CN210367504U - Extraction element of epsilon-polylysine - Google Patents

Extraction element of epsilon-polylysine Download PDF

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CN210367504U
CN210367504U CN201920572237.5U CN201920572237U CN210367504U CN 210367504 U CN210367504 U CN 210367504U CN 201920572237 U CN201920572237 U CN 201920572237U CN 210367504 U CN210367504 U CN 210367504U
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polylysine
epsilon
microfiltration membrane
pipe
feed
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方威
陈磊
刘怀红
张南南
李国学
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Nanjing Jay Environmental Protection Technology Co ltd
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Nanjing Jay Environmental Protection Technology Co ltd
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Abstract

The utility model discloses an extraction element of epsilon-polylysine, include the zymotic fluid piggy bank, micro-filtration membrane device, the ion exchange adsorption equipment, desorption device, active carbon decoloration device, receive and strain enrichment facility, spout dry device and receiving device that connect gradually through the pipeline. Compared with the prior art, the utility model discloses device simple structure has lower capital construction cost, and degree of automation is high, and control process is simple, and personnel intensity of labour and use amount significantly reduce can save 50% labour cost, and economic benefits is showing. In addition, the extraction device can stably produce epsilon-polylysine products with high concentration and high titer in batches, the product quality is stable, the recovery rate of the epsilon-polylysine is more than 96.2 percent, and the production efficiency, the recovery rate and the filtration precision are improved.

Description

Extraction element of epsilon-polylysine
Technical Field
The utility model belongs to the field of biological instruments, concretely relates to extraction element of epsilon-polylysine.
Background
In the screening of Dragendo-Positive (abbreviated as DP) material from microorganisms by S.Shima and H.Sakai in 1977, it was found that one strain of actinomycete No.346 produces a large amount of stable DP material, which was confirmed by analysis and structural analysis of acid hydrolysis products to be a homo-type monomer polymer containing 25 to 30 lysine residues, called epsilon-polylysine (epsilon-PL).
The epsilon-polylysine is a polypeptide with bacteriostatic effect, and the biological preservative is applied to food preservation for the first time in the 80 s. Epsilon-polylysine can be decomposed into lysine in the human body, and lysine is one of 8 amino acids essential to the human body and is also an amino acid allowed to be enriched in food in countries all over the world. Therefore, the epsilon-polylysine is a nutritional bacteriostatic agent, has higher safety than other chemical preservatives, and has the acute oral toxicity of 5 g/kg.
The epsilon-polylysine has a broad antibacterial spectrum, and can be used for treating Candida acutifolia, Rhodotorula Farfarae, Pichia pastoris and Sporobolomyces rosea of Saccharomyces; heat-resistant Bacillus stearothermophilus, Bacillus coagulans and Bacillus subtilis in gram-positive bacteria; the gram-negative bacteria such as the aerobacter aerogenes and the escherichia coli have obvious inhibiting and killing effects. The polylysine has obvious inhibition effect on the growth of gram-positive micrococcus, lactobacillus bulgaricus, streptococcus thermophilus, gram-negative escherichia coli, salmonella and saccharomycetes, and the polylysine and acetic acid compound reagent has obvious inhibition effect on bacillus subtilis.
The action mechanism of epsilon-polylysine is mainly shown in the following 3 aspects:
(1) acting on cell wall and cell membrane systems;
(2) acting on genetic material or genetic microparticulate structures;
(3) acting on enzymes or functional proteins.
The antibacterial performance of polylysine is researched, and the epsilon-PL is found to be capable of inhibiting micrococcus with high heat resistance and also has a very good antibacterial effect on Escherichia coli and salmonella of G & lt- & gt which is not easy to inhibit other natural preservatives (such as Nisin), and can inhibit the growth of Lactobacillus bulgaricus, Streptococcus thermophilus and saccharomycetes. But the single use of the epsilon-PL has no obvious inhibition on the bacillus subtilis and the aspergillus niger, the composite treatment of the epsilon-PL and acetic acid enhances the inhibition on the bacillus subtilis, and the epsilon-PL after the high-temperature treatment still has the antibacterial activity on micrococcus.
