CN106006594B - A kind of production method of medicinal calcium phosphate dibasic anhydrous - Google Patents
A kind of production method of medicinal calcium phosphate dibasic anhydrous Download PDFInfo
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- CN106006594B CN106006594B CN201610346346.6A CN201610346346A CN106006594B CN 106006594 B CN106006594 B CN 106006594B CN 201610346346 A CN201610346346 A CN 201610346346A CN 106006594 B CN106006594 B CN 106006594B
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- 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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/322—Preparation by neutralisation of orthophosphoric acid
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Abstract
The present invention relates to a kind of preparation of calcium monohydrogen phosphate, the production method of specifically a kind of pharmaceutical grade anhydrous calcium monohydrogen phosphate includes the following steps：（1）Prepare phosphoric acid solution；（2）Calcium carbonate slurry is prepared, is reacted with phosphoric acid solution, obtains slurries one；（3）Compound concentration is 10 15% milk of limes, and step is added to the rate of 1.0 2.5L/min（2）It in the slurries one of gained, is stirred while adding in milk of lime with the rate of 130 200rpm, after milk of lime adds, the pH for continuing to stir 15 20min to solution is 6.0 7.0, stands 1 1.5h of heat preservation, obtains slurries two；（4）By step（3）The slurries two of gained carry out separation of solid and liquid, and recycling solid is dried, and obtains calcium phosphate dibasic anhydrous.Present invention process is simple, low for equipment requirements, reaction raw materials is carried out with special process processing, the yield height of the calcium phosphate dibasic anhydrous of gained, purity are high, can reach the requirement of pharmaceutical grade, production cost is low.
Description
Technical field
The present invention relates to a kind of preparation of calcium monohydrogen phosphate, the producer of specifically a kind of pharmaceutical grade anhydrous calcium monohydrogen phosphate
Method belongs to excipient substance production field.
Background technology
Calcium phosphate dibasic anhydrous is a kind of white, odorless, tasteless powder or crystal, it exists with the crystal of anorthic system.
Pharmaceutical grade anhydrous calcium monohydrogen phosphate is mainly used as the diluent of hydrophobic medicinal tablet and capsule, it be both a kind of pharmaceutic adjuvant and
A kind of calcium replenishing nutrient.
The preparation of traditional calcium phosphate dibasic anhydrous, such as calcium monohydrogen phosphate a kind of disclosed in Patent No. CN201210562254.3
Production technology, but the following problem of generally existing：1. low yield, impurity is more, and purity is undesirable；2. by-product is also easy to produce, especially
During high-temperature process is dehydrated by dicalcium phosphate dihydrate to sewage calcium monohydrogen phosphate, calcium monohydrogen phosphate can occur it is intermolecular dehydration from
And become pyrophosphoric acid hydrogen calcium；3. the regulation current edition of pharmacopeia and the requirement of American-European pharmacopeia etc. is not achieved, these existing problems are very
Application of the calcium phosphate dibasic anhydrous in medicinal applications is limited in big degree.
Invention content
The present invention provides a kind of pharmaceutical grade anhydrous calcium monohydrogen phosphate, and using direct neutralisation, the technique of every section of Discrete control is joined
Number, with reference to the specially treated to reactant, reaches the product calcium phosphate dibasic anhydrous of high yield, high-purity, reaches the mark of pharmaceutical grade
Standard controls production cost.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of production method of medicinal calcium phosphate dibasic anhydrous, includes the following steps：
（1）Compound concentration is added in for 15-30% phosphoric acid solutions in reaction kettle, is warming up to 40-50 DEG C；
（2）Compound concentration is starched for 20-25% calcium carbonate, is added in reaction kettle with the rate of 1.5-3.5L/min, simultaneously will
Solution is warming up to 65-70 DEG C in reaction kettle, and is constantly stirred with the rate of 200-250rpm, and calcium carbonate is reacted with phosphoric acid solution,
It is 5.0-5.5 that calcium carbonate slurry, which continues to stir after adding to the pH of solution, stops stirring, and temperature is down to 50-60 DEG C, stands heat preservation
0.5-1.5h obtains slurries one；
（3）Compound concentration is 10-15% milk of limes, and step is added to the rate of 1.0-2.5L/min（2）The slurries of gained
It in one, is stirred while adding in milk of lime with the rate of 130-200rpm, after milk of lime adds, continues to stir 15-20min to molten
The pH of liquid is 6.0-7.0, stands heat preservation 1-1.5h, obtains slurries two；
（4）By step（3）The slurries two of gained carry out separation of solid and liquid, and recycling solid is dried, and obtains anhydrous phosphoric acid hydrogen
Calcium.
