CN103011113B - Method for co-producing industrial grade diammonium phosphate during production of industrial grade monoammonium phosphate of phosphoric acid by wet process - Google Patents
Method for co-producing industrial grade diammonium phosphate during production of industrial grade monoammonium phosphate of phosphoric acid by wet process Download PDFInfo
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- CN103011113B CN103011113B CN201210575796.4A CN201210575796A CN103011113B CN 103011113 B CN103011113 B CN 103011113B CN 201210575796 A CN201210575796 A CN 201210575796A CN 103011113 B CN103011113 B CN 103011113B
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- phosphoric acid
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Abstract
The invention discloses a method for co-producing industrial grade diammonium phosphate during the production of industrial grade monoammonium phosphate of phosphoric acid by a wet process. The method comprises the steps of: making filtrate obtained after carrying out desulfurization on calcium hydrophosphate and wet-process phosphoric acid neutralize with ammonia gas or ammonia water to obtain ammonium phosphate slurry, making ammonium sulfide react with the ammonium phosphate slurry, and concentrating, crystallizing and drying the filtrate to obtain an industrial grade monoammonium phosphate product; secondly, making a primary mother solution obtained through filtering after crystallizing secondarily neutralize with the ammonia gas or ammonia water; and finally, concentrating, crystallizing and drying the filtrate obtained through secondary neutralizing to obtain an industrial grade diammonium phosphate product, and returning a secondary mother solution obtained through filtering after crystallizing to a concentrating tank and continuously concentrating. The method is used for co-producing the diammonium phosphate during the production of the monoammonium phosphate, has the advantages of saving production cost, reducing energy consumption, reducing pollution and ensuring quality of the monoammonium phosphate and the diammonium phosphate through effective impurity removal, and has good economic benefits.
Description
Technical field
The present invention relates to the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammonium.
Background technology
Industrial grade monoammonium phosphate and diammonium phosphate all have a wide range of applications in fire-fighting, drip irrigation fertilizer, medicine and food etc.The production of current industrial level monoammonium phosphate and diammonium phosphate is all generally adopt thermal phosphoric acid or purifying phosphoric acid technique, and shortcoming is that production cost is high, technique is more complicated, energy consumption is high, pollution is large.There is part producer also to adopt wet method phosphoric acid manufacture process, but there is some problems at dedoping step, as in product, metal content is high, can, along with phosphoric acid quality change, make quality product be difficult to ensure.In the prior art, production equipment and the production technique of technical grade phosphorus ammonium are comparatively single, can only manufacture level monoammonium phosphate or PHOSPHORIC ACID TECH.GRADE two ammonium, and do not realize the technique of industrial grade monoammonium phosphate coproduction PHOSPHORIC ACID TECH.GRADE two ammonium.
Summary of the invention
The object of the present invention is to provide the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammonium, solve in prior art and produce monoammonium phosphate, features of DAP production cost and energy consumption is high, it is large to pollute, problem that is unstable product quality.
The object of the invention is to be achieved through the following technical solutions.
