CN113086957A - Method for producing ammonium dihydrogen phosphate - Google Patents
Method for producing ammonium dihydrogen phosphate Download PDFInfo
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- CN113086957A CN113086957A CN202110485552.6A CN202110485552A CN113086957A CN 113086957 A CN113086957 A CN 113086957A CN 202110485552 A CN202110485552 A CN 202110485552A CN 113086957 A CN113086957 A CN 113086957A
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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
- C01B25/28—Ammonium phosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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Abstract
The invention provides a method for producing ammonium dihydrogen phosphate, which relates to the technical field of ammonium dihydrogen phosphate production and comprises the following steps: step 1, reacting sulfuric acid and ammonium bisulfate with phosphate concentrate powder and water, wherein the molar ratio of the ammonium bisulfate to the phosphate concentrate powder is 3: 1, obtaining a reaction solution, and filtering the reaction solution to obtain a first filtrate and a first filter cake; step 2, adding ammonia into the first filtrate, adjusting the pH value of the obtained mixed solution to 1-2.5, and then filtering to obtain a second filtrate; and 3, adding ammonium sulfide into the second filtrate for reaction, wherein the molar ratio of the ammonium sulfide to the ammonium bisulfate is 1.3: 6, then adding ammonia to enable the pH value of the mixed solution to be 4-4.5, and filtering to obtain a third filtrate; and 4, evaporating and crystallizing the third filtrate, and separating crystals in the obtained crystallization liquid to obtain ammonium dihydrogen phosphate, so that the fluorine content is greatly reduced, and the production cost is saved.
Description
Technical Field
The invention relates to the technical field of ammonium dihydrogen phosphate production, in particular to a method for producing ammonium dihydrogen phosphate.
Background
At present, ammonium dihydrogen phosphate is produced mainly by adopting a neutralization slurry concentration process, namely, phosphate rock powder is firstly decomposed by sulfuric acid, crude phosphoric acid is separated out, then phosphoric acid is prepared after purification, then ammonia gas is introduced for neutralization to obtain ammonium dihydrogen phosphate slurry, and evaporation concentration and cooling are carried out after impurity removalCrystallizing to obtain industrial-grade ammonium dihydrogen phosphate, neutralizing P (as P) in slag2O5Calculated) and the content of N can not reach the standard of agricultural ammonium dihydrogen phosphate (namely, the total nutrient is more than or equal to 55 percent, the N is more than or equal to 10 percent, and the P is less than or equal to2O5Not less than 45 percent), mixing with dilute phosphoric acid after size mixing, and introducing ammonia gas to prepare agricultural ammonium dihydrogen phosphate.
Therefore, the production process cost of the ammonium dihydrogen phosphate is high at present, and meanwhile, the produced agricultural ammonium dihydrogen phosphate has high fluorine content and has the problem of pollution to soil.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for producing ammonium dihydrogen phosphate, which greatly reduces the fluorine content and saves the production cost.
The invention is realized by the following technical scheme:
a method for producing ammonium dihydrogen phosphate, comprising the steps of:
step 1, reacting sulfuric acid and ammonium bisulfate with phosphate concentrate powder and water, wherein the molar ratio of the ammonium bisulfate to the phosphate concentrate powder is 3: 1, obtaining a reaction solution, and filtering the reaction solution to obtain a first filtrate and a first filter cake;
step 2, adding ammonia into the first filtrate, adjusting the pH value of the obtained mixed solution to 1-2.5, and then filtering to obtain a second filtrate;
and 3, adding ammonium sulfide into the second filtrate for reaction, wherein the molar ratio of the ammonium sulfide to the ammonium bisulfate is 1.3: 6, then adding ammonia to enable the pH value of the mixed solution to be 4-4.5, and filtering to obtain a third filtrate;
and 4, evaporating and crystallizing the third filtrate, and separating crystals in the obtained crystallization liquid to obtain ammonium dihydrogen phosphate.
Preferably, the sulfuric acid and the ammonium bisulfate react with the phosphate concentrate powder and the water at the temperature of 80-85 ℃ in the step 1.
Further, sulfuric acid, ammonium bisulfate, phosphate concentrate powder and water react for 6-8h at the temperature.
Preferably, the washing liquid after the first cake washing is returned to the reaction of step 1, and thereafter, the subsequent processes are continued.
Preferably, the molar ratio of the sulfuric acid to the ammonium bisulfate to the phosphate concentrate powder to the water in the step 1 is (4-6): 6: 2: (7.5-15).
