CN105001078A - Clean production method for extracting citric acid from citric acid fermented clear liquid - Google Patents
Clean production method for extracting citric acid from citric acid fermented clear liquid Download PDFInfo
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- CN105001078A CN105001078A CN201510416497.XA CN201510416497A CN105001078A CN 105001078 A CN105001078 A CN 105001078A CN 201510416497 A CN201510416497 A CN 201510416497A CN 105001078 A CN105001078 A CN 105001078A
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- citric acid
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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
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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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- 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
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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
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
Abstract
The invention is suitable for the technical field of organic acid production and provides a clean production method for extracting citric acid from a citric acid fermented clear liquid. The method comprises the following steps: (1) carrying out concentration at a reduced pressure and crystallization on the citric acid fermented clear liquid at a predetermined temperature and pressure and separating the citric acid fermented clear liquid to obtain a solid phase and a liquid phase; (2) dissolving the solid phase obtained in the step (1) at the predetermined temperature and carrying out subsequent refining and purification treatment to obtain a critic acid finished product; and (3) carrying out a common calcium salt extraction or chromatographic purification method on the liquid phase obtained in the step (1) and then carrying out subsequent purification treatment to prepare the citric acid finished product. According to citric acid prepared from the citric acid fermented clear liquid by virtue of the method provided by the invention, the yield is greatly improved, the energy consumption is lowered, the consumption of auxiliary materials is reduced, the output of wastes such as calcium sulfate, carbon dioxide and the like are reduced, and the total output is greatly improved.
Description
Technical field
The present invention relates to fermentative Production organic acid technical field, particularly relate to a kind of clean preparation method extracting citric acid from citric acid fermentation aqueous solution.
Background technology
Citric acid is a kind of important organic acid, is widely used in food, beverage, daily use chemicals and medicine and other fields.China is the big producing country of citric acid, and extracting method main at present has calcium salt method, chromatography, membrane separation process, extraction process.Due to the production of chromatography, membrane separation process and utility appliance cost higher, and the residual solvent in extraction process not easily removes the quality affecting citric acid product, and these production methods do not have large-scale application and universal.The main production method of current citric acid is calcium salt method, and the supplementary product onsumptions such as calcium salt method is produced citric acid and had that yield is low, calcium carbonate and sulfuric acid are large, calcium sulfate, carbonic acid gas the like waste produce the problems such as difficult removal.Therefore, study that a kind of yield is high, energy consumption is low, pollute less, process for cleanly preparing that cost is low is one of problem of urgently studying of current citric acid industry.
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 clean preparation method extracting citric acid from citric acid fermentation aqueous solution, first by citric acid fermentation aqueous solution through condensing crystal process, most of citric acid is collected, the liquid phase of remainder is again through calcium salt method or chromatography purity operation, obtained citric acid, the present invention makes that the yield of citric acid significantly improves, energy consumption reduces, supplementary product onsumption is low, and decrease calcium sulfate, carbonic acid gas the like waste generation, aggregated capacity increases substantially.
To achieve these goals, the invention provides a kind of clean preparation method extracting citric acid from citric acid fermentation aqueous solution, it comprises the following steps: citric acid fermentation aqueous solution is carried out concentrating under reduced pressure, crystallization treatment by (1) at predetermined temperature and pressure, is separated and obtains solid phase and liquid phase; (2) solid phase obtained obtained in step (1) is dissolved at a predetermined temperature, carry out follow-up refining purification processes, obtain citric acid finished product; (3) liquid phase obtained in step (1) is extracted or chromatography purity method by common calcium salt, then through subsequent purification process, obtained citric acid finished product.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, also comprise before described step (1): citric acid fermentation aqueous solution is carried out Plate Filtration process.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (1), the described method being separated employing is separated with whizzer, and the centrifugal rotating speed of described whizzer is 500r/min ~ 800r/min, and the time is 5min ~ 15min.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (1), the centrifugal rotating speed of described feed liquid is 600r/min, and the time is 10min.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (1), the preset temperature of described citric acid fermentation aqueous solution concentrating under reduced pressure is 60 DEG C ~ 80 DEG C, and pressure is-0.08MPa ~-0.05MPa.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (1), the preset temperature of described citric acid fermentation aqueous solution concentrating under reduced pressure is 70 DEG C, and pressure is-0.065MPa.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (1), the citric acid fermentation aqueous solution crystallizing cycle after concentrating under reduced pressure is 10h ~ 12h.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (1), the citric acid fermentation aqueous solution crystallizing cycle after concentrating under reduced pressure is 11h.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (2), the preset temperature of described solid-solution is between 40 DEG C ~ 50 DEG C.
