reduced by nearly 45 percent.
As shown in fig. 2, this embodiment further provides a method for purifying acarbose, which includes the following steps: s1: filtering the acarbose fermentation liquor by using a plate-and-frame filter, collecting filter residues as a fertilizer, and performing S2: performing resin desalting treatment on the filtrate obtained by filtering in the step S1, wherein the step S3: and (3) carrying out monosaccharide-disaccharide removal treatment on the acarbose neutralized liquid obtained after the resin desalination treatment in the step S2 by adopting the acarbose monosaccharide-disaccharide removal method, wherein S4: and (4) performing chromatographic separation on the acarbose analysis solution obtained after the treatment of the step S3, wherein the chromatographic separation is performed in S5: concentrating the eluate obtained after the treatment in the step S4, and S6: and (4) carrying out spray drying on the concentrated solution obtained after the treatment of the step S5 to obtain the acarbose.
According to the invention, according to different adsorption forces of the resin on acarbose and monosaccharide, the effluent is monosaccharide and disaccharide, the acarbose is adsorbed on the resin, the worked resin enters the regeneration zone along with the rotation of the system, and the separation column can continue to work after the regeneration zone is regenerated and leached. The steps of feeding, washing, resolving, alkali regeneration, backwashing, acid regeneration, flushing and the like which are carried out according to the time lapse in the traditional production are realized in a continuous production method, and the product is continuously fed and discharged. In the continuous operation of the continuous ion exchange unit of the present invention, the sequential switching of the various fluid distribution valves, each separation unit will pump in sequence liquids of different media such as: raw materials, water, different chemical reagents, etc.
The invention has the following beneficial effects:
1. integrates the procedures, simplifies the production method, reduces the production cost, improves the production efficiency, shortens the production period and has high product yield and purity.
2. And errors caused by manual operation are reduced.
3. Continuously running and continuously discharging.
4. The continuous ion exchange technology has the following advantages:
1) due to continuous operation, the product components and concentration are kept stable, and the matching of a downstream working section is facilitated.
2) Because of improving production efficiency, the resin column, the storage tank and the matching scale are very small, the equipment is compact, the resin column, the storage tank and the matching scale are easy to install at any position, the resin column is easy to match with the old production process and the equipment, and the occupied area is only about one third of the same scale.
3) The rotation speed can be automatically adjusted according to the requirements of the production process along with the change of the mass and the flow rate of the inflow fluid, thereby ensuring the operation under the economically optimal state.
4) The acid and alkali consumption is reduced, the wastewater discharge is reduced, and the subsequent environmental protection pressure is relieved.
5) Due to the adoption of a plurality of separation units, the production method flow can be flexibly changed.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art; the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for removing monosaccharide and disaccharide from acarbose is characterized in that,
and (3) adopting a continuous ion exchange device filled with cationic resin, and realizing the removal of the monosaccharide and the disaccharide from the acarbose through the continuous ion exchange device.
2. A method for removing monosaccharide and disaccharide from acarbose is characterized in that,
the continuous ion exchange device comprises at least 30 resin columns, and each resin column is filled with cation resin;
the continuous ion exchange device is divided into a feeding area, a top material processing area, a backwashing purification area, an analysis area, a first acid washing area, a backwashing area, an alkali regeneration area, an alkali washing area, an acid regeneration area and a second acid washing area;
the feeding area comprises a first stage to a third stage which are sequentially connected in series from left to right, each stage comprises at least 3 resin columns which are connected in parallel, and acarbose neutralization solution enters from the first stage of the feeding area in a forward feeding mode;
the material ejection processing area comprises at least two resin columns connected in series, and the effluent of the material ejection processing area enters the third stage of the material feeding area;
the backwashing purification area comprises a resin column, liquid is fed in a reverse feeding mode, and the liquid is acarbose resolution liquid;
the analysis area comprises a first stage to a second stage which are sequentially connected in series from left to right, each stage comprises at least 3 resin columns which are connected in series, acid liquor enters from the first stage of the analysis area in a forward feeding mode, and the second stage effluent of the analysis area is acarbose analysis liquor;
the first acid washing area comprises a resin column, water is fed in a forward feeding mode, and the effluent of the first acid washing area is mixed with the first-stage effluent of the analysis area and then enters the second stage of the analysis area;
the backwashing area comprises a resin column and adopts a reverse feeding mode to feed water;
the alkali regeneration zone comprises at least two resin columns which are connected in series, and alkali is fed in by adopting a forward feeding mode;
the alkali washing zone comprises at least three resin columns which are connected in series, water is fed in a forward feeding mode, and the effluent of the alkali washing zone is mixed with the effluent of the first resin column of the alkali regeneration zone and then enters the second resin column of the alkali regeneration zone;
the acid regeneration zone comprises at least three resin columns which are connected in series, and acid is fed in a forward mode;
the second acid washing area comprises at least two resin columns which are connected in series, water is fed in a forward feeding mode, and the effluent of the second acid washing area is mixed with the effluent of the first resin column in the acid regeneration area and then enters the second resin column in the acid regeneration area.
