CN106744764A - A kind of method for producing potassium dihydrogen phosphate - Google Patents
A kind of method for producing potassium dihydrogen phosphate Download PDFInfo
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- CN106744764A CN106744764A CN201611004641.XA CN201611004641A CN106744764A CN 106744764 A CN106744764 A CN 106744764A CN 201611004641 A CN201611004641 A CN 201611004641A CN 106744764 A CN106744764 A CN 106744764A
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- phosphoric acid
- calcium
- dihydrogen phosphate
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- potassium
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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
- C01B25/301—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
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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
Abstract
The present invention relates to a kind of method for producing potassium dihydrogen phosphate, calcium hydrophosphate fodder is first carried out into predecomposition reaction with PHOSPHORIC ACID TECH.GRADE, adding potassium acid sulfate carries out metathesis reaction, filter out calcium sulfate and filtrate, crystallisation by cooling is concentrated after carrying out purified treatment to filtrate, potassium dihydrogen phosphate product is prepared, crystalline mother solution is circulated operation in returning to calcium hydrophosphate fodder, or for the production without chlorine composite fertilizer.Compared with prior art, the inventive method takes phosphoric acid and the calcium hydrophosphate fodder to carry out the rate of recovery that pre-reaction is greatly improved phosphorus in calcium hydrophosphate fodder, reaches more than 95%, and the yield of potassium reaches 99.5% in potassium acid sulfate in addition, simultaneously, phosphoric acid in the present invention realizes recycling, and without discharging of waste liquid, this technological process is simple, phosphorus and potassium high income in raw material, production cost can be greatly reduced, environmental protection is sustainable, with great competitive advantage.
Description
Technical field
The present invention relates to phosphatic preparation, more particularly, to a kind of method for producing potassium dihydrogen phosphate.
Background technology
Potassium dihydrogen phosphate, is trapezoid body of a kind of colourless or white with gloss, can be dissolved in water, and its aqueous solution is micro- in acidity
Alcohol is dissolved in, there is moisture absorption hygroscopy.
Potassium dihydrogen phosphate is widely used in industry, agricultural, food service industry, medicine：Agriculturally, it is used as one kind
Controlling crop diseases and insect pests with notable volume increase, drought resisting, cold-resistant function, and are also had special by the senior phosphorus potassium compound fertilizer of high concentration
Effect, in addition because it has nutritional ingredient (P, K active ingredient high>90%), stable chemical nature, it is odorless, it is tasteless, it is nontoxic, easily
Water is dissolved in, is not lumpd, thus suitable for various soil and crop；It is used as the mineral element of supplement phosphorus and potassium in feed addictive
Additive, it is commonly used particularly in fish meal；Industrially, it is usually used in casate, makes Yeast Cultivation agent；In food
Potassium dihydrogen phosphate is one of important kind of phosphoric acid for food salt in product additive, as quality improver, fermentation accelerant, seasoning
Agent, buffer and with dipotassium hydrogen phosphate and be used as leavening agent.The production method of potassium dihydrogen phosphate have neutralisation, extraction,
Ion-exchange, double decomposition, direct method, crystallisation and electrolysis etc., the potassium dihydrogen phosphate of China is mainly by hot method at present
Prepared by the neutralization reaction of phosphoric acid and potash, account for more than the 90% of national potassium dihydrogen phosphate total productive capacity, the method technique skill
Art is ripe, but its production cost is high.
There is document report that the technique of potassium dihydrogen phosphate, document and patent are prepared using calcium hydrophosphate fodder and potassium acid sulfate
In preparation technology, be to be carried out in the double decomposition stage, potassium hydrogen sulfate solution to be added directly into the slurry of calcium hydrophosphate fodder
Metathesis reaction, reaction equation is as follows：
KHSO4+CaHPO4·2H2O→KH2PO4+CaSO4·2H2O↓
Reactant calcium monohydrogen phosphate is insoluble in water in the reaction, and the calcium sulfate of generation is also insoluble in water, and calcium sulfate is easily in phosphorus
Sour hydrogen calcium surface sediment, forms parcel so that the dissolving of calcium monohydrogen phosphate is difficult, and causing the resolution ratio of calcium monohydrogen phosphate phosphorus reduces.It is former
The utilization rate of material is low, production cost is increased；Meanwhile, this kind of metathesis process causes sulphur in the filtered fluid after metathesis reaction
Acid group concentration is high, influences the purity of final potassium dihydrogen phosphate product, if increasing filtrate dedoping step, will cause overall manufacturing into
This increase.