The method of preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammonium, that phosphoric acid is raw material in a wet process, concentrated after series of chemical, crystallization, dry obtained monoammonium phosphate and diammonium phosphate, it is characterized in that: the filtrate obtained after carrying out desulphurization reaction with secondary calcium phosphate and phosphoric acid by wet process and ammonia or ammoniacal liquor carry out neutralization reaction, obtain phosphor ammonium slurry, with ammonium sulfide and phosphor ammonium slurry reaction gained filtrate concentrated again, crystallization, drying obtains industrial grade monoammonium phosphate product, then mother liquor crystallization and filtration obtained and ammonia or ammoniacal liquor carry out Two-step neutralization reaction, the concentrating filter liquor finally Two-step neutralization obtained, crystallization, drying obtains PHOSPHORIC ACID TECH.GRADE two ammonium product, the secondary mother liquid that crystallization and filtration obtains returns in thickener and continues to concentrate, described Production Flow Chart is:
(1) desulfurization: phosphoric acid by wet process is warming up to 60 ~ 80 DEG C in desulfurizer, adds secondary calcium phosphate, filters after stirring reaction 30 ~ 60min, and filter cake is that calcium sulfate is delivered to special stockyard, and filtrate is that neutralizing well is sent in desulfurization acid;
(2) in and removal of impurities: add ammonia or ammoniacal liquor in the desulfurization phosphoric acid in neutralizing well under whipped state, the pH value of solution is neutralized to 3.9 ~ 4.3, while hot by slurry filtration, filter cake is that agricultural grade phosphorus ammonium delivers to compound fertilizer facility production energy composite fertilizer, and filtrate is that phosphor ammonium slurry delivers to purification tank;
(3) purify: in purification tank, add ammonium sulfide stirring reaction, through centrifugation filter residue after the assay was approved, filtrate sends into thickener A;
(4) one ammonium condensing crystals: the slip after purification is concentrated into slip proportion to 1.30 ~ 1.35 with steam in thickener A, send in crystallisation by cooling groove A and be cooled to less than the 40 DEG C crystallizations of slurry temperature value, slurry filtration after crystallization is separated and obtains a mother liquor and crystal, crystal is sent into drying machine A inner drying and is obtained industrial grade monoammonium phosphate product, and one time mother liquor is sent in secondary and groove;
(5) Two-step neutralization: add ammonia or ammoniacal liquor in time mother liquor of in Two-step neutralization groove, regulates pH=7.9 ~ 8.0, after pH value is stable, send into thickener B;
(6) two ammonium condensing crystals: the slip of Two-step neutralization is concentrated into slip proportion in the scope of 1.25 ~ 1.30 with steam in thickener B, send in crystallisation by cooling groove B and be cooled to slurry temperature crystallization below 40 DEG C, slip after crystallization is separated by filtration and obtains secondary mother liquid and crystal, crystal is sent into drying machine inner drying and is obtained PHOSPHORIC ACID TECH.GRADE two ammonium product, and secondary mother liquid then returns in thickener B and continues to concentrate.
In described step (1), phosphoric acid is P
2o
5concentration 20 ~ 35% phosphoric acid by wet process.
Before adding secondary calcium phosphate, need first sampling analysis wherein sulfate radical content in described step (1), the add-on of secondary calcium phosphate is 0.85 ~ 1.0 times of sulfate radical amount.
Detecting qualified method before centrifugal in described step (3) is dark solution filtered, and drips ammonium sulfide, when solution no longer shows black and qualified in filtrate.
Negative pressure is adopted to concentrate in described step (6) during two ammonium condensing crystals, the ammonia that in the ammonia of overflowing in concentration process and step (5), Two-step neutralization overflow need absorb with phosphoric acid washing, with removal of impurities operation in carrying out in the neutralizing well that the slip after absorption delivers to step (2).
According to the character of ammonification slip, at the PH of slurry solution in 4.0 ~ 4.5 scopes, impurity in phosphoric acid and ammonia and phosphoric acid generation chemical reaction can generate a series of insoluble compound, just the impurity in phosphoric acid can be removed after filtration, the industrial grade monoammonium phosphate that filtrate monoammonium phosphate slip is clean, concentrated again.Isolate an industrial ammonium mother liquor and neutralize to obtain PHOSPHORIC ACID TECH.GRADE two ammonium through further ammonia.In the present invention, the main chemical reaction occurred is the generation of monoammonium phosphate and diammonium phosphate, and reaction equation is:
H
3PO
4＋NH
3=NH
4H
2PO
4
H
3PO
4＋NH
3=（NH
4）
2HPO
4
Beneficial effect of the present invention: produce monoammonium phosphate co-producing diammonium phosphate, saved production cost, reduced energy consumption, reduced pollution, ensure that the quality of monoammonium phosphate and diammonium phosphate through effective removal of impurities, there is good economic benefit.Adopt secondary calcium phosphate and wet-process phosphoric acid reaction to remove sulfate radical, while removing impurity, the phosphate radical in secondary calcium phosphate is converted into phosphoric acid, finally generates ammonium phosphate salt, not only can not introduce impurity and also create good economic benefit.Adopt ammonium sulfide desulfurization can remove the heavy metal such as arsenic, lead in phosphoric acid by wet process and partly other metallic cations further, improve the quality of products.In process of production, filter residue after neutralization can be used for fertilizer grade monoammonium phosphate and produces, and purification slag can be used for extracting metal, and one time mother liquor continues to add in ammonia or liquefied ammonia and manufacture level diammonium phosphate, secondary mother liquid returns crystal system recycle and reclaims, without waste residue, discharging of waste liquid.With manufacture level diammonium phosphate in utilizing manufacture level monoammonium phosphate mother liquor to continue, technical grade two ammonium production cost can be reduced.In and, in heating evaporation, crystallisation by cooling process, the effusion of ammonia is all recycled, and does not have ammonia to overflow in process of production, greatly reduces ammonia loss, and can not impact human body and environment.Coproduction PHOSPHORIC ACID TECH.GRADE two ammonium on the basis of manufacture level monoammonium phosphate, increases product diversity, in similar production, enhances competitive power.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention;
Fig. 2 is equipment flowsheet of the present invention;
In figure: 1-desulfurizer, 2-neutralizing well, 3-purification tank, 4-thickener A, 5-crystallisation by cooling groove A, 6-drying machine A, 7-Two-step neutralization groove, 8-thickener B, 9-crystallisation by cooling groove B, 10-drying machine B.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with drawings and Examples, the present invention is described in further detail, but do not form limiting the scope of the present invention.
Fig. 1 is general flow chart of the present invention, and Fig. 2 is equipment flowsheet of the present invention.As shown in Figure 1 and Figure 2, the present invention filters after carrying out desulphurization reaction in secondary calcium phosphate and phosphoric acid by wet process feeding desulfurizer 1, and gained filtrate enters in neutralizing well 2 carries out neutralization reaction with ammonia or ammoniacal liquor; Again filtering the filtrate obtained enters in purification tank 3, react with the ammonium sulfate added and filter, the filtrate obtained is delivered in thickener A4 and is carried out concentrated rear feeding crystallisation by cooling groove A5 crystallization, and the crystal obtained is delivered to the process of drying machine A6 inner drying and obtained industrial grade monoammonium phosphate finished product; The liquid obtained is a mother liquor, deliver in Two-step neutralization groove 7 and carry out Two-step neutralization reaction with ammonia or ammoniacal liquor, the filtrate obtained is delivered in thickener B8 concentrated, deliver to again in crystallisation by cooling groove B9 through crystallisation by cooling, gained crystal is delivered to the process of drying machine B10 inner drying after filtering and is obtained PHOSPHORIC ACID TECH.GRADE two ammonium product, gained filtrate is secondary mother liquid, delivers in thickener B8 and continues to concentrate.
Embodiment 1
By P
2o
5concentration is in the phosphoric acid by wet process feeding desulfurizer of 25%, sampling analysis is sulfate radical content wherein, the add-on of secondary calcium phosphate is 0.85 ~ 1.0 times of sulfate radical amount, adding after secondary calcium phosphate carries out desulphurization reaction sends in neutralizing well by filtrate, ammonia is passed under agitation, when the pH value of slip stops logical ammonia 4.3 time, slip filtered while hot in neutralizing well, compound fertilizer facility production composite fertilizer delivered to by filter cake, and filtrate enters purification tank; Ammonium sulfide solution is added in purification tank, stirring reaction removal of impurities, through after the assay was approved, crosses and filters filter residue, for extracting wherein metal after residue collection, filtrate enters in condensing crystal groove, stops concentrated when proportion reaches 1.32, sends into crystallisation by cooling groove intercrystalline, when temperature is down to 35 DEG C, filter centrifugation, crystal enters drying machine inner drying and obtains industrial grade monoammonium phosphate product, and mother liquor sends into Two-step neutralization groove; In Two-step neutralization groove, add ammonia, stop logical ammonia when neutralizer PH is neutralized to 8.0, send in two ammonium condensing crystal grooves concentrated, stop concentrated after proportion reaches 1.25, send into cooling in two ammonium crystallisation by cooling grooves; Temperature is sent in whizzer centrifugal 38 DEG C time, and crystal obtains PHOSPHORIC ACID TECH.GRADE two ammonium product after entering drying machine inner drying, and filtrate returns the concentrated utilization of two ammonium condensing crystal groove internal recycle.Acceptable end product requirement is all reached through inspection industrial grade monoammonium phosphate and PHOSPHORIC ACID TECH.GRADE two ammonium product indices.