Above-mentioned technical proposal using direct neutralization reaction, obtains calcium monohydrogen phosphate, from the concentration of reaction raw materials to each step
Technological parameter is accurately controlled, the addition rate of each step reactant, the reaction temperature in reaction process, stir speed (S.S.) etc.,
All there is extreme influence to the yield of product and quality, especially the addition rate of calcium carbonate slurry, the addition rate of milk of lime are to production
The purity of object has an impact；In step（2）、（3）In, if there is standing incubation step, the yield of product is influenced by very big, passes through increasing
The standing in the technical program is added to keep the temperature, the yield of last calcium phosphate dibasic anhydrous can be improved at least three point.
Preferably, the preparation method of the milk of lime includes：A. it is 1 in mass ratio by quick lime and water：5-7 is mixed,
1-1.5h is stirred to react with the rate of 45-60rpm, obtains the thick liquid of lime white, the temperature of the water is 60-65 DEG C；B. by described in
The thick liquid of lime white obtains lime white through removal of impurities processing and filtration treatment；The removal of impurities processing is using adsorbent.
The milk of lime prepared by the above method removes the impurity such as heavy metal in quick lime, for the system of calcium monohydrogen phosphate
It is standby, the purity of calcium monohydrogen phosphate is improved, meets medicinal requirement.
Preferably, the grain size of the quick lime is 35-45cm, the generation efficiency of grain diameter influence's milk of lime of quick lime,
Grain size is excessive, is unfavorable for reacting, and grain size is too small, can wrap up quick lime due to the supersaturation of the lime of generation, prevent the life of lime
Into, and then influence the yield and purity of calcium monohydrogen phosphate.
Preferably, step（4）Middle drying when, inlet air temperature be 120-150 DEG C, leaving air temp be 75-90 DEG C, can
It to dicalcium phosphate dihydrate high efficiency drying, and will not cause calcium monohydrogen phosphate that intermolecular dehydration occurs, improve calcium phosphate dibasic anhydrous
Purity.
Preferably, the concrete operations of the removal of impurities processing are that the thick liquid stream of milk of lime is filled through to the absorption of adsorbent
Column, the flow velocity of the thick liquid of milk of lime is 0.5-1 L/min, and impurity-eliminating effect is more preferable.
Preferably, the adsorbent includes the component of following parts by weight：13-20 parts of chitosan, embedding yeast 25-40
Part, 20-30 parts of diatom, 5-12 parts of bagasse, 5-10 parts of silica gel.
The adsorbent that component disclosed in said program obtains is adsorbed, especially for the impurity component in milk of lime
To do not meet it is medicinal as defined in such as beavy metal impurity, can play significant suction-operated, cooperation using adsorption column form,
The thick flow velocity of milk of lime of 0.5-1 L/min, removal of impurities treated milk of lime purity is high, can reach after reaction generation calcium monohydrogen phosphate
Pharmaceutical grades.
In component, many hydroxyls, amino are dispersed on chitosan macromolecular chain, is formed by hydrogen bond or sat linkage with similar
The caged of reticular structure, diatom have the specific surface area and porosity of super large, can not only be high by the cage structure of chitosan
Effect absorption heavy metal ion, and adsorb and stablize, yeast, silica gel auxiliary absorption promote the adsorption effect of diatom, bagasse is not only
Itself there is adsorption function, and the bagasse of appropriate particle size can be that adsorbent improves stable support force, improve adsorbent
Stability.
Preferably, the adsorbent is made by the steps：1. chitosan is mixed with diatom, through ultrasonic wave
Processing, obtains mixture one；The processing frequency of ultrasonic wave is 20-35kHz, and processing 1min, interval 1min are repeated 3-5 times；It 2. will
The mixture one is mixed with embedding yeast, is added in silica gel while stirring, is obtained mixture two；3. by the mixture two with it is sweet
Bagasse mixes, and obtains adsorbent；The grain size of the bagasse is 10nm-50nm.
