CN105174238B - A kind of phosphoric acid by wet process prepares dipotassium hydrogen phosphate method - Google Patents
A kind of phosphoric acid by wet process prepares dipotassium hydrogen phosphate method Download PDFInfo
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- CN105174238B CN105174238B CN201510604846.0A CN201510604846A CN105174238B CN 105174238 B CN105174238 B CN 105174238B CN 201510604846 A CN201510604846 A CN 201510604846A CN 105174238 B CN105174238 B CN 105174238B
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- phosphoric acid
- wet process
- dipotassium hydrogen
- hydrogen phosphate
- potassium hydroxide
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Abstract
The present invention relates to phosphoric acid by wet process to prepare phosphate technical field, especially a kind of phosphoric acid by wet process prepares dipotassium hydrogen phosphate method, by being detected and analyzed to the amount of the sulfate radical in phosphoric acid by wet process, add a certain amount of ground phosphate rock thereto again, so that ground phosphate rock reacts with sulfate radical, ammonia is passed through again or adds ammoniacal liquor, by the pH value for adjusting slurry, so that the sulfate radical of phosphoric acid by wet process and substantial amounts of Fe, the cations such as Al and F, the anionic impurities such as Si generation precipitation, after filtering, remove the sulfate radical remained in phosphoric acid by wet process and substantial amounts of Fe, the cations such as Al and F, the anionic impurities such as Si, improve the quality of phosphoric acid by wet process, improve the purity of phosphoric acid by wet process；Add potassium hydroxide thereto again, and the dosage of potassium hydroxide is defined, and then improve the utilization rate of potassium ion, reduce production cost, saved resource.
Description
Technical field
The present invention relates to phosphoric acid by wet process to prepare phosphate technical field, and especially a kind of phosphoric acid by wet process prepares dipotassium hydrogen phosphate
Method.
Background technology
Dipotassium hydrogen phosphate, also known as dikalium phosphate, potassium phosphate,monobasic, it is one of sylvite acid salt of phosphoric acid generation, is colourless
Tetragonal crystal system crystallizes or white crystalline powder.Soluble in water, the aqueous solution is in alkalescence, is slightly soluble in alcohol, there is a hygroscopicity, and temperature is higher
When self-dissolving.Dipotassium hydrogen phosphate is mainly used in medical (penicillin, the nutrient chemical of streptomysin) industry, also acts as the deferrization of talcum powder
Agent, pH adjusting agent etc..
In the prior art, the production of dipotassium hydrogen phosphate is concentrated mainly on liquor kalii caustici neutralising phosphoric acid and is made or uses potassium carbonate
Solution neutralising phosphoric acid and obtain.Wherein, liquor kalii caustici neutralising phosphoric acid is that solid caustic potash is made into 30% aqueous solution, clarified,
Impurity is filtered to remove, is added after metering in corrosion-resistant retort, 50% appropriate phosphoric acid solution is added slowly with stirring, 90
Neutralization reaction, control of reaction end point pH8.5~9.0 are carried out at~100 DEG C (untill just showing red with phenolphthalein indicator).Heating
Concentrated to 120~124 DEG C, insoluble matter is filtered to remove after reaching claimed range to solution concentration.Clear filtrate is cooled to
Less than 20 DEG C separate out crystallization, then are centrifuged, and slightly air-dry, and dipotassium hydrogen phosphate finished product are made, mother liquor returns after filtering to be made
With.Its reaction equation is as follows：
H3PO4+2KOH→K2HPO4+2H2O
It is in the case where being stirred continuously with solution of potassium carbonate neutralising phosphoric acid, solution of potassium carbonate is added anti-in 30% phosphoric acid solution
Should, neutralization terminal is pH value 8.5~9.0 (phenolphthalein indicator just shows red)；Neutralizer is crossed after being concentrated into 120~124 DEG C and filtered out
Insoluble matter is removed, is subsequently cooled to 20~C crystallization below；Centrifuge, be dry that product, mother liquor deliver to neutralization step reuse.Instead
Answer equation as follows：
K2CO3+H3PO4→K2HPO4+H2O+CO2↑
But phosphoric acid is broadly divided into phosphoric acid by wet process and thermal phosphoric acid, because the cost of thermal phosphoric acid is higher so that wet method phosphorus
The production of acid has obtained large range of promotion and application, but, because phosphoric acid by wet process is with phosphorus ore and inorganic acid, according to strong acid
Produce what the principle of weak acid was prepared, and phosphorus ore, according to different qualities, its impurity level contained is also different, method phosphorus
Impurity content in acid is higher, and this not only affects phosphoric acid by wet process and potassium hydroxide or carbonic acid nak response production dipotassium hydrogen phosphate
The quality of product, and also result in the impurity in phosphoric acid by wet process and can be reacted with potassium ion, generate the sediment of complexity, Jin Erzao
Utilization rate into potassium ion is relatively low, adds the cost that phosphoric acid by wet process prepares dipotassium hydrogen phosphate.