Embodiment 2
P is added in neutralizing well
2o
5concentration is in the phosphoric acid by wet process feeding desulfurizer of 35%, sampling analysis is sulfate radical content wherein, the add-on of secondary calcium phosphate is 0.85 ~ 1.0 times of sulfate radical amount, adding after secondary calcium phosphate carries out desulphurization reaction sends in neutralizing well by filtrate, add the ammoniacal liquor that mass concentration is 25% while stirring, the pH value of phosphor ammonium slurry stops adding ammoniacal liquor, slip filtered while hot 4.2 time, compound fertilizer facility production composite fertilizer delivered to by filter cake, and filtrate sends into purification tank; The further removal of impurities of ammonium sulfide solution is added in purification tank, enter in thickener concentrated filtrate after the assay was approved, thickener internal ratio weigh 1.29 time stop concentrated, send in crystallisation by cooling groove, during temperature 35 DEG C, filter centrifugation, crystal enters drying machine inner drying and obtains industrial grade monoammonium phosphate product, and mother liquor is sent in Two-step neutralization groove; In Two-step neutralization groove, add ammonia, when neutralizer PH stops logical ammonia to when being neutralized to 8.0, send in two ammonium condensing crystal grooves concentrated, stop concentrated after proportion reaches 1.30, send into cooling in two ammonium crystallisation by cooling grooves; Temperature is sent in whizzer centrifugal 35 DEG C time, and crystal obtains PHOSPHORIC ACID TECH.GRADE two ammonium product after entering drying machine inner drying, and filtrate returns the concentrated utilization of two ammonium condensing crystal groove internal recycle.Acceptable end product requirement is all reached through inspection industrial grade monoammonium phosphate and PHOSPHORIC ACID TECH.GRADE two ammonium product indices.
Claims (1)
1. the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammonium, that phosphoric acid is raw material in a wet process, concentrated after series of chemical, crystallization, dry obtained monoammonium phosphate and diammonium phosphate, it is characterized in that: the filtrate obtained after carrying out desulphurization reaction with secondary calcium phosphate and phosphoric acid by wet process and ammonia or ammoniacal liquor carry out neutralization reaction, obtain phosphor ammonium slurry, with ammonium sulfide and phosphor ammonium slurry reaction gained filtrate concentrated again, crystallization, drying obtains industrial grade monoammonium phosphate product, then mother liquor crystallization and filtration obtained and ammonia or ammoniacal liquor carry out Two-step neutralization reaction, the concentrating filter liquor finally Two-step neutralization obtained, crystallization, drying obtains PHOSPHORIC ACID TECH.GRADE two ammonium product, the secondary mother liquid that crystallization and filtration obtains returns in thickener and continues to concentrate, described Production Flow Chart is:
(1) desulfurization: phosphoric acid by wet process is warming up to 60 ~ 80 DEG C in desulfurizer, adds secondary calcium phosphate, filters after stirring reaction 30 ~ 60min, and filtrate is that neutralizing well is sent in desulfurization acid;
(2) in and removal of impurities: add ammonia or ammoniacal liquor in the desulfurization phosphoric acid in neutralizing well under whipped state, the pH value of solution is neutralized to 3.9 ~ 4.3, while hot by slurry filtration, filtrate is that phosphor ammonium slurry delivers to purification tank;
(3) purify: in purification tank, add ammonium sulfide stirring reaction, through centrifugation filter residue after the assay was approved, filtrate sends into thickener A;