It adsorbent is prepared by above-mentioned technique, can give full play to the effect of each component, chitosan not only performance itself
Suction-operated also using the cage structure of itself is gone to provide spatial distribution net for diatom, improves the adsorption effect of diatom, ultrasonic wave
After processing, it is more notable to promote amplitude；The bagasse that this programme discloses grain size can be that adsorbent improves stable support force, improve
The stability of adsorbent is functioned using other absorbed components.
Preferably, the bagasse carries out just handling before use, the concrete operations just handled are：By bagasse in temperature
It spends in the alkaline solution for 40-65 DEG C and impregnates 2.5-4h, the pH of the alkaline solution is 7.5-8.0.
In the present solution, being handled using alkaline solution bagasse, soaking time and temperature are controlled, conducive to being fully extended
The fiber in bagasse is opened, if pH is excessively high, destroys bagasse fibre, the adsorptivity of itself is not only resulted in and declines even funeral
It loses, and it assists the effect of other component adsorption capacities also to weaken or even have opposite inhibition inhibition, pH is low, and fiber is stretched
Exhibition does not reach requirement, function limitation, too low to obtain acidity, loss of function.
Preferably, the embedding yeast is embedded using sodium alginate, conducive to maintaining, stablizing the effect of yeast.
By implementing above-mentioned technical proposal, the present invention has following advantageous effect：Present invention process is simple, will to equipment
It asks low, reaction raw materials is carried out with special process processing, the yield height of the calcium phosphate dibasic anhydrous of gained, purity are high, can reach medicinal
The requirement of grade, production cost are low.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.
Embodiment 1：
A kind of production method of medicinal calcium phosphate dibasic anhydrous, includes the following steps：
（1）Compound concentration is added in for 15% phosphoric acid solution in reaction kettle, is warming up to 40 DEG C；
（2）Compound concentration is 25% calcium carbonate slurry, is added in reaction kettle with the rate of 1.5L/min, while by reaction kettle
Interior solution is warming up to 65 DEG C, and is constantly stirred with the rate of 200rpm, and calcium carbonate is reacted with phosphoric acid solution, after calcium carbonate slurry adds
It is 5.0 to continue to stir to the pH of solution, stops stirring, and temperature is down to 60 DEG C, stands heat preservation 1.5h, obtains slurries one；
（3）Compound concentration is 15% milk of lime, and step is added to the rate of 2.5L/min（2）In the slurries one of gained, add
It is stirred while entering milk of lime with the rate of 150rpm, after milk of lime adds, the pH for continuing to stir 20min to solution is 6.0, quiet
Heat preservation 1.5h is put, obtains slurries two；
（4）By step（3）The slurries two of gained carry out separation of solid and liquid, and recycling solid is dried, the air inlet of drying device
Temperature is 150 DEG C, and leaving air temp is 90 DEG C, obtains calcium phosphate dibasic anhydrous,
Yield reaches 95%, and purity reaches 99.9%, burns vehement weightless stable 7.5%.