Further, adding phosphate concentrate powder into the first filtrate for desulfurization reaction, wherein the mass of the phosphate concentrate powder is 10% of that of the phosphate concentrate powder in the step 1, so as to obtain a mixed system, and then adding ammonia into the filtrate obtained by filtering the mixed system for the process of the step 2.
Further, a filter cake obtained by filtering the mixed system is returned to the reaction of the step 1, and then the subsequent processes are continued.
Preferably, step 4 evaporates the third filtrate at 90 ℃.
Preferably, step 4 is to cool the concentrated solution obtained by evaporation to 25 ℃ for crystallization.
Preferably, the crystallization liquid is centrifuged in step 4 to obtain ammonium dihydrogen phosphate.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a method for producing ammonium dihydrogen phosphate, which comprises the steps of firstly reacting sulfuric acid and ammonium bisulfate with phosphate concentrate powder and water, wherein the sulfuric acid and the ammonium bisulfate react with the phosphate concentrate powder and the water by the following reaction Ca5F(PO4)3+3NH4HSO4+2H2SO4+5nH2O＝5CaSO4.nH2O+3NH4H2PO4+ HF, SiO carried in phosphate concentrate powder2The metal oxide and the metal carbonate are dissolved, and the side reaction equation is as follows: 6HF + SiO2＝H2SiF6+2H2O，Fe2O3+3H2SO4＝Fe2(SO4)3+3H2O，Al2O3+3H2SO4＝Al2(SO4)3+3H2O，CaCO3+H2SO4＝CaSO4+H2O+CO2，MgCO3+H2SO4＝MgSO4+H2O+CO2Thus phosphorus concentrateCompletely removing the powder, adding ammonia to the first filtrate, and adjusting pH of the obtained mixture to 1-2.5 at which CaF is due to solubility product2、MgF2Can be separated out, so that the impurities can be removed, and after the precipitation is completed, the fluoride filter residue (namely CaF) can be removed by filtering2、MgF2) Adding ammonium sulfide into the second filtrate, regulating and controlling the molar ratio of ammonium sulfide to ammonium bisulfate, and adding ammonia to adjust the pH value of the mixed solution to 4-4.5, wherein Fe2S3Will separate out, the aluminum ion will be hydrolyzed to generate Al (OH)3，H2SiF6Can generate complicated changes to form SiO2Since the silicon impurities are at pH>When 4, it will be SiO2And (4) separating out in a form, removing impurities for the second time, filtering after complete precipitation to obtain filtrate containing ammonium dihydrogen phosphate, evaporating, crystallizing, and separating crystals in the obtained crystallization liquid to obtain the ammonium dihydrogen phosphate. The invention uses the mixture of sulfuric acid and ammonium bisulfate to react with the phosphate concentrate powder to obtain the ammonium dihydrogen phosphate solution in one step, and compared with the existing wet-process phosphoric acid slurry neutralization and concentration process by introducing ammonia gas, the production cost is saved.
Drawings
FIG. 1 is a flow chart of the present invention for producing ammonium dihydrogen phosphate.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention discloses a method for producing low-fluorine ammonium dihydrogen phosphate with low cost, which comprises the following steps as shown in figure 1:
1) reacting 98% by mass of sulfuric acid solution and ammonium bisulfate with phosphate concentrate powder and water, wherein the molar ratio of the sulfuric acid to the ammonium bisulfate to the phosphate concentrate powder to the water in the sulfuric acid solution is (4-6): 6: 2: (7.5-15), filtering the reaction solution to obtain a filtrate A and a filter cake A;
in the industrial production, the phosphorus concentrate slurry containing the above-mentioned content of phosphorus concentrate powder is used;
the main reaction equation is as follows:
Ca5F(PO4)3+3NH4HSO4+2H2SO4+5nH2O＝5CaSO4.nH2O+3NH4H2PO4+HF
SiO carried in phosphate concentrate powder2The metal oxide and the metal carbonate are dissolved, and the side reaction equation is as follows:
6HF+SiO2＝H2SiF6+2H2O
Fe2O3+3H2SO4＝Fe2(SO4)3+3H2O
Al2O3+3H2SO4＝Al2(SO4)3+3H2O
CaCO3+H2SO4＝CaSO4+H2O+CO2
MgCO3+H2SO4＝MgSO4+H2O+CO2
