CN105883739A - Preparation method of medicinal potassium dihydrogen phosphate - Google Patents
Preparation method of medicinal potassium dihydrogen phosphate Download PDFInfo
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- CN105883739A CN105883739A CN201610354655.8A CN201610354655A CN105883739A CN 105883739 A CN105883739 A CN 105883739A CN 201610354655 A CN201610354655 A CN 201610354655A CN 105883739 A CN105883739 A CN 105883739A
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- dihydrogen phosphate
- potassium dihydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/305—Preparation from phosphorus-containing compounds by alkaline treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a preparation method of medicinal potassium dihydrogen phosphate. The preparation method comprises the following steps: a, preparing raw materials, namely preparing a phosphoric acid solution and a potassium hydroxide solution; b, carrying out synthesis reaction, namely adding the obtained phosphoric acid solution into a reaction kettle, heating, and slowly dropwise adding the potassium hydroxide solution until reaction is completed; c, decolorizing, filtering and concentrating, namely heating, adding activated carbon, stirring for decolorizing under the condition of thermal insulation, filtering and carrying out reduced pressure condensation in a concentration kettle; d, crystallizing and filtering in a throwing manner, namely transferring the concentrated solution into a crystallizing tank in a clean zone, and carrying out low-temperature crystallization and centrifugal filtration in the throwing manner, thus obtaining crude products, namely a potassium dihydrogen phosphate wet product and filtrate; e, drying the crude products, namely drying the crude product, namely the potassium dihydrogen phosphate wet product, into a vacuum drying oven; f, refining the crude products, namely carrying out refiltration and recrystallization to obtain the refined potassium dihydrogen phosphate wet product; and g, drying and packaging, namely drying and packaging the refined potassium dihydrogen phosphate wet product, discharging, packaging, warehousing and storing. On the whole, the preparation method disclosed by the invention has the advantages that technology is simple, manufacturing cost is low and market demand can be met.
Description
Technical field
The invention belongs to pharmaceutical synthesis field, relate to the synthesis preparation method of a kind of crude drug, the preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate.
Background technology
Potassium dihydrogen phosphate (KH2PO4), colourless tetragonal crystal or white crystalline powder, relative density 2.338, fusing point 252.6 DEG C, soluble in water, when 100 DEG C, dissolubility is 83.5g/100ml water, aqueous solution is acidity, mass percent be the pH value of 1% potassium dihydrogen phosphate be 4.0, insoluble in alcohol, have hygroscopy, when being heated to 400 DEG C, fusing forms transparent liquid, is cured as dense glass shape potassium metaphosphate after cooling.
Potassium dihydrogen phosphate belongs to nutrition medication, supplement as phosphorus, phosphorus participates in the inverse phosphorylation in carbohydrate metabolism in human body, form the phospholipid in film component, it it is one of important component forming intracellular rna, DNA and many coenzyme, phosphorus also participates in the storage conversion of energy, conveying and the regulation of body fluid buffering function, has important effect.
At present, existing preparation technology is the most extensive in China, and production cost is higher, and product purity is it cannot be guaranteed that meet the prescription of medicinal potassium dihydrogen phosphate.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate, overcome deficiency of the prior art, improve the conversion ratio of raw material, the purity improving product makes to meet medicinal demand.
The object of the present invention is achieved like this: the preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate, and described preparation method comprises the following steps: a, configuration raw material: configuration phosphoric acid solution and potassium hydroxide solution；B, synthetic reaction: added by gained phosphoric acid solution in reactor, liter high-temperature, to 40-70 DEG C, is slowly added dropwise pH value in gained potassium hydroxide solution to solution PH reaches 3.5 ~ 4.5 and 20 minutes and no longer changes, and stops dropping and has i.e. reacted；C, decolorization filtering concentrate: be warming up to 80-100 DEG C, add medicinal carbon, insulated and stirred is decoloured 20-30 minute, use compressed air to pressurizeing in reactor and keeping pressure≤0.4MPa, make reactant liquor pass through filter to enter smoothly in concentration kettle, to concentration kettle evacuation pressure≤-0.08MPa in keeping still, concentration kettle heat temperature raising is concentrated until concentrated solution density reaches 1.3 ~ 1.4g/cm3Stop concentrating；Worry is got rid of in d, crystallization: concentrated solution is transferred to clean area crystallizer, crystallizer is carried out slow cooling to-5 ~ 0 DEG C, and keep the temperature crystallize 24 hours of-5 ~ 0 DEG C, be centrifuged getting rid of worry in blowing to centrifuge, use water to carry out drip washing, obtain crude product potassium dihydrogen phosphate wet product and filtrate；E, crude product are dried: crude product potassium dihydrogen phosphate wet product put in the drip pan being covered with medicinal Low Density Polyethylene bag uniformly, drip pan is put in vacuum drying oven, evacuation makes pressure≤-0.08MPa in baking oven, under conditions of carrying out intensification holding temperature 25 ~ 40 DEG C, dry and meet the requirements to product for 12 ~ 15 hours, take out crude product potassium dihydrogen phosphate after being down to room temperature to carry out weighing, packing, enclose material card stand-by；F, crude product refining: in refining kettle, add water and crude product potassium dihydrogen phosphate, stirring and dissolving, heats up and adds medicinal activated carbon decolorizing, carry out filtering, concentrating filtrate by filter, it is transferred to clean area carry out crystallization and crystallize and carry out centrifugal drying worry, obtains fine work potassium dihydrogen phosphate wet product；G, drying and packaging: fine work potassium dihydrogen phosphate wet product is loaded uniformly in the drip pan being covered with medicinal Low Density Polyethylene bag, drip pan is put in vacuum drying oven, make vacuum≤-0.08MPa, carry out vacuum drying drying until dipotassium hydrogen phosphate loss on drying≤0.2% under conditions of temperature 25 ~ 40 DEG C, be cooled to room temperature, carry out discharging, carry out weighing in clean area, subpackage enters in complex pocket, sealing, put into pail pack, warehouse-in deposits wait delivery.
