CN103011113A - 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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- CN103011113A CN103011113A CN2012105757964A CN201210575796A CN103011113A CN 103011113 A CN103011113 A CN 103011113A CN 2012105757964 A CN2012105757964 A CN 2012105757964A CN 201210575796 A CN201210575796 A CN 201210575796A CN 103011113 A CN103011113 A CN 103011113A
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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 ammoniums.
Background technology
Industrial grade monoammonium phosphate and diammonium phosphate all have a wide range of applications at aspects such as fire-fighting, drip irrigation fertilizer, medicine and food.The production of current industrial level monoammonium phosphate and diammonium phosphate generally all is to adopt thermal phosphoric acid or purifying phosphoric acid technique, and shortcoming is that production cost is high, technique is complicated, energy consumption is high, pollution is large.There is part producer also to adopt wet method phosphoric acid manufacture process, but has some problems in the removal of impurities process, high such as metal content in the product, can change along with phosphoric acid quality, make quality product be difficult to guarantee.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 ammoniums, and do not realize the technique of industrial grade monoammonium phosphate coproduction PHOSPHORIC ACID TECH.GRADE two ammoniums.
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 ammoniums, solve and to produce monoammonium phosphate, features of DAP production cost in the prior art and energy consumption is high, it is large to pollute, problem unstable product quality.
The objective 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 ammoniums, as raw material take phosphoric acid by wet process, concentrated after series of chemical, crystallization, drying makes monoammonium phosphate and diammonium phosphate, it is characterized in that: carry out the filtrate that obtains behind the desulphurization reaction and ammonia or ammoniacal liquor with secondary calcium phosphate and phosphoric acid by wet process and carry out neutralization reaction, obtain phosphor ammonium slurry, concentrate with ammonium sulfide and phosphor ammonium slurry reaction and with gained filtrate again, crystallization, drying obtains the industrial grade monoammonium phosphate product, the mother liquor that then crystallization and filtration is obtained and ammonia or ammoniacal liquor carry out the secondary neutralization reaction, the concentrating filter liquor that at last the secondary neutralization is obtained, crystallization, drying obtains PHOSPHORIC ACID TECH.GRADE two ammonium products, and the secondary mother liquid that crystallization and filtration obtains returns and continues in the thickener to concentrate; Described Production Flow Chart is:
(1) desulfurization: phosphoric acid by wet process is warming up to 60～80 ℃ in desulfurizer, adds secondary calcium phosphate, filter behind stirring reaction 30～60min, 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 under whipped state in the neutralizing well, the pH value of solution is neutralized to 3.9～4.3, with slurry filtration, filter cake is that agricultural grade phosphorus ammonium is delivered to compound fertilizer facility production energy composite fertilizer while hot, and filtrate is that phosphor ammonium slurry is delivered to purification tank;
(3) purify: in purification tank, add the ammonium sulfide stirring reaction, through centrifugation filter residue after the assay was approved, filtrate is sent into thickener A;
(4) one ammonium condensing crystals: the slip after the purification is concentrated into slip proportion to 1.30～1.35 with steam in thickener A, send into and be cooled to the crystallization below 40 ℃ of slurry temperature value in the crystallisation by cooling groove A, slurry filtration after the crystallization separates and obtains mother liquor and crystal, crystal is sent into drying machine A inner drying and is obtained the industrial grade monoammonium phosphate product, and one time mother liquor is sent in secondary and the groove;
(5) secondary neutralization: add ammonia or ammoniacal liquor in the mother liquor in the secondary neutralizing well, regulate pH=7.9～8.0, behind the pH value stabilization, send into thickener B;
(6) two ammonium condensing crystals: the slip of secondary neutralization is concentrated into slip proportion in 1.25～1.30 scope with steam in thickener B, send in the crystallisation by cooling groove B and be cooled to slurry temperature in crystallization below 40 ℃, slip after the crystallization is separated by filtration and obtains secondary mother liquid and crystal, crystal is sent into the drying machine inner drying and is obtained PHOSPHORIC ACID TECH.GRADE two ammonium products, and secondary mother liquid then returns and continues in the thickener B to concentrate.
Phosphoric acid is P in the described step (1)
2O
5Concentration is at 20～35% phosphoric acid by wet process.
Need wherein sulfate radical content of first sampling analysis in the described step (1) before adding secondary calcium phosphate, the add-on of secondary calcium phosphate is 0.85～1.0 times of sulfate radical amount.
The qualified method of centrifugal front detection is that dark solution is filtered in the described step (3), drips ammonium sulfide in filtrate, and is qualified when solution no longer shows black.
