CN109970587B - L-aspartic acid separation and purification device and method for separating and purifying L-aspartic acid - Google Patents
L-aspartic acid separation and purification device and method for separating and purifying L-aspartic acid Download PDFInfo
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- CN109970587B CN109970587B CN201910369761.7A CN201910369761A CN109970587B CN 109970587 B CN109970587 B CN 109970587B CN 201910369761 A CN201910369761 A CN 201910369761A CN 109970587 B CN109970587 B CN 109970587B
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- 229960005261 aspartic acid Drugs 0.000 title claims abstract description 87
- CKLJMWTZIZZHCS-UHFFFAOYSA-N D-OH-Asp Natural products OC(=O)C(N)CC(O)=O CKLJMWTZIZZHCS-UHFFFAOYSA-N 0.000 title claims abstract description 86
- CKLJMWTZIZZHCS-UWTATZPHSA-N L-Aspartic acid Natural products OC(=O)[C@H](N)CC(O)=O CKLJMWTZIZZHCS-UWTATZPHSA-N 0.000 title claims abstract description 86
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 title claims abstract description 86
- 238000000926 separation method Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000000746 purification Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 71
- 102000004190 Enzymes Human genes 0.000 claims abstract description 54
- 108090000790 Enzymes Proteins 0.000 claims abstract description 54
- 239000012528 membrane Substances 0.000 claims abstract description 54
- 238000004440 column chromatography Methods 0.000 claims abstract description 28
- 238000003860 storage Methods 0.000 claims abstract description 24
- 238000002425 crystallisation Methods 0.000 claims abstract description 22
- 230000008025 crystallization Effects 0.000 claims abstract description 21
- 238000001471 micro-filtration Methods 0.000 claims abstract description 16
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 13
- 238000005374 membrane filtration Methods 0.000 claims abstract description 13
- 238000010828 elution Methods 0.000 claims abstract description 12
- 238000001728 nano-filtration Methods 0.000 claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 69
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 239000003480 eluent Substances 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 20
- 230000001105 regulatory effect Effects 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 230000001276 controlling effect Effects 0.000 claims description 12
- 238000005086 pumping Methods 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000003456 ion exchange resin Substances 0.000 claims description 6
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 6
- 238000013375 chromatographic separation Methods 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 13
- 239000010865 sewage Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000000855 fermentation Methods 0.000 description 4
- 230000004151 fermentation Effects 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 238000002955 isolation Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229940024606 amino acid Drugs 0.000 description 2
- 150000001413 amino acids Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000729 antidote Substances 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses an L-aspartic acid separation and purification device, which comprises an enzyme liquid storage tank, wherein the enzyme liquid storage tank is communicated with a column chromatography separation device, the column chromatography separation device is communicated with a filter membrane filtration device, and the filter membrane filtration device is communicated with a concentration crystallization device; the column chromatography separation device comprises a liquid disc, and a plurality of chromatography columns are communicated with the top of the liquid disc. The device disclosed by the invention solves the technical problems of low yield, high cost and large pollution in the prior art that an extraction device is adopted to separate and purify L-aspartic acid. Meanwhile, the invention provides a method for separating and purifying L-aspartic acid, which comprises four steps of column chromatography adsorption, elution, microfiltration membrane and nanofiltration membrane filtration and concentration crystallization. The technical scheme disclosed by the invention has the advantages of high separation efficiency, high yield, larger purity of the separated L-aspartic acid, and small amount of sewage and waste gas by adopting a column chromatography separation mode, thereby reducing the pollution of industrial production and reducing the environmental protection treatment cost.
Description
Technical Field
The invention relates to an amino acid extraction column chromatographic separation device, in particular to an L-aspartic acid separation and purification device and a method for separating and purifying L-aspartic acid.
Background
L-aspartic acid having the structure shown below:
L-aspartic acid can not only provide a source of amino acids to the human body, but also can be used as a pharmaceutical such as an ammonia antidote. Regarding the industrial preparation method of L-aspartic acid, the prior art is mostly prepared by adopting a chemical synthesis method, but the chemical synthesis has the defect of great pollution.
