KR101975187B1

KR101975187B1 - Method of preparaing diol

Info

Publication number: KR101975187B1
Application number: KR1020170055199A
Authority: KR
Inventors: 전상준; 남희근
Original assignee: 지에스칼텍스 주식회사
Priority date: 2017-04-28
Filing date: 2017-04-28
Publication date: 2019-05-07
Also published as: KR20180121040A; CN110573625A; WO2018199669A1

Abstract

The present invention relates to a process for the preparation of a diol comprising a separation and purification process. Specifically, the present invention provides a method for producing a fermentation broth comprising: producing a fermentation broth containing a diol; Removing impurities in the fermentation broth to produce a pretreatment liquid; And purifying the pretreatment liquid to obtain a diol.

Description

METHOD OF PREPARING DIOL [0002]

The present invention relates to a process for the production of diols. More particularly, the present invention relates to a process for preparing a diol comprising a separation and purification process.

For example, diols such as 2,3-butanediol have been utilized as industrial preparations such as fuel additives, antifreeze and plasticizers, and as home-use preparations such as cosmetics and medicinal ingredients. The above-mentioned diols can be industrially produced through a continuous chemical catalyst process using, for example, C-4 olefin, but their use has been limited due to problems such as a high cost manufacturing process, environmental pollution induction and isomer separation difficulty.

Recently, a process for producing 2,3-butanediol as a bio-base at low cost and environmentally friendly has been under development in 2,3-butanediol production process. As a result, the possibility of expanding commercial use of 2,3-butanediol is increasing. For example, 2,3-butanediol having a specific structure of a desired structure can be selectively produced by a bio-based process, and its use can also be developed specifically.

However, other diol by-products (e.g., propanediol, 1,3-butanediol, 1,4-butanediol, etc.) may be produced together in the process of producing a target diol such as 2,3- The separation and purification process should be developed to increase the yield.

In addition, not only diol by-products but also impurities such as various organic salts, inorganic salts and organic acids, microorganisms derived from the biogenic raw materials, and biochemical byproducts such as proteins can be produced together, and processes for removing the impurities and the by- There is a need.

For example, Korean Patent Publication No. 1575717 discloses an example of a method for purifying 2,3-butanediol containing reduced pressure distillation.

Korean Patent Registration No. 10-1575717 (Feb. 20, 2015)

An object of the present invention is to provide a process for producing a diol capable of producing a target diol with excellent yield and purity.

1. producing a fermentation broth comprising a diol; Generating a pretreatment liquid from which the impurities have been removed by continuous treatment of the fermentation broth with electrodialysis and ion exchange; And purifying said pretreatment liquid to obtain a diol.

2. The method for producing diol according to 1 above, wherein the inorganic salt and organic acid contained in the fermentation broth are removed by electrodialysis and ion exchange.

3. The method of claim 1, wherein the ion exchange comprises sequentially passing the fermentation broth through a cation exchange resin column and an anion exchange resin column.

4. The method of claim 1, further comprising filtering the fermentation broth prior to electrodialysis and ion exchange treatment.

5. The process of claim 4, wherein said filtration comprises continuous treatment of micro-filtration and ultra-filtration.

6. The method of producing a diol according to 5 above, wherein the microfiltration is performed using a polymer or ceramic membrane having a pore size of 0.05 to 10 mu m.

7. The method of claim 5, wherein the ultrafiltration uses an organic polymer membrane or an organic hollow fiber laminate having a pore size ranging from 1,000 to 100,000 in Molecular Weight Cut Off (MWCO).

8. The method for producing a diol according to 5 above, wherein the microbial-derived cells and solid components contained in the fermentation broth are removed through the microfiltration, and the protein is removed by the ultrafiltration.

9. The process for producing a diol according to the above 5, wherein the electrodialysis and the ion exchange continuous treatment are performed immediately after the continuous treatment of the microfiltration and the ultrafiltration.

10. The method for producing diol according to any one of 1 to 4 above, further comprising the step of concentrating the pretreatment liquid to remove water.