At present, most polylysine products in the market exist in the form of hydrochloride, while polylysine products in an alkaline form (epsilon-polylysine) are less, but the epsilon-polylysine has higher biological activity compared with the hydrochloride, so that the preparation of the epsilon-polylysine further utilizes the polylysine generated by fermentation, the production efficiency is improved, and higher economic benefit is generated.
The traditional extraction method is to obtain crude epsilon-polylysine by fermentation liquor centrifugation, vacuum concentration and organic solvent elution, and freeze drying. These methods have the following disadvantages:
(1) the fermentation liquor is not subjected to pre-filtration and is directly adsorbed by resin, theoretically, but residual thalli, protein, culture medium residues and the like in the fermentation liquor can seriously pollute the resin, reduce the adsorption quantity and the service life of the resin, only can be scientifically researched, and cannot be applied to actual production.
(2) And the high-purity epsilon-polylysine is difficult to obtain, the recovery rate is low, and the purity is low.
(3) The operation process is complicated, the workload is large, the yield is low, the period is long, and the efficiency is low.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that to prior art not enough, provide an extraction element of epsilon-polylysine that the energy consumption is low, efficient, economic benefits is showing to solve the not good scheduling problem of effect that prior art exists.
In order to achieve the purpose, the utility model adopts the following technical scheme:
an extraction device of epsilon-polylysine comprises a fermentation liquor storage tank, a microfiltration membrane device, an ion exchange adsorption device, a desorption device, an activated carbon decoloring device, a nanofiltration concentration device, a spray drying device and a material receiving device;
wherein, the feed liquid in the fermentation liquid storage tank enters the microfiltration membrane device through a feed liquid inlet pipe of the microfiltration membrane device;
the trapped fluid of the microfiltration membrane device returns to the microfiltration membrane device through a return pipe of the microfiltration membrane device, and the permeate enters the ion exchange adsorption device through a liquid inlet pipe of the ion exchange adsorption device;
adsorbing epsilon-polylysine in the feed liquid by using the adsorption resin in the ion exchange adsorption device, and introducing the adsorption resin adsorbed with the epsilon-polylysine into a desorption device through a feed pipe of the desorption device for desorption;
the sodium chloride solution in the desorption device is used for desorbing epsilon-polylysine in the resin, and then the epsilon-polylysine enters the activated carbon decolorization device through a feed pipe of the activated carbon decolorization device for decolorization;
the feed liquid decolorized in the activated carbon decolorization device enters a nanofiltration concentration device through a feed pipe of the nanofiltration concentration device;
trapped liquid of the nanofiltration concentration device enters the spray drying device through a feed pipe of the spray drying device after being concentrated, and permeate liquid is discharged outwards through a discharge pipe;
and the dried materials in the spray drying device enter the material receiving device through the material receiving pipe to be collected and stored.
Furthermore, a microfiltration membrane feeding pump is arranged on the microfiltration membrane device liquid inlet pipe.
The feed pipe of the desorption device is provided with a feed pump of the desorption device.
The feeding pipe of the activated carbon decoloring device is provided with a feeding pump of the activated carbon decoloring device.
The nanofiltration concentration device is characterized in that a nanofiltration concentration device feeding pump is arranged on a nanofiltration concentration device feeding pipe.
Preferably, the microfiltration membrane in the microfiltration membrane device is a ceramic microfiltration membrane, the average membrane pore size is 5-500 nm, the fermentation liquor of epsilon-polylysine is filtered by the ceramic membrane, thallus and epsilon-polylysine can be effectively separated, the filtering precision is high, the structure of epsilon-polylysine can not be broken, the activity of epsilon-polylysine is maintained, and meanwhile, part of macromolecular protein is removed.
The adsorption resin in the ion exchange adsorption device is weak acid cation exchange resin, and the model is Dow chemical Amberlite IRC-50.