The side that a kind of calcium hydrophosphate fodder produces potassium dihydrogen phosphate is disclosed in Chinese patent CN 103879980B
Method, the method carries out extractive reaction with sulfuric acid again with calcium hydrophosphate fodder as raw material after carrying out conversion reaction with phosphoric acid solution,
Obtained after filtering filtrate PHOSPHORIC ACID TECH.GRADE regulation PH be 7.1~8.5, after again in filtrate add potassium carbonate and potassium hydroxide
Solution carries out neutralization reaction, and it is 8.5~9.5 that PH is adjusted after the completion of reaction, and filtering gained filtrate continues to adjust by PHOSPHORIC ACID TECH.GRADE
Section PH is 4~4.5, adjusts reaction solution density, and centrifugal drying obtains potassium dihydrogen phosphate after crystal is all separated out.Phosphorus in the patent
Acid participates in reaction in the form of reactant, while production cost is very high under the technique.
It is anti-that Chinese patent CN 103058158A directly carry out double decomposition using the calcium monohydrogen phosphate of fertilizer grade with potassium acid sulfate
Should, there is no phosphoric acid to participate in decomposing the reaction of calcium monohydrogen phosphate；Meanwhile, phosphoric acid, the effect of Recycling Mother Solution are not contained in its crystalline mother solution
It is only in that the yield for improving potassium dihydrogen phosphate product.
Chinese patent CN 104944397A are by purification of wet process phosphoric acid and calcium oxide or calcium hydroxide or calcium carbonate reaction preparation
Synthos, then metathesis reaction is carried out using potassium acid sulfate or potassium sulfate solution, process adds polyoxyethylene alkyl amine and third
The composite assistant of diol block polyethers composition to reduce plane of crystal free energy, after being filtered to remove calcium sulfate, filtered fluid is concentrated,
Crystallization, washing obtain potassium dihydrogen phosphate after drying.
Patent CN 105819939A disclose a kind of production method of water soluble fertilizer, including following technical process：To contain
One section of neutralization that calcium dihydrogen phosphate produces calcium hydrophosphate fodder for the double superhosphate of main component, with mid low grade phosphate rock is clear
Liquid and agricultural potassium sulfate are raw material, carry out metathesis reaction, generate the solution of phosphoric acid potassium dihydrogen；Filter after once being filtered
Slag supplements p and ses as the raw material of production double superphosphate；Filtrate phosphoric acid potassium dihydrogen is the solution of main component, then uses hydrogen
Potassium oxide or liquefied ammonia carry out neutralizing removal of impurities reaction, and after carrying out secondary filter, filter residue enters calcium hydrophosphate fodder as supplement
Raw material or the raw material as production fertilizer grade DAP etc..Patent CN 105819939A, are by one using phosphoric acid by wet process
Clear liquid after Duan Zhonghe removal precipitations carries out metathesis reaction with agricultural potassium sulfate, generates the solution of phosphoric acid potassium dihydrogen, and this is molten
Liquid prepares water soluble fertilizer (potassium dihydrogen phosphate, or ammonium potassium dihydrogen phosphate) through removal of impurities.Phosphoric acid is participated in patent CN 105819939A
Subsequently with the neutralization reaction of potassium hydroxide or liquefied ammonia.
The content of the invention
The present invention proposes a kind of method of new production potassium dihydrogen phosphate, is raw material to solve calcium monohydrogen phosphate and potassium acid sulfate
The raw material availability that is faced in the technique for preparing potassium dihydrogen phosphate is low and production cost problem high.The method of the present invention is in subdivision
Phosphrus reagent during solution reaction reaches more than 95%, and the yield of potassium reaches 99.5% in potassium acid sulfate；The raising of phosphrus reagent, makes simultaneously
The content for obtaining sulfate radical in filtrate diminishes, and reduces cost when filtrate purifies；Additionally, mother liquid recycling in the present invention, both
The recycling of phosphoric acid is realized, the concentration and evaporation amount of follow-up potassium dihydrogen phosphate is reduced again.The present invention is pollution-free simultaneously
Discharging of waste liquid, the sustainable value of production process environmental protection.