According to the clean preparation method extracting citric acid from citric acid fermentation aqueous solution of the present invention, in described step (2), the preset temperature of described solid-solution is 45 DEG C.
The invention provides a kind of clean preparation method extracting citric acid from citric acid fermentation aqueous solution, it comprises the following steps: citric acid fermentation aqueous solution is carried out concentrating under reduced pressure, crystallization treatment by (1) at predetermined temperature and pressure, is separated and obtains solid phase and liquid phase; (2) solid phase obtained obtained in step (1) is dissolved at a predetermined temperature, carry out follow-up refining purification processes, obtain citric acid finished product; (3) liquid phase obtained in step (1) is extracted or chromatography purity method by common calcium salt, then through subsequent purification process, obtained citric acid finished product.First most of citric acid is collected, the liquid phase of remainder is again through calcium salt method or chromatography purity operation, obtained citric acid, the present invention makes that the yield of citric acid significantly improves, energy consumption reduces, supplementary product onsumption is low, and decrease calcium sulfate, carbonic acid gas the like waste generation, aggregated capacity increases substantially.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the embodiment of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, 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
See the flow chart of steps of Fig. 1, this example is for illustration of a kind of clean preparation method extracting citric acid from citric acid fermentation aqueous solution provided by the invention, it comprises the following steps: citric acid fermentation aqueous solution is carried out concentrating under reduced pressure, crystallization treatment by (1) at predetermined temperature and pressure, is separated and obtains solid phase and liquid phase; (2) solid phase obtained obtained in step (1) is dissolved at a predetermined temperature, carry out follow-up refining purification processes, obtain citric acid finished product; (3) liquid phase obtained in step (1) is extracted or chromatography purity method by common calcium salt, then through subsequent purification process, obtained citric acid finished product.
Further, also comprise before step (1): citric acid fermentation aqueous solution is carried out Plate Filtration process.
Further, in step (1), the described method being separated employing is separated with whizzer, and the centrifugal rotating speed of described whizzer is 500r/min ~ 800r/min, and the time is 5min ~ 15min.
Further, in step (1), the preset temperature of described citric acid fermentation aqueous solution concentrating under reduced pressure is 60 DEG C ~ 80 DEG C, and pressure is-0.08MPa ~-0.05MPa.
Further, in step (1), the citric acid fermentation aqueous solution crystallizing cycle after concentrating under reduced pressure is 10h ~ 12h.
Further, in step (2), the preset temperature of described solid-solution is between 40 DEG C ~ 50 DEG C.
Specifically comprise the steps:
1, by acidity be 18% citric acid fermentation broth 180kg, be heated to 55 DEG C, carry out Plate Filtration, obtain citric acid fermentation aqueous solution.
2, fermentation clear liquid through filter laggard enter concentrating pan, controlling concentrating pan temperature is 60 DEG C, and pressure is-0.08MPa, acidity is brought up to 80% by 18%, obtains 0.224m
3concentrated solution.
3, be added in crystallizer by citric acid concentrated solution, carry out crystallization treatment, whole crystallizing cycle is 10 hours.
4, crystallization feed liquid is carried out centrifugal washing process, centrifugal rotational speed is 500r/min, centrifugation time 5 minutes, washing time 30 seconds, and the solid phase obtaining weight in wet base after centrifugal is 199kg and 0.51m
3liquid phase.
