CN105152912A - Citric acid fermentation solution pretreatment method - Google Patents
Citric acid fermentation solution pretreatment method Download PDFInfo
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- CN105152912A CN105152912A CN201510415923.8A CN201510415923A CN105152912A CN 105152912 A CN105152912 A CN 105152912A CN 201510415923 A CN201510415923 A CN 201510415923A CN 105152912 A CN105152912 A CN 105152912A
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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
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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- 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
- C12P7/44—Polycarboxylic acids
- C12P7/48—Tricarboxylic acids, e.g. citric acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/91—Bacteria; Microorganisms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2603—Application of an electric field, different from the potential difference across the membrane
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention is suitable for the technical field of organic acid production technologies, and provides a citric acid fermentation solution pretreatment method. The method comprises the following steps: carrying out low temperature heat treatment on a fermented citric acid fermentation solution to make the temperature of the citric acid fermentation reach a predetermined temperature; and allowing the citric acid fermentation solution with the predetermined temperature to go through an electric field cross-flow membrane filter device in order to carry out filtering and sterilizing treatment. The electric field cross-flow membrane filter device is formed by combining high voltage pulse electric field with a ceramic membrane, and the filtering performance, the pollution resistance and the penetration flux of the micro-filter membrane of the ceramic membrane are improved under the reinforcement action of the high voltage pulse unidirectional current electric field. Aspergillus niger cell mycelia, suspending solid impurities and other macromolecular substances are intercepted through treatment, so the final thallus mortality reaches 99.5% or more, the acidity of the purified citric acid fermentation solution is higher than 16%, the turbidity is lower than 8NTU, and the problems of high energy consumption and large energy waste of present citric acid fermentation solution pretreatment technologies are solved.
Description
Technical field
The present invention relates to fermentative Production organic acid processing technology field, particularly relate to a kind of citric acid fermentation broth pretreatment process.
Background technology
Citric acid is a kind of important organic acid, has a very wide range of purposes in industry, grocery trade, cosmetic industry etc.Present stage, China's citric acid production technique was generally that bacterial classification adopts tank fermentation method to produce citric acid and purifies by calcium salt extraction method with aspergillus niger.After having fermented, carry out heat germicidal treatment rapidly, kill aspergillus niger, then Plate Filtration is passed through, remove black-koji mould filament and other solid residues, the clarified broth obtained, for a neutralization reaction, adopts calcium salt method (hydrogen calcium technique) to extract citric acid further.Carry out heat-sterilization process to the fermented liquid after fermentation ends, have several respects reason: after having fermented, citric acid content has reached the highest, kills aspergillus niger rapidly, can prevent aspergillus niger from continuing to utilize citric acid to carry out metabolism; Make aspergillus niger cell rupture, a small amount of citric acid in release cells; By high temperature, the protein denaturation in fermented liquid is solidified, viscosity reduces, and improves Plate Filtration speed; Calcium salt method neutralization reaction also needs higher temperature of reaction, is about 55 DEG C ~ 60 DEG C.The defect of this technological process is that Citric Acid Fermentation temperature is between 35 DEG C ~ 40 DEG C, adopt thermal sterilization process fermented liquid after fermentation ends and adopt calcium salt method to extract citric acid, need first broth temperature to be increased to about 70 DEG C, consume a large amount of heat energy, although can be reclaimed this part heat by heat exchange, but reclaim heat exchange efficiency and can not reach 100%, part energy will inevitably be caused to lose; And Plate Filtration needs the manual operations such as disassembly, cleaning filter cloth, operational efficiency is relatively low.
In summary, obviously there is inconvenience and defect in actual use in prior art, so be necessary to be improved.
Summary of the invention
For above-mentioned defect, the object of the present invention is to provide a kind of citric acid fermentation broth pretreatment process, by process, citric acid fermentation broth is played to the effect of sterilization and filtration, it can retain solid impurity and other macromolecular substance of aspergillus niger cell mycelium and suspension, the citric acid fermentation liquid acidity after purifying can be made higher than 16%, turbidity is lower than 8NTU, final thalline mortality ratio is made to reach more than 99.5% microfiltration of ceramic membrane under the electric field-enhanced effect of high-voltage pulse Unidirectional direct-current electric field, the strainability of film makes moderate progress, antifouling property increases, permeation flux increases greatly simultaneously.
To achieve these goals, the invention provides a kind of citric acid fermentation broth pretreatment process, it comprises the following steps: step a: the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, makes citric acid fermentation broth reach preset temperature.Step b: by the citric acid fermentation broth after low-temperature heat treatment by the process of electric field crossflow membrane filtration device filter sterilization, described electric field crossflow membrane filtration device to be combined with ceramic membrane by pulsed electric field and to form.
