WO1997015545A1 - Method of citric acid purification and concentration - Google Patents
Method of citric acid purification and concentration Download PDFInfo
- Publication number
- WO1997015545A1 WO1997015545A1 PCT/SK1996/000015 SK9600015W WO9715545A1 WO 1997015545 A1 WO1997015545 A1 WO 1997015545A1 SK 9600015 W SK9600015 W SK 9600015W WO 9715545 A1 WO9715545 A1 WO 9715545A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- stage
- weight parts
- permeate
- citnc
- acid
- Prior art date
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 27
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000746 purification Methods 0.000 title claims description 5
- 239000012466 permeate Substances 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims abstract description 13
- 239000012141 concentrate Substances 0.000 claims abstract description 10
- 238000001728 nano-filtration Methods 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 22
- 235000000346 sugar Nutrition 0.000 claims description 15
- 150000008163 sugars Chemical class 0.000 claims description 15
- 238000000855 fermentation Methods 0.000 abstract description 7
- 230000004151 fermentation Effects 0.000 abstract description 7
- 150000007524 organic acids Chemical class 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 235000005985 organic acids Nutrition 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 5
- 108090000623 proteins and genes Proteins 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 241000738583 Senna artemisioides Species 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000011026 diafiltration Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
Definitions
- the invention relates to a method for cit ⁇ c acid purification and concentration of cit ⁇ c- hquors from citric acid fermentation
- cit ⁇ c-hquor is used for solution obtained after fermentation at citnc acid production
- citnc- quors contam except for 10 to 20 % w/w of water and organic acids also proteins in amount of 0 1 to 1 % w/w and reducing sugars in amount of 0 5 to 5 % w/w from which the compounds are formed at mcreased temperature e g 60° C in evaporator, assigned as readily carbonisable substances
- the presence of these substances in product serves as an indicator of citnc acid punty
- Permeate from the second stage is divided to three technological flows according to residual content of citnc acid Technological flow with content of 0 01 to 1 % w/w of citnc acid may be used as a source of water for fermentation Technological flow with content of 1 to 10 % w/w of citnc acid may be used for washing out the citnc acid residue from concentrate at pre-treatment/diafiltration/, while the permeate from diafiitration enters again nanofiltration Technological flow with content of 10 to 20 % w/w is returned for nanofiltration
- Concentration and pu ⁇ fication of citnc acid from citnc-hquors obtained after citnc acid fermentation by nanofiltration through polymenc membranes may be performed regarding to different permeability and selectivity towards the compounds in citnc-hquors Exactly expressed, the pu ⁇ fication effect is provided by higher selectivity of membranes towards citric acid as to reducing sugars In this way both separation effect and concentration effect are secured
- the claims for energy consumption are twenty time lower regarding to different energy consumption at water separation by classical method - evaporator
- the method according to the invention represents an economic solution of the part of technology for citnc acid production, considered for an important product assigned especially for food and pharmaceutical industry
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
Citric-liquors representing a solution of citric acid after fermentation undergo two stage nanofiltration on polymeric membranes. In the first stage, nanofiltration is performed on polymeric membranes with the nominal molecular weight cut-off 10,000 to 20,000 daltons and in the second stage on polymeric membranes with nominal molecular weight cut-off 200 to 400 daltons. The resulting concentrate from the second stage undergoes appropriate crystallisation and permeate is recycled into particular stages of technological process.
Description
METHOD OF CITRIC ACID PURIFICATION AND CONCENTRATION.