The described titanium rod filter that the filter in step c is 5 μm, the titanium rod accurate filter that filter is 0.22 μm in described f step.
Described water is purified water.
Described washing water temperature is-5 ~ 0 DEG C.
The described complex pocket in step g is polyester-aluminium-polythene drug packaging complex pocket.
The concentration of described phosphoric acid solution is 35-50%.
The concentration of described potassium hydroxide is 15-30%.
The beneficial effect comprise that: raw material phosphoric acid of the present invention is the peroxophosphoric acid of high concentration, it is acidified potassium hydroxide direct preparing phosphoric acid hydrogen dipotassium by peroxophosphoric acid, compared with traditional handicraft, the technical processs such as condensing crystallizing separation are lacked, simplify production process, reduce the production cost of product and the energy consumption of product simultaneously.
Detailed description of the invention
Below to embodiments of the present invention further instruction.
Embodiment:
A kind of preparation method of pharmaceutical grade potassium dihydrogen phosphate, preparation method comprises the following steps:
A, configuration raw material: configure phosphoric acid solution and the potassium hydroxide solution of 20% concentration of 40% concentration；
The phosphoric acid solution of proportioning 40% concentration is to be slowly added in 14.22kg purified water by 12.53kg industrial phosphoric acid, and stir dissolving gained；The potassium hydroxide solution of proportioning 20% concentration is to be added in 26.8kg purified water by 6.7kg industrial hydrogen potassium oxide, and stir dissolving gained.
B, synthetic reaction: added by gained phosphoric acid solution in reactor, liter high-temperature, to about 55 DEG C, is slowly added dropwise pH value in gained potassium hydroxide solution to solution PH reaches 4.0 and 20 minutes and no longer changes, and stops dropping and has i.e. reacted；
C, decolorization filtering concentrate: be warming up to 80 DEG C, add medicinal carbon, insulated and stirred is decoloured 20 minutes, use compressed air to pressurizeing in reactor and keeping pressure≤0.4MPa, by the titanium rod filter of 5 μm, make reactant liquor pass through filter to enter smoothly in concentration kettle, to concentration kettle evacuation pressure≤-0.08MPa in keeping still, concentration kettle heat temperature raising is concentrated until concentrated solution density reaches 1.3g/cm3Stop concentrating；
Worry is got rid of in d, crystallization: concentrated solution is transferred to clean area crystallizer, crystallizer is carried out slow cooling to-5 DEG C, and keep the temperature crystallize 24 hours of-5 DEG C, be centrifuged getting rid of worry in blowing to centrifuge, use purified water to carry out drip washing, obtain crude product potassium dihydrogen phosphate wet product and filtrate；
E, crude product are dried: crude product potassium dihydrogen phosphate wet product put in the drip pan being covered with medicinal Low Density Polyethylene bag uniformly, drip pan is put in vacuum drying oven, evacuation makes pressure≤-0.08MPa in baking oven, under conditions of carrying out intensification holding temperature 40 DEG C, dry and meet the requirements to product for 12 hours, take out crude product potassium dihydrogen phosphate after being down to room temperature to carry out weighing, packing, enclose material card stand-by；
The raw materials used rate of charge of synthetic reaction:
| Name of material | Rank | Rate of charge | Inventory | Purity | Molecular formula | Molecular weight |
| Phosphoric acid | Industry | 1 | 12.53kg | 85.4% | H3PO4 | 98 |
| Potassium hydroxide | Industry | 0.53 | 6.7kg | 90.7% | KOH | 56.11 |
| Medicinal charcoal | Medicinal | 0.13 | 1.04kg | / | C | 12.01 |
| Purified water | Industry | 3.27 | 41.02kg | / | H2O | 18.01 |
F, crude product refining: in refining kettle, add purified water water and crude product potassium dihydrogen phosphate, stirring and dissolving, intensification adds medicinal activated carbon decolorizing, carry out filtering, filtrate being concentrated by the titanium rod accurate filter that filter is 0.22 μm, it is transferred to clean area carry out crystallization and crystallize and carry out centrifugal drying worry, obtains fine work potassium dihydrogen phosphate wet product；
Refined raw materials used rate of charge:
| Name of material | Rank | Rate of charge | Inventory | Molecular formula | Molecular weight |
| Potassium dihydrogen phosphate crude product | / | 1 | / | KH2PO4 | 136.09 |
| Purified water | Industry | 2 | / | H2O | 18.01 |
| Medicinal charcoal | Medicinal | 0.06 | 0.66kg | C | 12.01 |
G, drying and packaging: fine work potassium dihydrogen phosphate wet product is loaded uniformly in the drip pan being covered with medicinal Low Density Polyethylene bag, drip pan is put in vacuum drying oven, carry out drying until dipotassium hydrogen phosphate Monitoring Data meets the requirements, it is cooled to room temperature, carry out discharging, carry out weighing in clean area, subpackage enters in complex pocket, seal, putting into pail pack, warehouse-in deposits wait delivery.
