CN1144794A - Method for extracting citric acid - Google Patents
Method for extracting citric acid Download PDFInfo
- Publication number
- CN1144794A CN1144794A CN 94110642 CN94110642A CN1144794A CN 1144794 A CN1144794 A CN 1144794A CN 94110642 CN94110642 CN 94110642 CN 94110642 A CN94110642 A CN 94110642A CN 1144794 A CN1144794 A CN 1144794A
- Authority
- CN
- China
- Prior art keywords
- citric acid
- inorganic salt
- hour
- extraction methods
- decolouring
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 title claims abstract description 151
- 238000000034 method Methods 0.000 title abstract description 14
- 238000000855 fermentation Methods 0.000 claims abstract description 11
- 230000004151 fermentation Effects 0.000 claims abstract description 11
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 10
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 238000000605 extraction Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 5
- 159000000007 calcium salts Chemical class 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005342 ion exchange Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 235000015165 citric acid Nutrition 0.000 description 37
- 235000010633 broth Nutrition 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to a method for extracting citric acid, and is characterized by that under the action of tributyl phosphate and inorganic salt the filtered fermentation liquor can be used for separating citric acid from the fermentation liquor, then the citric acid can be made into the invented product through the processes of water-washing, decolouring, concentration, crystallization and drying, so that it can overcome the defects of poor operation safety, environmental pollution and short equipment life, etc. which are resulted from using chemical raw materials of acid, alkali and salt, etc. by calcium salt ion-exchange method, and can reduce production cost, save raw material, save energy source, raise yield of citric acid by above 10%, and its economic benefit and social benefit are obvious.
Description
The present invention relates to a kind of use extraction process and extract methods of citric acid.
Citric acid as a kind of application of foodstuff additive more and more widely is subject to people's attention day by day.At present, the production technique of citric acid extensively adopts calcium salt from the friendship method, by microorganism to after the starch material fermentation, use lime carbonate to carry out neutralization reaction, citric acid and lime carbonate generate citrate of lime and separate out, after the filtration, carry out acidolysis with sulfuric acid, make citric acid dissociate out, by ion exchange column citric acid is purified out again, form through concentrated, crystallization, oven dry.Because need sulfuric acid during acidolysis, process resin need be used hydrochloric acid and sodium hydroxide, workman's processing safety is poor, equipment corrosion is serious, and work-ing life is short, serious environment pollution, and in the use lime carbonate and the time can not make whole citric acid generate calcium salt to separate out, whole citrate of lime acidolysis during ion-exchange, also can not there be the part citric acid loss during acidolysis, thereby calcium salt is lower from the method for friendship yield, a large amount of citric acids are lost, waste grain, waste resource.
The purpose of this invention is to provide a kind of use extraction process and extract methods of citric acid,, the citric acid in the fermented liquid all is dissolved in the extraction agent, strip through deionized water and extract citric acid by the effect of extraction agents such as tributyl phosphate and inorganic salt.
The present invention realizes like this, raw material is under action of microorganisms, make citric acid fermentation broth, citric acid fermentation broth after filtration, decolouring, concentrate and make the citric acid concentrated solution, after in the citric acid concentrated solution, adding 6-15 tributyl phosphate doubly, the 10-40% inorganic salt that add the citric acid concentrated solution while stirring, extract 1-1.5 hour after-filtration, adding the 10-35% deionized water that filters liquid measure in filtered liquid strips, stirred after 0.2～1 hour standing demix 1-2 hour, isolate lower floor's aqueous citric acid solution, after the resin column decolouring, concentrate, crystallization, oven dry.
The present invention has advantages such as technology is simple, cost is low, less investment, can reduce production costs significantly, the technological operation high safety, the anacidity alkali pollution, equipment life height, the recovery rate of finished product reaches 85%, improves more than 10% from the friendship method than calcium salt, economical, societal benefits are remarkable, have broad prospect for its application.
Accompanying drawing is a technological process block-diagram of the present invention.
In order to understand better and to implement, by reference to the accompanying drawings, in detail the technology step is described below:
1, raw material makes citric acid fermentation broth after the microorganism fermentation, with lemon Lemon acid zymotic fluid is warming up to 80 ℃, filters after 10-15 minute.
2, filtrate is squeezed into the decolouring tank, the powdery that adds 1-3% in tank is lived The property charcoal, be warming up to 70-80 ℃, stir after 45 minutes and to filter.
3, the citric acid filtered liquid is squeezed into thickener, be evaporated to acid content more than 72%.
4, the citric acid concentrated solution is squeezed in the extractor, add citric acid and concentrate liquid measure 6-15 tributyl phosphate doubly, the inorganic salt that add the 10-40% of citric acid concentrated solution while stirring reach supersaturation, stir 1-2 hour after-filtration of extraction, it can be calcium chloride, sal epsom, sodium sulfate, zinc sulfate etc. that inorganic salt help the collection agent.
5, the citric acid filtered liquid is squeezed in the jar of stripping, behind the 10-35% deionized water of adding citric acid filtrate amount, stirred 0.2-1 hour, standing demix 1-2 hour, isolate lower floor's aqueous citric acid solution.