2) the product of the washed filter cake A is gypsum, the washing liquid returns to the reaction of 1) for continuous circulation, and because the ammonium dihydrogen phosphate has strong water solubility, the filter cake A contains a certain amount of water, so that the filter cake A can not avoid containing ammonium dihydrogen phosphate and other impurities and can be recycled;
in order to avoid sulfuric acid which is not completely reacted in the step 1), adding phosphate concentrate powder into the filtrate A for desulfurization reaction, wherein the mass of the phosphate concentrate powder is 10 percent of that of the phosphate concentrate powder in the step 1), filtering after complete reaction to obtain filtrate B and filter cake B, carrying out subsequent process on the filtrate B, and the filter cake B contains an unreacted substance SiO2Returning to the reaction of 1) for continuous circulation;
the reaction equation for this step is as follows:
Fe2O3+3H2SO4＝Fe2(SO4)3+3H2O
Al2O3+3H2SO4＝Al2(SO4)3+3H2O
CaCO3+H2SO4＝CaSO4+H2O+CO2
MgCO3+H2SO4＝MgSO4+H2O+CO2
3) adding ammonia into the filtrate B, adjusting pH to 1-2.5, at which CaF is due to solubility product2、MgF2Separating out to remove impurities, precipitating completely, filtering to obtain filtrate C, and filtering to obtain fluoride (CaF)2、MgF2)。
Liquid ammonia is generally used in experiments, and ammonia is used in industrial production.
4) Adding ammonium sulfide into the filtrate C, wherein the ratio of the ammonium sulfide to the ammonium bisulfate in the filtrate C is 1.3 mol:6mol, adding ammonia to adjust the pH value of the mixed solution to 4-4.5, Fe2S3Will separate out, the aluminum ion will be hydrolyzed to generate Al (OH)3Silicon impurity at pH>When 4, it will be SiO2Separating out, removing impurities for the second time, precipitating completely, filtering to obtain filtrate D, and collecting the residue as Fe2S3、Al(OH)3And SiO2。
5) Evaporating and concentrating the filtrate D, cooling and crystallizing, pumping into a centrifugal machine by a pump for centrifugal separation to obtain a product ammonium dihydrogen phosphate, recovering evaporated secondary condensed water as washing water, and washing the filter cake A obtained in the step 2).
In particular, the amount of the solvent to be used,
the invention relates to a method for producing low-fluorine ammonium dihydrogen phosphate with low cost, which comprises the following steps:
1) adding 98 mass percent of sulfuric acid solution, ammonium bisulfate and water into the phosphate concentrate powder, wherein the ratio of the phosphate concentrate powder, the ammonium bisulfate, the sulfuric acid and the water is 2mol:6mol (4-6 mol): (7.5-15) mol, stirring and reacting for 6-8h at the reaction temperature of 80-85 ℃, and filtering the reaction liquid to obtain a filtrate A and a filter cake A.
2) Washing the filter cake A to obtain gypsum, and returning the washing liquid to the reaction of 1) for continuous circulation;
adding phosphate concentrate powder into the filtrate A for desulfurization reaction, wherein the mass of the phosphate concentrate powder is 1) 10% of that of the phosphate concentrate powder, filtering after complete reaction to obtain filtrate B and a filter cake B, performing subsequent process on the filtrate B, and returning the filtrate B to the reaction of 1) for continuous circulation;
3) adding ammonia into the filtrate B, adjusting pH to 1-2.5, precipitating completely, filtering to obtain filtrate C, and filtering to obtain CaF as filter residue2、MgF2。
4) Adding ammonium sulfide into the filtrate C to react for 10-30 min, wherein the ratio of the ammonium sulfide to the ammonium bisulfate in the filtrate 1) is 1.3 mol:6mol, adding liquid ammonia to adjust the pH value of the mixed solution to 4-4.5, filtering to obtain filtrate D, wherein the filter residue is Fe2S3、Al(OH)3And SiO2。
5) Evaporating the filtrate D under reduced pressure at the evaporation temperature of 90 ℃, cooling to 25 ℃ for crystallization, then performing centrifugal separation, manually pouring the filtrate D into a centrifugal machine for centrifugal separation during experiments, pumping the filtrate D into the centrifugal machine during industrialization, and drying to obtain ammonium dihydrogen phosphate with the quality meeting the industrial standard HG/T4133-2010; the secondary condensed water evaporated is recovered as washing water, and the filter cake A obtained in the step 2) is washed.
