CN111099988A - Separation and extraction method of sodium gluconate mother liquor - Google Patents

Separation and extraction method of sodium gluconate mother liquor Download PDF

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Publication number
CN111099988A
CN111099988A CN201910784079.4A CN201910784079A CN111099988A CN 111099988 A CN111099988 A CN 111099988A CN 201910784079 A CN201910784079 A CN 201910784079A CN 111099988 A CN111099988 A CN 111099988A
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sodium gluconate
mother liquor
separating
content
solution
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Inventor
程文才
刘海亮
崔洪文
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Weifang Jianbao Biotechnology Co Ltd
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Weifang Jianbao Biotechnology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
    • C12P7/58—Aldonic, ketoaldonic or saccharic acids
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/59—Biological synthesis; Biological purification

Abstract

The invention discloses a separation and extraction method of sodium gluconate mother liquor, and relates to the technical field of chemical engineering. The method comprises the steps of preparing sodium gluconate, catalyzing, separating polysaccharide, decoloring, crystallizing and electrodialysis, wherein the separated secondary recovered mother liquor is used for separating and extracting sodium gluconate from sodium gluconate mother liquor by a homogeneous membrane electrodialysis method to obtain sodium gluconate concentrated liquor.

Description

Separation and extraction method of sodium gluconate mother liquor
Technical Field
The invention relates to the technical field of chemical engineering, in particular to a method for separating and extracting sodium gluconate mother liquor.
Background
The sodium gluconate has wide industrial application, can be used as a high-efficiency chelating agent in the industries of construction, textile printing and dyeing, metal surface treatment, water treatment and the like, a steel surface cleaning agent, a glass bottle cleaning agent, aluminum oxide coloring in the electroplating industry, a high-efficiency retarder, a high-efficiency water reducing agent and the like in the concrete industry, and is prepared by taking glucose as a raw material, adopting fermented sodium gluconate liquid, filtering, decolorizing, concentrating, crystallizing and centrifugally separating the sodium gluconate-containing liquid, namely the sodium gluconate mother liquid.
After the sodium gluconate mother liquor is repeatedly crystallized and separated for multiple times, the solid content in the liquor is 40% -60%, 30% -40% of sodium gluconate is contained, 5% -15% of polysaccharide and 1% -5% of glucose are contained, and the efficient utilization of the sodium gluconate mother liquor is always a research subject, and CN201610710054.6 discloses that an electrodialysis method is used for extracting the sodium gluconate in the mother liquor, but the residual polysaccharide in the mother liquor cannot be fully converted and extracted.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the separation and extraction method of the sodium gluconate mother liquor, disaccharide and polysaccharide in the mother liquor are fully converted into sodium gluconate, the influence of the polysaccharide on electrodialysis separation of the sodium gluconate is reduced, the yield and the recovery period of products in the mother liquor are improved, and the energy consumption is reduced.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a separation and extraction method of sodium gluconate mother liquor comprises the following steps:
s1, preparation of sodium gluconate: taking corn starch as a raw material, adding a certain amount of nutrient substances after liquefaction and saccharification, sterilizing, cooling to a proper temperature, introducing the mixture into a fermentation tank, adding an Aspergillus niger seed solution with a volume fraction of 10%, fermenting for about 28 hours under stirring and ventilation conditions, oxidizing glucose into gluconic acid by Aspergillus niger, continuously pumping NaOH to convert the gluconic acid into sodium gluconate through neutralization reaction, finishing fermentation when residual sugar is reduced to less than 10g/L, filtering out impurities such as thalli from the fermentation liquor through a plate-and-frame filter press, adjusting pH of the filtrate, heating, primarily filtering and secondary filtering through the plate-and-frame filter press, performing four-effect evaporation, concentration and crystallization, discharging, centrifuging, separating, and drying through a fluidized bed to obtain a finished product of the sodium gluconate;
