CN101698640A - Method for extracting citric acid - Google Patents
Method for extracting citric acid Download PDFInfo
- Publication number
- CN101698640A CN101698640A CN200910148286A CN200910148286A CN101698640A CN 101698640 A CN101698640 A CN 101698640A CN 200910148286 A CN200910148286 A CN 200910148286A CN 200910148286 A CN200910148286 A CN 200910148286A CN 101698640 A CN101698640 A CN 101698640A
- Authority
- CN
- China
- Prior art keywords
- reaction
- citric acid
- neutralization
- reaction tank
- solution
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for extracting citric acid, which comprises the following steps: adopting citric acid sterile clear solution and calcium carbonate and/or calcium hydroxide, simultaneously continuously adding into a multi-stage reaction tank, carrying out neutralization reaction, obtaining calcium citrate, continuously feeding and continuously discharging after the full neutralization reaction; and then carrying out acid hydrolysis for obtaining acid hydrolysis solution of the citric acid, wherein the neutralization reaction is carried out continuously as follows: simultaneously continuously adding the citric acid sterile clear solution and the calcium carbonate and/or the calcium hydroxide into the first-stage reaction tank for carrying out the neutralization reaction, starting to enter into the second-stage reaction tank when reaction solution in the reaction tank achieves the limited liquid level, continuing the neutralization reaction of the reaction solution in the second-stage reaction tank, starting to enter into the third-stage reaction tank when the reaction solution in the reaction tank achieves the limited liquid level, simultaneously continuously adding the calcium carbonate and/or the calcium hydroxide into the third-stage reaction tank till the full neutralization of the citric acid sterile clear solution, and starting to discharge continuously when the reaction solution in the third-stage reaction tank achieves the limited liquid level.
Description
Technical field
The present invention relates to the food chemical field, especially adopt continuous neutralisation citric acid in the fermented liquid to be carried out the extracting method of a kind of citric acid of extraction separation.
Background technology
Citric acid is a kind of organic acid that is widely used in industries such as beverage, food and medicine, and China is citric acid production big country, have 20 surplus family factory, output is above 500,000 tons.At present, the extracting method of domestic citric acid is mainly calcium salt method.
The shortcoming of tradition calcium salt method technology is:
One, citric acid per ton consumes about 0.9 ton of sulfuric acid and 0.9 ton of lime carbonate, supplementary product onsumption height;
Two, citrate of lime throw out specific surface area is big, and particle is inhomogeneous, and absorption impurity is many, must adopt go up row's wash water technology, causes leaching requirement big, and hot water consumption is many, in and yield is the highest can only reach 94%, yield is low;
Three, batch technology, level of automation is low, unstable product quality, double team has lime carbonate in the citrate of lime, has increased sulfuric acid, lime carbonate consumption;
Four, occupation area of equipment is big, facility investment is big, and utilization ratio is low;
Five, intermittently in and labor capacity big, poor working environment.
Summary of the invention
The extracting method that the purpose of this invention is to provide a kind of citric acid has not only solved the problems referred to above, and has improved yield, has saved auxiliary material, improved level of automation.
The objective of the invention is to be achieved through the following technical solutions:
A kind of extracting method of citric acid, adopt citric acid sterilization clear liquid and lime carbonate and/or calcium hydroxide to add continuously simultaneously in the reaction of high order jar, the pH value of solution value is carried out neutralization reaction at 3-6 in the control retort, obtain citrate of lime, continue reinforced and lasting discharging after complete neutralization reaction; After acidolysis, obtain citric acid acidolysis liquid then.
Described neutralization reaction is what carry out continuously: in citric acid sterilization clear liquid and lime carbonate and/or the continuous simultaneously adding first class reaction pot of calcium hydroxide, carry out neutralization reaction and keep that pH value is stabilized in the setting range in the retort, the flow of control citric acid sterilization clear liquid and lime carbonate and/or calcium hydroxide is in set(ting)value, reaction solution in the retort arrives the qualification liquid level and the reaction times begins to enter the second order reaction jar above after the limiting time, reaction solution continues neutralization reaction in the second order reaction jar, the flow of material is in set(ting)value in the control second order reaction jar, reaction solution in the retort arrives the qualification liquid level and the reaction times begins to enter the third order reaction jar above after the limiting time, successive adds lime carbonate and/or calcium hydroxide in the third order reaction jar simultaneously, pH value is stable in the maintenance third order reaction jar, neutralize fully up to citric acid sterilization clear liquid, reaction solution arrival qualification liquid level in the third order reaction jar and reaction times are above beginning to continue discharging after the limiting time.