5, the warm water of solid phase with 40 DEG C is dissolved, lysate obtains citric acid product 165.4kg through refining steps such as ion-exchange, concentrated, centrifugal, oven dry.
6, the liquid phase in step 4 is passed through calcium salt method or chromatography purity technique, then obtain citric acid 10.1kg through refining step.
7, the citric acid product obtained by step 5 and step 6 amounts to 175.5kg, and product yield is 97.5%.
Wherein, the yield formula in the present invention is:
Yield=(the citric acid quality that citric acid quality+liquid phase that solid phase obtains obtains)/citric acid fermentation broth total mass.
Embodiment 2
Specifically comprise the steps:
1, by acidity be 18% citric acid fermentation broth 180kg, be heated to 55 DEG C, carry out Plate Filtration, obtain citric acid fermentation aqueous solution.
2, fermentation clear liquid through filter laggard enter concentrating pan, concentrating pan temperature is 80 DEG C, and acidity is brought up to 80% by 18%, obtained 0.235m by pressure-0.05MPa
3concentrated solution.
3, be added in crystallizer by citric acid concentrated solution, carry out crystallization treatment, whole crystallizing cycle is 12 hours.
4, crystallization feed liquid is carried out centrifugal washing process, centrifugal rotational speed is 800r/min, centrifugation time 15 minutes, washing time 50 seconds, and the solid phase obtaining weight in wet base after centrifugal is 202kg and 0.50m
3liquid phase.
5, the warm water of solid phase with 50 DEG C is dissolved, lysate obtains citric acid product 164.2kg through refining steps such as ion-exchange, concentrated, centrifugal, oven dry.
6, the liquid phase in step 4 is passed through calcium salt method or chromatography purity technique, then obtain citric acid 10.9kg through refining step.
7, the citric acid product obtained by step 5 and step 6 amounts to 175.1kg, and product yield is 97.3%.
Embodiment 3
Specifically comprise the steps:
1, by acidity be 18% citric acid fermentation broth 180kg, be heated to 55 DEG C, carry out Plate Filtration, obtain citric acid fermentation aqueous solution.
2, fermentation clear liquid through filter laggard enter concentrating pan, concentrating pan temperature is 70 DEG C, and acidity is brought up to 80% by 18%, obtained 0.225m by pressure-0.065MPa
3concentrated solution.
3, be added in crystallizer by citric acid concentrated solution, carry out crystallization treatment, whole crystallizing cycle is 11 hours.
4, crystallization feed liquid is carried out centrifugal washing process, centrifugal rotational speed is 600r/min, centrifugation time 10 minutes, washing time 35 seconds, and the solid phase obtaining weight in wet base after centrifugal is 202kg and 0.52m
3liquid phase.
5, the warm water of solid phase with 45 DEG C is dissolved, lysate obtains citric acid product 165.5kg through refining steps such as ion-exchange, concentrated, centrifugal, oven dry.
6, the liquid phase in step 4 is passed through calcium salt method or chromatography purity technique, then obtain citric acid 10.2kg through refining step.
7, the citric acid product obtained by step 5 and step 6 amounts to 175.7kg, and product yield is 97.6%.
Embodiment 4
Specifically comprise the steps:
1, by acidity be 18% citric acid fermentation broth 180kg, be heated to 55 DEG C, carry out Plate Filtration, obtain citric acid fermentation aqueous solution.
2, fermentation clear liquid through filter laggard enter concentrating pan, concentrating pan temperature is 66 DEG C, and acidity is brought up to 80% by 18%, obtained 0.227m by pressure-0.07MPa
3concentrated solution.
3, be added in crystallizer by citric acid concentrated solution, carry out crystallization treatment, whole crystallizing cycle is 11 hours.
4, crystallization feed liquid is carried out centrifugal washing process, centrifugal rotational speed is 650r/min, centrifugation time 12 minutes, washing time 44 seconds, and the solid phase obtaining weight in wet base after centrifugal is 203kg and 0.54m
3liquid phase.