11. The process of claim 10, wherein the concentration comprises evaporation under reduced pressure, wherein 90 to 95% of the water contained in the pretreatment liquid is removed.

12. The process for producing diol according to 1 above, wherein the step of purifying the pretreatment liquid comprises a vacuum distillation.

13. The process of claim 12, wherein the reduced pressure distillation comprises a first reduced pressure distillation and a second reduced pressure distillation, wherein the second reduced pressure distillation is performed at a higher temperature than the first reduced pressure distillation.

14. The process of claim 1, wherein the diol is 2,3-butanediol.

15. The method of claim 1, wherein the step of producing the fermentation broth comprises:

Preparing a saccharified liquid using a bio raw material; And producing a fermentation broth by using a strain in the glycated solution.

16. The method of producing a diol according to 15 above, wherein the bio raw material comprises cassava, and the strain comprises Klebsiella.

According to embodiments of the present invention, pretreatment including, for example, pre-purification of target diol through reduced pressure distillation, electrodialysis and ion exchange may be performed to effectively remove components such as inorganic salts and organic acids present in the fermentation broth have. Thus, the purity of the target diol in the purification process can be significantly improved.

Further, prior to the pretreatment including electrodialysis and ion exchange, continuous treatment of microfiltration and ultrafiltration can be further performed. Therefore, prior to the removal of the inorganic salt and the organic acid, the bio-byproducts including the cells derived from the microorganism, the solid content, the protein and the like can be removed in advance and the pretreatment efficiency can be improved.

In addition, the fermentation broth can use specific raw materials and strains having specificity to 2,3-butanediol, and can reduce the production of other diols or alcohols in the fermentation broth step so that the recovery rate of 2,3-butanediol in the reduced- .

Further, the purity of the target diol can be further increased by combining with the above-described separation, purification, extraction and / or decolorization and deodorization processes.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic flow diagram illustrating a method for manufacturing a diol in accordance with one exemplary embodiment of the present invention. FIG.
2 is a schematic flow diagram illustrating a method for manufacturing a diol in accordance with some embodiments of the present invention.
3 is a schematic flow diagram for illustrating a method of manufacturing a diol in accordance with some embodiments of the present invention.
4 is a schematic flow diagram illustrating a method for manufacturing a diol in accordance with some embodiments of the present invention.
5 is a schematic flow diagram illustrating a method for manufacturing a diol in accordance with some embodiments of the present invention.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, It will be obvious to those skilled in the art that such modifications and variations are within the scope of the appended claims.

1 to 3 are schematic flow charts for explaining a method of manufacturing a diol according to exemplary embodiments of the present invention.

Referring to FIG. 1, the method for producing diol comprises preparing a fermentation broth containing a diol mixture (S10), removing impurities (S20), increasing the concentration of diol through concentration (S30) A diol is obtained (S30), and a further decolorization or deodorization step (S40) can be further carried out.

Preparation of fermentation broth (S10)

The fermentation broth can be obtained by fermenting a bio raw material with a strain. The bio-raw material may be a kernel, woody and / or starch-based material. Examples of the starch-based material include starch-containing cereals such as corn, rye, cassava, raw sugar, glucose, and the like. Etc. may be used.

As the strain, a microorganism capable of producing a diol-containing fermentation product can be utilized without particular limitation. For example, Klebsiella, Bacillus, Serratia, Enterobacter, Clostridium, yeast, E. coli and the like are utilized as the microorganisms .

The above-mentioned bio raw materials and strains can be selected in consideration of a desired target diol. In exemplary embodiments of the present invention, the target diol may be 2,3-butanediol. In one embodiment, the target diol may comprise 2R, 3S-butanediol in the optical isomer of 2,3-butanediol.

In some embodiments, cassava as the bio-raw material and Klebsiella as the strain may be used for the production of 2,3-butanediol. For example, K. oxytoca, K. pneumoniae and the like can be used as the above-mentioned strains, and K. oxytoca (K. oxytoca) .