Adopt during two ammonium condensing crystals negative pressure concentrated in the described step (6), in the ammonia of overflowing in the concentration process and the step (5) in the secondary and the ammonia of overflowing need to absorb with phosphoric acid washing, during the slip after the absorption is delivered to and is carried out in the neutralizing well of step (2) and the removal of impurities operation.
Character according to the ammonification slip, at the PH of slurry solution in 4.0～4.5 scopes, impurity in the phosphoric acid and ammonia and phosphoric acid generation chemical reaction can generate a series of insoluble compounds, just can remove after filtration the impurity in the phosphoric acid, filtrate monoammonium phosphate slip is clean, concentrated industrial grade monoammonium phosphate again.Isolate an industrial ammonium mother liquor through further ammonia PHOSPHORIC ACID TECH.GRADE two ammoniums that neutralize to get.The main chemical reaction that occurs is the generation of monoammonium phosphate and diammonium phosphate among the present invention, 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 the monoammonium phosphate co-producing diammonium phosphate, saved production cost, reduced energy consumption, reduced pollution, guaranteed the quality of monoammonium phosphate and diammonium phosphate through effective removal of impurities, have good economic benefit.Adopt secondary calcium phosphate and wet-process phosphoric acid reaction to remove sulfate radical, when removing impurity, the phosphate radical in the secondary calcium phosphate is converted into phosphoric acid, finally generate ammonium phosphate salt, not only can not introduce impurity and also produce good economic benefit.Adopt the ammonium sulfide desulfurization can further remove the heavy metal such as arsenic in the phosphoric acid by wet process, lead and other metallic cations partly, improve the quality of products.In process of production, filter residue after the neutralization can be used for the production of fertilizer grade monoammonium phosphate, and purification slag can be used for extracting metal, and one time mother liquor continues to add in ammonia or the liquefied ammonia and manufacture level diammonium phosphate, secondary mother liquid returns the crystal system recycle and reclaims, without waste residue, discharging of waste liquid.Utilize in the continuation of manufacture level monoammonium phosphate mother liquor and manufacture level diammonium phosphate, can reduce technical grade two ammonium production costs.In neutralization, 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 the ammonia loss, and can not impact human body and environment.Coproduction PHOSPHORIC ACID TECH.GRADE two ammoniums on the basis of manufacture level monoammonium phosphate increase product diversity, have strengthened competitive power in similar production.
Description of drawings
Fig. 1 is process flow diagram of the present invention;
Fig. 2 is equipment flowsheet of the present invention;
Among the figure: 1-desulfurizer, 2-neutralizing well, 3-purification tank, 4-thickener A, 5-crystallisation by cooling groove A, 6-drying machine A, 7-secondary neutralizing well, 8-thickener B, 9-crystallisation by cooling groove B, 10-drying machine B.
Embodiment
In order to deepen the understanding of the present invention, the present invention is described in further detail below in conjunction with drawings and Examples, but do not consist of the restriction to protection domain 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 sends into secondary calcium phosphate and phosphoric acid by wet process to carry out in the desulfurizer 1 filtering behind the desulphurization reaction, and gained filtrate enters in the neutralizing well 2 carries out neutralization reaction with ammonia or ammoniacal liquor; Again filtering the filtrate that obtains enters in the purification tank 3, with the ammonium sulfate reaction and the filtration that add, send into crystallisation by cooling groove A5 crystallization after the filtrate that obtains is delivered to and concentrated in the thickener A4, the crystal that obtains is delivered to the processing of drying machine A6 inner drying and is obtained the industrial grade monoammonium phosphate finished product; The liquid that obtains is a mother liquor, deliver in the secondary neutralizing well 7 and carry out the secondary neutralization reaction with ammonia or ammoniacal liquor, the filtrate that obtains is delivered in the thickener B8 concentrated, deliver to again in the crystallisation by cooling groove B9 through crystallisation by cooling, the gained crystal is delivered to after filtering the processing of drying machine B10 inner drying and is obtained PHOSPHORIC ACID TECH.GRADE two ammonium products, gained filtrate is secondary mother liquid, delivers to and continues in the thickener B8 to concentrate.
With P
2O
5Concentration is that 25% phosphoric acid by wet process is sent in the desulfurizer, 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 secondary calcium phosphate carries out behind the desulphurization reaction filtrate being sent in the neutralizing well, under agitation condition, in neutralizing well, pass into ammonia, when the pH value of slip stops logical ammonia, slip filtered while hot 4.3 the time, filter cake is delivered to compound fertilizer facility production composite fertilizer, and filtrate enters purification tank; In purification tank, add ammonium sulfide solution, the stirring reaction removal of impurities through after the assay was approved, removes by filter filter residue, after collecting, filter residue is used for extracting wherein metal, filtrate enters in the condensing crystal groove, stops to concentrate when proportion reaches 1.32, sends into crystallisation by cooling groove intercrystalline, when temperature is down to 35 ℃, filter centrifugally, crystal enters the drying machine inner drying and gets the industrial grade monoammonium phosphate product, and mother liquor is sent into the secondary neutralizing well; In the secondary neutralizing well, add ammonia, when neutralizer PH is neutralized to 8.0, stop logical ammonia, send into two ammonium condensing crystal grooves interior concentrated, stop to concentrate after proportion reaches 1.25, send into cooling in the two ammonium crystallisation by cooling grooves; Temperature is sent in the whizzer centrifugal in the time of 38 ℃, and crystal gets PHOSPHORIC ACID TECH.GRADE two ammonium products after entering the drying machine inner drying, and filtrate is returned the concentrated utilization of two ammonium condensing crystal groove internal recycle.All reach the acceptable end product requirement through check industrial grade monoammonium phosphate and PHOSPHORIC ACID TECH.GRADE two ammonium product indices.
In neutralizing well, add P
2O
5Concentration is that 35% phosphoric acid by wet process is sent in the desulfurizer, 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 secondary calcium phosphate carries out behind the desulphurization reaction filtrate being sent in the neutralizing well, add while stirring mass concentration and be 25% ammoniacal liquor, the pH value of phosphor ammonium slurry stopped to add ammoniacal liquor, slip filtered while hot at 4.2 o'clock, filter cake is delivered to compound fertilizer facility production composite fertilizer, and filtrate is sent into purification tank; In purification tank, add the further removal of impurities of ammonium sulfide solution, enter in the thickener concentrated at the rear filtrate that is up to the standards, weigh in the thickener internal ratio and to stop to concentrate in 1.29 o'clock, send in the crystallisation by cooling groove, during 35 ℃ of temperature, filter centrifugally, crystal enters the drying machine inner drying and gets the industrial grade monoammonium phosphate product, and mother liquor is sent in the secondary neutralizing well; In the secondary neutralizing well, add ammonia, when neutralizer PH stops logical ammonia when being neutralized to 8.0, send in the two ammonium condensing crystal grooves concentratedly, stop to concentrate after proportion reaches 1.30, send into cooling in the two ammonium crystallisation by cooling grooves; Temperature is sent in the whizzer centrifugal in the time of 35 ℃, and crystal gets PHOSPHORIC ACID TECH.GRADE two ammonium products after entering the drying machine inner drying, and filtrate is returned the concentrated utilization of two ammonium condensing crystal groove internal recycle.All reach the acceptable end product requirement through check industrial grade monoammonium phosphate and PHOSPHORIC ACID TECH.GRADE two ammonium product indices.
Claims (5)
1. the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammoniums, as raw material take phosphoric acid by wet process, concentrated after series of chemical, crystallization, drying makes monoammonium phosphate and diammonium phosphate, it is characterized in that: carry out the filtrate that obtains behind the desulphurization reaction and ammonia or ammoniacal liquor with secondary calcium phosphate and phosphoric acid by wet process and carry out neutralization reaction, obtain phosphor ammonium slurry, concentrate with ammonium sulfide and phosphor ammonium slurry reaction and with gained filtrate again, crystallization, drying obtains the industrial grade monoammonium phosphate product, the mother liquor that then crystallization and filtration is obtained and ammonia or ammoniacal liquor carry out the secondary neutralization reaction, the concentrating filter liquor that at last the secondary neutralization is obtained, crystallization, drying obtains PHOSPHORIC ACID TECH.GRADE two ammonium products, and the secondary mother liquid that crystallization and filtration obtains returns and continues in the thickener to concentrate; Described Production Flow Chart is:
(1) desulfurization: phosphoric acid by wet process is warming up to 60～80 ℃ in desulfurizer, adds secondary calcium phosphate, filter behind stirring reaction 30～60min, 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 under whipped state in the neutralizing well, the pH value of solution is neutralized to 3.9～4.3, while hot with slurry filtration, filtrate is that phosphor ammonium slurry is delivered to purification tank;
(3) purify: in purification tank, add the ammonium sulfide stirring reaction, through centrifugation filter residue after the assay was approved, filtrate is sent into thickener A;
(4) one ammonium condensing crystals: the slip after the purification is concentrated into slip proportion to 1.30～1.35 with steam in thickener A, send into and be cooled to the crystallization below 40 ℃ of slurry temperature value in the crystallisation by cooling groove A, slurry filtration after the crystallization separates and obtains mother liquor and crystal, crystal is sent into drying machine A inner drying and is obtained the industrial grade monoammonium phosphate product, and one time mother liquor is sent in secondary and the groove;
(5) secondary neutralization: add ammonia or ammoniacal liquor in the mother liquor in the secondary neutralizing well, regulate pH=7.9～8.0, behind the pH value stabilization, send into thickener B;
(6) two ammonium condensing crystals: the slip of secondary neutralization is concentrated into slip proportion in 1.25～1.30 scope with steam in thickener B, send in the crystallisation by cooling groove B and be cooled to slurry temperature in crystallization below 40 ℃, slip after the crystallization is separated by filtration and obtains secondary mother liquid and crystal, crystal is sent into the drying machine inner drying and is obtained PHOSPHORIC ACID TECH.GRADE two ammonium products, and secondary mother liquid then returns and continues in the thickener B to concentrate.