Described first class reaction pot continue to add citric acid sterilization clear liquid and lime carbonate and/or calcium hydroxide, in all retort the reaction time of neutralizer in setting range, reach limit liquid level after, the third order reaction jar begins lasting discharging.
The feed liquid temperature of reaction is the 75-85 degree in described all retort, keeps suitable stirring velocity in the neutralization reaction process.
Described employing reaction of high order jar repeats neutralization reaction, makes citric acid composition in the citric acid sterilization clear liquid generation citrate of lime that neutralizes gradually, up to neutralization fully; Along with the carrying out of neutralization reaction, the pH value raises gradually in the next stage retort.
The beneficial effect of the extracting method of citric acid of the present invention is: the level of automation height, and adopt the continuous feeding and discharging mode to carry out neutralization reaction, with respect to being easy to carry out automatization control with technology in the traditional batch, improve working conditions, reduce labour intensity.
The citrate of lime steady quality: adopt continuous discharge method can make neutralization pot pH value stabilization in the scope of control, can avoid because of in terminal point pH de-stabilising effect citrate of lime quality.
The lime carbonate double team is few, and sulfuric acid consumption is low: in adopting continuously and technology, lime carbonate and citric acid remove thalline secondary fermentation liquid sufficient reacting, and the double team amount is low, can effectively reduce sulfuric acid consumption.
Energy consumption is low: the citrate of lime uniform particles of producing, and be easy to particle and separate with impurity, can reduce the consumption of hot water during washing, and then reduce steam consumption.
Facility investment is low: adopt continuous feeding and discharging, and the equipment continuous operation, the usage ratio of equipment height under the identical condition of production capacity, can reduce facility investment and maintenance cost.
Embodiment
The extracting method of the described citric acid of the embodiment of the invention,
Embodiment 1 is:
1, simultaneously continuously add in first class reaction pot with lime carbonate 158KG citric acid sterilization clear liquid (containing citric acid 200KG), carry out neutralization reaction, control pH value is 3.0～3.8, temperature of reaction is at 70～80 degree, after the feed liquid residence time reaches 30-40 minute and arrive to limit liquid level in the retort, start the dnockout pump, reaction solution is squeezed into (first class reaction pot continuous charging this moment) in the second order reaction jar; Temperature is controlled at 70～80 degree in the second order reaction jar, open and stir, after control reaction time 10 minutes and arrival limit liquid level, start the dnockout pump, reaction solution is squeezed in the third order reaction jar (this moment first class reaction pot continuous charging and continue to enter the second order reaction jar, second order reaction jar internal reaction liquid continues to enter the third order reaction jar); Temperature is controlled at 70～80 degree in the third order reaction jar, in the third order reaction jar, add lime carbonate 5.5KG, the pH value is 4.8～5.2 in the control retort, after control reaction time 20-30 minute and retort liquid level reach set(ting)value, starts the continuous discharging of dnockout pump (citrate of lime).
2, the reaction solution that obtains of separating step 1, and adopt 1500 liters of hot wash solid phases, obtain purified citrate of lime and in and 3000 liters of waste water, the citrate of lime after the washing enters hydrolysis procedure, the easy charcoal multiple of acid hydrolysis solution is 2.2, in and waste water contain citric acid
%.
Compare the data synopsis with batch technology:
| Continuously and technology | Intermittently and technology (on average) | |
| Lime carbonate consumes (ton/ton citric acid) | ??0.82 | ??0.9 |
| Wash hot water amount's (ton/ton citric acid) of citrate of lime | ??7.5 | ??13 |
| In and wastewater volume (m 3/ ton citric acid) | ??15 | ??20.5 |
| In and waste water in residual citric acid (%) | ??0.12 | ??0.11 |
| Continuously and technology | Intermittently and technology (on average) | |
| The easy charcoal multiple of acid hydrolysis solution | ??2.2 | ??2.8 |
| The neutralization reaction time (h) | ??1 | ??1.5 |
Table is compared with traditional batch technology with technology in continuously as can be seen thus: 1. 0.08 ton of/ton citric acid of lime carbonate consumption reduction.2. the hot water amount who washes citrate of lime reduces by 5.5 tons of/ton citric acids.3. the citric acid yield can improve 2.3%.4. the acid hydrolysis solution quality increases.5. because the neutralization reaction time shortens, the neutralized system production capacity is improved.