3. The process for the removal of mono-and disaccharides using acarbose according to claim 1,
an intermediate tank is arranged between the second stage and the third stage of the feeding area, and the second stage effluent of the feeding area and the effluent of the material ejection processing area enter the third stage of the feeding area after being transferred into the intermediate tank.
4. The process for the removal of mono-and disaccharides using acarbose according to claim 1,
the running period of the continuous ion exchange device is 2880 s;
the filling amount of the cation resin of each resin column is 300-500 ml;
the treatment capacity of each cationic resin is 7-10L/h;
the cationic resin is PT151 resin.
5. The process for the removal of mono-and disaccharides using acarbose according to claim 1,
the feeding speed of the feeding area is 120-160 ml/min;
the feeding speed of the top material treatment area is 5-10 ml/min;
the feeding speed of the backwashing purification area is 8-10 ml/min;
the feeding speed of the resolving area is 25-30 ml/min;
the feeding speed of the first acid washing area is 5-10 ml/min;
the feeding speed of the backwashing area is 20-40 ml/min;
the feeding speed of the alkali regeneration zone is 20-40 ml/min;
the feeding speed of the alkali washing area is 30-50 ml/min;
the feeding speed of the acid regeneration zone is 20-40 ml/min;
the feeding speed of the second acid washing area is 30-50 ml/min.
6. The process for the removal of mono-and disaccharides using acarbose according to claim 1,
the PH of the effluent of the first resin column in the second acid washing area is more than 6, and the conductivity is less than 100 us/cm.
7. The process for the removal of mono-and disaccharides using acarbose according to claim 1,
the PH of the effluent of the first resin column in the acid regeneration area is less than 2.
8. The process for the removal of mono-and disaccharides using acarbose according to claim 1,
the pH of the effluent of the first resin column effluent of the alkali regeneration area is more than 13, and the conductivity is less than 50 us/cm.
9. The process for the removal of mono-and disaccharides using acarbose according to claim 1,
the acid adopted in the resolving area is 0.05-0.15mol/L hydrochloric acid;
the acid used in the acid regeneration zone is 1-2mol/L hydrochloric acid.
The alkali used in the alkali regeneration zone is 1-2mol/L sodium hydroxide.
10. The acarbose purification method is characterized by comprising the following steps:
s1: filtering the acarbose fermentation liquor by using a plate-and-frame filter, and collecting filter residues as a chemical fertilizer;
s2: performing resin desalting treatment on the filtrate obtained by filtering in the step S1;
s3: carrying out monosaccharide-disaccharide removal treatment on the acarbose neutralized liquid obtained after the resin desalting treatment in the step S2 by adopting the acarbose monosaccharide-disaccharide removal method according to any one of claims 1 to 9;
s4: performing chromatographic chromatography on the acarbose analysis solution obtained after the treatment of the step S3;
s5: concentrating the eluent obtained after the treatment of the step S4;
s6: and (4) carrying out spray drying or freeze drying on the concentrated solution obtained after the treatment of the step S5 to obtain the acarbose.
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