6, after aqueous citric acid solution decolours by the decolorizing resin post, be evaporated to acid content 72% above citric acid concentrated solution.
7, the citric acid concentrated solution is made finished product through crystallization, oven dry, packing, and technological process finishes.
Embodiment 1: 50 tons of citric acid fermentation broths, 60 tons of tributyl phosphates, sodium sulfate 1500kg, 1.2 hours extraction time, 12 tons of deionized waters, churning time 0.5 hour.
Embodiment 2: 100 tons of citric acid fermentation broths, 110 tons of tributyl phosphates, zinc sulfate 2000kg, 1 hour extraction time, 20 tons of deionized waters, churning time 1 hour.
Embodiment 3: 33 tons of citric acid fermentation broths, 30 tons of tributyl phosphates, sal epsom 700kg, 1.5 hours extraction time, 3.7 tons of deionized waters, churning time 0.5 hour.
Technological process is described in detail as follows by embodiment 3:
Producing one day fermented liquid of 500 tons of Citric Acid Plant per year is 33 tons, fermented liquid is warming up to 80 ℃, leave standstill 10 minutes after-filtration, filtered liquid is squeezed in the bleacher, add 350kg gac powder, under 70 ℃ of temperature, stir decolouring 45 minutes, the use flame filter press filters, and filtrate is squeezed into and is evaporated to citric acid content in the double-effect evaporator is 80% concentrated solution, and concentrated solution is squeezed into extractor, add 30 tons of tributyl phosphates, stir the back adding and help the agent sal epsom 700kg that comes together, stir extraction and filter with flame filter press after 1.5 hours, then filtrate is squeezed in the reextraction jar, add 3.7 tons of deionized waters, stirred 0.5 hour, standing demix 2 hours is isolated lower floor's aqueous citric acid solution, the tributyl phosphate on upper strata is recycled and reused, aqueous citric acid solution is concentrated into acid content 80%, through crystallization by the decolouring of resin decolorization post after the decolouring, oven dry, packing forms.
Claims (5)
1, a kind of by citric acid fermentation broth after filtration, decolouring, concentration extraction methods of citric acid, after it is characterized in that in the citric acid concentrated solution, adding 6-15 tributyl phosphate doubly, add the 10-40% inorganic salt of citric acid concentrated solution while stirring.Extract 1-2 hour after-filtration, filter the back and in filtrate, add the 10-35% deionized water that filters liquid measure, stirred after 0.2～1 hour standing demix 1-2 hour, isolate lower floor's aqueous citric acid solution, decolouring, concentrated, crystallization, oven dry.
2, a kind of extraction methods of citric acid according to claim 1 is characterized in that inorganic salt are calcium chloride.
3, a kind of extraction methods of citric acid according to claim 1 is characterized in that inorganic salt are sal epsom.
4, a kind of extraction methods of citric acid according to claim 1 is characterized in that inorganic salt are sodium sulfate.
5, a kind of extraction methods of citric acid according to claim 1 is characterized in that inorganic salt are zinc sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94110642 CN1144794A (en) | 1994-05-27 | 1994-05-27 | Method for extracting citric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94110642 CN1144794A (en) | 1994-05-27 | 1994-05-27 | Method for extracting citric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1144794A true CN1144794A (en) | 1997-03-12 |
Family
ID=5034589
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94110642 Pending CN1144794A (en) | 1994-05-27 | 1994-05-27 | Method for extracting citric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1144794A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817740A (en) * | 2010-04-22 | 2010-09-01 | 武汉大学 | Emulsion for extracting citric acid from fermentation liquor and using method thereof |
| CN101979368A (en) * | 2010-10-19 | 2011-02-23 | 大连理工大学 | A method for salting out and extracting organic acids in fermentation broth |
| CN114276235A (en) * | 2021-12-21 | 2022-04-05 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting citric acid from fermentation liquor containing citric acid |
-
1994
- 1994-05-27 CN CN 94110642 patent/CN1144794A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817740A (en) * | 2010-04-22 | 2010-09-01 | 武汉大学 | Emulsion for extracting citric acid from fermentation liquor and using method thereof |
| CN101817740B (en) * | 2010-04-22 | 2013-03-06 | 武汉大学 | Emulsion for extracting citric acid from fermentation liquor and using method thereof |
| CN101979368A (en) * | 2010-10-19 | 2011-02-23 | 大连理工大学 | A method for salting out and extracting organic acids in fermentation broth |
| WO2012051774A1 (en) * | 2010-10-19 | 2012-04-26 | 大连理工大学 | Process for salting out and extracting organic acid from fermentation broth |
| CN101979368B (en) * | 2010-10-19 | 2014-11-12 | 大连理工大学 | Method for extracting and salting organic acids out of fermentation liquor |
| CN114276235A (en) * | 2021-12-21 | 2022-04-05 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting citric acid from fermentation liquor containing citric acid |
| CN114276235B (en) * | 2021-12-21 | 2024-05-07 | 安徽丰原发酵技术工程研究有限公司 | Method for extracting citric acid from fermentation broth containing citric acid |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |