CN1680256A - Extracting production of refining calcium lactate by supercritical fluid carbon dioxide - Google Patents
Extracting production of refining calcium lactate by supercritical fluid carbon dioxide Download PDFInfo
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- CN1680256A CN1680256A CNA2005100181915A CN200510018191A CN1680256A CN 1680256 A CN1680256 A CN 1680256A CN A2005100181915 A CNA2005100181915 A CN A2005100181915A CN 200510018191 A CN200510018191 A CN 200510018191A CN 1680256 A CN1680256 A CN 1680256A
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- calcium lactate
- carbon dioxide
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
Production of refined calcium lactate by supercritical fluid carbon dioxide extraction is carried out by ionic exchanging for fermenting lactic acid, removing inorganic salt, obtaining calcium lactate, laying lamellar or granular calcium lactate on filtering layer of extracting pot at pressure 25-30MPa and 40-45deg.C, inducing supercritical fluid carbon dioxide into extracting pot at high pressure, extracting organics impurity of calcium lactate, continuous releasing organics impurity of calcium lactate into fluid carbon dioxide, fluid carbon dioxide induced into extracting pot flowing from bottom of extracting pot, entering into de-pressuring separating pot, reducing pressure, releasing dissolved organics impurity, collecting by de-pressuring separating pot, reducing pressure of fluid carbon dioxide to 4-5Mpa, pressurizing carbon dioxide, delivering into extracting pot, circulating using, recovering carbon dioxide in extracting pot after 90mins, and obtaining refined calcium lactate. It achieves reasonable process and low cost.
Description
Technical field
The present invention relates to a kind of production process of chemical product, particularly extracting production of refining calcium lactate by supercritical fluid carbon dioxide.This production technique, utilize lactic acid-fermenting after inorganic salt are removed in ion-exchange, to go out calcium lactate as raw material production after, utilize supercritical fluid carbon dioxide to extract wherein organic impurities again, it is a kind of process for refining of obtain lactic acid calcium.Be applicable to food grade calcium lactate or the refining processing of calcium lactate work in-process (comprising L-calcium lactate or DL-calcium lactate), make it to reach the British Pharmacopoeia standard.
Background technology
Calcium lactate is comparatively broad range of food additive and a calcium-nutrition intensifying agent of a kind of purposes, and its chemical molecular formula is Ca (CH
3CHOHCOO)
25H
2O is white crystalline or graininess powder, littlely deposits weathering.Dissolving, easily molten in boiling water in water, the aqueous solution are neutral, are dissolved in ethanol hardly.On the market, food grade calcium lactate market price is 7000 yuan/ton at home, and pharmaceutical grade calcium lactate market price is 15000 yuan/ton, advances the product calcium lactate and reaches 22000 yuan/ton.In the international market, because the calcium lactate food grade standard of our China and pharmaceutical grade standard have than big difference with the external corresponding standard of calcium lactate is not approved.Therefore, calcium lactate often is used as the feed grade outlet.According to the knowledge of the applicant, present manufacturer produces highly purified refining calcium lactate and adopts refining heat-resisting level lactic acid (15000 yuan/ton of market prices) and medical calcium carbonate reaction to produce usually, its basic production technology is: 1) will make with extra care heat-resisting level lactic acid and be diluted to 20-30%, under heated condition, add pharmaceutical grade lime carbonate (powdery), add an amount of aqua calcis after reacting completely, the adjusting pH value is 6.5-7.5.2) above-mentioned calcium lactate solution is concentrated into 50-55% after, cooling granulation or film-making become finished product with its hot-air seasoning again.The advantage that this purified reaches the calcium lactate technology of pharmaceutical grade is with short production cycle, and technology is simpler, and shortcoming is because the market price of fine purification of lactic acid is very high, causes the manufacturing cost of this refining calcium lactate also very high.The applicant finds that under study for action the lactic acid that the raw material of refining calcium lactate should adopt fermentation to produce is because its inorganic salt content after ion-exchange meets the pharmaceutical grade requirement.But still contain organic impurities such as reducing sugar, lipid acid, soluble protein in this lactic acid after ion-exchange.Therefore, though the calcium lactate inorganic salt content of producing with this lactic acid and pharmaceutical grade calcium carbonate reaction is qualified, materials such as dried color and the voltaile fatty acid of failing to remove, reducing sugar can cause its local flavor, physical and chemical index defective.Therefore, obtain purified pharmaceutical grade calcium lactate, just must reprocess, remove organic impurities wherein it.Also should make the precision work cost cheap simultaneously.
Summary of the invention
The objective of the invention is,, carry out process modification, propose extracting production of refining calcium lactate by supercritical fluid carbon dioxide at the higher deficiency of existing refining calcium lactate production technique manufacturing cost.By using low cost raw material, adopt rational technical process, remove the organic impurities in the work in-process calcium lactate, obtain purity and meet the calcium lactate that pharmaceutical grade requires, and reduce the production cost of refining calcium lactate.
Technical solution of the present invention is, the employing calcium lactate is a raw material, calcium lactate is to adopt the calcium lactate of producing through the lactic acid-fermenting of ion-exchange and calcium hydroxide reaction, or the calcium lactate made of the lactic acid-fermenting of employing ion-exchange or food grade lactic acid and pharmaceutical grade calcium carbonate reaction; The technical process that calcium lactate is made is: with the positive resin of lactic acid-fermenting process, inorganic salt are removed in negative resin ion-exchange earlier; Lactic acid solution being adjusted concentration is 25-30% again, adds lime carbonate and carry out neutralization reaction under 80-90 ℃ hot state, when reacting near terminal point, adjusts the calcium lactate solution pH value at 6.5-7.5 with aqua calcis; The calcium lactate solution heating that reacts completely is concentrated to 55-60%; after granulation or the film-making; hot-air seasoning is to the calcium lactate of content 98-103%; raw material as refining calcium lactate; it is characterized in that; fluid carbon dioxide under the use supercritical state extracts the organic impurities in the calcium lactate; obtain refining calcium lactate; organic impurities comprises lipid acid; soluble protein; reducing sugar; its basic technology is: with sheet or granular calcium lactate is that solid lactic acid calcium places on the filtering layer of extractor; pressure in the 25-30 MPa; under the 40-45 ℃ of temperature condition; high pressure feeds supercritical state in extractor fluid carbon dioxide extracts the organic impurities that contains in the calcium lactate; organic impurities in the calcium lactate is released in the fluid carbon dioxide constantly; the fluid carbon dioxide that feeds extractor flows out from the extractor bottom; enter the decompression separation jar; by decompression; discharge the dissolved organic impurities; it is collected by the decompression separation jar as resistates; the pressure of fluid carbon dioxide reduces to the 4-5 MPa; the pressurized extractor of sending into again of carbonic acid gas recycles afterwards; after 90 minutes; reclaim the carbonic acid gas in the extractor; take out the calcium lactate after the above-mentioned operation of process is removed organic impurities, this calcium lactate is refining calcium lactate.
It is characterized in that, solid lactic acid calcium is put into extractor, use supercritical fluid carbon dioxide under high pressure conditions to the organic impurities in the calcium lactate---lipid acid, soluble protein, reducing sugar extracts.
It is characterized in that the carbonic acid gas after extraction is used can be forced into supercritical state again after discharging organic impurities under the non-supercritical state and becomes fluid carbon dioxide through being decompressed to, for repeated use.
Its feature in, the organic impurities that the supercritical fluid carbon dioxide that uses of extraction discharges is lipid acid, soluble protein, reducing sugar.
Its feature in, solid lactic acid calcium is placed on the husky core filtering layer of extractor, under air-tight state, high pressure feeds fluid carbon dioxide and soaks into calcium lactate.
Its feature in, the extractor internal pressure that feeds after the fluid carbon dioxide is not less than 25 MPas, temperature is not higher than 45 ℃.
The time that the calcium lactate of its feature in, extractor continued extraction is no less than 90 minutes.
Its feature in, 90 minutes is a production cycle, belongs to batch production.