According to exemplary embodiments, the preparation of the fermentation broth may comprise separate saccharification and fermentation processes. The saccharification step may be performed in a liquid phase. For example, the biosource material may be pulverized, mixed with a liquid such as fresh water, and a saccharification enzyme may be added to react with the biosource material to prepare a saccharification solution . The saccharifying enzyme may include, for example, an amylase-based enzyme.

Thereafter, the fermentation broth can be prepared by injecting the strain into the saccharified solution. The fermentation broth can be, for example, not only 2,3-butanediol, which is a target diol, but also monoalcohols and other glycols such as ethylene glycol, diethylene glycol, 1,3-propanediol, , Dipropylene glycol, and the like). In addition, the fermentation broth may contain various inorganic salts, organic acids, and impurities such as bio-by-products derived from the strain or its metabolites.

As described above, by separately performing the saccharification step and the fermentation step, the production of biodegradable products can be relatively reduced compared to, for example, simultaneous saccharification / fermentation, and the yield of diol production can be increased.

Impurity removal (S20)

The impurity removal step may be performed as a pretreatment step for the fermentation broth containing biosynthetic diol. Thus, the above-mentioned impurities contained in the fermentation broth can be removed.

As shown in FIG. 2, the impurity removing process may include an electrodialysis and an ion exchange process (S25). In some embodiments, the filtration step (S23) may be further performed before the electrodialysis and ion exchange treatment (S25) as shown in Fig.

Filtration step (S23)

According to exemplary embodiments of the present invention, the filtration process may include microfiltration and utrafiltration. The fermentation broth can be continuously passed through the microfiltration membrane and the ultrafiltration membrane in order to remove the biosubstance.

For example, the micro-filtration can remove microbial cells and microbial solid matter (suspended solid or solubilized solid matter) produced from the strain. The microfiltration can be performed by passing the fermentation broth through a polymer or ceramic membrane having a pore size of, for example, about 0.05 to 10 mu m, installed in the filter module. The fermentation broth can be repeatedly subjected to microfiltration through a circulation channel. In one embodiment, the pore size of the microfiltration membrane may be about 0.05 to 0.2 탆.

The microbial cells and solid matter in the fermentation broth can be removed by microfiltration, and the protein can be removed through ultrafiltration.

The ultrafiltration may be performed by passing the fermentation broth through an organic polymer membrane or an organic hollow fiber laminate having a pore size ranging from 1,000 to 100,000, for example, a molecular weight cut off (MWCO) have.

As described above, the cells and the solid matter derived from the microorganism of the strain can be firstly removed by continuous treatment of microfiltration and ultrafiltration, and then the protein can be removed. Thus, by removing the byproduct before the electrodialysis and the ion exchange treatment, the fouling by the byproduct of the biosensor is blocked, thereby improving the efficiency of the subsequent impurity removal process.

In addition, for example, microfiltration / ultrafiltration can be used without employing a nanofiltration mechanism, thereby improving the specificity of the filtration process targeting the biotreatment product. For example, when nanofiltration is used instead of microfiltration / ultrafiltration continuous treatment, the filtration rod is increased due to simultaneous removal of the microbial-derived cells, solids and protein, so that the desired diol is coagulated or adsorbed together with the bio- . Thus, the yield of the target diol obtained after the purification process can be lowered.

However, according to the exemplary embodiments of the present invention, microfiltration and ultrafiltration, which are specifically designed according to the filtration target, are sequentially performed, so that only the bio-by-product is selectively removed so that the subsequent inorganic salt, The efficiency of the target diol purification process can be improved.

Electrodialysis and ion exchange treatment (S25)

According to exemplary embodiments of the present invention, a desalination process in which an inorganic salt and an organic acid contained in a filtrate collected through microfiltration and ultrafiltration are sequentially removed through electrodialysis and sequential continuous treatment of ion exchange .

The electrodialysis can be performed using a membrane device including a cation exchange membrane and an anion exchange membrane. For example, a cation exchange membrane and an anion exchange membrane may be disposed between the anode and the cathode to divide the electrodialysis unit into a compartment, and a DC current may be supplied using the anode and the cathode.

For example, monovalent cations such as Na ⁺ and K ⁺ , divalent cations such as Ca ² ⁺ and Mg ² ⁺ can not pass through the anion exchange membrane and accumulate in the compartment, It can be diluted and discharged in a desalted state.

For example, the organic acid may be removed through the ion exchange treatment of the filtrate from which the inorganic salt has been removed.

The electrodialyzed filtrate may contain target diols and other alcohols, weak salts or organic acids present in the form of weaker ions. By the ion exchange treatment, a weak salt or an organic acid present in a weak ion form is removed, and a pretreatment liquid substantially containing a target diol and other alcohols can be obtained.

Examples of the ion exchanger used in the ion exchange treatment include an ion exchange resin, an ion exchange fiber, a gel ion exchanger, a liquid ion exchanger, a zeolite, and a carbonaceous ion exchanger. In the embodiments of the present invention, Ion exchange resins can be utilized.

For example, an ion exchange treatment utilizing a cation exchange resin and an anion exchange resin may be performed. The cation exchange resin can be regenerated into a weakly acidic solution such as hydrochloric acid and used as the H type. The anion exchange resin may be regenerated as a weakly alkaline solution such as sodium hydroxide and used as the OH type.

The desalting method by the ion exchange resin may include a batch method or a column method. According to exemplary embodiments, a columnar approach may be employed for repeated desalination. For example, the electrodialyzed filtrate may be passed through a column filled with a cation exchange resin, and then passed through a column filled with an anion exchange resin.

According to exemplary embodiments, the inorganic salts are removed through the electrodialysis process, and the organic acid and the residual inorganic salts can be removed together by the ion exchange treatment.

The efficiency of the desalination process of the filtrate from which the by-product of bio-by-filtration has been removed can be significantly increased through continuous and sequential execution of electrodialysis and ion exchange, and the selectivity and yield of target diol acquisition can be improved in subsequent concentration and purification processes .

As described above, when a biogenic raw material (e.g., cassava) and a strain (e.g., K. oxytoca) specific to 2,3-butanediol are used, general industrial production A large amount of organic and inorganic impurities can be produced in comparison with a bioprocess for the production of a process or other diol (for example, 1,3-propanediol).

Accordingly, when the oil and the inorganic impurities are removed only by ion exchange, the load of the ion exchange step is excessively increased, and sufficient desalination efficiency may not be ensured. Further, in order to secure the desired desalination efficiency, the number of steps (for example, the number of columns) in the ion exchange equipment is excessively increased to lower the process efficiency, and the target diol yield in the purification process may deteriorate.

However, according to the embodiments of the present invention, it is possible to reduce the load of ion exchange by performing electrodialysis first before ion exchange. Therefore, it is possible to design the number of stages required for ion exchange, for example, in a two-stage configuration of cation exchange resin and anion exchange resin. Therefore, desired desalting efficiency can be secured while preventing a decrease in target diol yield due to an increase in the number of ion exchange stages.

Concentration (S30)

The water in the pretreatment liquid after electrodialysis and ion exchange treatment can be removed through concentration. For example, concentration can be performed through a vacuum evaporation process. The removal rate of water by the concentration process can be set in consideration of the efficiency of the purification process of the subsequent target diol and the extraction process to be described later. If the removal rate of water is too high, the efficiency of the extraction process may be lowered. Also, if the water removal rate is too low, the efficiency of the purification process may be lowered and the yield of the target diol may be lowered.

For example, about 90 to 95% of the water contained in the pretreatment liquid can be removed through a concentration process. In one embodiment, the concentration of the fermentation product in the culture may be controlled to be about 500 to 900 g / L through the concentration process.

Target diol tablet (S40)

A concentrate containing the fermentation product is collected through a concentration process, and a target diol can be obtained from the concentrate through a purification process.