Example 1
The invention relates to a method for producing low-fluorine ammonium dihydrogen phosphate with low cost, which comprises the following steps:
1) adding 98 mass percent of sulfuric acid solution, ammonium bisulfate and water into the phosphate concentrate powder, wherein the molar numbers of the phosphate concentrate powder, the ammonium bisulfate, the sulfuric acid and the water are respectively 2mol, 6mol, 4mol and 7.5mol, stirring and reacting for 6 hours, reacting at the temperature of 85 ℃, and filtering the reaction liquid to obtain filtrate A and filter cake A.
2) Washing the filter cake A to obtain gypsum, and returning the washing liquid to the reaction of 1) for continuous circulation;
adding phosphate concentrate powder into the filtrate A for desulfurization reaction, wherein the mass of the phosphate concentrate powder is 1) 10% of that of the phosphate concentrate powder, filtering after complete reaction to obtain filtrate B and a filter cake B, performing subsequent process on the filtrate B, and returning the filtrate B to the reaction of 1) for continuous circulation;
3) adding liquid ammonia into the filtrate B,adjusting pH to 1, precipitating completely, filtering to obtain filtrate C, and filtering to obtain filter residue CaF2、MgF2。
4) Adding 1.3mol ammonium sulfide into the filtrate C, reacting for 10min, adding ammonia solution to adjust pH of the mixed solution to 4, filtering to obtain filtrate D, and the filter residue is Fe2S3、Al(OH)3And SiO2。
5) Evaporating the filtrate D under reduced pressure at the evaporation temperature of 90 ℃, cooling to 25 ℃ for crystallization, then performing centrifugal separation, manually pouring the filtrate D into a centrifugal machine for centrifugal separation during experiments, pumping the filtrate D into the centrifugal machine during industrialization, and drying to obtain ammonium dihydrogen phosphate with the quality meeting the industrial standard HG/T4133-2010; the secondary condensed water evaporated is recovered as washing water, and the filter cake A obtained in the step 2) is washed.
Example 2
The invention relates to a method for producing low-fluorine ammonium dihydrogen phosphate with low cost, which comprises the following steps:
1) adding 98 mass percent of sulfuric acid solution, ammonium bisulfate and water into the phosphate concentrate powder, wherein the molar numbers of the phosphate concentrate powder, the ammonium bisulfate, the sulfuric acid and the water are respectively 2mol, 6mol, 5mol and 10mol, stirring and reacting for 7 hours, reacting at the temperature of 83 ℃, and filtering the reaction liquid to obtain filtrate A and filter cake A.
2) Washing the filter cake A to obtain gypsum, and returning the washing liquid to the reaction of 1) for continuous circulation;
adding phosphate concentrate powder into the filtrate A for desulfurization reaction, wherein the mass of the phosphate concentrate powder is 1) 10% of that of the phosphate concentrate powder, filtering after complete reaction to obtain filtrate B and a filter cake B, performing subsequent process on the filtrate B, and returning the filtrate B to the reaction of 1) for continuous circulation;
3) adding liquid ammonia into the filtrate B, adjusting pH to 2, precipitating completely, filtering to obtain filtrate C, and filtering to obtain CaF as filter residue2、MgF2。
4) Adding 1.3mol ammonium sulfide into the filtrate C, reacting for 20min, adding ammonia solution to adjust pH of the mixed solution to 4.5, filtering to obtain filtrate D, and the filter residue is Fe2S3、Al(OH)3And SiO2。
5) Evaporating the filtrate D under reduced pressure at the evaporation temperature of 90 ℃, cooling to 25 ℃ for crystallization, then performing centrifugal separation, manually pouring the filtrate D into a centrifugal machine for centrifugal separation during experiments, pumping the filtrate D into the centrifugal machine during industrialization, and drying to obtain ammonium dihydrogen phosphate with the quality meeting the industrial standard HG/T4133-2010; the secondary condensed water evaporated is recovered as washing water, and the filter cake A obtained in the step 2) is washed.
Example 3
The invention relates to a method for producing low-fluorine ammonium dihydrogen phosphate with low cost, which comprises the following steps:
1) adding 98 mass percent of sulfuric acid solution, ammonium bisulfate and water into the phosphate concentrate powder, wherein the molar numbers of the phosphate concentrate powder, the ammonium bisulfate, the sulfuric acid and the water are respectively 2mol, 6mol and 15mol, stirring and reacting for 8 hours, the reaction temperature is 80 ℃, and filtering the reaction liquid to obtain filtrate A and filter cake A.