Its feature in, the fluid carbon dioxide of dissolved organic matter impurity through being decompressed to 5 MPas when following, but discharge recirculation utilization behind the organism.
The invention has the advantages that, adopt the organic impurities that under the supercritical fluid carbon dioxide condition, extracts in the calcium lactate, produce the refining calcium lactate that reaches the pharmaceutical grade standard.Its technology is reasonable, refining low processing cost is used common low price raw material, does not add catalyzer, can obtain highly purified refining calcium lactate (being that purity meets the calcium lactate that pharmaceutical grade requires) by consumption of power and amounts of carbon dioxide (leakage loss), its physical and chemical index reaches the British Pharmacopoeia standard.
Embodiment
Below, describe embodiments of the invention in detail.
The technical scheme that proposes according to the present invention, embodiments of the invention are undertaken by following processing step:
1, learnt from else's experience 550 liters of lactic acid-fermentings (the about 20-30% of content) after the ion-exchange, place 1500 liters enamel reactor, be heated to 85-90 ℃ by chuck, continue to add powdery pharmaceutical grade lime carbonate and react under whipped state, pharmaceutical grade lime carbonate adds speed and does not overflow for good with the carbonic acid gas bubble that produces in the reaction process.
2, in the reaction process, when the PH of calcium lactate solution reaches 5.0-5.5, change and add 2% aqua calcis to the pH value of calcium lactate solution and reach 6.5-7.5.
3, calcium lactate solution is filtered by mineral membrane (0.2 micron), remove unreacted lime carbonate, it is utilized again.
4, calcium lactate solution is placed 1500 liters concentration tank, after heating is concentrated into content 50-55%, directly be spray dried to powder or particulate state calcium lactate.
5, about 200 kilograms powder or the even equal layering of particulate state calcium lactate are tiled on the husky core filtering layer of 1000 liters of extractors.Tiling thickness is not more than 50 millimeters.Airtight extractor.Go into the fluid carbonic acid gas from the fluid inlet high-pressure pump, reach 25 MPas or surpass 25 MPas to the extractor internal pressure, and when making calcium lactate by complete submergence, it is 20 liters/minute that control fluid carbon dioxide pump is gone into speed, open the following tapping valve of extractor, fluid carbon dioxide is imported the decompression separation jar, the velocity of discharge also is 20 liters/minute, by the chuck heating and cooling, temperature is at 40-45 ℃ in the control extractor simultaneously.
6, from beginning discharge opeing timing, after 90 minutes, stop to pump into fluid carbon dioxide.Reclaim carbonic acid gas from the following tapping valve of extractor, when the extractor internal pressure is the 0.02-0.03 MPa, close tapping valve, open exhaust-valve, open extractor, take out the calcium lactate after the above-mentioned operation of process is removed organic impurities, this calcium lactate is refining calcium lactate.
7, in extraction process, the fluid carbon dioxide that imports the decompression separation jar is depressurized to below 5 MPas, discharges the organic impurities of extraction, and by the decompression separation jar it is collected, and carbonic acid gas reuses more than being forced into 25 MPas again afterwards.