According to embodiments of the present invention, the purification process may include distillation. The distillation step may include, for example, distillation, normal pressure distillation, thin film distillation, vacuum distillation, and the like. In some embodiments, a vacuum distillation process may be employed for targeted diol purification. The boiling point can be lowered by the distillation under reduced pressure, whereby the generation of impurities in the distillation step can be suppressed.

In some embodiments, the purification process may comprise a first vacuum distillation and a second vacuum distillation.

The second vacuum distillation can be carried out at a higher temperature than the first vacuum distillation. For example, the first vacuum distillation can be carried out in the range of about 40 to 70 degrees Celsius ( ^oC ) to discharge impurities of lower boiling point than the target diol (for example, 2,3-butanediol) to the top have. The second vacuum distillation for the concentrate containing the target diol can be carried out in the temperature range of about 100 to 130 degrees ( ^o C).

When the second vacuum distillation temperature is less than about 100 degrees, the recovery rate may be lowered. If the second vacuum distillation temperature is greater than about 130 degrees, the target diol (e.g., 2,3-butanediol) or remaining traces of organics can react to form byproducts.

Decolorization or deodorization (S50)

In embodiments of the present invention, a decolorization or deodorization process may be optionally performed depending on the use of the target diol. For example, if 2,3-butanediol is utilized as a component of a cosmetic or cosmetic composition, a further decolorizing or deodorizing process may be performed.

The extraction step (S32)

4 is a schematic flow diagram illustrating a method for making a diol in accordance with some embodiments of the present invention. For example, as shown in FIG. 4, the extraction process may be further performed to remove the remaining impurities.

In some embodiments, the extraction process may be performed between concentration processes. For example, the extraction process may be performed on the pretreatment liquid in which water is partially removed by the first concentration step (S31), and the extraction solvent used in the extraction step may be recovered through the second concentration step (S35) have.

The extraction process may include solvent extraction (or solvent precipitation), water-phase binary extraction, phase separation, and the like. The solvent extraction may include, for example, a mechanism to precipitate impurities using an extraction solvent. The above-mentioned bi-component extraction may include a mechanism for separating and removing the impurity phase through, for example, inorganic salt addition. The phase separation extraction may include a mechanism for increasing the yield of the target diol through separation of the organic phase and the inorganic phase.

In exemplary embodiments of the present invention, the solvent extraction process may be utilized in consideration of the prevention of residue due to the addition of additional components in the extraction process, ease of recovery process, and the like.

For example, a low-alcohol solvent can be added as an extraction solvent to the pretreatment solution through the first concentration step. With the above-mentioned extraction solvent, for example, inorganic salts and organic acid salts which have not been removed by the impurity removal step (S20) can form precipitates in the form of solid.

As the extraction solvent, a lower alcohol having 3 or less carbon atoms can be used for separation from a target diol such as 2,3-butanediol. For example, methanol, ethanol and / or isopropanol can be used as the extraction solvent, preferably isopropanol.

The precipitate may be removed by filtering the pretreatment solution that has undergone the extraction process. Thereafter, the extraction solvent can be recovered through the second concentration step (S35). The recovered extraction solvent may be recycled to be fed again to the extraction process.

Additional recovery process

5 is a schematic flow diagram illustrating a method for making a diol in accordance with some embodiments of the present invention. For example, further recovery may be performed through the residue produced after the target diol purification. The residue may be solvent washed as shown in Figure 5 (S45) and the washed residue may be recycled, for example, to the extraction process (S32) or the second concentration process (S35) to repeat the target diol purification.

In one embodiment, the solvent washing may be carried out by a mechanism that is substantially the same as or similar to the extraction process described above. For example, the residue may be washed with a solvent comprising isopropanol, the precipitate may be filtered off, and then the washed residue may be recycled.