In order to overcome the technical defect of chemical synthesis of L-aspartic acid, scientific researchers prepare fermentation liquor of L-aspartic acid precursor by adopting a biological fermentation method, and then carry out enzymolysis on the fermentation liquor to obtain the control enzyme conversion liquor rich in L-aspartic acid. However, in the process of obtaining L-aspartic acid by biological fermentation, the separation and control of L-aspartic acid in an enzymatic conversion solution has been a difficult technical problem.
In the prior art, in order to separate L-aspartic acid from a control enzyme conversion solution, an extraction means is mostly adopted, and the L-aspartic acid is obtained by an extraction mode.
However, in the above-mentioned extraction means, since the enzyme-converted solution is controlled to contain various impurities in addition to L-aspartic acid, L-aspartic acid can be obtained by repeating the extraction and the crystallization, and the yield of L-aspartic acid obtained by the above-mentioned repeated extraction and crystallization is extremely low.
For the separation and purification by an extraction means or the separation yield by the extraction means is low, the method of column chromatography separation is adopted at present.
Column chromatography separation technology, i.e., chromatographic separation by chromatography column, has been applied from small-sized chromatography columns used in laboratories to large-sized chromatography columns produced by industrial separation. Adding the separated liquid into a large chromatographic column, and separating substances in the separated liquid by chromatography with adsorbent such as silica gel. Because the large-scale chromatographic column produced in the industry has certain height and width, the theoretical plate number is larger, the separation efficiency is high, and the amount obtained by one-time separation is larger.
However, there has been no column chromatography apparatus and no suitable chromatography method which can be applied to L-aspartic acid. In the prior art, the traditional multi-extraction-crystallization technology is still adopted for separation, the amount of waste liquid generated by an extraction mode is large, so that the industrialized sewage treatment cost is high, and meanwhile, the extraction cost is high.
Disclosure of Invention
The invention aims to solve the technical problem of providing an L-aspartic acid separation and purification device and a method for separating and purifying L-aspartic acid.
The invention solves the technical problems through the following technical scheme:
The L-aspartic acid separation and purification device comprises an enzyme liquid storage tank, wherein the enzyme liquid storage tank is communicated with a column chromatography separation device, the column chromatography separation device is communicated with a filter membrane filtration device, and the filter membrane filtration device is communicated with a concentration crystallization device;
The column chromatography separation device comprises a liquid tray, wherein the top of the liquid tray is communicated with a plurality of chromatography columns, a first pipeline is communicated between the chromatography columns, the first pipeline is communicated with a second pipeline, and the second pipeline is communicated with an enzyme liquid storage tank;
The bottom of the liquid disc is communicated with a third pipeline, the third pipeline is communicated with a filter membrane filtering device, and the filter membrane filtering device is communicated with a concentration crystallization device;
the filter membrane filter device comprises a micro-filter membrane filter device and a nano-filter membrane filter device, and the top of the nano-filter membrane filter device is communicated with the top of the micro-filter membrane filter device through a fifth pipeline;
the bottom of the microfiltration membrane filtering device is communicated with a third pipeline, and the bottom of the nanofiltration membrane filtering device is communicated with a concentration crystallization device through a fourth pipeline;
The first pipeline, the second pipeline, the third pipeline, the fourth pipeline and the fifth pipeline are all provided with valves.
Preferably, 6 chromatographic columns are symmetrically distributed at the top of the liquid tray, and the chromatographic columns are symmetrically distributed at the side edge positions of the bottom of the liquid tray by taking the center of the liquid tray as a symmetry center;
The chromatographic columns at the diagonal positions are communicated through first pipelines, the first pipelines are communicated mutually in a penetrating way, and the penetrating part of the first pipelines is vertically communicated with a second pipeline upwards.
Preferably, the ends of the two ends of the first pipeline respectively penetrate through the tops of the corresponding chromatographic columns, and the ends of the two ends of the end of the first pipeline are respectively communicated with metal filter balls.