According to citric acid fermentation broth pretreatment process of the present invention, in described step a, described low-temperature heat treatment high-performance heat exchanger realizes, and described high-performance heat exchanger is any one in spiral-plate exchanger, heat exchanger with oblate or two phase flow jet-type heat exchanger.
According to citric acid fermentation broth pretreatment process of the present invention, in described step a, described preset temperature is 55 DEG C ~ 65 DEG C.
According to citric acid fermentation broth pretreatment process of the present invention, in described step a, described preset temperature 60 DEG C.
According to citric acid fermentation broth pretreatment process of the present invention, in described step b, described pulsed electric field is Unidirectional direct-current electric field, its strength of electric field is between 80kv/cm ~ 120kv/cm, pulse-repetition is between 90Hz ~ 130Hz, pulse width is between 2 μ s ~ 20 μ s, and the treatment time is between 10s ~ 60s.
According to citric acid fermentation broth pretreatment process of the present invention, described pulsed electric field is Unidirectional direct-current electric field, and its strength of electric field is between 90kv/cm ~ 110kv/cm, and pulse-repetition is 110Hz, pulse width is between 5 μ s ~ 20 μ s, and the treatment time is between 15s ~ 55s.
According to citric acid fermentation broth pretreatment process of the present invention, described pulsed electric field is Unidirectional direct-current electric field, and its strength of electric field is 100kv/cm, and pulse-repetition is 115Hz, and pulse width is 11 μ s, and the treatment time is 40s.
According to citric acid fermentation broth pretreatment process of the present invention, in described step b, described ceramic membrane is microfiltration membrane.
According to citric acid fermentation broth pretreatment process of the present invention, in described step b, described ceramic membrane filter be configured to that plate and frame filters, tubular filter or multi-channel type filter in any one.
The present invention is by this citric acid fermentation broth pretreatment process, and it comprises the following steps: the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, makes citric acid fermentation broth reach preset temperature.To the citric acid fermentation broth of preset temperature be reached by the process of electric field crossflow membrane filtration device filter sterilization again, electric field crossflow membrane filtration device to be combined with ceramic membrane by pulsed electric field and to form, microfiltration of ceramic membrane film is under the electric field-enhanced effect of high-voltage pulse Unidirectional direct-current electric field, the strainability of film makes moderate progress, antifouling property increases, permeation flux increases greatly simultaneously, solid impurity and other macromolecular substance of aspergillus niger cell mycelium and suspension can be retained by process, final thalline mortality ratio is made to reach more than 99.5%, make the citric acid fermentation liquid acidity after purifying higher than 16%, turbidity is lower than 8NTU.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
A kind of citric acid fermentation broth pretreatment process, comprises the following steps:
Step a: the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, makes citric acid fermentation broth reach preset temperature;
Step b: by the citric acid fermentation broth after low-temperature heat treatment by the process of electric field crossflow membrane filtration device filter sterilization, described electric field crossflow membrane filtration device to be combined with ceramic membrane by pulsed electric field and to form.
Particularly, in step a, described low-temperature heat treatment high-performance heat exchanger realizes, and described high-performance heat exchanger is any one in spiral-plate exchanger, heat exchanger with oblate or two phase flow jet-type heat exchanger.
Particularly, in described step a, described preset temperature is 55 DEG C ~ 65 DEG C.
Particularly, in described step b, described pulsed electric field is Unidirectional direct-current electric field, its strength of electric field is between 80kv/cm ~ 120kv/cm, pulse-repetition is between 90Hz ~ 130Hz, and pulse width is between 2 μ s ~ 20 μ s, and the treatment time is between 10s ~ 60s.
Particularly, in described step b, described pulsed electric field is Unidirectional direct-current electric field, and its strength of electric field is between 90kv/cm ~ 110kv/cm, and pulse-repetition is 110Hz, and pulse width is between 5 μ s ~ 20 μ s, and the treatment time is between 15s ~ 55s.
Particularly, in described step b, ceramic membrane is microfiltration membrane, and it is configured to any one in plate and frame filtration, tubular filter or multi-channel type filtration.
Such as, in the present embodiment, select spiral plate type high-performance heat exchanger that the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, citric acid fermentation liquid temp is made to reach 55 DEG C, the strength of electric field of the Unidirectional direct-current electric field pulsed electric field passed through is 80kv/cm, pulse-repetition is 90Hz, and pulse width is 2 μ s, and the treatment time is 10s; Ceramic membrane is microfiltration membrane, and its structure is preferably plate and frame.