Embodiment 2：
A kind of production method of medicinal calcium phosphate dibasic anhydrous, includes the following steps：
（1）Compound concentration is added in for 20% phosphoric acid solution in reaction kettle, is warming up to 45 DEG C；
（2）Compound concentration is 20% calcium carbonate slurry, is added in reaction kettle with the rate of 3.5L/min, while by reaction kettle
Interior solution is warming up to 70 DEG C, and is constantly stirred with the rate of 250rpm, and calcium carbonate is reacted with phosphoric acid solution, after calcium carbonate slurry adds
It is 5.5 to continue to stir to the pH of solution, stops stirring, and temperature is down to 55 DEG C, stands heat preservation 0.5h, obtains slurries one；
（3）Compound concentration is 10% milk of lime, and step is added to the rate of 1.0L/min（2）In the slurries one of gained, add
It is stirred while entering milk of lime with the rate of 130rpm, after milk of lime adds, the pH for continuing to stir 15min to solution is 6.5, quiet
Heat preservation 1h is put, obtains slurries two；
The preparation method of milk of lime is as follows：A. it is 1 in mass ratio by quick lime and water：5 mixing, are stirred with the rate of 60rpm
Reaction 1h is mixed, obtains the thick liquid of lime white, the temperature of the water is 60 DEG C；B. the thick liquid of the lime white is handled and filtered through removal of impurities
Processing, obtains lime white；Using adsorbent, concrete operations are that the thick liquid stream of milk of lime has been filled through adsorbent for the removal of impurities processing
Adsorption column, the flow velocity of the thick liquid of milk of lime is 1 L/min；
Adsorbent includes the component of following parts by weight：15 parts of chitosan, 25 parts of yeast of embedding, 25 parts of diatom, bagasse 12
Part, 5 parts of silica gel；It is made by the steps：1. chitosan is mixed with diatom, through ultrasonication, mixture is obtained
One；The processing frequency of ultrasonic wave is 25kHz, and processing 1min, interval 1min are repeated 3 times；2. by the mixture one and embedding ferment
Mother's mixing, adds in silica gel, obtains mixture two while stirring；3. the mixture two is mixed with bagasse, adsorbent is obtained；
The grain size of the bagasse is 10nm-30nm；
（4）By step（3）The slurries two of gained carry out separation of solid and liquid, and recycling solid is dried, the air inlet of drying device
Temperature is 120 DEG C, and leaving air temp is 75 DEG C, obtains calcium phosphate dibasic anhydrous, and yield reaches 95%, and purity reaches 99.8%, vehement mistake of burning
Stablize again 7.8%.
Embodiment 3：
A kind of production method of medicinal calcium phosphate dibasic anhydrous, includes the following steps：
（1）Compound concentration is added in for 30% phosphoric acid solution in reaction kettle, is warming up to 50 DEG C；
（2）Compound concentration is 21% calcium carbonate slurry, is added in reaction kettle with the rate of 2.0L/min, while by reaction kettle
Interior solution is warming up to 68 DEG C, and is constantly stirred with the rate of 225rpm, and calcium carbonate is reacted with phosphoric acid solution, after calcium carbonate slurry adds
It is 5.3 to continue to stir to the pH of solution, stops stirring, and temperature is down to 50 DEG C, stands heat preservation 1.0h, obtains slurries one；
（3）Compound concentration is 12% milk of lime, and step is added to the rate of 2.0L/min（2）In the slurries one of gained, add
It is stirred while entering milk of lime with the rate of 200rpm, after milk of lime adds, the pH for continuing to stir 16min to solution is 7.0, quiet
Heat preservation 80min is put, obtains slurries two；
The preparation method of milk of lime is as follows：A. it is 1 in mass ratio by quick lime and water：6 mixing, are stirred with the rate of 45rpm
Reaction 1.5h is mixed, obtains the thick liquid of lime white, the temperature of the water is 65 DEG C；B. by the thick liquid of the lime white through removal of impurities processing and mistake
Filter is handled, and obtains lime white；Using adsorbent, concrete operations are that the thick liquid stream of milk of lime has been filled through absorption for the removal of impurities processing
The adsorption column of agent, the flow velocity of the thick liquid of milk of lime is 0.5L/min；
Adsorbent includes the component of following parts by weight：13 parts of chitosan, 40 parts of the yeast of sodium alginate embedding, diatom 20
Part, 10 parts of bagasse, 10 parts of silica gel；It is made by the steps：1. chitosan is mixed with diatom, at ultrasonic wave
Reason, obtains mixture one；The processing frequency of ultrasonic wave is 35kHz, and processing 1min, interval 1min are repeated 5 times；2. by described mixed
It closes object one to mix with embedding yeast, adds in silica gel while stirring, obtain mixture two；3. the mixture two is mixed with bagasse
It closes, obtains adsorbent；The grain size of the bagasse is 30nm-50nm；Bagasse carries out just handling before use, and bagasse is existed
Temperature is that 2.5h is impregnated in 65 DEG C of alkaline solution, and the pH of the alkaline solution is 7.5；
（4）By step（3）The slurries two of gained carry out separation of solid and liquid, and recycling solid is dried, the air inlet of drying device
Temperature is 130 DEG C, and leaving air temp is 80 DEG C, obtains calcium phosphate dibasic anhydrous, and yield reaches 96.6%, and purity reaches 99.82%, is burnt vehement
Weightlessness is stablized 7.0%.