Generally, it is simple that the present invention has technique, low cost of manufacture, the advantage meeting the market demand.
Claims (8)
1. a preparation method for pharmaceutical grade potassium dihydrogen phosphate, described preparation method comprises the following steps: a, configuration raw material: configuration phosphoric acid solution and potassium hydroxide solution；B, synthetic reaction: added by gained phosphoric acid solution in reactor, liter high-temperature, to 40-70 DEG C, is slowly added dropwise pH value in gained potassium hydroxide solution to solution PH reaches 3.5 ~ 4.5 and 20 minutes and no longer changes, and stops dropping and has i.e. reacted；C, decolorization filtering concentrate: be warming up to 80-100 DEG C, add medicinal carbon, insulated and stirred is decoloured 20-30 minute, use compressed air to pressurizeing in reactor and keeping pressure≤0.4MPa, make reactant liquor pass through filter to enter smoothly in concentration kettle, to concentration kettle evacuation pressure≤-0.08MPa in keeping still, concentration kettle heat temperature raising is concentrated until concentrated solution density reaches 1.3 ~ 1.4g/cm3Stop concentrating；Worry is got rid of in d, crystallization: concentrated solution is transferred to clean area crystallizer, crystallizer is carried out slow cooling to-5 ~ 0 DEG C, and keep the temperature crystallize 24 hours of-5 ~ 0 DEG C, be centrifuged getting rid of worry in blowing to centrifuge, use water to carry out drip washing, obtain crude product potassium dihydrogen phosphate wet product and filtrate；E, crude product are dried: crude product potassium dihydrogen phosphate wet product put in the drip pan being covered with medicinal Low Density Polyethylene bag uniformly, drip pan is put in vacuum drying oven, evacuation makes pressure≤-0.08MPa in baking oven, under conditions of carrying out intensification holding temperature 25 ~ 40 DEG C, dry and meet the requirements to product for 12 ~ 15 hours, take out crude product potassium dihydrogen phosphate after being down to room temperature to carry out weighing, packing, enclose material card stand-by；F, crude product refining: in refining kettle, add water and crude product potassium dihydrogen phosphate, stirring and dissolving, heats up and adds medicinal activated carbon decolorizing, carry out filtering, concentrating filtrate by filter, it is transferred to clean area carry out crystallization and crystallize and carry out centrifugal drying worry, obtains fine work potassium dihydrogen phosphate wet product；G, drying and packaging: fine work potassium dihydrogen phosphate wet product is loaded uniformly in the drip pan being covered with medicinal Low Density Polyethylene bag, drip pan is put in vacuum drying oven, make vacuum≤-0.08MPa, carry out vacuum drying drying until dipotassium hydrogen phosphate loss on drying≤0.2% under conditions of temperature 25 ~ 40 DEG C, be cooled to room temperature, carry out discharging, carry out weighing in clean area, subpackage enters in complex pocket, sealing, put into pail pack, warehouse-in deposits wait delivery.
The preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate the most according to claim 1, it is characterised in that: the described titanium rod filter that the filter in step c is 5 μm, the titanium rod accurate filter that filter is 0.22 μm in described f step.
The preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate the most according to claim 1, it is characterised in that: described clean area is D level clean area.
The preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate the most according to claim 1, it is characterised in that: described water is purified water.
The preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate the most according to claim 1, it is characterised in that: described washing water temperature is 0 ~-5 DEG C.
The preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate the most according to claim 1, it is characterised in that: the described complex pocket in step g is polyester-aluminium-polythene drug packaging complex pocket.
The preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate the most according to claim 1, it is characterised in that: the concentration of described phosphoric acid solution is 35-50%.
The preparation method of a kind of pharmaceutical grade potassium dihydrogen phosphate the most according to claim 1, it is characterised in that: the concentration of described potassium hydroxide is 15-30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610354655.8A CN105883739B (en) | 2016-05-26 | 2016-05-26 | A kind of preparation method of pharmaceutical grade potassium dihydrogen phosphate |
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| CN201610354655.8A CN105883739B (en) | 2016-05-26 | 2016-05-26 | A kind of preparation method of pharmaceutical grade potassium dihydrogen phosphate |
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| CN105883739A true CN105883739A (en) | 2016-08-24 |
| CN105883739B CN105883739B (en) | 2018-03-06 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107804832A (en) * | 2017-11-16 | 2018-03-16 | 达州瓮福蓝剑化工有限责任公司 | A kind of neutralized by the heating of dense mother liquor obtains the method for potassium dihydrogen phosphate |
| CN109045744A (en) * | 2018-08-30 | 2018-12-21 | 山东亚邦化工科技有限公司 | The method and apparatus for preparing acesulfame potassium crystallization of continuous-stable |
| CN109078359A (en) * | 2018-08-30 | 2018-12-25 | 山东亚邦化工科技有限公司 | A kind of technique and device for acesulfame potassium sulfonation hydrolysis liquid continuous extration |
| CN109133021A (en) * | 2018-11-07 | 2019-01-04 | 武汉联德化学品有限公司 | A kind of preparation method for fire-retardant biphosphate potassium granular formulation |
| CN113336209A (en) * | 2021-04-07 | 2021-09-03 | 山东鼎欣生物科技有限公司 | Method for preparing monopotassium phosphate by constant pH |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101186A (en) * | 1986-02-21 | 1987-01-31 | 沈阳化学工业污染防治研究中心 | A kind of novel method of producing potassium primary phosphate |
| CN102101661A (en) * | 2010-12-29 | 2011-06-22 | 武汉同源药业有限公司 | Method for preparing high-purity monopotassium phosphate crude medicine |
| CN102249204A (en) * | 2011-06-15 | 2011-11-23 | 安徽恒星制药有限公司 | Method for preparing dipotassium phosphate |
| CN102285649A (en) * | 2011-06-15 | 2011-12-21 | 安徽恒星制药有限公司 | Method for preparing monopotassium phosphate |
-
2016
- 2016-05-26 CN CN201610354655.8A patent/CN105883739B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101186A (en) * | 1986-02-21 | 1987-01-31 | 沈阳化学工业污染防治研究中心 | A kind of novel method of producing potassium primary phosphate |
| CN102101661A (en) * | 2010-12-29 | 2011-06-22 | 武汉同源药业有限公司 | Method for preparing high-purity monopotassium phosphate crude medicine |
| CN102249204A (en) * | 2011-06-15 | 2011-11-23 | 安徽恒星制药有限公司 | Method for preparing dipotassium phosphate |
| CN102285649A (en) * | 2011-06-15 | 2011-12-21 | 安徽恒星制药有限公司 | Method for preparing monopotassium phosphate |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107804832A (en) * | 2017-11-16 | 2018-03-16 | 达州瓮福蓝剑化工有限责任公司 | A kind of neutralized by the heating of dense mother liquor obtains the method for potassium dihydrogen phosphate |
| CN109045744A (en) * | 2018-08-30 | 2018-12-21 | 山东亚邦化工科技有限公司 | The method and apparatus for preparing acesulfame potassium crystallization of continuous-stable |
| CN109078359A (en) * | 2018-08-30 | 2018-12-25 | 山东亚邦化工科技有限公司 | A kind of technique and device for acesulfame potassium sulfonation hydrolysis liquid continuous extration |
| CN109078359B (en) * | 2018-08-30 | 2020-11-06 | 山东亚邦化工科技有限公司 | Process and device for continuous extraction of acesulfame potassium sulfonated hydrolysate |
| CN109045744B (en) * | 2018-08-30 | 2021-04-27 | 山东亚邦化工科技有限公司 | Method and device for continuously and stably preparing acesulfame potassium crystals |
| CN109133021A (en) * | 2018-11-07 | 2019-01-04 | 武汉联德化学品有限公司 | A kind of preparation method for fire-retardant biphosphate potassium granular formulation |
| CN113336209A (en) * | 2021-04-07 | 2021-09-03 | 山东鼎欣生物科技有限公司 | Method for preparing monopotassium phosphate by constant pH |
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| CN105883739B (en) | 2018-03-06 |
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