(4) one ammonium condensing crystals: the slip after purification is concentrated into slip proportion to 1.30 ~ 1.35 with steam in thickener A, send in crystallisation by cooling groove A and be cooled to less than the 40 DEG C crystallizations of slurry temperature value, slurry filtration after crystallization is separated and obtains a mother liquor and crystal, crystal is sent into drying machine A inner drying and is obtained industrial grade monoammonium phosphate product, and one time mother liquor is sent in Two-step neutralization groove;
(5) Two-step neutralization: add ammonia or ammoniacal liquor in time mother liquor of in Two-step neutralization groove, regulates pH=7.9 ~ 8.0, after pH value is stable, send into thickener B;
(6) two ammonium condensing crystals: the slip of Two-step neutralization is concentrated into slip proportion in the scope of 1.25 ~ 1.30 with steam in thickener B, send in crystallisation by cooling groove B and be cooled to slurry temperature crystallization below 40 DEG C, slip after crystallization is separated by filtration and obtains secondary mother liquid and crystal, crystal is sent into drying machine inner drying and is obtained PHOSPHORIC ACID TECH.GRADE two ammonium product, and secondary mother liquid then returns in thickener B and continues to concentrate;
In described step (1), phosphoric acid is P
2o
5concentration, at the phosphoric acid by wet process of 20 ~ 35%, needs first sampling analysis wherein sulfate radical content before adding secondary calcium phosphate, and the add-on of secondary calcium phosphate is 0.85 ~ 1.0 times of sulfate radical amount;
Detecting qualified method before centrifugal in described step (3) is dark solution filtered, and drips ammonium sulfide, when solution no longer shows black and qualified in filtrate;
Negative pressure is adopted to concentrate in described step (6) during two ammonium condensing crystals, the ammonia that in the ammonia of overflowing in concentration process and step (5), Two-step neutralization overflow need absorb with phosphoric acid washing, with removal of impurities operation in carrying out in the neutralizing well that the slip after absorption delivers to step (2).
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| CN201210575796.4A CN103011113B (en) | 2012-12-25 | 2012-12-25 | Method for co-producing industrial grade diammonium phosphate during production of industrial grade monoammonium phosphate of phosphoric acid by wet process |
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| CN104340963A (en) * | 2013-07-23 | 2015-02-11 | 耿兆翔 | Efficient ammonium biphosphate production method |
| CN103613083B (en) * | 2013-11-28 | 2015-10-21 | 贵州开磷集团股份有限公司 | A kind of phosphoric acid by wet process and high-purity phosphoric acid are in conjunction with the method for manufacture level monoammonium phosphate |
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| CN110877901B (en) * | 2019-12-16 | 2023-02-28 | 瓮福达州化工有限责任公司 | Method and system for producing industrial-grade monoammonium phosphate and industrial-grade diammonium phosphate by wet-process phosphoric acid |
| CN111498821A (en) * | 2020-04-23 | 2020-08-07 | 湖北兴发化工集团股份有限公司 | Process and device for producing diammonium hydrogen phosphate and ammonium dihydrogen phosphate by taking phosphoric acid as raw material |
| CN112624074B (en) * | 2020-12-31 | 2022-11-22 | 四川龙蟒磷化工有限公司 | Method for producing industrial grade monoammonium phosphate, monopotassium phosphate and fertilizer grade monoammonium phosphate from raffinate |
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2012
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| US4610853A (en) * | 1985-03-08 | 1986-09-09 | Chisso Corporation | Process for producing purified monoammonium phosphate from wet process phosphoric acid |
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