The purpose of the present invention can be achieved through the following technical solutions：
The present invention provides a kind of method for producing potassium dihydrogen phosphate, and concrete scheme is：By calcium hydrophosphate fodder elder generation and work
Industry level phosphoric acid carries out predecomposition reaction, and adding potassium acid sulfate carries out metathesis reaction, calcium sulfate and filtrate is filtered out, to filtrate
Crystallisation by cooling is concentrated after carrying out purified treatment, the potassium dihydrogen phosphate product of the technical grade Grade A for meeting national standard is prepared,
Crystalline mother solution is circulated operation in returning to calcium hydrophosphate fodder, or for the production without chlorine composite fertilizer.
Further, when calcium hydrophosphate fodder and PHOSPHORIC ACID TECH.GRADE carry out predecomposition and react, phosphoric acid and calcium monohydrogen phosphate
Mol ratio is 0.2~0.3：1.The reaction mechanism of predecomposition reaction is the calcium monohydrogen phosphate portions turn that will be insoluble in water to be slightly soluble in
The calcium dihydrogen phosphate of water, predecomposition reaction promotes the decomposition of calcium monohydrogen phosphate, can increase substantially the phosphorus in metathesis reaction stage
Yield.
Further, calcium hydrophosphate fodder and PHOSPHORIC ACID TECH.GRADE carry out predecomposition react when, reaction temperature be 50 DEG C~
70 DEG C, the reaction time is 1h~2h.
Further, the potassium phosphorus mol ratio of potassium acid sulfate and calcium hydrophosphate fodder is 0.9~1.1：1.
Further, add potassium acid sulfate when carrying out metathesis reaction, reaction temperature is 50 DEG C~70 DEG C, the reaction time is
2~4h.
The mode that calcium hydrophosphate fodder and PHOSPHORIC ACID TECH.GRADE predecomposition reaction mix in the present invention, it is preferred to use below two
The mode of kind：
Mode one, calcium hydrophosphate fodder adds water after mashing, obtains calcium hydrophosphate fodder slurry, adds PHOSPHORIC ACID TECH.GRADE
Predecomposition reaction is carried out with calcium hydrophosphate fodder slurry；
Calcium hydrophosphate fodder adds water mashing when preparing calcium hydrophosphate fodder slurry, the level phosphoric acid hydrogen per kilogram of feed
It is 2.5~5 liters that calcium adds the volume of water.
Mode two, PHOSPHORIC ACID TECH.GRADE and the mixed phosphoric acid solution of water are mixed with calcium hydrophosphate fodder, mashing it is same
Shi Jinhang predecomposition is reacted.
When PHOSPHORIC ACID TECH.GRADE and water are mixed, the phosphoric acid solution mass percent being configured to is preferably 20%~40%.
When crystalline mother solution is returned to is circulated operation in calcium hydrophosphate fodder, crystalline mother solution can substitute industrial phosphorus
Acid, during crystalline mother solution is returned to through the pretreated calcium hydrophosphate fodder slurry of peroxophosphoric acid, potassium hydrogen sulfate solution is added to knot
In brilliant mother liquor and calcium hydrophosphate fodder slurry mixed liquor；
When crystalline mother solution is used for the production without chlorine composite fertilizer, potassium hydrogen sulfate solution is added directly into and is pre-processed through peroxophosphoric acid
In calcium hydrophosphate fodder slurry afterwards.
Potassium acid sulfate is added preferably in the form of potassium hydrogen sulfate solution, and potassium hydrogen sulfate solution mass percent is preferably 30%
~50%.
In the present invention, described calcium hydrophosphate fodder is prepared through three sections of neutralisations by phosphoric acid by wet process.
In the present invention, described PHOSPHORIC ACID TECH.GRADE can be thermal phosphoric acid, or phosphoric acid by wet process.
In the present invention, yield to more than 95%, the K yields of metathesis reaction stage phosphorus are more than 99.5%.Namely cross
P loss lates are≤5%, K loss late≤0.5% in the calcium sulfate for leaching.
In the present invention, purified treatment is carried out to filtrate and uses conventional treatment method, further the remaining sulfate radical of removing and calcium
The impurity such as ion.It is removed because the multiple stage of reaction sulfate radical overwhelming majority forms calcium sulfate, significantly reduces and be cleaned into
This.