Embodiment 2 is:
1. simultaneously continuously add in first class reaction pot with lime carbonate 100KG citric acid sterilization clear liquid (containing citric acid 200KG), carry out neutralization reaction, control pH value is 3.0～3.8, temperature of reaction is at 70～80 degree, the feed liquid residence time reaches 30-40 minute and after the retort liquid level reaches set(ting)value in the retort, start the dnockout pump, reaction solution is squeezed into (first class reaction pot continuous charging this moment) in the second order reaction jar; Temperature is controlled at 70～80 degree in the second order reaction jar, open and stir, after control reaction time 10 minutes and retort liquid level reach set(ting)value, start the dnockout pump, reaction solution is squeezed in the third order reaction jar (this moment, first class reaction pot continuous charging and continue to enter the second order reaction jar continued to enter the third order reaction jar in the second order reaction reaction flow container); Temperature is controlled at 70～80 degree in the third order reaction jar, in the third order reaction jar, add lime carbonate 10KG, the pH value is 4.8～5.2 in the control retort, after control reaction time 20-30 minute and retort liquid level reach set(ting)value, starts the continuous discharging of dnockout pump (citrate of lime).
2, the reaction solution that obtains of separating step 1, and adopt 1500 liters of hot wash solid phases, obtain purified citrate of lime and in and 3000 liters of waste water, the citrate of lime after the washing enters hydrolysis procedure, the easy charcoal multiple of acid hydrolysis solution is 2.0, in and waste water contain citric acid 0.09%.
Testing data is as follows:
| Continuously and technology | Intermittently and technology (on average) | |
| Calcium hydroxide consumes (ton/ton citric acid) | ??0.55 | ??0.60 |
| Wash hot water amount's (ton/ton citric acid) of citrate of lime | ??7.0 | ??12.5 |
| In and wastewater volume (m 3/ ton citric acid) | ??14.5 | ??20.0 |
| In and waste water in residual citric acid (%) | ??0.09 | ??0.10 |
| The easy charcoal multiple of acid hydrolysis solution | ??2.0 | ??2.7 |
| The neutralization reaction time (h) | ??1 | ??1.5 |
Table is compared with traditional batch technology with technology in continuously as can be seen thus: 1. 0.05 ton of/ton citric acid of calcium hydroxide consumption reduction.2. the hot water amount who washes citrate of lime reduces by 5.5 tons of/ton citric acids.3. the citric acid yield can improve 3.5%.4. the acid hydrolysis solution quality increases.5. because the neutralization reaction time shortens, the neutralized system production capacity is improved.
Above-described embodiment, the present invention embodiment a kind of more preferably just, the common variation that those skilled in the art carries out in the technical solution of the present invention scope and replacing all should be included in protection scope of the present invention.
Claims (3)
1. the extracting method of a citric acid, it is characterized in that: adopt citric acid sterilization clear liquid and lime carbonate and/or calcium hydroxide to add in the reaction of high order jar continuously simultaneously, carry out neutralization reaction, obtain citrate of lime, continue reinforced and lasting discharging after complete neutralization reaction; After acidolysis, obtain citric acid acidolysis liquid then.
2. the extracting method of citric acid according to claim 1, it is characterized in that: described neutralization reaction is what carry out continuously: described primary reaction jar continues to add citric acid sterilization clear liquid and lime carbonate and/or calcium hydroxide, control the liquid level and the reaction time of neutralizer in all retort, control that feed temperature is the 75-85 degree in all retort, keep suitable stirring velocity in the neutralization reaction process, the final stage retort continues discharging.