Embodiment 2
As different from Example 1, in the present embodiment, select spiral plate type high-performance heat exchanger that the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, make citric acid fermentation liquid temp reach 65 DEG C, the strength of electric field of the Unidirectional direct-current electric field pulsed electric field passed through is 120kv/cm, and pulse-repetition is 130Hz, pulse width is 20 μ s, treatment time is 60s, and ceramic membrane is microfiltration membrane, and its structure is preferably plate and frame.
Embodiment 3
With above embodiment unlike, in the present embodiment, select spiral plate type high-performance heat exchanger that the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, citric acid fermentation liquid temp is made to reach 57 DEG C, the strength of electric field of the Unidirectional direct-current electric field pulsed electric field passed through is 101kv/cm, pulse-repetition is 113Hz, and pulse width is 9 μ s, and the treatment time is 20s; Ceramic membrane is microfiltration membrane, and its structure is preferably plate and frame.
Embodiment 4
With above embodiment unlike, in the present embodiment, select spiral plate type high-performance heat exchanger that the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, citric acid fermentation liquid temp is made to reach 59 DEG C, the strength of electric field of the Unidirectional direct-current electric field pulsed electric field passed through is 96kv/cm, pulse-repetition is 123Hz, and pulse width is 15 μ s, and the treatment time is 33s; Ceramic membrane is microfiltration membrane, and its structure is preferably plate and frame.
Embodiment 5
With above embodiment unlike, in the present embodiment, select spiral plate type high-performance heat exchanger that the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, citric acid fermentation liquid temp is made to reach 57 DEG C, the strength of electric field of the Unidirectional direct-current electric field pulsed electric field passed through is 101kv/cm, pulse-repetition is 113Hz, and pulse width is 9 μ s, and the treatment time is 20s; Ceramic membrane is microfiltration membrane, and its structure is preferably plate and frame.
Embodiment 6
With above embodiment unlike, in the present embodiment, select spiral plate type high-performance heat exchanger that the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, citric acid fermentation liquid temp is made to reach 60 DEG C, the strength of electric field of the Unidirectional direct-current electric field pulsed electric field passed through is 100kv/cm, pulse-repetition is 120Hz, and pulse width is 11 μ s, and the treatment time is 25s; Ceramic membrane is microfiltration membrane, and its structure is preferably plate and frame.
Contrast experiment
With the citric acid fermentation broth without above-mentioned pretreatment process that same citric acid fermentation technique obtains.
Assay
The citric acid fermentation broth produced embodiment 1 ~ embodiment 6 and contrast experiment carries out microscopy statistics mortality ratio according to " GB478915-2010 national food safety standard food microbiological analysis moulds and yeasts count " to thalline, basis " GB/T9736-2008 chemical reagent acidity and Basicity Determination universal method " detects acidity, carries out Turbidity measurement according to " GB13200-91 water turbidity mensuration ", and check data result is in table 1.
The every check data result contrast of table 1 citric acid fermentation broth
As can be seen from the above table, citric acid fermentation broth pretreatment process of the present invention can make the citric acid fermentation liquid acidity after purifying higher than 16%, turbidity is lower than 8NTU, final thalline mortality ratio reaches more than 99.5%, wherein, the effect of embodiment 6 is better, namely select spiral plate type high-performance heat exchanger that the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment to make to reach 60 DEG C, the strength of electric field of the Unidirectional direct-current electric field pulsed electric field passed through is 100kv/cm, pulse-repetition is 120Hz, pulse width is 11 μ s, treatment time is 25s, ceramic membrane is selected as plate and frame microfiltration membrane is preferred embodiment.
With the fermented liquid after method process provided by the invention, its temperature is between 55 DEG C ~ 60 DEG C, meet a neutralization reaction temperature, without the need to additionally heating again, microfiltration of ceramic membrane is under the electric field-enhanced effect of high-voltage pulse Unidirectional direct-current electric field, the strainability of film makes moderate progress, antifouling property increases, permeation flux increases greatly simultaneously, the effect of microfiltration of ceramic membrane replaces traditional Plate Filtration, solid impurity and other macromolecular substance of aspergillus niger cell mycelium and suspension can be retained, allow citric acid molecule to pass simultaneously, thus make citric acid obtain extraction and cleaning, concrete membrane pore size and film pressure at both sides are depending on processing requirement, make the citric acid feed acidity after purifying higher than 16%, turbidity is lower than 8NTU.