Claims (8)
1, the critical fluids carbon dioxide abstraction is produced refining calcium lactate, the employing calcium lactate is a raw material, calcium lactate is to adopt the calcium lactate of producing through the lactic acid-fermenting of ion-exchange and calcium hydroxide reaction, or the calcium lactate made of the lactic acid-fermenting of employing ion-exchange or food grade lactic acid and pharmaceutical grade calcium carbonate reaction; The technical process that calcium lactate is made is: with the positive resin of lactic acid-fermenting process, inorganic salt are removed in negative resin ion-exchange earlier; Lactic acid solution being adjusted concentration is 25-30% again, adds lime carbonate and carry out neutralization reaction under 80-90 ℃ hot state, when reacting near terminal point, adjusts the calcium lactate solution pH value at 6.5-7.5 with aqua calcis; The calcium lactate solution heating that reacts completely is concentrated to 55-60%; after granulation or the film-making; hot-air seasoning is to the calcium lactate of content 98-103%; raw material as refining calcium lactate; it is characterized in that; fluid carbon dioxide under the use supercritical state extracts the organic impurities in the calcium lactate; obtain refining calcium lactate; organic impurities comprises lipid acid; soluble protein; reducing sugar; its basic technology is: with sheet or granular calcium lactate is that solid lactic acid calcium places on the filtering layer of extractor; pressure in the 25-30 MPa; under the 40-45 ℃ of temperature condition; high pressure feeds supercritical state in extractor fluid carbon dioxide extracts the organic impurities that contains in the calcium lactate; organic impurities in the calcium lactate is released in the fluid carbon dioxide constantly; the fluid carbon dioxide that feeds extractor flows out from the extractor bottom; enter the decompression separation jar; by decompression; discharge the dissolved organic impurities; it is collected by the decompression separation jar as resistates; the pressure of fluid carbon dioxide reduces to the 4-5 MPa; the pressurized extractor of sending into again of carbonic acid gas recycles afterwards; after 90 minutes; reclaim the carbonic acid gas in the extractor; take out the calcium lactate after the above-mentioned operation of process is removed organic impurities, this calcium lactate is refining calcium lactate.
2, extracting production of refining calcium lactate by supercritical fluid carbon dioxide according to claim 1, it is characterized in that, carbonic acid gas after extraction is used can be forced into supercritical state again after discharging organic impurities under the non-supercritical state and becomes fluid carbon dioxide through being decompressed to, for repeated use.
3, extracting production of refining calcium lactate by supercritical fluid carbon dioxide according to claim 1, its feature in, the organic impurities that the supercritical fluid carbon dioxide that uses of extraction discharges is lipid acid, soluble protein, reducing sugar.
4, extracting production of refining calcium lactate by supercritical fluid carbon dioxide according to claim 1, its feature in, solid lactic acid calcium is placed on the husky core filtering layer of extractor, under air-tight state, high pressure feeds fluid carbon dioxide and soaks into calcium lactate.
5, extracting production of refining calcium lactate by supercritical fluid carbon dioxide according to claim 1, its feature in, the extractor internal pressure that feeds after the fluid carbon dioxide is not less than 25 MPas, temperature is not higher than 45 ℃.
6, extracting production of refining calcium lactate by supercritical fluid carbon dioxide according to claim 1, the time that the calcium lactate of its feature in, extractor continued extraction is no less than 90 minutes.
7, extracting production of refining calcium lactate by supercritical fluid carbon dioxide according to claim 1, its feature in, 90 minutes is a production cycle, belongs to batch production.
8, extracting production of refining calcium lactate by supercritical fluid carbon dioxide according to claim 1, its feature in, the fluid carbon dioxide of dissolved organic matter impurity through being decompressed to 5 MPas when following, but discharge recirculation utilization behind the organism.
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| CNA2005100181915A CN1680256A (en) | 2005-01-25 | 2005-01-25 | Extracting production of refining calcium lactate by supercritical fluid carbon dioxide |
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| CNA2005100181915A CN1680256A (en) | 2005-01-25 | 2005-01-25 | Extracting production of refining calcium lactate by supercritical fluid carbon dioxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109160877A (en) * | 2018-10-09 | 2019-01-08 | 武汉三江航天固德生物科技有限公司 | The production method of medical calcium lactate |
| CN111604009A (en) * | 2020-05-27 | 2020-09-01 | 苏州大学 | Multifunctional supercritical fluid processor for materials |
-
2005
- 2005-01-25 CN CNA2005100181915A patent/CN1680256A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109160877A (en) * | 2018-10-09 | 2019-01-08 | 武汉三江航天固德生物科技有限公司 | The production method of medical calcium lactate |
| CN111604009A (en) * | 2020-05-27 | 2020-09-01 | 苏州大学 | Multifunctional supercritical fluid processor for materials |
| CN111604009B (en) * | 2020-05-27 | 2022-08-12 | 苏州大学 | Multifunctional supercritical fluid processor for materials |
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