Preferably, the chromatographic column comprises a top cover, a bottom cover and a column body, wherein the top cover is connected with the top of the column body, the bottom cover is connected with the bottom of the column body, an inner cavity is formed in the top cover, the metal filter ball is positioned in the inner cavity of the top cover, a chromatographic cavity is formed in the column body and is communicated with the inner cavity of the top cover, and an anti-impact disc is connected to the top of the chromatographic cavity;
the anti-impact disc is provided with a plurality of through holes, the through holes are communicated with the chromatographic cavity, and the through holes are fixedly connected with a filter screen;
An inner cavity is formed in the bottom cover, the inner cavity of the bottom cover is communicated with the chromatographic cavity, the bottom cover is communicated with the top of the liquid tray through a liquid discharge pipe, and the liquid discharge pipe is provided with a valve.
Preferably, the chromatography cavity is filled with ion exchange resin.
Preferably, the concentrating and crystallizing device comprises a concentrating and crystallizing kettle, wherein a stirring device is arranged in the concentrating and crystallizing kettle, and the concentrating and crystallizing kettle is communicated with a vacuum device.
Preferably, the liquid disc is hollow, and a glass observation area is arranged on the side wall of the liquid disc.
Preferably, the glass observation area is provided with scale marks.
Preferably, a layer of circular filter screen is fixedly connected to the bottom in the liquid tray, and the circular filter screen covers the bottom surface in the liquid tray.
The invention also discloses a method for separating and purifying L-aspartic acid by using the L-aspartic acid separating and purifying device, which comprises the following steps:
S1, pumping 50L of regulating enzyme conversion solution with the concentration content of L-aspartic acid of 160-210g/L into an enzyme solution storage tank, regulating the pH value of the regulating enzyme conversion solution to 4-8, opening a valve, adding the regulating enzyme conversion solution into a column chromatography separation device for adsorption, adsorbing the L-aspartic acid in the column chromatography separation device, and controlling the flow rate of the regulating enzyme conversion solution flowing into the column chromatography separation device to be 100-2000mL/min;
S2, after adsorption is finished, pumping sodium hydroxide solution into an enzyme solution storage tank, taking the sodium hydroxide solution as eluent, opening a valve, and controlling the elution flow rate of sodium hydroxide to be 100-2000mL/min by utilizing the L-aspartic acid adsorbed in a sodium hydroxide eluting column chromatographic separation device;
S3, in the eluting process, a valve is opened, and eluent sequentially enters a microfiltration membrane filtering device and a nanofiltration membrane filtering device for filtration and then enters a concentration crystallization device;
S4, concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5-3.0, adding L-aspartic acid seed crystal, crystallizing, filtering and drying to obtain pure L-aspartic acid.
Compared with the prior art, the invention has the following advantages:
The device disclosed by the invention solves the technical problems of low yield, high cost and large pollution of the prior art that the L-aspartic acid is separated and purified by an extraction means. The device disclosed by the invention provides a device suitable for separating L-aspartic acid by using industrialized column chromatography, which is used for separating L-aspartic acid by using the device, and has the advantages of high separation efficiency, high yield, high purity of the separated L-aspartic acid, and low sewage and waste gas, reduces industrialized pollution and reduces environmental protection treatment cost.
The separation and purification method disclosed by the invention replaces the traditional extraction method used in industrialization, and has the advantages of high yield, purity up to 99.9% and simple method.
Drawings
FIG. 1 is a schematic overall structure of an embodiment of the present invention;
FIG. 2 is a schematic diagram of a concentrating crystallization device and a membrane filtration device according to an embodiment of the present invention;
FIG. 3 is a schematic diagram showing the structure of a column chromatography separation apparatus according to an embodiment of the present invention;
FIG. 4 is a cross-sectional view of a chromatography column in an embodiment of the invention;
FIG. 5 is a schematic view of a part of the FIG. 4A enlarged structure according to an embodiment of the present invention;
FIG. 6 is a schematic view of the structure of an impact-resistant disc in an embodiment of the present invention;
FIG. 7 is a diagram of the connection relationship between a first pipe and a second pipe in an embodiment of the present invention;
FIG. 8 is an infrared spectrum of the purified L-aspartic acid obtained by crystallization in example 2 of the present invention.
Detailed Description
The following describes in detail the examples of the present invention, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples.