2. the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammoniums according to claim 1 is characterized in that: phosphoric acid is P in the described step (1)
2O
5Concentration is at 20～35% phosphoric acid by wet process.
3. the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammoniums according to claim 1, it is characterized in that: need wherein sulfate radical content of first sampling analysis in the described step (1) before adding secondary calcium phosphate, the add-on of secondary calcium phosphate is 0.85～1.0 times of sulfate radical amount.
4. the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammoniums according to claim 1, it is characterized in that: the qualified method of centrifugal front detection is that dark solution is filtered in the described step (3), in filtrate, drip ammonium sulfide, qualified when solution no longer shows black.
5. the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid coproduction PHOSPHORIC ACID TECH.GRADE two ammoniums according to claim 1, it is characterized in that: adopt during two ammonium condensing crystals negative pressure concentrated in the described step (6), in the ammonia of overflowing in the concentration process and the step (5) in the secondary and the ammonia of overflowing need to absorb with phosphoric acid washing, during the slip after the absorption is delivered to and is carried out in the neutralizing well of step (2) and the removal of impurities operation.
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| CN103613083A (en) * | 2013-11-28 | 2014-03-05 | 贵州开磷（集团）有限责任公司 | Method for producing industrial grade monoammonium phosphate through combination of wet process phosphoric acid and high-purity phosphoric acid |
| CN104340963A (en) * | 2013-07-23 | 2015-02-11 | 耿兆翔 | Efficient ammonium biphosphate production method |
| CN106904586A (en) * | 2017-01-19 | 2017-06-30 | 赵常然 | A kind of active charcoal bag membrane material and the ammonium of crystal phosphoric acid one, the co-production of two ammoniums |
| CN110697670A (en) * | 2019-10-17 | 2020-01-17 | 昆明理工大学 | Method for desulfurizing phosphate slurry, co-producing ammonium phosphate and recycling phosphate slurry |
| CN110844897A (en) * | 2019-12-13 | 2020-02-28 | 中山市中环环保废液回收有限公司 | Waste phosphoric acid treatment method and flow line treatment line |
| CN110877901A (en) * | 2019-12-16 | 2020-03-13 | 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 |
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| CN112624074A (en) * | 2020-12-31 | 2021-04-09 | 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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| CN104340963A (en) * | 2013-07-23 | 2015-02-11 | 耿兆翔 | Efficient ammonium biphosphate production method |
| CN103613083A (en) * | 2013-11-28 | 2014-03-05 | 贵州开磷（集团）有限责任公司 | Method for producing industrial grade monoammonium phosphate through combination of wet process phosphoric acid and high-purity phosphoric acid |
| CN106904586A (en) * | 2017-01-19 | 2017-06-30 | 赵常然 | A kind of active charcoal bag membrane material and the ammonium of crystal phosphoric acid one, the co-production of two ammoniums |
| CN106904586B (en) * | 2017-01-19 | 2019-02-19 | 赵常然 | A kind of co-production of active charcoal bag membrane material and crystal phosphoric acid monoammonium, diammonium |
| CN110697670A (en) * | 2019-10-17 | 2020-01-17 | 昆明理工大学 | Method for desulfurizing phosphate slurry, co-producing ammonium phosphate and recycling phosphate slurry |
| CN112378898A (en) * | 2019-11-07 | 2021-02-19 | 陕西彩虹新材料有限公司 | Method for measuring content of nonmagnetic metal substances in positive electrode material |
| CN110844897A (en) * | 2019-12-13 | 2020-02-28 | 中山市中环环保废液回收有限公司 | Waste phosphoric acid treatment method and flow line treatment line |
| CN110844897B (en) * | 2019-12-13 | 2023-08-29 | 中山市中环环保废液回收有限公司 | Treatment method of waste phosphoric acid on running water treatment line |
| CN110877901A (en) * | 2019-12-16 | 2020-03-13 | 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 |
| 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 |
| CN112624074A (en) * | 2020-12-31 | 2021-04-09 | 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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