The filtering precision of the activated carbon decoloring device is 100-1000 meshes.
The nanofiltration membrane in the nanofiltration concentration device has the intercepted molecular weight of 100-1000 Da, and the epsilon-polylysine clear liquid is concentrated by the nanofiltration membrane device, so that the titer of the epsilon-polylysine is effectively improved, the epsilon-polylysine can be concentrated by 5-6 times, the purity and the yield of the epsilon-polylysine are improved, the amount of evaporated water is reduced, and the purity of the epsilon-polylysine is further improved by adding water for dialysis of inorganic salts.
Has the advantages that:
the extraction device of the utility model can stably produce high-concentration and high-titer epsilon-polylysine products in batches, the equipment is stable in operation, the product quality is stable, the recovery rate of the epsilon-polylysine is more than 94 percent, and the production efficiency, the recovery rate and the product purity are further improved; compared with the traditional production process, the extraction device has the advantages that the energy is saved, the automation degree is high, the control process is simple, the labor intensity and the use amount of personnel are greatly reduced, about 60 percent of labor cost can be saved, and the economic benefit is remarkable; and by adopting the membrane separation device, the occupied area of equipment is reduced, and the capital construction and energy consumption cost is reduced.
Drawings
These and/or other advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings and the following detailed description.
Fig. 1 is a schematic view of the overall structure of the extraction apparatus.
Wherein each reference numeral represents: 1 fermentation liquor storage tank, 2 microfiltration membrane device, 3 ion exchange adsorption device, 4 desorption device, 5 active carbon decolorization device, 6 nanofiltration concentration device, 7 spray drying device, 8 microfiltration membrane feed pump, 9 desorption device feed pump, 10 active carbon decolorization device feed pump, 11 nanofiltration concentration device feed pump, 12 material receiving device, 13 microfiltration membrane device feed liquor pipe, 14 microfiltration membrane device return pipe, 15 ion exchange adsorption device feed liquor pipe, 16 desorption device feed pipe, 17 active carbon decolorization device feed pipe, 18 nanofiltration concentration device feed pipe, 19 spray drying device feed pipe, 20 material discharge pipe and 21 material receiving pipe.
Detailed Description
The invention will be better understood from the following examples.
The drawings in the specification show the structure, ratio, size, etc. only for the purpose of matching with the content disclosed in the specification, so as to be known and read by those skilled in the art, and not for the purpose of limiting the present invention, so the present invention does not have the essential meaning in the art, and any structure modification, ratio relationship change or size adjustment should still fall within the scope covered by the technical content disclosed in the present invention without affecting the function and achievable purpose of the present invention. Meanwhile, the terms "upper", "lower", "front", "rear", "middle", and the like used in the present specification are for the sake of clarity only, and are not intended to limit the scope of the present invention, and changes or adjustments of the relative relationship thereof are also considered to be the scope of the present invention without substantial changes in the technical content.
The following examples were all conducted using an apparatus as shown in FIG. 1 to extract epsilon-polylysine. The device comprises a fermentation liquor storage tank 1, a microfiltration membrane device 2, an ion exchange adsorption device 3, a desorption device 4, an active carbon decolorization device 5, a nanofiltration concentration device 6, a spray drying device 7 and a material receiving device 12.
Wherein, the feed liquid in the fermentation liquid storage tank 1 enters the microfiltration membrane device 2 through a microfiltration membrane device liquid inlet pipe 13; the trapped fluid of the microfiltration membrane device 2 returns to the microfiltration membrane device 2 through a microfiltration membrane device return pipe 14, and the permeate enters the ion exchange adsorption device 3 through an ion exchange adsorption device liquid inlet pipe 15; the adsorption resin in the ion exchange adsorption device 3 adsorbs epsilon-polylysine in the feed liquid, and then the adsorption resin adsorbed with the epsilon-polylysine is introduced into the desorption device 4 through the feed pipe 16 of the desorption device for desorption; the sodium chloride solution in the desorption device 4 is used for desorbing epsilon-polylysine in the resin, and then the epsilon-polylysine enters the activated carbon decolorization device 5 through a feed pipe 17 of the activated carbon decolorization device for decolorization; the feed liquid decolorized in the activated carbon decolorization device 5 enters the nanofiltration concentration device 6 through a feed pipe 18 of the nanofiltration concentration device; the trapped liquid of the nanofiltration concentration device 6 enters the spray drying device 7 through a feed pipe 19 of the spray drying device after being concentrated, and the permeate liquid is discharged outwards through a discharge pipe 20; the dried material in the spray drying device 7 enters the material receiving device 12 through the material receiving pipe 21 to be collected and stored.