It can be seen that the technique that phosphoric acid by wet process is prepared to dipotassium hydrogen phosphate product is improved so that phosphoric acid by wet process prepares phosphoric acid
Yield increase in sylvite product process, purity is higher, reduces the consumption of potassium ion, and it is key as this area to reduce cost
The problem of；Based on this, this researcher combines production practices for many years, and preparing potassium phosphate for phosphoric acid by wet process provides a kind of new think of
Road.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides a kind of phosphoric acid by wet process and prepares phosphoric acid hydrogen
Dipotassium method.
It is achieved particular by following technical scheme：
A kind of phosphoric acid by wet process prepares dipotassium hydrogen phosphate method, comprises the following steps：
(1) phosphoric acid by wet process that phosphorus pentoxide concentration is 15-35% is taken, by analyzing the content of sulfate radical therein, and
Add ground phosphate rock thereto, it with the mass ratio of the content of sulfate radical is (1~1.2) that the addition of ground phosphate rock, which is,:1, treat its reaction
After 30-60min, then ammoniacal liquor being added thereto or is passed through ammonia, regulation pH value is 3~7, filtering, obtains slurry and filter residue；
(2) potassium hydroxide is taken, potassium hydroxide is added in slurry, in the addition and phosphoric acid by wet process that control potassium hydroxide
The mol ratio of the amount of phosphorus pentoxide is 4:1, after the completion for the treatment of that it feeds intake, it is 0-0.01MPa to control vacuum, use temperature for
85-95 DEG C of evaporative crystallization, treat occur a large amount of crystal in solution, stop evaporation, be cooled to room temperature, filter, obtain mother liquor and phosphoric acid hydrogen
Dipotassium.
Described dipotassium hydrogen phosphate, its purity are 98.3-99%.
Described filter residue sends to composite fertilizer production line；Described mother liquor sends to composite fertilizer production line.
Described evaporative crystallization, after caused gas carries out absorption processing using phosphoric acid,diluted in this process, return to step
(1) mixed in phosphoric acid by wet process.
Described phosphoric acid,diluted, its concentration are 15-35%.
The purity of above-mentioned dipotassium hydrogen phosphate, it is that the dipotassium hydrogen phosphate crystal that will be obtained is placed in drier after drying, then
It is sampled analysis.
The most important advantage of the present invention is, uses vacuum to control the supersaturation in solution for 0-0.01MPa size
Degree, control the crystalline rate of dipotassium hydrogen phosphate so that the dipotassium hydrogen phosphate product quality of preparation is more excellent, and purity is higher, and quality is steady
It is fixed.
The granular size of above-mentioned ground phosphate rock is 60-130 mesh.
The content of phosphorus pentoxide in above-mentioned ground phosphate rock must not be less than 9%.
Above-mentioned potassium hydroxide is that solid is added in ammonium phosphate salt solution, or after potassium hydroxide is configured to liquid
Add.
Above-mentioned potassium hydroxide can be replaced using potassium carbonate, can also be replaced using saleratus.