Embodiment 4：
A kind of production method of medicinal calcium phosphate dibasic anhydrous, includes the following steps：
（1）Compound concentration is added in for 25% phosphoric acid solution in reaction kettle, is warming up to 48 DEG C；
（2）Compound concentration is starched for 20-25% calcium carbonate, is added in reaction kettle with the rate of 1.8L/min, while will reaction
Solution is warming up to 66 DEG C in kettle, and is constantly stirred with the rate of 245rpm, and calcium carbonate is reacted with phosphoric acid solution, and calcium carbonate slurry adds
It is 5.1 to continue to stir afterwards to the pH of solution, stops stirring, and temperature is down to 52 DEG C, stands heat preservation 1.2h, obtains slurries one；
（3）Compound concentration is 14% milk of lime, and step is added to the rate of 1.6L/min（2）In the slurries one of gained, add
It is stirred while entering milk of lime with the rate of 160rpm, after milk of lime adds, the pH for continuing to stir 15min to solution is 6.4, quiet
Heat preservation 1.3h is put, obtains slurries two；
The preparation method of milk of lime is as follows：A. it is 1 in mass ratio by quick lime and water：7 mixing, are stirred with the rate of 55rpm
Reaction 1.2h is mixed, obtains the thick liquid of lime white, the temperature of the water is 63 DEG C；B. by the thick liquid of the lime white through removal of impurities processing and mistake
Filter is handled, and obtains lime white；Using adsorbent, concrete operations are that the thick liquid stream of milk of lime has been filled through absorption for the removal of impurities processing
The adsorption column of agent, the flow velocity of the thick liquid of milk of lime is 0.8 L/min；
Adsorbent includes the component of following parts by weight：20 parts of chitosan, 30 parts of the yeast of sodium alginate embedding, diatom 30
Part, 5 parts of bagasse, 8 parts of silica gel；It is made by the steps：1. chitosan is mixed with diatom, through ultrasonication,
Obtain mixture one；The processing frequency of ultrasonic wave is 30kHz, and processing 1min, interval 1min are repeated 4 times；2. by the mixture
One mixes with embedding yeast, adds in silica gel while stirring, obtains mixture two；3. the mixture two is mixed with bagasse,
Obtain adsorbent；The grain size of the bagasse is 10nm-50nm；Bagasse carries out just handling before use, by bagasse in temperature
It spends in the alkaline solution for 45 DEG C and impregnates 54h, the pH8.0 of the alkaline solution；
（4）By step（3）The slurries two of gained carry out separation of solid and liquid, and recycling solid is dried, the air inlet of drying device
Temperature is 135 DEG C, and leaving air temp is 85 DEG C, obtains calcium phosphate dibasic anhydrous, and yield reaches 97.5%, and purity reaches 99.98%, is burnt vehement
Weightlessness is stablized 7.0%.
Claims (6)
1. a kind of production method of medicinal calcium phosphate dibasic anhydrous, includes the following steps：
（1）Compound concentration is added in for 15-30% phosphoric acid solutions in reaction kettle, is warming up to 40-50 DEG C；
（2）Compound concentration is starched for 20-25% calcium carbonate, is added in reaction kettle with the rate of 1.5-3.5L/min, while will reaction
Solution is warming up to 65-70 DEG C in kettle, and is constantly stirred with the rate of 200-250rpm, and calcium carbonate is reacted with phosphoric acid solution, carbonic acid
It is 5.0-5.5 that calcium slurry, which continues to stir after adding to the pH of solution, stops stirring, and temperature is down to 50-60 DEG C, stands heat preservation 0.5-
1.5h obtains slurries one；
（3）Compound concentration is 10-15% milk of limes, and step is added to the rate of 1.0-2.5L/min（2）The slurries one of gained
In, it is stirred while adding in milk of lime with the rate of 130-200rpm, after milk of lime adds, continues to stir 15-20min to solution
PH for 6.0-7.0, stand heat preservation 1-1.5h, obtain slurries two；
（4）By step（3）The slurries two of gained carry out separation of solid and liquid, and recycling solid is dried, and obtains calcium phosphate dibasic anhydrous；
The preparation method of the milk of lime includes：A. it is 1 in mass ratio by quick lime and water：5-7 is mixed, with the speed of 45-60rpm
Rate is stirred to react 1-1.5h, obtains the thick liquid of lime white, the temperature of the water is 60-65 DEG C；B. by the thick liquid of the lime white through removing
Reason and filtration treatment are lived together, obtains lime white；The removal of impurities processing is using adsorbent；
The concrete operations of the removal of impurities processing are that the thick liquid stream of milk of lime is filled through to the adsorption column of adsorbent, the thick liquid of milk of lime
Flow velocity is 0.5-1 L/min；The adsorbent includes the component of following parts by weight：13-20 parts of chitosan, embedding yeast 25-40
Part, 20-30 parts of diatom, 5-12 parts of bagasse, 5-10 parts of silica gel.