A microfiltration membrane feeding pump 8 is arranged on the microfiltration membrane device liquid inlet pipe 13; a desorption device feed pump 9 is arranged on the desorption device feed pipe 16; the feeding pipe 17 of the activated carbon decoloring device is provided with a feeding pump 10 of the activated carbon decoloring device; the feed pipe 18 of the nanofiltration concentration device is provided with a feed pump 11 of the nanofiltration concentration device.
The microfiltration membrane in the microfiltration membrane device 2 is a ceramic microfiltration membrane, and the average membrane pore size is 5-500 nm.
The adsorption resin in the ion exchange adsorption device 3 is cation exchange resin with the model of Dow chemical Amberlite eIRC-50.
The filtering precision of the activated carbon decoloring device 5 is 100-1000 meshes.
The intercepted molecular weight of the nanofiltration membrane in the nanofiltration concentration device 6 is 100-1000 Da.
Example 1
The trapped liquid of the microfiltration membrane device 2 flows back to the fermentation liquid storage tank 1 for circulation, the permeated liquid enters an ion exchange adsorption device 3 to adsorb epsilon-polylysine, and then the adsorption resin is conveyed into a desorption device 4 by the driving of a feed pump 9 of the desorption device to desorb the epsilon-polylysine by sodium chloride solution, and the resin is recovered; after desorption, adding activated carbon to adsorb pigment; the active carbon decolorization device is driven by a feed pump 10 to enter an active carbon decolorization device 5 for decolorization; the decolored clear liquid is driven by a feed pump 11 of a nanofiltration concentration device to enter a nanofiltration concentration device 6 to concentrate epsilon-polylysine extracting solution for 3-4 times, water is added to dialyze inorganic salt in the epsilon-polylysine extracting solution, the dialyzed water amount is 2-3 times of the total volume of the concentrated solution, the dialyzed concentrated solution enters a spray drying device 7 to be spray dried, and epsilon-polylysine solid products are collected through a material receiving device 12.
Wherein, in the microfiltration membrane device 2, the membrane aperture of the ceramic membrane is 500nm, and the operation conditions are controlled as follows: the flow rate of the membrane surface is 2m/s, the filtration temperature is 50 ℃, and the filtration pressure is 0.1 MPa.
In the nanofiltration concentration device 6, the molecular weight cut-off of the nanofiltration membrane is 1000Da, and the operation conditions are controlled as follows: the filtration temperature was 40 ℃ and the filtration pressure was 0.5 MPa.
In the embodiment, the ceramic membrane has larger pore size selection, unstable filtration flux to epsilon-polylysine fermentation liquor and obvious attenuation. The filtrate is not particularly clear and membrane fouling is rapid; the rejection rate of the nanofiltration membrane is low, and the rejection rate of the product of epsilon-polylysine is low. Resulting in greater product passage in the subsequent water dialysis, the overall yield of the final epsilon-polylysine product was 54.4% with a purity of 97.5%.