In the present invention, when concentration crystallisation by cooling is operated, crystallization process mixing speed is 80rpm/min~100rpm/min,
Crystallization temperature is 20~40 DEG C, and crystallization time is 3h~6h, prepares the biphosphate for meeting national standard technical grade Grade A
Potassium product.
The present invention carries out predecomposition reaction by adding phosphoric acid so that part calcium monohydrogen phosphate dissolves to form certain density containing
There is the solution of free phosphorus acid group and calcium ion；After adding potassium acid sulfate, sulfate radical reacts with the calcium ion in solution, forms phosphoric acid
Calcium precipitate；The formation of calcium sulfate, it is ensured that the continuation of decomposition reaction of the calcium monohydrogen phosphate in the presence of phosphoric acid.Due to forming calcium sulfate
Reaction occur in bulk solution, package action of the calcium sulfate to calcium hydrogen phosphate particle is controlled, so as to improve phosphoric acid hydrogen
The resolution ratio of calcium.Simultaneously as employing the method that phosphoric acid dissolves part calcium monohydrogen phosphate, the amount of solution of reaction system is controlled,
The concentration of potassium dihydrogen phosphate in double decomposition liquid is improve, concentrated cost is reduced.
After adding phosphoric acid, course of reaction is：
H3PO4→H2PO4 -+H+
CaHPO4·2H2O+H2PO4 -+H+→Ca2++2H2PO4 -+2H2O
SO4 2-+Ca2++2H2O→CaSO4·2H2O↓
When phosphoric acid is added without, the dissociation of calcium monohydrogen phosphate is mainly influenceed by calcium monohydrogen phosphate solubility, after adding phosphoric acid,
The dissociation of calcium monohydrogen phosphate is mainly influenceed by calcium dihydrogen phosphate solubility, and the solubility of calcium dihydrogen phosphate is more than calcium monohydrogen phosphate
Solubility, is more beneficial for the dissociation of calcium monohydrogen phosphate, and phosphrus reagent is increased substantially.
Compared with prior art, the inventive method is taken phosphoric acid to carry out pre-reaction with calcium hydrophosphate fodder and is increased substantially
The rate of recovery of phosphorus, reaches more than 95% in calcium hydrophosphate fodder, and in addition the yield of potassium reaches 99.5%, pole in potassium acid sulfate
The big utilization rate that improve raw material, reduces cost of material；Meanwhile, the phosphoric acid in the present invention realizes recycling, without useless
Liquid is discharged, and the production technology of the other potassium dihydrogen phosphates of contrast, this raw materials technology is easy to get and low cost, and flow is simple, in raw material
Phosphorus and potassium high income, can be greatly reduced production cost, environmental protection is sustainable, with great competitive advantage.It is specific and
Speech,
1st, compared with background technology Patent CN 103879980B, its advantage and disadvantage is technical solution of the present invention：
Calcium hydrophosphate fodder is added in phosphoric acid solution in patent CN 103879980B, and excessive phosphoric acid is by phosphoric acid hydrogen
Calcium is completely converted into calcium dihydrogen phosphate, and the concentration of the metathesis reaction liquid active ingredient potassium dihydrogen phosphate of formation is low, is preparing phosphorus
Before acid dihydride potassium product, big by the water for being concentrated by evaporation removal, concentrated cost is high.And present invention process is to add phosphoric acid to
In calcium hydrophosphate fodder, phosphoric acid is 0.2~0.3, only very least a portion of feed grade phosphoric acid hydrogen with the mol ratio of calcium monohydrogen phosphate
Calcium is converted into calcium dihydrogen phosphate, then the formation for passing through calcium sulfate, maintains the decomposition reaction of calcium monohydrogen phosphate；After metathesis reaction
Feed concentration is relatively higher.
Calcium hydrophosphate fodder is added in phosphoric acid solution in patent CN 103879980B, and functioning as phosphoric acid is anti-
Thing, and calcium hydrophosphate fodder reaction is answered to prepare biphosphate calcium solution, and the effect of sulfuric acid is precipitated calcium, and form phosphoric acid
Solution.It is and the present invention makes calcium hydrophosphate fodder decomposed using phosphoric acid then complete by metathesis reaction stage calcium monohydrogen phosphate
Part solves, and produces potassium dihydrogen phosphate.In the preparation process of potassium dihydrogen phosphate, phosphoric acid is not consumed, and serves similar to subdivision
The effect of solution reaction " catalyst ".