In sum, the present invention is by this citric acid fermentation broth pretreatment process, and it comprises the following steps: the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, makes citric acid fermentation broth reach preset temperature.To the citric acid fermentation broth of preset temperature be reached by the process of electric field crossflow membrane filtration device filter sterilization again, electric field crossflow membrane filtration device to be combined with ceramic membrane by pulsed electric field and to form, microfiltration of ceramic membrane film is under the electric field-enhanced effect of high-voltage pulse Unidirectional direct-current electric field, the strainability of film makes moderate progress, antifouling property increases, permeation flux increases greatly simultaneously, solid impurity and other macromolecular substance of aspergillus niger cell mycelium and suspension can be retained by process, final thalline mortality ratio is made to reach more than 99.5%, make the citric acid fermentation liquid acidity after purifying higher than 16%, turbidity is lower than 8NTU.
Certainly; the present invention also can have other various embodiments; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art are when making various corresponding change and distortion according to the present invention, but these change accordingly and are out of shape the protection domain that all should belong to the claim appended by the present invention.
Claims (9)
1. a citric acid fermentation broth pretreatment process, is characterized in that, comprises the following steps:
Step a: the citric acid fermentation broth after fermentation is carried out low-temperature heat treatment, makes citric acid fermentation broth reach preset temperature;
Step b: by the citric acid fermentation broth after low-temperature heat treatment by the process of electric field crossflow membrane filtration device filter sterilization, described electric field crossflow membrane filtration device to be combined with ceramic membrane by pulsed electric field and to form.
2. citric acid fermentation broth pretreatment process according to claim 1, it is characterized in that, in described step a, described low-temperature heat treatment high-performance heat exchanger realizes, and described high-performance heat exchanger is any one in spiral-plate exchanger, heat exchanger with oblate or two phase flow jet-type heat exchanger.
3. citric acid fermentation broth pretreatment technology according to claim 1, is characterized in that, in described step a, described preset temperature is 55 DEG C ~ 65 DEG C.
4. citric acid fermentation broth pretreatment process according to claim 3, is characterized in that, described preset temperature is 60 DEG C.
5. citric acid fermentation broth pretreatment process according to claim 1, it is characterized in that, in described step b, described pulsed electric field is Unidirectional direct-current electric field, its strength of electric field is between 80kv/cm ~ 120kv/cm, pulse-repetition is between 90Hz ~ 130Hz, and pulse width is between 2 μ s ~ 20 μ s, and the treatment time is between 10s ~ 60s.
6. citric acid fermentation broth pretreatment process according to claim 5, it is characterized in that, described pulsed electric field is Unidirectional direct-current electric field, its strength of electric field is between 90kv/cm ~ 110kv/cm, pulse-repetition is 110Hz, pulse width is between 5 μ s ~ 20 μ s, and the treatment time is between 15s ~ 55s.
7. citric acid fermentation broth pretreatment process according to claim 5, is characterized in that, described pulsed electric field is Unidirectional direct-current electric field, and its strength of electric field is 100kv/cm, and pulse-repetition is 115Hz, and pulse width is 11 μ s, and the treatment time is 40s.
8. citric acid fermentation broth pretreatment process according to claim 1, is characterized in that, in described step b, described ceramic membrane is microfiltration membrane.
9. citric acid fermentation broth pretreatment process according to claim 1, is characterized in that, in described step b, described ceramic membrane filter be configured to that plate and frame filters, tubular filter or multi-channel type filter in any one.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365985A (en) * | 2016-08-31 | 2017-02-01 | 江苏国信协联能源有限公司 | Deep filtering method for citric acid fermentation liquid |
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| CN103664579A (en) * | 2013-12-18 | 2014-03-26 | 潍坊英轩实业有限公司 | Purification treatment technology of citric acid crystallization mother liquor and treatment device |
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| WO1997015545A1 (en) * | 1995-10-27 | 1997-05-01 | Likospol S.R.O. | Method of citric acid purification and concentration |
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| CN101781190A (en) * | 2010-03-23 | 2010-07-21 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting refined citric acid from citric acid fermentation liquid |
| CN103664579A (en) * | 2013-12-18 | 2014-03-26 | 潍坊英轩实业有限公司 | Purification treatment technology of citric acid crystallization mother liquor and treatment device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365985A (en) * | 2016-08-31 | 2017-02-01 | 江苏国信协联能源有限公司 | Deep filtering method for citric acid fermentation liquid |
| CN106365985B (en) * | 2016-08-31 | 2019-03-05 | 江苏国信协联能源有限公司 | A kind of depth filtration approaches of citric acid fermentation broth |
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