Example 2
The trapped liquid of the microfiltration membrane device 2 flows back to the fermentation liquid storage tank 1 for circulation, the permeated liquid enters an ion exchange adsorption device 3 to adsorb epsilon-polylysine, and then the adsorption resin is conveyed into a desorption device 4 by the driving of a feed pump 9 of the desorption device to desorb the epsilon-polylysine by sodium chloride solution, and the resin is recovered; after desorption, adding activated carbon to adsorb pigment; the active carbon decolorization device is driven by a feed pump 10 to enter an active carbon decolorization device 5 for decolorization; the decolored clear liquid is driven by a feed pump 11 of a nanofiltration concentration device to enter a nanofiltration concentration device 6 to concentrate epsilon-polylysine extracting solution for 3-4 times, water is added to dialyze inorganic salt in the epsilon-polylysine extracting solution, the dialyzed water amount is 2-3 times of the total volume of the concentrated solution, the dialyzed concentrated solution enters a spray drying device 7 to be spray dried, and epsilon-polylysine solid products are collected through a material receiving device 12.
Wherein, in the microfiltration membrane device 2, the membrane aperture of the ceramic membrane is 5nm, and the operation conditions are controlled as follows: the flow rate of the membrane surface is 6m/s, the filtering temperature is 20 ℃, and the filtering pressure is 0.4-0.6 MPa.
In the nanofiltration concentration device 6, the molecular weight cut-off of the nanofiltration membrane is 100Da, and the operation conditions are controlled as follows: the filtration temperature was 20 ℃ and the filtration pressure was 2.0 MPa.
In the embodiment, the pore diameter of the ceramic membrane is 5nm, the filtration flux is relatively stable, the quality of the filtrate is good, but the flux is low due to the small pore diameter. The nanofiltration membrane has smaller molecular weight, higher retention rate on epsilon-polylysine and higher recovery rate, but simultaneously retains partial salt, pigment, micromolecular protein and other impurities, and the finally obtained epsilon-polylysine product has the total recovery rate of 98.4 percent and the purity of 95.8 percent.
Example 3
The trapped liquid of the microfiltration membrane device 2 flows back to the fermentation liquid storage tank 1 for circulation, the permeated liquid enters an ion exchange adsorption device 3 to adsorb epsilon-polylysine, and then the adsorption resin is conveyed into a desorption device 4 by the driving of a feed pump 9 of the desorption device to desorb the epsilon-polylysine by sodium chloride solution, and the resin is recovered; after desorption, adding activated carbon to adsorb pigment; the active carbon decolorization device is driven by a feed pump 10 to enter an active carbon decolorization device 5 for decolorization; the decolored clear liquid is driven by a feed pump 11 of a nanofiltration concentration device to enter a nanofiltration concentration device 6 to concentrate epsilon-polylysine extracting solution for 5-8 times, water is added to dialyze inorganic salt in the epsilon-polylysine extracting solution, the dialyzed water amount is 2-3 times of the total volume of the concentrated solution, the dialyzed concentrated solution enters a spray drying device 7 to be spray dried, and epsilon-polylysine solid products are collected through a material receiving device 12.
Wherein, in the microfiltration membrane device 2, the membrane aperture of the ceramic membrane is 50nm, and the operation conditions are controlled as follows: the flow rate of the membrane surface is 5m/s, the filtering temperature is 40 ℃, and the filtering pressure is 0.4-MPa.
In the nanofiltration concentration device 6, the molecular weight cut-off of the nanofiltration membrane is 200Da, and the operation conditions are controlled as follows: the filtration temperature was 35 ℃ and the filtration pressure was 1.2 MPa.
In the embodiment, the aperture of the ceramic membrane is 50nm, the flux of the fermentation liquor for filtering epsilon-polylysine is relatively stable, and the pollution to the membrane surface is relatively slow. The fermentation liquor can be concentrated by 5-8 times. The nanofiltration membrane has the molecular weight of 200Da, the flux is large, the retention rate of epsilon-polylysine is high, most inorganic salt can permeate through the nanofiltration membrane, and the conductivity of 18000us/cm is reduced to 350us/cm through 4 times of elutriation. The effect is superior to that of the examples 1 and 2, and the total recovery rate of the finally obtained epsilon-polylysine product is 97.9 percent, and the purity is 98.6 percent.