In some embodiments, the washed residue may be recovered to the extraction process (S32) and the above-described solvent extraction process may be performed again. In some embodiments, the washed residue is recovered to a second concentration step (S35) and the solvent is removed by vacuum distillation, and then the target diol may be re-collected by the purification step (S40). In some embodiments, the washed residue may be directly introduced into the target diol purification process (S40).

In some embodiments, the residue produced in the form of, for example, sludge or cake after discoloration / deodorization (S50) may be further recovered. As shown in FIG. 5, the product may be recycled to an extraction, concentration, and / or purification process after solvent wash (S45) of decolorizing / deodorizing residues.

Hereinafter, the processes of the diol production method according to the embodiments of the present invention will be described in detail with reference to specific experimental examples. It should be noted that the embodiments and the comparative examples included in the experimental examples are illustrative of the present invention but are not intended to limit the scope of the appended claims and various changes and modifications may be made to the embodiments within the scope and spirit of the present invention It is obvious to those skilled in the art that such variations and modifications are within the scope of the appended claims.

Experimental Example

1) Preparation of fermentation broth

Cassava was pulverized as a raw material, saccharified and used as a carbon source, and K. oxytoca GSC112 LK strain was used to prepare a fermentation broth containing 2,3-butanediol as a target diol. Specifically, 1 mL of the K. oxytoca GSC112 (KCTC 11888BP) LK strain stored in a 15% glycerol solution at -70 ° C was inoculated into a 20-mL complex medium containing 10 g / L of the saccharified raw material, After culturing at 150 rpm for 8 hours, 3.0 mL of the above culture was transferred to a 300 mL complex medium containing 10 g / L saccharified raw material, and then re-cultured at 37 DEG C and 150 rpm for 8 hours. LK means a strain in which the ldhA gene encoding the lactate dehydrogenase enzyme involved in the production of lactic acid in the strain is removed. The fermentation was carried out by inoculating 300 mL of the cultured medium into a bioreactor containing a complex medium of 2.7 L containing 10 g / L of the raw material. The culturing conditions were 300 mM of saccharified raw material, 37 DEG C of culture temperature, The stirring speed was 150 rpm.

The cell concentration during culture was estimated by using a spectrophotometer using the absorbance (OD600) measured beforehand and the weight verification line of the dry cell. The concentrations of various organic acids and other alcohols, including succinic acid, produced as metabolites during the culture, were obtained by periodically sampling a bioreactor and centrifuging at 13,000 rpm at 4 ° C for 10 minutes. The supernatant was analyzed by liquid chromatography (HPLC) Respectively.

As a result, as shown in Table 1, a fermentation broth in which about 120 g / L of 2,3-butanediol was contained as a target product as a target diol was obtained.

division 2,3-butanediol Formic acid ethanol Lactic acid Suche mountain Acetic acid Acetone content
(g / L) 120.1 3.88 0.92 0.17 0.21 4.56 3.98

2) Filtration process

2-1) Micro-filtration

The fermentation broth was first passed through a microfiltration membrane having a pore size of 0.05 μm at a system pressure of 2 to 3 bar at 30 to 40 ^° C. at a flow rate of 25 L / m ² / h.

2-2) Ultrafiltration

After the microfiltration, the culture was continuously passed through an ultrafiltration membrane of MWCO 10,000 hollow fiber type. The system temperature and pressure were maintained at 30-40 ^° C and 5-6 bar, respectively. The flow rate of the culture liquid was maintained at 20 L / m ² / h.

After the microfiltration, about 99% or more of the total amount of cells and solids contained in the fermentation broth was removed. After the ultrafiltration, about 70% of proteins were removed from the fermentation broth. The amount of protein removed was determined by the Bradford assay protein determination method.

3) Electrodialysis and ion exchange treatment

The fermentation broth having undergone the above microfiltration and ultrafiltration was introduced into an electrodialysis device containing three compartments with a cation exchange resin membrane and an anion exchange resin membrane embedded therein. 180V DC power was applied to the anode and cathode, and the flow rate in the compartment was kept at 60 ~ 80 LPM (L / min).