s2, enzyme catalyzed: detecting 100Kg of sodium gluconate mother liquor, wherein the sodium gluconate content is 34 wt%, the disaccharide content is 6 wt% and the other polysaccharide content is 3 wt% in the mother liquor, adding pullulanase 20U/g into the mother liquor, cooling to 30 ℃, adding aspergillus niger, introducing sterile air, reacting for 6 hours, adding NaOH to adjust the pH value to be 7-8, and obtaining reaction liquid I;
s3, polysaccharide separation: ba (OH) is added to the reaction solution I20.5Kg, a small amount of unreacted polysaccharide was precipitated, Na was added2CO30.5Kg, precipitating unreacted barium ions, separating, and removing solid matters; obtaining a reaction solution II;
s4, decoloring: adding 2.0-4.0 wt% of activated carbon when the temperature of the reaction liquid II is 60 ℃, keeping the temperature for 30 minutes when the temperature is increased to 65 ℃, and then starting to filter to obtain a reaction liquid III;
s5, crystallization: concentrating the reaction liquid III at 60-80 ℃ until the glucose content is 60-80%, standing, cooling, crystallizing and separating to obtain a sodium gluconate product and a secondary recovered mother liquid;
s6, electrodialysis: and separating the separated secondary recovered mother liquor by using a homogeneous membrane electrodialysis method to extract sodium gluconate from the sodium gluconate mother liquor to obtain a sodium gluconate concentrated solution.
Further optimizing the technical scheme, the aspergillus niger seed liquid with the volume fraction of 10% is inoculated in the step S1, the pH value is maintained at 5.5-6.0 at the moment, and the temperature is maintained at 37-40 ℃.
Further optimizing the technical scheme, in the step S2, the sodium gluconate mother liquor is detected, wherein the content range of the sodium gluconate is 30% -40%, the content range of the disaccharide is 4% -12%, and the content range of the tri-pentasaccharide or more is 1% -3%.
Further optimizing the technical scheme, in the step S2, 20U/g of pullulanase is added into the mother liquor, and the closed anaerobic reaction is carried out for 2 hours at the temperature of 55-65 ℃.
Further optimizing the technical scheme, in the step S3, Ba (OH) is added into the reaction solution I20.5Kg, stirred and reacted for 20 min.
Further optimizing the technical scheme, the conditions of the homogeneous membrane electrodialysis method in the step S6 are as follows: the size of a diaphragm of the electrodialyzer is 10cm multiplied by 20cm, the electrode liquid (2mol/L sodium sulfate), the initial concentrated solution (pure water) is 0.5L, the flow feeding is adjusted to be 20L/h, the flow velocity of the electrode liquid is 10L/h, the voltage is 14V, the concentrated sodium gluconate solution is obtained, and the concentrated sodium gluconate solution is crystallized and separated to obtain a sodium gluconate product.
Further optimizing the technical scheme, the total amount of the sodium gluconate products obtained in the steps S5 and S6 is 40kg, which exceeds 34 wt% of the sodium gluconate in the initial sodium gluconate mother liquor.
(III) advantageous effects
Compared with the prior art, the invention provides a method for separating and extracting sodium gluconate mother liquor, which has the following beneficial effects:
according to the method for separating and extracting the sodium gluconate mother liquor, the sodium gluconate mother liquor is extracted and separated by using the electrodialysis method, electricity is used as power, no exogenous chemical medicine is added, and the sodium gluconate in the sodium gluconate mother liquor is recovered.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The sodium gluconate mother liquor is produced after separating sodium gluconate prepared by a conventional method, and the method for preparing the sodium gluconate is the prior art and comprises the following steps:
the method comprises the steps of taking corn starch as a raw material, adding a certain amount of nutrient substances after liquefaction and saccharification, sterilizing, cooling to a proper temperature, entering a fermentation tank, inoculating Aspergillus niger seed liquid with the volume fraction of 10%, keeping the pH value at 5.5-6.0 and the temperature at 37-40 ℃, fermenting for about 28 hours under the conditions of stirring and ventilation, oxidizing glucose into gluconic acid by Aspergillus niger, continuously pumping NaOH to convert the gluconic acid into sodium gluconate through neutralization reaction, finishing fermentation when the residual sugar is reduced to be less than 10g/L, filtering thalli and other impurities of fermentation liquor by a plate-and-frame filter press, adjusting the pH of filtrate, heating, performing plate-and-frame primary filtration and secondary filtration, performing four-effect evaporation concentration crystallization, discharging, centrifuging, separating, and drying by a fluidized bed to obtain a finished product of the sodium gluconate.
The sodium gluconate mother liquor generated by the process is detected, and the solid components are shown in table 1:
TABLE 1
Composition (I) Sodium gluconate Disaccharides Three-five sugar above
Content (wt.) 30％-40％ 4％-12％ 1％-3％
1) Enzyme catalysis: detecting 100Kg of sodium gluconate mother liquor, wherein the content of sodium gluconate in the mother liquor is 34 wt%, the content of disaccharide is 6 wt%, and the content of other polysaccharides is 3 wt%, adding pullulanase 20U/g into the mother liquor, carrying out closed anaerobic reaction at 55-65 ℃ for 2h, cooling to 30 ℃, adding aspergillus niger, introducing sterile air, reacting for 6h, adding NaOH to adjust the pH value to 7-8, and obtaining a reaction solution I;
2) and (3) separating polysaccharide: ba (OH) is added to the reaction solution I20.5Kg, stirring and reacting for 20min to separate out a small amount of unreacted polysaccharide, adding Na2CO30.5Kg, precipitating unreacted barium ions, separating, and removing solid matters; obtaining a reaction solution II;
3) and (3) decoloring: adding 2.0-4.0 wt% of activated carbon when the temperature of the reaction liquid II is 60 ℃, keeping the temperature for 30 minutes when the temperature is increased to 65 ℃, and then starting to filter to obtain a reaction liquid III;
4) and (3) crystallization: concentrating the reaction liquid III at 60-80 ℃ until the glucose content is 60-80%, standing, cooling, crystallizing and separating to obtain a sodium gluconate product and a secondary recovered mother liquid;
5) electrodialysis: separating the separated secondary recovered mother liquor from sodium gluconate in the sodium-extracted mother liquor by using a homogeneous membrane electrodialysis method to obtain a sodium gluconate concentrated solution, wherein the conditions of the homogeneous membrane electrodialysis method are as follows: the size of a diaphragm of the electrodialyzer is 10cm multiplied by 20cm, the electrode solution (2mol/L sodium sulfate), the initial concentrated solution (pure water) is 0.5L, the flow feeding is adjusted to be 20L/h, the flow velocity of the electrode solution is 10L/h, the voltage is 14V, the concentrated sodium gluconate solution is obtained, and the concentrated sodium gluconate solution is crystallized and separated to obtain a sodium gluconate product;
the total amount of the sodium gluconate products obtained in the step 4) and the step 5) is 40kg, which exceeds 34 wt% of the sodium gluconate in the initial sodium gluconate mother liquor.
The invention has the beneficial effects that: according to the method for separating and extracting the sodium gluconate mother liquor, the sodium gluconate mother liquor is extracted and separated by using the electrodialysis method, electricity is used as power, no exogenous chemical medicine is added, and the sodium gluconate in the sodium gluconate mother liquor is recovered.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A separation and extraction method of sodium gluconate mother liquor is characterized by comprising the following steps:
s1, preparation of sodium gluconate: taking corn starch as a raw material, adding a certain amount of nutrient substances after liquefaction and saccharification, sterilizing, cooling to a proper temperature, introducing the mixture into a fermentation tank, adding an Aspergillus niger seed solution with a volume fraction of 10%, fermenting for about 28 hours under stirring and ventilation conditions, oxidizing glucose into gluconic acid by Aspergillus niger, continuously pumping NaOH to convert the gluconic acid into sodium gluconate through neutralization reaction, finishing fermentation when residual sugar is reduced to less than 10g/L, filtering out impurities such as thalli from the fermentation liquor through a plate-and-frame filter press, adjusting pH of the filtrate, heating, primarily filtering and secondary filtering through the plate-and-frame filter press, performing four-effect evaporation, concentration and crystallization, discharging, centrifuging, separating, and drying through a fluidized bed to obtain a finished product of the sodium gluconate;
s2, enzyme catalyzed: detecting 100Kg of sodium gluconate mother liquor, wherein the sodium gluconate content is 34 wt%, the disaccharide content is 6 wt% and the other polysaccharide content is 3 wt% in the mother liquor, adding pullulanase 20U/g into the mother liquor, cooling to 30 ℃, adding aspergillus niger, introducing sterile air, reacting for 6 hours, adding NaOH to adjust the pH value to be 7-8, and obtaining reaction liquid I;
s3, polysaccharide separation: ba (OH) is added to the reaction solution I20.5Kg, a small amount of unreacted polysaccharide was precipitated, Na was added2CO30.5Kg, precipitation of unreacted barium ionSeparating and removing solid matters; obtaining a reaction solution II;
s4, decoloring: adding 2.0-4.0 wt% of activated carbon when the temperature of the reaction liquid II is 60 ℃, keeping the temperature for 30 minutes when the temperature is increased to 65 ℃, and then starting to filter to obtain a reaction liquid III;
s5, crystallization: concentrating the reaction liquid III at 60-80 ℃ until the glucose content is 60-80%, standing, cooling, crystallizing and separating to obtain a sodium gluconate product and a secondary recovered mother liquid;
s6, electrodialysis: and separating the separated secondary recovered mother liquor by using a homogeneous membrane electrodialysis method to extract sodium gluconate from the sodium gluconate mother liquor to obtain a sodium gluconate concentrated solution.
2. The method for separating and extracting sodium gluconate mother liquor as claimed in claim 1, wherein in step S1, aspergillus niger seed liquor with a volume fraction of 10% is inoculated, at which the PH is maintained at 5.5-6.0 and the temperature is maintained at 37-40 ℃.
3. The method for separating and extracting sodium gluconate mother liquor according to claim 1, wherein the sodium gluconate mother liquor is detected in step S2, wherein the content of sodium gluconate is 30% -40%, the content of disaccharide is 4% -12%, and the content of tri-pentasaccharide or higher is 1% -3%.
4. The method for separating and extracting sodium gluconate mother liquor as claimed in claim 1, wherein pullulanase 20U/g is added into the mother liquor in step S2, and the mother liquor undergoes a closed anaerobic reaction at 55-65 ℃ for 2 hours.
5. The method for separating and extracting sodium gluconate mother liquor as claimed in claim 1, wherein in step S3, Ba (OH) is added into the reaction solution I20.5Kg, stirred and reacted for 20 min.
6. The method for separating and extracting sodium gluconate mother liquor as claimed in claim 1, wherein the conditions of the homogeneous membrane electrodialysis in the step S6 are as follows: the size of a diaphragm of the electrodialyzer is 10cm multiplied by 20cm, the electrode liquid (2mol/L sodium sulfate), the initial concentrated solution (pure water) is 0.5L, the flow feeding is adjusted to be 20L/h, the flow velocity of the electrode liquid is 10L/h, the voltage is 14V, the concentrated sodium gluconate solution is obtained, and the concentrated sodium gluconate solution is crystallized and separated to obtain a sodium gluconate product.
7. The method as claimed in claim 1, wherein the total amount of the sodium gluconate products obtained in steps S5 and S6 is 40kg, which exceeds 34 wt% of the sodium gluconate in the initial sodium gluconate mother liquor.
CN201910784079.4A 2019-08-23 2019-08-23 Separation and extraction method of sodium gluconate mother liquor Withdrawn CN111099988A (en)

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