3. the extracting method of citric acid according to claim 1 and 2 is characterized in that: the reaction end pH value is stable in every order reaction jar, and along with the carrying out of neutralization reaction, the pH value of neutralizer can raise to some extent in every next stage retort.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910148286A CN101698640A (en) | 2009-06-22 | 2009-06-22 | Method for extracting citric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910148286A CN101698640A (en) | 2009-06-22 | 2009-06-22 | Method for extracting citric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101698640A true CN101698640A (en) | 2010-04-28 |
Family
ID=42147103
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910148286A Pending CN101698640A (en) | 2009-06-22 | 2009-06-22 | Method for extracting citric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101698640A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351687A (en) * | 2011-08-04 | 2012-02-15 | 中粮生物化学（安徽）股份有限公司 | Preparation method of calcium carbonate slurry and preparation method of citric acid |
| CN102863327A (en) * | 2012-09-21 | 2013-01-09 | 中粮生物化学（安徽）股份有限公司 | Production device and production method of calcium citrate |
| CN103961688A (en) * | 2014-04-30 | 2014-08-06 | 湖北神地农业科贸有限公司 | Eggshell source compound calcium citrate chewable tablet and preparation method thereof |
| CN105495069A (en) * | 2014-10-29 | 2016-04-20 | 张湉 | Preparation method of citric acid |
-
2009
- 2009-06-22 CN CN200910148286A patent/CN101698640A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351687A (en) * | 2011-08-04 | 2012-02-15 | 中粮生物化学（安徽）股份有限公司 | Preparation method of calcium carbonate slurry and preparation method of citric acid |
| CN102351687B (en) * | 2011-08-04 | 2013-10-30 | 中粮生物化学（安徽）股份有限公司 | Preparation method of calcium carbonate slurry and preparation method of citric acid |
| CN102863327A (en) * | 2012-09-21 | 2013-01-09 | 中粮生物化学（安徽）股份有限公司 | Production device and production method of calcium citrate |
| CN102863327B (en) * | 2012-09-21 | 2015-01-07 | 中粮生物化学（安徽）股份有限公司 | Production device and production method of calcium citrate |
| CN103961688A (en) * | 2014-04-30 | 2014-08-06 | 湖北神地农业科贸有限公司 | Eggshell source compound calcium citrate chewable tablet and preparation method thereof |
| CN103961688B (en) * | 2014-04-30 | 2016-05-25 | 湖北神地农业科贸有限公司 | A kind of eggshell source compound lemon acid Biocal and preparation method thereof |
| CN105495069A (en) * | 2014-10-29 | 2016-04-20 | 张湉 | Preparation method of citric acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101117315B (en) | Production method of citric acid | |
| CN102921711B (en) | Organic solid waste regeneration resource treatment method and apparatus system thereof | |
| CN101778944A (en) | Method for the conversion of biomass from renewable raw materials in anaerobic fermenters | |
| US20120135491A1 (en) | Method for producing biogas or sewage gas | |
| CN101585044A (en) | Food waste acidifying hydrolysis treatment method | |
| CN103627621A (en) | Solid-state vertical fertilization, self-circulation cooling and distillation integrated device and method | |
| CN101993900B (en) | Pretreatment process of citric acid raw material | |
| CN102703515A (en) | Method for producing biogas through anaerobic digestion of fruit and vegetable waste | |
| CN101698640A (en) | Method for extracting citric acid | |
| CN108569812B (en) | Treatment system and treatment method for wastewater containing low-concentration sulfuric acid | |
| CN106348562A (en) | Method for treating active sludge generated by sewage treatment and extracting protein | |
| CN102826691B (en) | Electrode foil formation section phosphoric acid waste liquor treatment technique | |
| CN1611464A (en) | Organic fertilizer using distillers' grains as raw material and its production process | |
| EP3630705B1 (en) | A method for conversion of poultry manure | |
| CN101643411A (en) | Neutralization method of citric acid | |
| CN112044919B (en) | Environment-friendly comprehensive utilization process for livestock and poultry manure without biogas slurry and biogas residues | |
| CN102268062A (en) | Process for clean production of saponin by utilizing turmeric | |
| CN104529115A (en) | Technology for producing marsh gas and recycling phosphorus in anaerobic fermentation mode through chicken manure | |
| CN101434436A (en) | Processing method for wastewater from cassava starch production | |
| CN104876817A (en) | Method for extracting succinic acid by employing succinic acid fermentation liquor | |
| CN210559929U (en) | Thermal hydrolysis recycling system for anaerobic digestion biogas slurry of livestock and poultry feces | |
| CN109022502B (en) | Method for producing citric acid by recycling anaerobic digestion solution | |
| CN107245035B (en) | Clean production device for low-carbon acid high-boiling-point alcohol ester and use process | |
| CN113846128A (en) | Process flow for preparing biodiesel by liquid enzyme method | |
| CN103483233B (en) | Method for recycling wastewater produced during methionine production process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100428 |