2) Washing the filter cake A to obtain gypsum, and returning the washing liquid to the reaction of 1) for continuous circulation;
adding phosphate concentrate powder into the filtrate A for desulfurization reaction, wherein the mass of the phosphate concentrate powder is 1) 10% of that of the phosphate concentrate powder, filtering after complete reaction to obtain filtrate B and a filter cake B, performing subsequent process on the filtrate B, and returning the filtrate B to the reaction of 1) for continuous circulation;
3) adding liquid ammonia into the filtrate B, adjusting pH to 2.5, precipitating completely, filtering to obtain filtrate C, and filtering to obtain CaF as filter residue2、MgF2。
4) Adding 1.3mol ammonium sulfide into the filtrate C, reacting for 30min, adding liquid ammonia to adjust pH of the mixed solution to 4.5, filtering to obtain filtrate D, wherein the filter residue is Fe2S3、Al(OH)3And SiO2。
5) Evaporating the filtrate D under reduced pressure at the evaporation temperature of 90 ℃, cooling to 25 ℃ for crystallization, then performing centrifugal separation, manually pouring the filtrate D into a centrifugal machine for centrifugal separation during experiments, pumping the filtrate D into the centrifugal machine during industrialization, and drying to obtain ammonium dihydrogen phosphate with the quality meeting the industrial standard HG/T4133-2010; the secondary condensed water evaporated is recovered as washing water, and the filter cake A obtained in the step 2) is washed.
Claims (10)
1. A method for producing ammonium dihydrogen phosphate, which is characterized by comprising the following steps:
step 1, reacting sulfuric acid and ammonium bisulfate with phosphate concentrate powder and water, wherein the molar ratio of the ammonium bisulfate to the phosphate concentrate powder is 3: 1, obtaining a reaction solution, and filtering the reaction solution to obtain a first filtrate and a first filter cake;
step 2, adding ammonia into the first filtrate, adjusting the pH value of the obtained mixed solution to 1-2.5, and then filtering to obtain a second filtrate;
and 3, adding ammonium sulfide into the second filtrate for reaction, wherein the molar ratio of the ammonium sulfide to the ammonium bisulfate is 1.3: 6, then adding ammonia to enable the pH value of the mixed solution to be 4-4.5, and filtering to obtain a third filtrate;
and 4, evaporating and crystallizing the third filtrate, and separating crystals in the obtained crystallization liquid to obtain ammonium dihydrogen phosphate.
2. The method for producing ammonium dihydrogen phosphate according to claim 1, wherein said sulfuric acid and ammonium bisulfate in step 1 are reacted with phosphate concentrate powder and water at 80-85 ℃.
3. The method for producing ammonium dihydrogen phosphate according to claim 2, wherein sulfuric acid, ammonium bisulfate, phosphate concentrate powder and water are reacted at said temperature for 6-8 h.
4. The method for producing ammonium dihydrogen phosphate according to claim 1, wherein the washing liquid after washing the first filter cake is returned to the reaction in step 1, after which the subsequent processes are continued.
5. The method for producing ammonium dihydrogen phosphate according to claim 1, wherein the molar ratio of said sulfuric acid, ammonium bisulfate, phosphate concentrate powder and water in step 1 is (4-6): 6: 2: (7.5-15).
6. The method for producing ammonium dihydrogen phosphate according to claim 5, wherein said method comprises adding phosphate concentrate powder to said first filtrate to conduct desulfurization, wherein the phosphate concentrate powder is 10% by weight of the phosphate concentrate powder obtained in step 1, to obtain a mixed system, and then adding ammonia to said filtrate obtained by filtering said mixed system to conduct the process of step 2.
7. The method for producing ammonium dihydrogen phosphate according to claim 6, wherein the filter cake obtained by filtering the mixed system is returned to the reaction in step 1, after which the subsequent processes are continued.
8. The method for producing ammonium dihydrogen phosphate according to claim 1, wherein step 4 comprises evaporating the third filtrate at 90 ℃.
9. The method for producing ammonium dihydrogen phosphate according to claim 1, wherein step 4 comprises cooling the concentrated solution obtained by evaporation to 25 ℃ for crystallization.
10. The method for producing ammonium dihydrogen phosphate according to claim 1, wherein step 4 comprises centrifuging the crystallized solution to obtain ammonium dihydrogen phosphate.
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