Compared with prior art, technique effect of the invention is embodied in：
By being detected and analyzed to the amount of the sulfate radical in phosphoric acid by wet process, then a certain amount of phosphorus ore is added thereto
Powder so that ground phosphate rock reacts with sulfate radical, then is passed through ammonia or adds ammoniacal liquor, by the pH value for adjusting slurry so that wet method
The anionic impurity such as the cation such as the sulfate radical of phosphoric acid and substantial amounts of Fe, Al and F, Si generation precipitation, after filtering, removes residual
The anionic impurity such as cation and F, Si such as sulfate radical and substantial amounts of Fe, Al in phosphoric acid by wet process, improves phosphoric acid by wet process
Quality, improve the purity of phosphoric acid by wet process；Add potassium hydroxide thereto again, and the dosage of potassium hydroxide be defined,
And then the utilization rate of potassium ion is improved, production cost is reduced, has saved resource.
The present invention under tiny structure environment especially by being evaporated crystallization so that Ammonia valatilization comes out, dipotassium hydrogen phosphate
Product formation, and then improve the crystal formation of dipotassium hydrogen phosphate crystallization, improves the quality of dipotassium hydrogen phosphate so that dipotassium hydrogen phosphate it is pure
Degree reaches 98.3-99%.
The discharge of waste liquid, waste gas, waste residue is not present in the whole technique of the present invention, and the mother liquor reclaimed is used with filter residue is crossed
In the production of composite fertilizer, and it disclosure satisfy that the indices of composite fertilizer；The ammonia evaporated is absorbed with reference to using phosphoric acid,diluted
Return to step 1, and then cause ammonia to be recycled utilization, resource consumption is reduced, reduces the production cost of dipotassium hydrogen phosphate.
Embodiment
Limited with reference to specific embodiment technical scheme is further, but claimed
Scope is not only limited to made description.
The present invention reaction principle be：Sulfate radical is first reacted with ground phosphate rock, formed sulfate insoluble matter, and pass through to
Wherein it is passed through ammonia or adds ammoniacal liquor adjustment pH value so that phosphoric acid is reacted with ammonia or ammoniacal liquor, forms ammonium phosphate salt
Slurry, then ammonium phosphate salt slurry and potassium hydroxide (saleratus or potassium carbonate) are reacted, dipotassium hydrogen phosphate is obtained, specifically
Reaction equation is related to：
SO4 2-+Ca2+→CaSO4
NH4H2PO4+2KOH→K2HPO4+NH3↑+2H2O
NH4H2PO4+2KHCO3→K2HPO4+NH3↑+2CO2↑+2H2O
NH4H2PO4+K2CO3→K2HPO4+NH3↑+CO2↑+H2O
Embodiment 1
A certain amount of phosphoric acid by wet process is taken, the phosphoric acid by wet process phosphorus pentoxide content is 15%, and to the sulphur in phosphoric acid by wet process
Acid group is tested and analyzed, and obtains the content of sulfate radical, is 1 according still further to ground phosphate rock and sulfate radical content ratio:1 adds ground phosphate rock,
After reacting 30min, then it is 3 to add ammoniacal liquor thereto or be passed through ammonia regulation pH, is filtered after the completion of reaction, obtains slurry and filter
Slag, filter residue send to composite fertilizer production line；Potassium hydroxide is slowly added into slurry again, the addition of potassium hydroxide is phosphoric acid by wet process
4 times of the amount of middle phosphorus pentoxide material, after the completion of addition, it is 01MPa to control vacuum, and adjusts after temperature is 85 DEG C and carry out
Evaporative crystallization, and then to control the degree of supersaturation of solution by controlling the size of vacuum, it is further to control in solution
The crystalline rate of dipotassium hydrogen phosphate, and when occurring a large amount of crystal in crystallization process to be evaporated, in solution, stop evaporative crystallization, will
It is cooled to normal temperature environment, by its filtration treatment, obtains mother liquor and dipotassium hydrogen phosphate, mother liquor sends to composite fertilizer production line；Upper
It is the phosphoric acid,diluted that absorption gas uses after being absorbed using phosphoric acid,diluted in return to step 1 to state caused gas in evaporation and crystal process
Concentration be 15%；Above-mentioned ground phosphate rock is 60 mesh, and the content of the phosphorus pentoxide in ground phosphate rock is not less than 13%.It is above-mentioned
Potassium hydroxide to add after it is prepared into solution with water.