Patent CN 103879980B are to prepare phosphorus by the neutralization reaction of prepared phosphoric acid and potassium carbonate and potassium hydroxide
Acid dihydride potassium, after neutralization reaction, crystallization separates out potassium dihydrogen phosphate, and the main component in crystalline mother solution is potassium dihydrogen phosphate, circulation
The purpose of the mother liquor is the yield of the potassium dihydrogen phosphate for improving the process.And the present invention passes through phosphoric acid predecomposition phosphoric acid hydrogen
Calcium, then directly prepares potassium dihydrogen phosphate in double decomposition mode.Analysis whole preparation process, phosphoric acid is not consumed, by the knot
The circulation of brilliant mother liquor, realizes the efficient utilization in preparation process of phosphoric acid, while technological process of the invention is more succinct.
In addition, the potassium in patent CN 103879980B comes from potassium carbonate and potassium hydroxide, and present invention process potassium comes from
In potassium acid sulfate, cost is lower.
2nd, compared with background technology Patent CN 105819939A, its advantage and disadvantage is technical solution of the present invention：
In documents CN 105819939A, the clear liquid after one section of neutralization mainly contains the calcium monohydrogen phosphate of dissolving and dissociates
Phosphoric acid, with potassium sulfate metathesis reaction, obtain potassium dihydrogen phosphate.And after phosphoric acid take part in patent CN 105819939A
The continuous neutralization reaction with potassium hydroxide or liquefied ammonia.
The present invention is to add a small amount of phosphoric acid in suspension to calcium hydrophosphate fodder, part calcium monohydrogen phosphate is converted into phosphorus
Acid dihydride calcium dissolves, and being subsequently adding potassium acid sulfate carries out metathesis reaction, with the generation of calcium sulfate precipitation, undissolved phosphoric acid
Hydrogen calcium continues to dissolve and participate in metathesis reaction in the presence of phosphoric acid.From in terms of mechanism, both courses of reaction are different.
In addition, using nitration mixture in documents CN 105819939A：Phosphoric acid and sulfuric acid so that calcium monohydrogen phosphate is complete
Dissolving, rises different similar to the mechanism of action of metathesis reaction " catalyst " from phosphoric acid in the present invention.
Meanwhile, compared with documents CN 105819939A, both initiation materials are different, the phosphorus obtained by preparation
The product purity of acid dihydride potassium is different.One is fertilizer grade, and one is feed grade or technical grade.
Brief description of the drawings
Fig. 1 is the process chart of present invention production potassium dihydrogen phosphate.
Specific embodiment
A kind of method for producing potassium dihydrogen phosphate, the process chart with reference to shown in Fig. 1, concrete technology is：
1st, calcium hydrophosphate fodder and water are beaten, prepare slurry, add the volume and calcium hydrophosphate fodder of water
Mass ratio is 2.5~5L/kg.
2nd, PHOSPHORIC ACID TECH.GRADE is configured to the phosphoric acid solution that mass percent is 20%~40%, to adding phosphoric acid in slurry
Solution carries out predecomposition reaction, and reaction temperature is 50 DEG C~70 DEG C, the calcium monohydrogen phosphate in the phosphoric acid mole and slurry of addition
Mol ratio is 0.2~0.3.The reaction mechanism of predecomposition reaction is the calcium monohydrogen phosphate portions turn that will be insoluble in water to be slightly soluble in water
Calcium dihydrogen phosphate, predecomposition reaction promotes the decomposition of calcium monohydrogen phosphate, and the phosphorus that can increase substantially the metathesis reaction stage is received
Rate.
3rd, after predecomposition reaction carries out 1h~2h, potassium acid sulfate is configured to the sulfuric acid that mass percent is 30%~50%
Hydrogen potassium solution, is slow added into, and carries out metathesis reaction, and calcium monohydrogen phosphate in the potassium acid sulfate mole of addition and slurry rubs
You are than being 0.9~1.1.
4th, after metathesis reaction carries out 2h~4h, calcium sulfate and filtrate are filtered out.The yield of metathesis reaction stage phosphorus is extremely
More than 95%, K yield are more than 99.5%.
5th, purified treatment is carried out to filtrate, further the remaining impurity such as sulfate radical and calcium ion of removing.Because double decomposition is anti-
Answer stage sulfuric acid eradication major part to form calcium sulfate to be removed, significantly reduce purification cost.