The culture solution after electrodialysis was subjected to continuous ion exchange treatment. Specifically, the weak basic anion exchange resin and the strongly acidic cation exchange resin were charged in the column, and the electrodialyzed culture liquid was passed through the pump at 5 LPM at room temperature in the order of the cation resin and the anion resin. The components of the pretreatment solution after completion of the electrodialysis and ion exchange treatment (pretreatment) were analyzed by HPLC and IC, as shown in Table 2 below.

division Organic acid Divalent cation Monovalent cation sulfate phosphate chloride ammonia Before pretreatment
(ppm) 2,498 62 3,313 66 4,355 31 1,300 After preprocessing
(ppm) 130 5 51 8 17 2 51

Referring to Table 2, about 95% or more of the organic acid was removed by continuous electrodialysis and ion exchange, and about 90 to 99% or more of ions / salts were also removed.

On the other hand, when the ion exchange was carried out under the same conditions except for the electrodialysis, the final ion concentration reached a similar level, but when the same amount of resin was used, the throughput of the fermentation broth was reduced to less than 50%. Therefore, in this case, the dilution ratio of 2,3-butanediol to increase the regeneration wastewater and the same recovery rate as the operation batch is increased should be increased.

4) Concentration

After the electrodialysis and ion exchange treatment, the pretreatment solution was changed to 50 ^{o A} 50 wt% or more diol concentrate was prepared by removing 90% of water through evaporation under reduced pressure at 50 mbar.

5) Target Diol Tablet

The concentrate was subjected to a first distillation under a pressure of 50 mbar and 40 ^o C to remove impurities having a lower boiling point than 2,3-butanediol, followed by a second distillation under a pressure of 50 mbar and 105 ^o C 2,3-butanediol was recovered.

As a result of the purification, 2,3-butanediol having a purity of 99.5% was obtained at a recovery rate of about 85% as compared with the fermentation broth.

Claims

Producing a fermentation broth comprising a diol;
The fermentation broth is filtered through continuous treatment of micro-filtration and ultrafiltration to remove microbial-derived cells and solid components contained in the fermentation broth through the microfiltration, Removing the protein through filtration;
Continuously filtering the filtered fermentation broth by electrodialysis and ion exchange to remove impurities to produce a pretreatment solution; And
And purifying said pretreatment liquid to obtain a diol.

The diol production method according to claim 1, wherein the inorganic salt and the organic acid contained in the fermentation broth are removed by electrodialysis and ion exchange.

The method of claim 1, wherein the ion exchange comprises passing the fermentation broth through a cation exchange resin column and an anion exchange resin column sequentially.

delete

[2] The method according to claim 1, wherein the microfiltration is performed using a polymer or ceramic membrane having a pore size of 0.05 to 10 [mu] m.

The method of claim 1, wherein the ultrafiltration uses an organic polymer membrane or an organic hollow fiber laminate having a pore size in the range of MWCO 1,000 to 100,000.

delete

The method of claim 1, wherein the electrodialysis and ion exchange continuous treatment is performed immediately after the continuous treatment of microfiltration and ultrafiltration.

The method of claim 1, further comprising the step of concentrating the pretreatment liquid to remove water.

11. The method of claim 10, wherein the concentration comprises reduced pressure evaporation, wherein 90 to 95% of the moisture contained in the pretreatment liquid is removed.

The method of claim 1, wherein the step of purifying the pretreatment liquid comprises reduced pressure distillation.

The method of claim 12, wherein the reduced pressure distillation comprises a first reduced pressure distillation and a second reduced pressure distillation,
Wherein the second vacuum distillation is performed at a temperature higher than the first vacuum distillation.

The method of claim 1, wherein the diol is 2,3-butanediol.

The method of claim 1, wherein the step of producing the fermentation broth comprises:
Preparing a saccharified liquid using a bio raw material; And
And producing a fermentation broth by using a strain in the glycated solution.

16. The method of claim 15, wherein the bio-raw material comprises cassava and the strain comprises Klebsiella.