Sampling analysis is carried out by being placed in dipotassium hydrogen phosphate obtained above in drier after drying, its result is phosphoric acid
The content of hydrogen dipotassium is 98.3%.
Embodiment 2
A certain amount of phosphoric acid by wet process is taken, the phosphoric acid by wet process is using the concentration that phosphorus pentoxide is counted as 35%, and to phosphoric acid by wet process
In sulfate radical tested and analyzed, obtain the content of sulfate radical, be 1.2 according still further to ground phosphate rock and sulfate radical content ratio:1 adds
Ground phosphate rock, treat that its reaction time reaches 60min, then it is 7 to add ammoniacal liquor thereto or be passed through ammonia regulation pH, then carried out
After filtering, slurry and filter residue are obtained, filter residue sends to composite fertilizer production line；Potassium hydroxide is added into slurry again, potassium hydroxide
Addition is 4 times of the amount of phosphorus pentoxide material in phosphoric acid by wet process, to be slowly added to during potassium hydroxide is added,
After the completion of addition, then it is 0.01MPa to control vacuum, and adjusts after temperature is 95 DEG C and carry out evaporative crystallization, and then to pass through
The size of vacuum is controlled to control the degree of supersaturation of solution, the further crystalline rate for controlling dipotassium hydrogen phosphate in solution,
And when occurring a large amount of crystal in crystallization process to be evaporated, in solution, stop evaporative crystallization, normal temperature environment is cooled to, by it
Filtration treatment, obtains mother liquor dipotassium hydrogen phosphate, and mother liquor sends to composite fertilizer production line；The caused gas in above-mentioned evaporation and crystal process
Body is after being absorbed using phosphoric acid,diluted in return to step 1, and the concentration for the phosphoric acid,diluted that absorption gas uses is 35%；Above-mentioned ground phosphate rock
For 130 mesh, and the content of the phosphorus pentoxide in ground phosphate rock is not less than 9%.
Sampling analysis is carried out by being placed in dipotassium hydrogen phosphate obtained above in drier after drying, its result is phosphoric acid
The content of hydrogen dipotassium is 98.5%.
Embodiment 3
A certain amount of phosphoric acid by wet process is taken, the phosphoric acid by wet process is using the concentration that phosphorus pentoxide is counted as 20%, and to phosphoric acid by wet process
In sulfate radical tested and analyzed, obtain the content of sulfate radical, be 1.1 according still further to ground phosphate rock and sulfate radical content ratio:1 adds
Ground phosphate rock, treat that its reaction time reaches 50min, then it is 5 to add ammoniacal liquor thereto or be passed through ammonia regulation pH, then carried out
After filtering, slurry and filter residue are obtained, filter residue sends to composite fertilizer production line；Potassium hydroxide is added into slurry again, potassium hydroxide
Addition is 4 times of the amount of phosphorus pentoxide material in phosphoric acid by wet process, to be slowly added to during potassium hydroxide is added,
After the completion of addition, then it is 0.005MPa to control vacuum, and adjusts after temperature is 90 DEG C and carry out evaporative crystallization, and then to pass through
The size of vacuum is controlled to control the degree of supersaturation of solution, the further crystalline rate for controlling dipotassium hydrogen phosphate in solution,
And when occurring a large amount of crystal in crystallization process to be evaporated, in solution, stop evaporative crystallization, normal temperature environment is cooled to, by it
Filtration treatment, obtains mother liquor and dipotassium hydrogen phosphate, and mother liquor sends to composite fertilizer production line；Caused by above-mentioned evaporation and crystal process
Gas is after being absorbed using phosphoric acid,diluted in return to step 1, and the concentration for the phosphoric acid,diluted that absorption gas uses is 20%；Above-mentioned phosphorus ore
Powder is 90 mesh, and the content of the phosphorus pentoxide in ground phosphate rock is not less than 17%.Above-mentioned potassium hydroxide is by itself and water system
It is standby into adding after solution.
Sampling analysis is carried out by being placed in dipotassium hydrogen phosphate obtained above in drier after drying, its result is phosphoric acid
The content of hydrogen dipotassium is 98.8%.
Embodiment 4
On the basis of embodiment 1, potassium hydroxide is replaced using saleratus, wherein potassium ion and above-mentioned use
Potassium content in potassium hydroxide is equal.