6th, the filtrate after purifying carries out concentration crystallisation by cooling, and crystallization process mixing speed is 80rpm/min~100rpm/
Min, crystallization temperature is 20~40 DEG C, and crystallization time is 3h~6h, prepares the phosphoric acid for meeting national standard technical grade Grade A
Potassium dihydrogen product.
7th, crystalline mother solution can substitute industrial phosphoric acid, to return to and carry out predecomposition reaction in calcium hydrophosphate fodder slurry,
It is circulated operation, it is also possible to for the production without chlorine composite fertilizer.
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1：
The water of 315kg calcium hydrophosphate fodders and 787.5kg is well mixed in a kettle., 174.43kg mass is added
Percentage is 20% phosphoric acid solution, and reaction temperature is 50 DEG C, and it is 30% to add 727.07kg mass percents after reaction 1h
Potassium hydrogen sulfate solution, reaction temperature is 50 DEG C, and the reaction time is 2h；Reaction is filtered after terminating, and obtains calcium sulfate and phosphoric acid two
The filtered fluid of hydrogen potassium, the loss late of phosphorus and potassium is respectively 4.93% and 0.26% in calcium sulfate；Filtrate is by after purification, crossing and filtering
Decontamination, gained filtrate carries out condensing crystallizing, and crystallization process mixing speed is 80rpm/min, and crystallization temperature is 20 DEG C, stirring knot
After brilliant 3h, 136.01kg potassium dihydrogen phosphate products and 494.81kg mother liquors are filtrated to get, mother liquor is returned in reactor, followed
Ring is operated；Biphosphate potassium content is 98.3% in product, meets the requirement of potassium dihydrogen phosphate technical grade Grade A.
Embodiment 2：
The water of 230kg calcium hydrophosphate fodders and 1150kg is well mixed in a kettle., 95.52kg mass hundred is added
Fraction is 40% phosphoric acid solution, and reaction temperature is 70 DEG C, and it is 50% to be added by 389.31kg mass percents after reaction 2h
Potassium hydrogen sulfate solution, reaction temperature is 70 DEG C, and the reaction time is 4h；Reaction is filtered after terminating, and obtains calcium sulfate and filtrate, sulfuric acid
The loss late of phosphorus and potassium is respectively 4.89% and 0.34% in calcium；Filtrate is entered by after purification, being filtered to remove impurity, gained filtrate
Row condensing crystallizing, crystallization process mixing speed is 100rpm/min, and crystallization temperature is 40 DEG C, after stirred crystallization 6h, is filtrated to get
The potassium dihydrogen phosphate product and 545.44kg mother liquors of 32.90kg, mother liquor are returned in reactor, are circulated operation；In product
Biphosphate potassium content is 98.4%, meets the requirement of potassium dihydrogen phosphate technical grade Grade A.
Embodiment 3：
The water of 180kg calcium hydrophosphate fodders and 647.50kg is well mixed in a kettle., adds 426.87kg's
Mother liquor, reaction temperature is 70 DEG C, is added after reaction 1h by the potassium hydrogen sulfate solution that 304.68kg mass percents are 50%, reaction
Temperature is 70 DEG C, and the reaction time is 4h；Reaction is filtered after terminating, and obtains calcium sulfate and filtrate, the loss of phosphorus and potassium in calcium sulfate
Rate is respectively 4.91% and 0.42%；Filtrate carries out condensing crystallizing by after purification, being filtered to remove impurity, gained filtrate, crystallization
Process mixing speed is 100rpm/min, and crystallization temperature is 40 DEG C, after stirred crystallization 6h, is filtrated to get 114.01kg biphosphates
The mother liquor of potassium product and 477.91kg, mother liquor is returned in reactor, is circulated operation；Biphosphate potassium content is in product
98.34%, meet the requirement of potassium dihydrogen phosphate technical grade Grade A.
The above-mentioned description to embodiment is to be understood that and use invention for ease of those skilled in the art.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel announcement of the invention, does not depart from improvement that scope made and modification all should be of the invention
Within protection domain.