Example 1L-aspartic acid separation and purification apparatus
As shown in figures 1-7, the L-aspartic acid separation and purification device comprises an enzyme liquid storage tank 1, wherein the enzyme liquid storage tank 1 is communicated with a column chromatography separation device 2 (the column chromatography separation device 2 is positioned below the enzyme liquid storage tank 1), the column chromatography separation device 2 is communicated with a filter membrane filtration device 3 (the filter membrane filtration device 3 is positioned below the column chromatography separation device 2), and the filter membrane filtration device 3 is communicated with a concentration crystallization device 4 (the concentration crystallization device 4 is positioned below the filter membrane filtration device 3).
In the above device: the filter membrane filter device 3 comprises a micro-filter membrane filter device 31 and a nano-filter membrane filter device 32 (the micro-filter membrane filter device 31 and the nano-filter membrane filter device 32 are communicated with each other), wherein the micro-filter membrane filter device 31 and the nano-filter membrane filter device 32 are conventional micro-filter membrane filter equipment and nano-filter membrane filter equipment disclosed in the prior art, the main structure of the main structure comprises a corresponding micro-filter membrane and a nano-filter membrane, and a specific structure and a working principle of the micro-filter membrane filter device 31 and the nano-filter membrane filter device 32 disclosed by the invention can be known by a person skilled in the art through consulting a technical manual or a technical dictionary.
Meanwhile, the concentrating and crystallizing device 4 is a conventional concentrating and crystallizing kettle disclosed in the prior art, and the main structure of the concentrating and crystallizing kettle comprises a kettle body, a stirring device arranged on the kettle body, and a vacuum device, such as a vacuum pump, communicated with the top of the kettle body, wherein eluent in the kettle body is concentrated by the vacuum device.
The improvement points of the invention are that:
The column chromatography separation device 2 is arranged, specifically, the column chromatography separation device 2 comprises a liquid disc 22 (the inside of the liquid disc 22 is hollow, a glass observation area is arranged on the side wall of the liquid disc 22, toughened glass is arranged in the glass observation area, scale marks 221 are arranged on the glass observation area, liquid levels in the liquid disc 22 are marked by the scale marks 221), 6 chromatographic columns 21 are symmetrically distributed at the top of the liquid disc 22 (the length of each chromatographic column 21 is 6.5m and the radius is 1 m), and the chromatographic columns 21 are symmetrically distributed at the side edge positions of the top of the liquid disc 22 by taking the center of the liquid disc 22 as the symmetry center. The bottom of the chromatographic column 21 is communicated with a liquid tray 22 (the bottom of the chromatographic column 21 is communicated with a liquid discharge pipe, and the liquid discharge pipe is communicated with the liquid tray 22).
Two chromatographic columns 21 positioned at diagonal positions (two chromatographic columns 21 are respectively positioned at two ends of a diameter line) are communicated through a first pipeline 211 (the top covers of the chromatographic columns 21 are communicated through the first pipeline 211), the first pipelines 211 are communicated in a crossing way, and the crossing part of the first pipeline 211 is vertically communicated with a second pipeline 212 upwards. (meanwhile, each first pipeline 211 is provided with 2 valves, and the valves are respectively positioned at two ends of the first pipeline 211 near the position of the top cover 201 on the chromatographic column 21).
The structure of the chromatographic column 21 is specifically:
The chromatographic column 21 comprises a top cover 201, a bottom cover 202 and a column body, wherein the top cover 201 is connected with the top of the column body, the bottom cover 202 is connected with the bottom of the column body, an inner cavity is formed in the top cover 201, the end parts of the two ends of the first pipeline 211 penetrate through and extend into the inner cavity of the top cover 201, and the end parts are communicated with a metal filter ball 2111 (the metal filter ball 2111 is woven by a metal filter screen, the end parts of the first pipeline 211 extend into the metal filter ball 2111, and the purpose of the metal filter ball 2111 is to prevent insoluble matters from entering into a chromatographic cavity and affecting the chromatographic effect).