Embodiment 5
On the basis of embodiment 1, potassium hydroxide is replaced using potassium carbonate, wherein potassium ion and the hydrogen of above-mentioned use
Potassium content in potassium oxide is equal.
Embodiment 6
On the basis of embodiment 2, potassium hydroxide is replaced using potassium bicarbonate solution, wherein potassium ion is adopted with above-mentioned
Potassium content in potassium hydroxide is equal.
Embodiment 7
On the basis of embodiment 2, potassium hydroxide is replaced using solution of potassium carbonate, wherein potassium ion and above-mentioned use
Potassium hydroxide in potassium content it is equal.
Claims (4)
1. a kind of phosphoric acid by wet process prepares dipotassium hydrogen phosphate method, it is characterised in that comprises the following steps：
(1) take the phosphoric acid by wet process that phosphorus pentoxide concentration is 15-35%, by analyzing the content of sulfate radical therein, and to its
Middle addition ground phosphate rock, it with the mass ratio of the content of sulfate radical is (1~1.2) that the addition of ground phosphate rock, which is,:1, treat that it reacts 30-
After 60min, then ammoniacal liquor being added thereto or is passed through ammonia, regulation pH value is 5~7, filtering, obtains slurry and filter residue；
(2) take potassium hydroxide, potassium hydroxide be added in slurry, control potassium hydroxide addition and phosphoric acid by wet process in five oxygen
The mol ratio for changing the amount of two phosphorus is 4:1, after the completion for the treatment of that it feeds intake, it is 0-0.01MPa to control vacuum, uses temperature as 85-95
DEG C evaporative crystallization, the tail gas being evaporated are washed with a certain amount of phosphoric acid,diluted, treat occur a large amount of crystal in solution, stop evaporation,
Room temperature is cooled to, filters, obtains mother liquor and dipotassium hydrogen phosphate；
Described evaporative crystallization, after caused gas carries out absorption processing using phosphoric acid,diluted in this process, in return to step (1)
Mixed with phosphoric acid by wet process.
2. phosphoric acid by wet process as claimed in claim 1 prepares dipotassium hydrogen phosphate method, it is characterised in that described phosphoric acid hydrogen two
Potassium, its purity are 98.3-98.8%.
3. phosphoric acid by wet process as claimed in claim 1 prepares dipotassium hydrogen phosphate method, it is characterised in that described filter residue is sent to multiple
Hefei production line；Described mother liquor sends to composite fertilizer production line.
4. phosphoric acid by wet process as claimed in claim 1 prepares dipotassium hydrogen phosphate method, it is characterised in that described phosphoric acid,diluted, its
Concentration is 15-35%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079205A (en) * | 1993-05-13 | 1993-12-08 | 王昌志 | The method of producing trisodium phosphate and ammonium salt by metathesis |
| CN1174812A (en) * | 1996-08-26 | 1998-03-04 | 四川联合大学 | Industrial monoammonium phosphate and productive method for industrial monoammunium phosphate and calcium hydrogen phosphate fodder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100528744C (en) * | 2007-07-30 | 2009-08-19 | 四川宏达股份有限公司 | Technique for preparing sodium pyrophosphate from wet method phosphoric acid |
| CN101613095B (en) * | 2009-08-07 | 2011-03-30 | 中国-阿拉伯化肥有限公司 | Method for producing ammonium polyphosphate by using wet phosphoric acid |
| CN102942166A (en) * | 2012-11-14 | 2013-02-27 | 贵州开磷（集团）有限责任公司 | Method for preparing toothpaste/food/medicine grade calcium hydrophosphate from phosphoric acid by wet process |
| CN102963874B (en) * | 2012-11-26 | 2015-04-15 | 贵州川恒化工有限责任公司 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079205A (en) * | 1993-05-13 | 1993-12-08 | 王昌志 | The method of producing trisodium phosphate and ammonium salt by metathesis |
| CN1174812A (en) * | 1996-08-26 | 1998-03-04 | 四川联合大学 | Industrial monoammonium phosphate and productive method for industrial monoammunium phosphate and calcium hydrogen phosphate fodder |
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