5, the warm water of solid phase with 47 DEG C is dissolved, lysate obtains citric acid product 163.3kg through refining steps such as ion-exchange, concentrated, centrifugal, oven dry.
6, the liquid phase in step 4 is passed through calcium salt method or chromatography purity technique, then obtain citric acid 10.2kg through refining step.
7, the citric acid product obtained by step 5 and step 6 amounts to 173.5kg, and product yield is 96.4%.
Embodiment 5
Specifically comprise the steps:
1, by acidity be 18% citric acid fermentation broth 180kg, be heated to 55 DEG C, carry out Plate Filtration, obtain citric acid fermentation aqueous solution.
2, fermentation clear liquid through filter laggard enter concentrating pan, concentrating pan temperature is 71 DEG C, and acidity is brought up to 80% by 18%, obtained 0.230m by pressure-0.07MPa
3concentrated solution.
3, be added in crystallizer by citric acid concentrated solution, carry out crystallization treatment, whole crystallizing cycle is 10 hours.
4, crystallization feed liquid is carried out centrifugal washing process, centrifugal rotational speed is 560r/min, centrifugation time 14 minutes, washing time 37 seconds, and the solid phase obtaining weight in wet base after centrifugal is 201kg and 0.54m
3liquid phase.
5, the warm water of solid phase with 48 DEG C is dissolved, lysate obtains citric acid product 165.0kg through refining steps such as ion-exchange, concentrated, centrifugal, oven dry.
6, the liquid phase in step 4 is passed through calcium salt method or chromatography purity technique, then obtain citric acid 10.1kg through refining step.
7, the citric acid product obtained by step 5 and step 6 amounts to 175.1kg, and product yield is 97.3%.
Embodiment 6
Specifically comprise the steps:
1, by acidity be 18% citric acid fermentation broth 180kg, be heated to 55 DEG C, carry out Plate Filtration, obtain citric acid fermentation aqueous solution.
2, fermentation clear liquid through filter laggard enter concentrating pan, concentrating pan temperature is 75 DEG C, and acidity is brought up to 80% by 18%, obtained 0.234m by pressure-0.053MPa
3concentrated solution.
3, be added in crystallizer by citric acid concentrated solution, carry out crystallization treatment, whole crystallizing cycle is 10 hours.
4, crystallization feed liquid is carried out centrifugal washing process, centrifugal rotational speed is 610r/min, centrifugation time 9 minutes, washing time 37 seconds, and the solid phase obtaining weight in wet base after centrifugal is 201kg and 0.53m
3liquid phase.
5, the warm water of solid phase with 43 DEG C is dissolved, lysate obtains citric acid product 165.2kg through refining steps such as ion-exchange, concentrated, centrifugal, oven dry.
6, the liquid phase in step 4 is passed through calcium salt method or chromatography purity technique, then obtain citric acid 10.4kg through refining step.
7, the citric acid product obtained by step 5 and step 6 amounts to 175.6kg, and product yield is 97.6%.
As can be seen from embodiment 1 ~ embodiment 6, the yield of embodiment 3 is the highest, namely select the effect under this condition best: thickening temperature is 70 DEG C, pressure is-0.07MPa, crystallization time is 11h, centrifugal rotational speed is 600r/min, centrifugation time is 10min, washing time is 35 seconds, and solid-solution temperature is 45 DEG C.
In sum, the invention provides a kind of clean preparation method extracting citric acid from citric acid fermentation aqueous solution, it comprises the following steps: citric acid fermentation aqueous solution is carried out concentrating under reduced pressure, crystallization treatment by (1) at predetermined temperature and pressure, is separated and obtains solid phase and liquid phase; (2) solid phase obtained obtained in step (1) is dissolved at a predetermined temperature, carry out follow-up refining purification processes, obtain citric acid finished product; (3) liquid phase obtained in step (1) is extracted or chromatography purity method by common calcium salt, then through subsequent purification process, obtained citric acid finished product.Present method produces the method for citric acid, and its advantage is:
1, yield is high: first through condensing crystal process, is collected by most of citric acid, and remaining liquid phase is again by calcium salt method or chromatography purity operation, and refining step obtains citric acid.