A chromatographic cavity (the chromatographic cavity is filled with ion exchange resin, the ion exchange resin is 732 type cation exchange resin) is arranged in the column body, the chromatographic cavity is communicated with the inner cavity of the top cover 201, the top of the chromatographic cavity is connected with an anti-impact disc 213 (a plurality of through holes 2131 are formed in the anti-impact disc 213, the through holes 2131 are communicated with the chromatographic cavity, a filter screen is fixedly connected to the through holes 2131, and the anti-impact disc 213 is designed to prevent the eluent from impacting and deforming the filled ion exchange resin powder at the moment of adding into the chromatographic cavity). The ion exchange resin is filled in the chromatographic cavity, and then the anti-impact plate 213 is screwed at the cavity opening position of the chromatographic cavity (an external thread part 2132 is arranged on the side wall of the anti-impact plate 213, and a corresponding internal thread is arranged on the inner wall of the cavity opening of the corresponding chromatographic cavity). In the conventional manner, the overcap 201 is designed to be detachably coupled to the column, such as by screwing the overcap 201 to the top of the column.
Similarly, an inner cavity is arranged in the bottom cover 202, the inner cavity of the bottom cover 202 is communicated with the chromatographic cavity, the bottom cover 202 is communicated with the top of the liquid tray 22 through a liquid discharge pipe, and the liquid discharge pipe is provided with a valve.
Since the two chromatographic columns 21 positioned at the diagonal positions are communicated through the first pipelines 211, the 6 chromatographic columns 21 are provided with 3 first pipelines 211,3, the first pipelines 211 are positioned on the same horizontal plane, the 3 first pipelines 211 are crossed, the crossing positions are the joint communication positions of the three first pipelines 211, the second pipelines 212 are vertically communicated at the crossing positions upwards, and the second pipelines 212 are communicated with the bottom of the enzyme liquid storage tank 1.
The bottom center intercommunication of liquid dish 22 (the bottom fixedly connected with one deck circular filter screen in the liquid dish 22, circular filter screen covers the bottom surface in the liquid dish 22, circular filter screen's effect is filtered, prevent to stop up microfiltration membrane filter 31 and nanofiltration membrane filter 32, circular filter screen is not drawn in the figure) has third pipeline 312, third pipeline 312 intercommunication is in the bottom of microfiltration membrane filter 31, the top of microfiltration membrane filter 31 is through the top of fifth pipeline 311 intercommunication nanofiltration membrane filter 32, the bottom of nanofiltration membrane filter 32 is through fourth pipeline 321 intercommunication concentration crystallization device 4.
The first pipe 211, the second pipe 212, the third pipe 312, the fourth pipe 321, and the fifth pipe 311 are all provided with valves.
EXAMPLE 2 method for isolation and purification of L-aspartic acid
As shown in FIGS. 1 to 7, the method for separating and purifying L-aspartic acid comprises the following steps:
S1, pumping 50L of an enzyme conversion solution with the concentration content of L-aspartic acid of 160g/L into an enzyme solution storage tank 1, opening a valve on a second pipeline 212 after regulating the pH value of the enzyme conversion solution to 4, enabling the enzyme conversion solution to enter a first pipeline 211 through the second pipeline 212, and selecting the number of the valves on the first pipeline 211 according to the liquid amount of the enzyme conversion solution actually regulated, namely selecting the number of the chromatographic columns 21. Controlling and regulating the flow rate of the enzyme conversion solution flowing into the chromatographic column 21 to be 100mL/min;
S2, after adsorption is finished, pumping sodium hydroxide solution into the enzyme solution storage tank 1, taking the sodium hydroxide solution as eluent, opening a valve on the second pipeline 212 and a valve on a drain pipe at the bottom of the chromatographic column 21, separating the sodium hydroxide solution from the chromatographic column 21 with L-aspartic acid, and controlling the elution flow rate of sodium hydroxide to be 100mL/min by feeding the L-aspartic acid eluent into the liquid tray 22;
S3, in the elution process, a valve on a third pipeline 312 is opened, the L-aspartic acid eluent enters the microfiltration membrane filter device 31 from the third pipeline 312, is filtered by the microfiltration membrane filter device 31, enters the nanofiltration membrane filter device 32 from a fifth pipeline 311, and enters the concentration crystallization device 4 from a fourth pipeline 321 for reduced pressure concentration;
S4, concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5, adding L-aspartic acid seed crystal, crystallizing, filtering and drying to obtain pure L-aspartic acid. The purity was 99.9% by HPLC and the yield was 91.6%.