The utility model provides a thinking and a method of epsilon-polylysine's extraction element specifically realize that this technical scheme's method and approach are many, above only the utility model discloses a preferred embodiment should point out, to the ordinary technical personnel in this technical field, not deviating from the utility model discloses under the prerequisite of principle, can also make a plurality of improvements and moist decorations, these improvements should also regard as with moist decorations the utility model discloses a protection scope. All the components not specified in the present embodiment can be realized by the prior art.

Claims (9)

1. The extraction device of epsilon-polylysine is characterized by comprising a fermentation liquor storage tank (1), a microfiltration membrane device (2) for filtering, an ion exchange adsorption device (3) for purifying, a desorption device (4), an active carbon decolorization device (5), a nanofiltration concentration device (6) for concentrating, a spray drying device (7) and a material receiving device (12);
wherein, the feed liquid in the fermentation liquid storage tank (1) enters the microfiltration membrane device (2) through a microfiltration membrane device feed liquid pipe (13);
the trapped fluid of the microfiltration membrane device (2) returns to the microfiltration membrane device (2) through a return pipe (14) of the microfiltration membrane device, and the permeate enters the ion exchange adsorption device (3) through a liquid inlet pipe (15) of the ion exchange adsorption device;
the adsorption resin in the ion exchange adsorption device (3) adsorbs epsilon-polylysine in the feed liquid, and then the adsorption resin adsorbed with the epsilon-polylysine is introduced into a desorption device (4) through a feed pipe (16) of the desorption device for desorption;
the sodium chloride solution in the desorption device (4) is used for resolving epsilon-polylysine in the resin, and then the epsilon-polylysine enters the activated carbon decolorization device (5) through a feed pipe (17) of the activated carbon decolorization device for decolorization;
the feed liquid decolorized in the activated carbon decolorization device (5) enters a nanofiltration concentration device (6) through a nanofiltration concentration device feed pipe (18);
trapped liquid of the nanofiltration concentration device (6) enters the spray drying device (7) through a feed pipe (19) of the spray drying device after being concentrated, and permeated liquid is discharged outwards through a discharge pipe (20);
the dried materials in the spray drying device (7) enter the material receiving device (12) through the material receiving pipe (21) to be collected and stored.
2. The extraction apparatus of epsilon-polylysine as defined in claim 1, wherein a microfiltration membrane feeding pump (8) is provided on the inlet pipe (13) of the microfiltration membrane device.
3. The extraction apparatus of epsilon-polylysine as defined in claim 1, wherein said desorber feed line (16) is provided with a desorber feed pump (9).
4. The extraction device of epsilon-polylysine as defined in claim 1, wherein a feeding pump (10) of the activated carbon decolorization device is arranged on the feeding pipe (17) of the activated carbon decolorization device.
5. The epsilon-polylysine extraction device according to claim 1, wherein a nanofiltration concentration device feed pump (11) is provided on the nanofiltration concentration device feed pipe (18).
6. The extraction device of epsilon-polylysine as defined in claim 1, wherein the microfiltration membrane of the microfiltration membrane device (2) is a ceramic microfiltration membrane, and the average membrane pore size is 5-500 nm.
7. The extraction apparatus of epsilon-polylysine according to claim 1, wherein the adsorption resin in said ion-exchange adsorption means (3) is a cation exchange resin.
8. The extraction device of epsilon-polylysine according to claim 1, characterized in that the filtration precision of the activated carbon decolorization device (5) is 100 to 1000 meshes.
9. The extraction device of epsilon-polylysine as defined in claim 1, wherein the nanofiltration membrane in the nanofiltration concentration device (6) has a molecular weight cutoff of 100-1000 Da.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114181388A (en) * 2021-11-30 2022-03-15 河北圣雪大成制药有限责任公司 Method for extracting polylysine from fermentation liquor

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114181388A (en) * 2021-11-30 2022-03-15 河北圣雪大成制药有限责任公司 Method for extracting polylysine from fermentation liquor
CN114181388B (en) * 2021-11-30 2023-12-01 河北圣雪大成制药有限责任公司 Method for extracting polylysine from fermentation liquor

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