CN104529737A - Method for rectifying vitamin K1 by supercritical carbon dioxide continuous extraction - Google Patents
Method for rectifying vitamin K1 by supercritical carbon dioxide continuous extraction Download PDFInfo
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- CN104529737A CN104529737A CN201410820068.4A CN201410820068A CN104529737A CN 104529737 A CN104529737 A CN 104529737A CN 201410820068 A CN201410820068 A CN 201410820068A CN 104529737 A CN104529737 A CN 104529737A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C46/00—Preparation of quinones
- C07C46/10—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2602/00—Systems containing two condensed rings
- C07C2602/02—Systems containing two condensed rings the rings having only two atoms in common
- C07C2602/04—One of the condensed rings being a six-membered aromatic ring
- C07C2602/10—One of the condensed rings being a six-membered aromatic ring the other ring being six-membered, e.g. tetraline
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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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- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for rectifying vitamin K1 by supercritical carbon dioxide continuous extraction, which comprises the following steps: vitamin K1 enters an extraction column through an extraction column feed port; supercritical carbon dioxide is compressed to 18-30 MPa by a compressor, and anhydrous ethanol is added into an extraction kettle through a gas inlet; after extraction, waste is discharged through an extraction column waste port, and the extraction material enters a supercritical rectification column feed port through a discharge port to enter a supercritical rectifier; the rectified waste liquid is discharged through a rectification column waste port and recycled; the rectification material enters a product collection unit through a discharge port; the pressure of the supercritical carbon dioxide is reduced to 3-6 MPa through a pressure relief valve of the product collection unit; the vitamin K1 is precipitated in an collection kettle and discharged through a product collection port; and the decompressed supercritical carbon dioxide returns to the compressor for cyclic use through a pipeline. The method implements integration and continuity of extraction and rectification, and greatly enhances the production efficiency.
Description
Technical field
The invention belongs to separation field, relate in particular to a kind of method of supercritical continuous carbon dioxide extraction rectifying vitamin K1.
Background technology
Vitamin k 1 (another name: phytonadione; 2-methyl-3-(3,7,11,15-tetramethyl-16-2-thiazolinyl)-1,4-naphthoquinone) belong to vitamin medicaments, be the necessary material of liver composition-factor II, VII, Ⅸ, Ⅹ.Vitamin K 1 injection is 2009 editions National essential drugs list kinds, is mainly used in the treatment of the hemorrhagic diseases that various vitamin K deficiency causes.For synthesizing the required material of thrombogen in liver, blood coagulation disorders can be caused when lacking.When in blood during vitamin K 1 injection prothrombin deficiency, it is slow that the solidifying of blood just there will be, and at this moment, supplements appropriate vitamin K1 and liver can be impelled to synthesize thrombogen, play the effect of hemostasis.Vitamin K1 is as pharmaceutical preparation, be applied to the too low disease of zymoplasm, vitamin K1 deficiency disease, newborn infant's nature control of hemorrhage and obstructive jaundice, leak, chronic diarrhoea etc. clinically caused hemorrhage, the Hypoprothrombinemia that coumarins, sodium salicylate etc. are caused.VITAMIN also has analgesia, alleviates the effect of bronchospasm, has obvious effect to the angina that visceral smooth muscle angina, cholepathia spastica, enterospasm cause.Vitamin K1 can also be used for the additive of multidimensional food and poultry and livestock feed.
Supercritical carbon dioxide extraction (SFE) utilizes the dissolving power of supercutical fluid and the relation of its density, namely utilizes pressure and temperature to carry out the impact of supercutical fluid dissolving power.In the supercritical state, supercutical fluid is contacted with material to be separated, make it selectively the composition of polarity size, boiling point height and molecular size range be extracted successively.
The principle of supercritical carbon dioxide extraction (SFE) sepn process utilizes the dissolving power of supercutical fluid and the relation of its density, namely utilizes pressure and temperature to carry out the impact of supercutical fluid dissolving power.In the supercritical state, supercutical fluid is contacted with material to be separated, make it selectively the composition of polarity size, boiling point height and molecular size range be extracted successively.Certainly, the extract that corresponding each pressure range obtains can not be single, but control condition can obtain the mixing element of optimum proportion, then the method by decompression, intensification makes supercutical fluid become common gases, be extracted material then to separate out completely or substantially, thus reach the object of separating-purifying, so supercritical carbon dioxide extraction process is combined by extraction and fractionation process.