The infrared spectrum of the pure L-aspartic acid is shown in FIG. 8.
EXAMPLE 3 method for isolation and purification of L-aspartic acid
As shown in FIGS. 1 to 7, the method for separating and purifying L-aspartic acid comprises the following steps:
s1, pumping 50L of an enzyme conversion solution with the concentration of L-aspartic acid of 210g/L into an enzyme solution storage tank 1, adjusting the pH value of the enzyme conversion solution to 8, opening a valve on a second pipeline 212, allowing the enzyme conversion solution to enter a first pipeline 211 through the second pipeline 212, and selecting the number of the valves on the first pipeline 211 according to the liquid amount of the enzyme conversion solution actually adjusted, namely selecting the number of the chromatographic columns 21. Controlling and regulating the flow rate of the enzyme conversion solution flowing into the chromatographic column 21 to 2000mL/min;
s2, after adsorption is finished, pumping sodium hydroxide solution into an enzyme solution storage tank 1, taking the sodium hydroxide solution as eluent, opening a valve on a second pipeline 212 and a valve on a liquid discharge pipe at the bottom of a chromatographic column 21, separating the sodium hydroxide solution from the chromatographic column 21 with L-aspartic acid, and controlling the elution flow rate of sodium hydroxide to be 500mL/min by feeding the L-aspartic acid eluent into a liquid tray 22;
S3, in the elution process, a valve on a third pipeline 312 is opened, the L-aspartic acid eluent enters the microfiltration membrane filter device 31 from the third pipeline 312, is filtered by the microfiltration membrane filter device 31, enters the nanofiltration membrane filter device 32 from a fifth pipeline 311, and enters the concentration crystallization device 4 from a fourth pipeline 321 for reduced pressure concentration;
S4, concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5, adding L-aspartic acid seed crystal, crystallizing, filtering and drying to obtain pure L-aspartic acid. The purity was 99.9% by HPLC and the yield was 90.5%.
EXAMPLE 4 method for isolation and purification of L-aspartic acid
As shown in FIGS. 1 to 7, the method for separating and purifying L-aspartic acid comprises the following steps:
s1, pumping 50L of an enzyme conversion solution with the concentration content of L-aspartic acid of 180g/L into an enzyme solution storage tank 1, opening a valve on a second pipeline 212 after regulating the pH value of the enzyme conversion solution to 8, enabling the enzyme conversion solution to enter a first pipeline 211 through the second pipeline 212, and selecting the number of the valves on the first pipeline 211 according to the liquid amount of the enzyme conversion solution actually regulated, namely selecting the number of the chromatographic columns 21. Controlling and regulating the flow rate of the enzyme conversion solution flowing into the chromatographic column 21 to be 500mL/min;
S2, after adsorption is finished, pumping sodium hydroxide solution into the enzyme solution storage tank 1, as eluent, opening a valve on the second pipeline 212 and a valve on a drain pipe at the bottom of the chromatographic column 21, separating sodium hydroxide solution from the chromatographic column 21 with L-aspartic acid, and controlling the elution flow rate of sodium hydroxide to be 100mL/min by feeding the L-aspartic acid eluent into the liquid tray 22;
S3, in the elution process, a valve on a third pipeline 312 is opened, the L-aspartic acid eluent enters the microfiltration membrane filter device 31 from the third pipeline 312, is filtered by the microfiltration membrane filter device 31, enters the nanofiltration membrane filter device 32 from a fifth pipeline 311, and enters the concentration crystallization device 4 from a fourth pipeline 321 for reduced pressure concentration;
S4, concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 2.8, adding L-aspartic acid seed crystal, crystallizing, filtering and drying to obtain pure L-aspartic acid. The purity was 99.9% by HPLC and the yield was 90.3%.