Technical Field
The invention relates to a method for citπc acid purification and concentration of citπc- hquors from citric acid fermentation
Background Art
Separation of citric acid from citπc-hquors after fermentation with classical process of isolation is made by the known separation methods as mechanical separation, 1 e filtration, centrifugation, etc Consequently, vaπous chemical methods of purification are used 1 e precipitation, breakdown and concentration of punfied solution in evaporators
The term citπc-hquor is used for solution obtained after fermentation at citnc acid production These citnc- quors contam except for 10 to 20 % w/w of water and organic acids also proteins in amount of 0 1 to 1 % w/w and reducing sugars in amount of 0 5 to 5 % w/w from which the compounds are formed at mcreased temperature e g 60° C in evaporator, assigned as readily carbonisable substances The presence of these substances in product serves as an indicator of citnc acid punty
Disclosure of Invention
It was observed that the higher punty of citnc acid may be reached by punficauon, using concentration of citnc-hquors as given in the mvention The principle of this process lies in two stage nanofiltration of citnc-hquors on polymenc membranes In the first stage, nanofiltration on polymenc membranes is performed with nominal molecular weight cut-off 10,000 to 20,000 daltons and in the second stage on polymenc membranes with nommal molecular weight cut-off 200 to 400 daltons Permeate from the first stage enters directly to the second stage and the concentrate from the second stage undergoes crystallisation Permeate from the second stage, accordmg to residual content of reducmg sugars, recycles into particular stages ofthe technological process
Concentrate from the second stage may be directly used as a final product if concentration of citric acid reaches 50 % w/w / liquid citnc acid/ or it is further treated by the obvious method for citric acid crystallisation
Permeate from the second stage is divided to three technological flows according to residual content of citnc acid Technological flow with content of 0 01 to 1 % w/w of citnc acid may be used as a source of water for fermentation Technological flow with content of 1 to 10 % w/w of citnc acid may be used for washing out the citnc acid residue from concentrate at pre-treatment/diafiltration/, while the permeate from diafiitration enters again nanofiltration Technological flow with content of 10 to 20 % w/w is returned for nanofiltration
Concentrate from the first stage representing the waste product undergoes appropπate diafiitration and is discharged
Concentration and puπfication of citnc acid from citnc-hquors obtained after citnc acid fermentation by nanofiltration through polymenc membranes may be performed regarding to different permeability and selectivity towards the compounds in citnc-hquors Exactly expressed, the puπfication effect is provided by higher selectivity of membranes towards citric acid as to reducing sugars In this way both separation effect and concentration effect are secured
At method in accordance with the mvention, higher punty and higher concentration are reached before entrance to evaporator, as a result of separation of certain part of water Separated permeates with lower content of citnc acid may be further utilised in framework of technological process
At nanofiltration performed by method in accordance with the invention, the claims for energy consumption are twenty time lower regarding to different energy consumption at water separation by classical method - evaporator
The following example of performance illustrates but does not limit citnc acid puπfication and concentration accordmg to the invention
Best Mode for Carrying Out the Invention
Example 1
5,000 weight parts of citnc-hquors contammg 5 weight parts of proteins, 750 weight parts of citπc acid and 25 weight parts of reducmg sugars are divided in the first stage at temperature 25°C and pressure 0 5 MPa on membrane with nominal molecular weight cut¬ off 10,000 to 20,000 daltons at formation of
- 4,500 weight pans of permeate consisting of 675 weight parts of citnc acid and 22 5 weight parts of reducing sugars
- 500 weight parts of concentrate containing 5 weight parts of proteins, 75 weight parts of organic acids and 2 5 weight parts of reducmg sugars
4,500 weight parts of permeate from the first stage are divided in the second stage at temperature 25°C and pressure 4 0 MPa on membrane with nominal molecular weight cut¬ off 200 to 400 daltons as follows
- 2,000 weight parts of permeate compnsing of 56 2 weight parts of citnc acid and 4 9 weight parts of reducing sugars / it is used at preparation of fermentation broth in further batch/
- 1 ,000 weight parts of permeate containing of 46 0 weight parts of citnc acid and 3 4 weight parts of reducing sugars / it is used for diafiitration/
- 800 weight parts of permeate compnsing of 64 0 weight parts of citπc acid and 4 0 weight parts of reducmg sugars / it is used further as an mput to the second stage/