2. a kind of production method of medicinal calcium phosphate dibasic anhydrous according to claim 1, which is characterized in that the quick lime
Grain size is 35-45cm.
A kind of 3. production method of medicinal calcium phosphate dibasic anhydrous according to claim 1, which is characterized in that step（4）In do
When dry, inlet air temperature is 120-150 DEG C, and leaving air temp is 75-90 DEG C.
4. a kind of production method of medicinal calcium phosphate dibasic anhydrous according to claim 1, which is characterized in that the adsorbent leads to
Following steps are crossed to be prepared：1. chitosan is mixed with diatom, through ultrasonication, mixture one is obtained；The place of ultrasonic wave
Reason frequency is 20-35kHz, and processing 1min, interval 1min are repeated 3-5 times；2. the mixture one is mixed with embedding yeast,
Silica gel is added in while stirring, obtains mixture two；3. the mixture two is mixed with bagasse, adsorbent is obtained；It is described sweet
The grain size of bagasse is 10nm-50nm.
5. a kind of production method of medicinal calcium phosphate dibasic anhydrous according to claim 4, which is characterized in that the bagasse exists
It is just handled using preceding progress, the concrete operations just handled are：Bagasse is impregnated in alkaline solution of the temperature for 40-65 DEG C
2.5-4h, the pH of the alkaline solution is 7.5-8.0.
A kind of 6. production method of medicinal calcium phosphate dibasic anhydrous according to claim 1, which is characterized in that the embedding yeast
It is embedded using sodium alginate.
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| JP6164628B1 (en) | 2017-03-30 | 2017-07-19 | 富田製薬株式会社 | Anhydrous calcium hydrogen phosphate and method for producing the same |
| CN111268661A (en) * | 2020-03-19 | 2020-06-12 | 江苏瑞丰医药有限公司 | Production method of superfine calcium hydrophosphate |
| CN113353905B (en) * | 2021-06-29 | 2024-05-17 | 湖北兴发化工集团股份有限公司 | Process for preparing medicinal coarse particle anhydrous calcium hydrophosphate |
| CN113548653B (en) * | 2021-07-14 | 2022-07-19 | 湖州展望药业有限公司 | Production process of pharmaceutic adjuvant anhydrous calcium hydrophosphate with direct-pressure function |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590286A (en) * | 2004-04-13 | 2005-03-09 | 贾振宇 | New production technology of feed grade calcium hydrogen phosphate |
| CN103496685A (en) * | 2013-10-14 | 2014-01-08 | 四川省化工设计院 | Method for continuously producing feed-grade dibasic calcium phosphate |
| CN104649242A (en) * | 2014-10-22 | 2015-05-27 | 昆明川金诺化工股份有限公司 | Method for obtaining high-quality superphosphate-enriched byproduct in feed-grade calcium hydrophosphate production process |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590286A (en) * | 2004-04-13 | 2005-03-09 | 贾振宇 | New production technology of feed grade calcium hydrogen phosphate |
| CN103496685A (en) * | 2013-10-14 | 2014-01-08 | 四川省化工设计院 | Method for continuously producing feed-grade dibasic calcium phosphate |
| CN104649242A (en) * | 2014-10-22 | 2015-05-27 | 昆明川金诺化工股份有限公司 | Method for obtaining high-quality superphosphate-enriched byproduct in feed-grade calcium hydrophosphate production process |
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