EXAMPLE 5 method for isolation and purification of L-aspartic acid
As shown in FIGS. 1 to 7, the method for separating and purifying L-aspartic acid comprises the following steps:
S1, pumping 50L of an enzyme conversion solution with the concentration of L-aspartic acid of 200g/L into an enzyme solution storage tank 1, adjusting the pH value of the enzyme conversion solution to 6, opening a valve on a second pipeline 212, allowing the enzyme conversion solution to enter a first pipeline 211 through the second pipeline 212, and selecting the number of the valves on the first pipeline 211 according to the liquid amount of the enzyme conversion solution actually adjusted, namely selecting the number of the chromatographic columns 21. Controlling and regulating the flow rate of the enzyme conversion solution flowing into the chromatographic column 21 to be 100mL/min;
s2, after adsorption is finished, pumping sodium hydroxide solution into an enzyme solution storage tank 1, taking the sodium hydroxide solution as eluent, opening a valve on a second pipeline 212 and a valve on a liquid discharge pipe at the bottom of a chromatographic column 21, separating the sodium hydroxide solution from the chromatographic column 21 with L-aspartic acid, and controlling the elution flow rate of sodium hydroxide to be 500mL/min by feeding the L-aspartic acid eluent into a liquid tray 22;
S3, in the elution process, a valve on a third pipeline 312 is opened, the L-aspartic acid eluent enters the microfiltration membrane filter device 31 from the third pipeline 312, is filtered by the microfiltration membrane filter device 31, enters the nanofiltration membrane filter device 32 from a fifth pipeline 311, and enters the concentration crystallization device 4 from a fourth pipeline 321 for reduced pressure concentration;
s4, concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 3.0, adding L-aspartic acid seed crystal, crystallizing, filtering and drying to obtain pure L-aspartic acid. The purity was 99.9% by HPLC and the yield was 92.7%.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (8)
1. The L-aspartic acid separation and purification device is characterized by comprising an enzyme liquid storage tank, wherein the enzyme liquid storage tank is communicated with a column chromatography separation device, the column chromatography separation device is communicated with a filter membrane filtration device, and the filter membrane filtration device is communicated with a concentration crystallization device;
The column chromatography separation device comprises a liquid tray, wherein the top of the liquid tray is communicated with a plurality of chromatography columns, a first pipeline is communicated between the chromatography columns, the first pipeline is communicated with a second pipeline, and the second pipeline is communicated with an enzyme liquid storage tank;
The bottom of the liquid disc is communicated with a third pipeline, the third pipeline is communicated with a filter membrane filtering device, and the filter membrane filtering device is communicated with a concentration crystallization device;
the filter membrane filter device comprises a micro-filter membrane filter device and a nano-filter membrane filter device, and the top of the nano-filter membrane filter device is communicated with the top of the micro-filter membrane filter device through a fifth pipeline;
the bottom of the microfiltration membrane filtering device is communicated with a third pipeline, and the bottom of the nanofiltration membrane filtering device is communicated with a concentration crystallization device through a fourth pipeline;
The first pipeline, the second pipeline, the third pipeline, the fourth pipeline and the fifth pipeline are all provided with valves;
The top of the liquid disc is symmetrically provided with 6 chromatographic columns, and the chromatographic columns are symmetrically distributed at the side edge positions of the bottom of the liquid disc by taking the center of the liquid disc as a symmetrical center;
The chromatographic columns at the diagonal positions are communicated through first pipelines, the first pipelines are communicated mutually in a penetrating way, and the penetrating part of the first pipelines is vertically communicated with a second pipeline upwards;
the ends of the two ends of the first pipeline respectively penetrate through the tops of the corresponding chromatographic columns, and the ends of the two ends of the end of the first pipeline are respectively communicated with metal filter balls.
2. The device for separating and purifying L-aspartic acid according to claim 1, wherein the chromatographic column comprises a top cover, a bottom cover and a column body, the top cover is connected with the top of the column body, the bottom cover is connected with the bottom of the column body, an inner cavity is formed in the top cover, the metal filter ball is positioned in the inner cavity of the top cover, a chromatographic cavity is formed in the column body and is communicated with the inner cavity of the top cover, and an anti-impact disc is connected to the top position of the chromatographic cavity;
the anti-impact disc is provided with a plurality of through holes, the through holes are communicated with the chromatographic cavity, and the through holes are fixedly connected with a filter screen;
An inner cavity is formed in the bottom cover, the inner cavity of the bottom cover is communicated with the chromatographic cavity, the bottom cover is communicated with the top of the liquid tray through a liquid discharge pipe, and the liquid discharge pipe is provided with a valve.
3. The L-aspartic acid separation and purification apparatus according to claim 2, wherein the chromatography cavity is filled with an ion exchange resin.
4. The device for separating and purifying L-aspartic acid according to claim 1, wherein the concentrating and crystallizing device comprises a concentrating and crystallizing kettle, a stirring device is arranged in the concentrating and crystallizing kettle, and a vacuum device is communicated with the concentrating and crystallizing kettle.
5. The L-aspartic acid separation and purification device according to claim 1, wherein the liquid tray is hollow, and a glass observation area is provided on a side wall of the liquid tray.
6. The apparatus according to claim 5, wherein the glass observation area is provided with scale marks.
7. The device for separating and purifying L-aspartic acid according to claim 6, wherein a circular filter screen is fixedly connected to the bottom of the liquid tray, and the circular filter screen covers the bottom surface of the liquid tray.
8. A method for separating and purifying L-aspartic acid using the L-aspartic acid separating and purifying apparatus according to any one of claims 1 to 7, comprising the steps of:
S1, pumping 50L of an enzyme conversion regulating solution with the concentration content of L-aspartic acid of 160-210 g/L into an enzyme solution storage tank, regulating the pH value of the enzyme conversion regulating solution to 4-8, opening a valve, adding the enzyme conversion regulating solution into a column chromatography separation device for adsorption, adsorbing the L-aspartic acid in the column chromatography separation device, and controlling the flow rate of the enzyme conversion regulating solution flowing into the column chromatography separation device to be 100-2000 mL/min;
S2, after adsorption is finished, pumping sodium hydroxide solution into an enzyme solution storage tank, taking the sodium hydroxide solution as eluent, opening a valve, and controlling the elution flow rate of sodium hydroxide to be 100-2000 mL/min by utilizing the L-aspartic acid adsorbed in a chromatographic separation device of a sodium hydroxide elution column;
S3, in the eluting process, a valve is opened, and eluent sequentially enters a microfiltration membrane filtering device and a nanofiltration membrane filtering device for filtration and then enters a concentration crystallization device;
S4, concentrating the eluent under reduced pressure, adding sulfuric acid to adjust the pH value of the concentrated solution to 1.5-3.0, adding L-aspartic acid seed crystal, crystallizing, filtering and drying to obtain pure L-aspartic acid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1165860A (en) * | 1996-03-29 | 1997-11-26 | 协和发酵工业株式会社 | Method for prepn. of L-aspartate |
| CN205907266U (en) * | 2016-06-30 | 2017-01-25 | 扬州工业职业技术学院 | L aspartic acid enzymolysis and purification device |
| CN209872831U (en) * | 2019-05-06 | 2019-12-31 | 宿州学院 | L-aspartic acid separation and purification device |
-
2019
- 2019-05-06 CN CN201910369761.7A patent/CN109970587B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1165860A (en) * | 1996-03-29 | 1997-11-26 | 协和发酵工业株式会社 | Method for prepn. of L-aspartate |
| CN205907266U (en) * | 2016-06-30 | 2017-01-25 | 扬州工业职业技术学院 | L aspartic acid enzymolysis and purification device |
| CN209872831U (en) * | 2019-05-06 | 2019-12-31 | 宿州学院 | L-aspartic acid separation and purification device |
Non-Patent Citations (2)
| Title |
|---|
| Ｌ-天冬氨酸的清洁提取工艺;章燕 等;《生物加工过程》;第5卷(第4期);第65-69页 * |
| 膜分离技术在低分子量生物产品分离纯化中的应用;姚红娟 等;《化工进展》(第2期);第146页1.1 膜分离类型 * |
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