1, supercritical extraction can extract under close to room temperature (35 ~ 40 DEG C) and CO2 gas blanket, effectively prevent oxidation and the loss of heat-sensitive substance.Therefore, in extract, remain the effective constituent of medicinal plant, and the material of high boiling point, low volatility, easily pyrolysis can be extracted under far below its boiling temperature;
2, SFE is used to be the cleanest extracting method, because whole process is without organic solvent, the therefore vehicle substance that absolutely not remains of extract, thus prevent the existence of harmful thing in leaching process and the pollution to environment, ensure that the pure natural property of 100%;
3, extraction and fractionation unites two into one, when the CO2 fluid of saturated solute enters separator, due to the decline of pressure or the change of temperature, CO2 and extract is made to become rapidly two-phase (gas-liquid separation) and separate immediately, the efficiency not only extracted is high but also energy consumption is less, improves production efficiency and also reduces expense cost;
4, CO2 is a kind of inactive gas, chemical reaction does not occur, and belong to non-flammable gases in extraction process, and tasteless, odorless, nontoxic, security is very good;
5, CO2 gas price is cheap, and purity is high, easily produces, and can recirculation use aborning, thus significantly reduces cost;
6, pressure and temperature can become the parameter regulating extraction process, reaches the object of extraction by changing temperature and pressure, and separating substances can come by changing temperature by pressure fixing too; Otherwise temperature fixed, make extract be separated by reducing pressure, therefore technique is simply easily grasped, and the speed of extraction is fast.
Summary of the invention
Technical problem to be solved by this invention overcomes current industrial supercritical carbon dioxide extraction not have serialization to realize the defect of extracting rectifying, provides a kind of method of supercritical continuous carbon dioxide extraction rectifying vitamin K1.It comprises the steps: by concentration be about 70% vitamin K1 enter extraction tower according to the speed of 4-10L/h by extraction tower opening for feed; Supercritical co is pressed onto 18-30MPa by compressor and adds 2-5% (with the weight ratio of vitamin K1 raw material) dehydrated alcohol and add extraction kettle by inlet mouth, carbon dioxide flow is 40-50Kg/h; Extraction tower temperature is set as 30-45 DEG C; After extraction, waste material is discharged by extraction tower waste material mouth, and extraction material enters overcritical rectifying tower opening for feed by discharge port and enters overcritical rectifier unit; The temperature setting of overcritical rectifying tower first warm area, the second warm area, three-temperature-zone, four-temperature region be respectively 35-45 DEG C, 45-55 DEG C, 55-65 DEG C, 65-75 DEG C; Waste liquid after rectifying is discharged by rectifying tower waste material mouth and is recycled; Rectifying material then enters product-collecting unit by discharge port; Supercritical co pressure is reduced to 3-6MPa by the reducing valve of product-collecting unit by rectifying material; Vitamin K1 is separated out in collection still, and is discharged by product-collecting mouth; Post-decompression supercritical co is got back to compressor cycle by pipeline and is used.
Product detects by high performance liquid chromatography.Method And Principle: trial-product and interior mark all make moving phase solution, enters high performance liquid chromatograph and carries out chromatographic separation, with ultraviolet absorption detector, detects the absorption value of vitamin K1 and interior mark dimethyl phthalate, calculate its content in wavelength 254nm place.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Specific embodiment
Embodiment 1:
By concentration be 70.7% vitamin K1 enter extraction tower according to the speed of 4L/h by extraction tower opening for feed; Supercritical co is pressed onto 22MPa by compressor and adds 2% (with the weight ratio of vitamin K1 raw material) dehydrated alcohol and add extraction kettle by inlet mouth, carbon dioxide flow is 40Kg/h; Extraction tower temperature is set as 35 DEG C; After extraction, waste material is discharged by extraction tower waste material mouth, and extraction material enters overcritical rectifying tower opening for feed by discharge port and enters overcritical rectifier unit; The temperature setting of overcritical rectifying tower first warm area, the second warm area, three-temperature-zone, four-temperature region is respectively 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C; Waste liquid after rectifying is discharged by rectifying tower waste material mouth and is recycled; Rectifying material then enters product-collecting unit by discharge port; Supercritical co pressure is reduced to 4MPa by the reducing valve of product-collecting unit by rectifying material; Vitamin K1 is separated out in collection still, and is discharged by product-collecting mouth; Post-decompression supercritical co is got back to compressor cycle by pipeline and is used.The vitamin K1 concentration obtained is 98.4%.