Claims (10)
1. a kind of method for producing potassium dihydrogen phosphate, it is characterised in that calcium hydrophosphate fodder is first carried out with PHOSPHORIC ACID TECH.GRADE
Predecomposition is reacted, and adding potassium acid sulfate carries out metathesis reaction, filters out calcium sulfate and filtrate, and purified treatment is carried out to filtrate
After concentrate crystallisation by cooling, prepare potassium dihydrogen phosphate product, crystalline mother solution is circulated behaviour in returning to calcium hydrophosphate fodder
Make, or for the production without chlorine composite fertilizer.
2. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that calcium hydrophosphate fodder and
When PHOSPHORIC ACID TECH.GRADE carries out predecomposition reaction, phosphoric acid is 0.2~0.3 with the mol ratio of calcium monohydrogen phosphate：1.
3. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that calcium hydrophosphate fodder and
When PHOSPHORIC ACID TECH.GRADE carries out predecomposition reaction, reaction temperature is 50 DEG C~70 DEG C, and the reaction time is 1h~2h.
4. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that potassium acid sulfate and feed grade
The potassium phosphorus mol ratio of calcium monohydrogen phosphate is 0.9~1.1：1.
5. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that add the potassium acid sulfate to carry out
During metathesis reaction, reaction temperature is 50 DEG C~70 DEG C, and the reaction time is 2~4h.
6. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that calcium hydrophosphate fodder adds
After water mashing, calcium hydrophosphate fodder slurry is obtained, add PHOSPHORIC ACID TECH.GRADE to carry out predecomposition with calcium hydrophosphate fodder slurry
Reaction；
Or, PHOSPHORIC ACID TECH.GRADE and the mixed phosphoric acid solution of water are mixed with calcium hydrophosphate fodder, carried out while mashing pre-
Decomposition reaction.
7. a kind of method for producing potassium dihydrogen phosphate according to claim 6, it is characterised in that calcium hydrophosphate fodder adds
When water mashing prepares calcium hydrophosphate fodder slurry, the volume that water is added per kilogram of feed calcium hydrophosphate is 2.5~5
Rise.
8. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that when crystalline mother solution is returned to
When being circulated operation in calcium hydrophosphate fodder, crystalline mother solution is returned to through the pretreated calcium hydrophosphate fodder of peroxophosphoric acid
In slurry, potassium hydrogen sulfate solution is added in crystalline mother solution and calcium hydrophosphate fodder slurry mixed liquor；
When crystalline mother solution is used for the production without chlorine composite fertilizer, potassium hydrogen sulfate solution is added directly into pretreated through peroxophosphoric acid
In calcium hydrophosphate fodder slurry.
9. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that described feed grade phosphoric acid
Hydrogen calcium is prepared through three sections of neutralisations by phosphoric acid by wet process.
10. a kind of method for producing potassium dihydrogen phosphate according to claim 1, it is characterised in that described technical grade phosphorus
Acid is thermal phosphoric acid or phosphoric acid by wet process.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188146A (en) * | 2017-07-18 | 2017-09-22 | 禄丰天宝磷化工有限公司 | A kind of production technology of feed grade potassium dihydrogen phosphate |
| CN110697671A (en) * | 2019-11-21 | 2020-01-17 | 江西渠成氟化学有限公司 | Process for producing potassium dihydrogen phosphate by using calcium hydrogen phosphate |
| CN113816351A (en) * | 2021-10-14 | 2021-12-21 | 太仓沪试试剂有限公司 | Preparation method of high-quality monopotassium phosphate |
| CN115092900A (en) * | 2022-06-28 | 2022-09-23 | 新希望化工投资有限公司 | Process for producing potassium dihydrogen phosphate and calcium sulfate whiskers by adopting phosphorite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107188146A (en) * | 2017-07-18 | 2017-09-22 | 禄丰天宝磷化工有限公司 | A kind of production technology of feed grade potassium dihydrogen phosphate |
| CN110697671A (en) * | 2019-11-21 | 2020-01-17 | 江西渠成氟化学有限公司 | Process for producing potassium dihydrogen phosphate by using calcium hydrogen phosphate |
| CN113816351A (en) * | 2021-10-14 | 2021-12-21 | 太仓沪试试剂有限公司 | Preparation method of high-quality monopotassium phosphate |
| CN115092900A (en) * | 2022-06-28 | 2022-09-23 | 新希望化工投资有限公司 | Process for producing potassium dihydrogen phosphate and calcium sulfate whiskers by adopting phosphorite |
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