2, energy consumption reduces: citric acid fermentation aqueous solution extracts most of citric acid by direct condensing crystal, replaces all utilizing calcium salt method or chromatography purity method, and energy consumption significantly reduces.
3, supplementary product onsumption is low: after condensing crystal process, major part citric acid is collected, and residue needs the citric acid amount extracted through calcium salt method or chromatography purity method to reduce, and the calcium carbonate consumption therefore needed reduces, the sulfuric acid amount used also reduces, and reduces the consumption of auxiliary material.
4, calcium sulfate, carbonic acid gas the like waste generation are few: production process major part no longer needs calcium salt extraction process, the also corresponding minimizing of the calcium sulfate therefore produced, carbonic acid gas the like waste.
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 (10)
1. from citric acid fermentation aqueous solution, extract a clean preparation method for citric acid, it is characterized in that, it comprises the following steps:
(1) citric acid fermentation aqueous solution is carried out concentrating under reduced pressure, crystallization treatment at predetermined temperature and pressure, be separated and obtain solid phase and liquid phase;
(2) solid phase obtained obtained in step (1) is dissolved at a predetermined temperature, carry out follow-up refining purification processes, obtain citric acid finished product;
(3) liquid phase obtained in step (1) is extracted or chromatography purity method by common calcium salt, then through subsequent purification process, obtained citric acid finished product.
2. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 1, is characterized in that, also comprises before described step (1):
Citric acid fermentation aqueous solution is carried out Plate Filtration process.
3. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 1, it is characterized in that, in described step (1), the described method being separated employing is separated with whizzer, the centrifugal rotating speed of described whizzer is 500r/min ~ 800r/min, and the time is 5min ~ 15min.
4. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 3, is characterized in that, in described step (1), the centrifugal rotating speed of described feed liquid is 600r/min, and the time is 10min.
5. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 1, it is characterized in that, in described step (1), the preset temperature of described citric acid fermentation aqueous solution concentrating under reduced pressure is 60 DEG C ~ 80 DEG C, and pressure is-0.08MPa ~-0.05MPa.
6. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 5, is characterized in that, in described step (1), the preset temperature of described citric acid fermentation aqueous solution concentrating under reduced pressure is 70 DEG C, and pressure is-0.065MPa.
7. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 1, is characterized in that, in described step (1), the citric acid fermentation aqueous solution crystallizing cycle after concentrating under reduced pressure is 10h ~ 12h.
8. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 7, is characterized in that, in described step (1), the citric acid fermentation aqueous solution crystallizing cycle after concentrating under reduced pressure is 11h.
9. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 1, is characterized in that, in described step (2), the preset temperature of described solid-solution is between 40 DEG C ~ 50 DEG C.
10. the clean preparation method extracting citric acid from citric acid fermentation aqueous solution according to claim 9, is characterized in that, in described step (2), the preset temperature of described solid-solution is 45 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256506A (en) * | 2019-07-19 | 2019-09-20 | 山东润德生物科技有限公司 | A method of preparing aminoglucose hydrochloride |
| CN114307389A (en) * | 2021-12-16 | 2022-04-12 | 潍坊英轩实业有限公司 | Filtering method for improving citric acid extraction yield and feed liquid quality |
-
2015
- 2015-07-15 CN CN201510416497.XA patent/CN105001078A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110256506A (en) * | 2019-07-19 | 2019-09-20 | 山东润德生物科技有限公司 | A method of preparing aminoglucose hydrochloride |
| CN114307389A (en) * | 2021-12-16 | 2022-04-12 | 潍坊英轩实业有限公司 | Filtering method for improving citric acid extraction yield and feed liquid quality |
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