Embodiment 2: by concentration be 70.7% vitamin K1 enter extraction tower according to the speed of 5L/h by extraction tower opening for feed; Supercritical co is pressed onto 22MPa by compressor and adds 4% (with the weight ratio of vitamin K1 raw material) dehydrated alcohol and add extraction kettle by inlet mouth, carbon dioxide flow is 50Kg/h; Extraction tower temperature is set as 40 DEG C; After extraction, waste material is discharged by extraction tower waste material mouth, and extraction material enters overcritical rectifying tower opening for feed by discharge port and enters overcritical rectifier unit; The temperature setting of overcritical rectifying tower first warm area, the second warm area, three-temperature-zone, four-temperature region is respectively 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C; Waste liquid after rectifying is discharged by rectifying tower waste material mouth and is recycled; Rectifying material then enters product-collecting unit by discharge port; Supercritical co pressure is reduced to 4MPa by the reducing valve of product-collecting unit by rectifying material; Vitamin K1 is separated out in collection still, and is discharged by product-collecting mouth; Post-decompression supercritical co is got back to compressor cycle by pipeline and is used.The vitamin K1 concentration obtained is 98.8%.
Claims (1)
1. a method for supercritical continuous carbon dioxide extraction rectifying vitamin K1, it is characterized in that comprising the steps: by concentration be about 70% vitamin K1 enter extraction tower according to the speed of 4-10L/h by extraction tower opening for feed; Supercritical co is pressed onto 18-30MPa by compressor and adds 2-5% (with the weight ratio of vitamin K1 raw material) dehydrated alcohol and add extraction kettle by inlet mouth, carbon dioxide flow is 40-50Kg/h; Extraction tower temperature is set as 30-45 DEG C; After extraction, waste material is discharged by extraction tower waste material mouth, and extraction material enters overcritical rectifying tower opening for feed by discharge port and enters overcritical rectifier unit; The temperature setting of overcritical rectifying tower first warm area, the second warm area, three-temperature-zone, four-temperature region be respectively 35-45 DEG C, 45-55 DEG C, 55-65 DEG C, 65-75 DEG C; Waste liquid after rectifying is discharged by rectifying tower waste material mouth and is recycled; Rectifying material then enters product-collecting unit by discharge port; Supercritical co pressure is reduced to 3-6MPa by the reducing valve of product-collecting unit by rectifying material; Vitamin K1 is separated out in collection still, and is discharged by product-collecting mouth; Post-decompression supercritical co is got back to compressor cycle by pipeline and is used.
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| CN201410820068.4A CN104529737A (en) | 2014-12-25 | 2014-12-25 | Method for rectifying vitamin K1 by supercritical carbon dioxide continuous extraction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104906262A (en) * | 2015-05-13 | 2015-09-16 | 北京化工大学常州先进材料研究院 | Method for rectification of tea polyphenol through supercritical carbon dioxide continuous extraction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4141799A (en) * | 1976-08-21 | 1979-02-27 | Bayer Aktiengesellschaft | Process for the purification of high-melting organic products |
| WO2006118167A1 (en) * | 2005-04-27 | 2006-11-09 | National University Corporation Toyohashi University Of Technology | Quinone profile method and the like utilizing quinone compound extracted using compressed carbon dioxide |
| CN101575279B (en) * | 2009-06-25 | 2012-09-19 | 河北理工大学 | Method for supercritical fluid extraction of juglone in walnut seed green skin waste residue |
-
2014
- 2014-12-25 CN CN201410820068.4A patent/CN104529737A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4141799A (en) * | 1976-08-21 | 1979-02-27 | Bayer Aktiengesellschaft | Process for the purification of high-melting organic products |
| WO2006118167A1 (en) * | 2005-04-27 | 2006-11-09 | National University Corporation Toyohashi University Of Technology | Quinone profile method and the like utilizing quinone compound extracted using compressed carbon dioxide |
| CN101575279B (en) * | 2009-06-25 | 2012-09-19 | 河北理工大学 | Method for supercritical fluid extraction of juglone in walnut seed green skin waste residue |
Non-Patent Citations (3)
| Title |
|---|
| 刘云等: "超临界CO2萃取浓缩天然维生素E的研究", 《化学工程》 * |
| 夏春辉等: "超临界CO2流体萃取新技术在医药中应用", 《医学信息》 * |
| 李雪: "超临界二氧化碳萃取茶多酚和维生素K1的实验研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104906262A (en) * | 2015-05-13 | 2015-09-16 | 北京化工大学常州先进材料研究院 | Method for rectification of tea polyphenol through supercritical carbon dioxide continuous extraction |
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Inventor after: Wu Hao Inventor after: Yu Enping Inventor after: Jin Junsu Inventor before: Wu Hao Inventor before: Yu Enping |
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Free format text: CORRECT: INVENTOR; FROM: WU HAO YU ENPING TO: WU HAO YU ENPING JIN JUNSU |
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Application publication date: 20150422 |