- 700 weight parts of concentrate containing 508 8 weight parts of citnc acid and 10 2 weight parts of reducing sugars / it is used for preparation of crystalline citπc acid or as a final product/
500 weight parts of concentrate contammg 5 weight parts of proteins, 75 weight parts of organic acids and 2 5 weight parts of reducing sugars are diafiltered two times with the second part of permeate from the second stage, while three technological flows are aπsing
- 500 weight parts of concentrate from diafiitration contammg 5 weight parts of proteins, 36 weight parts of organic acids and 1 9 weight parts of reducmg sugars / it may be used
for isolation of biologically valuable substances or liquidated in waste water treatment station/
- 500 weight parts of permeate from the first stage of diafiitration contammg 49 weight parts of organic acid and 2 1 weight parts of reducing sugars / it is used in further cycle as an input to the second stage/
- 500 weight parts of permeate from the second stage of diafiitration contammg 36 weight parts of organic acids and 1 9 weight parts of reducing sugars / it is used in further cycle of nanofiltration/
Industrial Applicability
The method according to the invention represents an economic solution of the part of technology for citnc acid production, considered for an important product assigned especially for food and pharmaceutical industry
Claims
THE CLAIMS
The method of citric acid purification and concentration of citric-liquors characterised in that , citπc-liquors undergo two stage nanofiltration on polymeric membranes, while the first stage is performed on polymeric membranes with nominal molecular weight cut-ofF 10,000 to 20,000 daltons and the second stage on polymeric membranes with nominal molecular weight cut-off 200 to 400 daltons, when the permeate from the first stage enters directly the second stage and the resulting concentrate from the second stage undergoes appropπate crystallisation, wherain the permeate from the second stage, regarding to residual content of citnc acid and reducing sugars recycles into particular stages of the technological process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AU73573/96A AU7357396A (en) | 1995-10-27 | 1996-10-25 | Method of citric acid purification and concentration |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SK1348-95A SK279219B6 (en) | 1995-10-27 | 1995-10-27 | Method of concentrate purification of citric acid from fermentative solution |
| SKPV1348-95 | 1995-10-27 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1997015545A1 true WO1997015545A1 (en) | 1997-05-01 |
Family
ID=20434466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/SK1996/000015 WO1997015545A1 (en) | 1995-10-27 | 1996-10-25 | Method of citric acid purification and concentration |
Country Status (4)
| Country | Link |
|---|---|
| AU (1) | AU7357396A (en) |
| CZ (1) | CZ111698A3 (en) |
| SK (1) | SK279219B6 (en) |
| WO (1) | WO1997015545A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152912A (en) * | 2015-07-15 | 2015-12-16 | 潍坊英轩实业有限公司 | Citric acid fermentation solution pretreatment method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1494414A (en) * | 1974-10-25 | 1977-12-07 | Benckiser Gmbh Joh A | Process for separating citrate or citric acid in aqueous solutions |
| EP0151470A2 (en) * | 1984-02-03 | 1985-08-14 | Jungbunzlauer Ladenburg GmbH | Process for the isolation of citric acid |
| EP0479084A2 (en) * | 1990-10-05 | 1992-04-08 | HAARMANN & REIMER CORP. | Method for the production of granular citric acid and salts thereof |
| US5492625A (en) * | 1994-04-07 | 1996-02-20 | Glitsch, Inc. | Method of recovering carboxylic acids from dilute solutions |
| WO1996008459A1 (en) * | 1994-09-12 | 1996-03-21 | Aeci Limited | Process for recovering citric acid |
-
1995
- 1995-10-27 SK SK1348-95A patent/SK279219B6/en unknown
-
1996
- 1996-10-25 AU AU73573/96A patent/AU7357396A/en not_active Abandoned
- 1996-10-25 CZ CZ981116A patent/CZ111698A3/en unknown
- 1996-10-25 WO PCT/SK1996/000015 patent/WO1997015545A1/en not_active Application Discontinuation
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1494414A (en) * | 1974-10-25 | 1977-12-07 | Benckiser Gmbh Joh A | Process for separating citrate or citric acid in aqueous solutions |
| EP0151470A2 (en) * | 1984-02-03 | 1985-08-14 | Jungbunzlauer Ladenburg GmbH | Process for the isolation of citric acid |
| EP0479084A2 (en) * | 1990-10-05 | 1992-04-08 | HAARMANN & REIMER CORP. | Method for the production of granular citric acid and salts thereof |
| US5492625A (en) * | 1994-04-07 | 1996-02-20 | Glitsch, Inc. | Method of recovering carboxylic acids from dilute solutions |
| WO1996008459A1 (en) * | 1994-09-12 | 1996-03-21 | Aeci Limited | Process for recovering citric acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152912A (en) * | 2015-07-15 | 2015-12-16 | 潍坊英轩实业有限公司 | Citric acid fermentation solution pretreatment method |
Also Published As
| Publication number | Publication date |
|---|---|
| CZ111698A3 (en) | 1998-07-15 |
| SK279219B6 (en) | 1998-08-05 |
| AU7357396A (en) | 1997-05-15 |
| SK134895A3 (en) | 1997-06-04 |
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