CN104828796A - Method for improving quality of diammonium phosphate product - Google Patents
Method for improving quality of diammonium phosphate product Download PDFInfo
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- CN104828796A CN104828796A CN201510270823.0A CN201510270823A CN104828796A CN 104828796 A CN104828796 A CN 104828796A CN 201510270823 A CN201510270823 A CN 201510270823A CN 104828796 A CN104828796 A CN 104828796A
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Abstract
The invention discloses a method for improving quality of a diammonium phosphate product. The method comprises the following steps: a remover, which is prepared by mixing wet-process phosphoric acid phosphogypsum heap backwater and sulfuric acid, is utilized to perform magnesium removal pretreatment on phosphorite slurry, so that magnesium ions are subjected to acidolysis to enter the liquid phase, thereby achieving the goal of removing magnesium ions; after the magnesium removal, cyclone grading is performed, and the obtained phosphorite slurry with the solid content of 50-70% can be used as a production raw material; after the residual part is subjected to natural settling, weak aqua ammonia is introduced into the liquid phase, and pressure filtration is performed to obtain the high-quality magnesium ammonium phosphate product, so that the magnesium ions are separated from the liquid phase; and finally, the liquid phase subjected to magnesium removal is used for wet-process phosphoric acid production, and the wet-process phosphoric acid slag slurry enters the phosphogypsum heap, thereby implementing cyclic utilization. The diammonium phosphate product obtained by the method can achieve the premium grade indexes; and the method enhances the amount of the premium-grade diammonium phosphate in the total product, and optimizes the product structure.
Description
Technical field
The invention belongs to phosphate ore pulp imurity-removal technical field, be specifically related to a kind ofly from the phosphate ore pulp of phosphoric acid by wet process, remove magnesium ion, and then promote the method for diammonium phosphate product quality.
Background technology
Phosphate rock resource and phosphorus ore quality are phosphatic fertilizer company issues that need special attention always, and phosphorus ore quality declines and has a strong impact on phosphate fertilizer production and quality.Phosphorus ore is produced in the process of phosphoric acid in extraction, and in phosphorus ore, the metal ion such as Fe, Al, Mg is dissolved in phosphoric acid in a large number, and brings in diammonium phosphate product.Along with phosphorus ore quality declines, the metal ions such as Fe, Al, Mg in phosphorus ore raise, and the metallic cations such as Fe, Al, Mg in phosphoric acid significantly raise, and can replace NH in produced diammonium phosphate
4 +ion, reduces nitrogen content.Simultaneously the metallic cation such as Fe, Al, Mg again with PO
4 3-in conjunction with generation indissoluble complex compound, magnesium ion impact particularly in phosphate ore pulp occupies largely in metal ion, the increase of magnesium ion increases the difficulty of production control, reduce the water-soluble phosphorus of diammonium phosphate product, product water is caused to have than lower than 90%, total nutrient is lower than 64%, and the diammonium phosphate produced does not reach premium grads index, only can produce acceptable end product diammonium phosphate (60%).How promoting the quality of diammonium phosphate product when using low-grade phosphate ore, just becoming problem demanding prompt solution, but in prior art, there is not yet terms of settlement well.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide one when using low-grade phosphate ore, the content of metal ion in phosphate ore pulp can be reduced, make the diammonium phosphate produced reach the method for premium grads.
Object of the present invention is achieved by the following technical programs.
Except as otherwise noted, percentage ratio of the present invention is mass percent.
Promote a method for diammonium phosphate product quality, comprise the following steps:
(1) obtain after the vitriol oil of 1 weight part being mixed with the ardealite storage yard backwater of 13 ~ 32 weight parts in tempering tank and remove agent;
(2) phosphorus ore raw ore is obtained fineness-200 order >=50% after fragmentation, ore grinding, classification, the phosphate ore pulp of solid content 40 ~ 50%;
(3) 1 part being removed agent slowly adds in 1 ~ 7 part of phosphate ore pulp, under 30 ~ 50 DEG C of conditions, react 1.0 ~ 2.0h, and the solid content controlling the rear slip of reaction is 25 ~ 35%;
(4) slip completing reaction obtains finished product phosphate ore pulp and the removing impurities liquid of 60 ~ 70% solid contents after cyclone classification;
(5) removing impurities liquid natural subsidence, bottom desilting introduces phosphate ore pulp storage tank, and supernatant liquid adds 1 ~ 2 part of NH
3as precipitation agent, regulate pH to be 6 ~ 8, mix rear standing 30 ~ 45min; Again through pressure filter press filtration, obtain magnesium ammonium phosphate and de-magging liquid phase;
(6) namely finished product phosphate ore pulp obtains phosphorus ammonium two ammonium premium grads through former features of DAP production device again.
Further, the de-magging liquid phase described in step (5) is introduced Wet Phosphoric Acid Plant production and application, enter ardealite storage yard with phosphogypsum slag slurry, ardealite storage yard backwater realizes recycle.
Relative to prior art, the present invention has the following advantages:
1, after process of the present invention, the P in finished product phosphate ore pulp
2o
5% can improve 0.5 ~ 2.0%, and content of MgO is lower than 1.0%, and phosphorous recovery is greater than 95%.
2, the present invention is mixed with ardealite storage yard backwater and phosphoric acid and removes agent, compared with the sulfuric acid removing agent that employing is single, has saved sulphuric acid cost; Achieve the working cycle of ardealite storage yard backwater → remove agent → de-magging liquid phase → production → ardealite storage yard backwater, save water resources.
3, after process of the present invention, the diammonium phosphate product of production reaches premium grads index, improves the accounting of premium grads diammonium phosphate in product population simultaneously, optimizes product structure.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described further, but drawings and Examples are not limited to the technical solution.
Embodiment 1
Preparation high-quality diammonium phosphate, removes the idiographic flow of magnesium ion in phosphate ore pulp as shown in Figure 1:
(1) get mass percentage concentration be 98% sulfuric acid mix with the ratio of ardealite storage yard backwater in 1:19, being mixed with compound, to remove agent stand-by.
(2) P is got
2o
5% content is 28.29%, and content of MgO is 2.37%, and granularity is 60% 1 part, the raw ore crossing 200 mesh sieves, is placed in reactor; Add the phosphate ore pulp that 1.2 parts of water make 45% solid content again.
(3) slowly add in the ore pulp of step (2) by the agent 1.5 parts that removes of step (1), control temperature is 30 ~ 50 DEG C, and stir speed (S.S.) is 300r/min, and reaction 60min, de-magging operation completes.
(4) by the reaction slurry of step (3) through one-level swirler cyclone classification, bottom desilting is finished product phosphate ore pulp, removing impurities liquid introduce subsider.
(5) finished product phosphate ore pulp in step (4) is analyzed, P in finished product phosphate ore pulp
2o
5% content is 28.82%, and content of MgO is 0.69%, and solid content is 61.33%.Compared with raw pulp before treatment, P
2o
5% content rises 0.52%, and content of MgO reduces by 1.68%, MgO decreasing ratio and reaches 70.9%.
(6), after the middle removing impurities liquid sedimentation of step (4), bottom desilting is collected into ore pulp storage tank; In supernatant liquid, add ammoniacal liquor, adjust ph 6 ~ 8, mix rear standing 45min, be then sent to pressure filter press filtration, obtain magnesium ammonium phosphate product, its purity is 92.37%.
(7) by the finished product phosphate ore pulp in step (4) for the production of in, the phosphorus ammonium two ammonium product analysis index produced is N%:17.30%, P
2o
5 is effective: 47.14%, P
2o
5 is water-soluble%:42.06%, total nutrient %:64.44%, moisture: 1.65%, water has ratio: 89.22%, reaches premium grads index.
Embodiment 2
Repeat embodiment 1, have following difference:
(1) get mass percentage concentration be 98% sulfuric acid and ardealite storage yard backwater in the ratio of 1:32, being mixed with compound, to remove agent stand-by.
(2) P is got
2o
5% content is 28.45%, and content of MgO is 2.28%, and granularity is 60% 1 part, the raw ore crossing 200 mesh sieves, is placed in reactor; Add the phosphate ore pulp that 1 part of water makes solid content 50% again.
(3) slowly add in the ore pulp of step (2) by the agent 2 parts that removes of step (1), control temperature is 30 ~ 50 DEG C, and stir speed (S.S.) is 300r/min, and reaction 90min, de-magging completes.
(4) by the reaction slurry of step (3) through one-level swirler cyclone classification, bottom desilting is finished product phosphate ore pulp, removing impurities liquid introduce subsider.
(5) finished product phosphate ore pulp in step (4) is analyzed, P in finished product phosphate ore pulp
2o
5% content is 29.12%, and content of MgO is 0.54%, and solid content is 60.98%.Compared with raw pulp before treatment, P
2o
5% content rises 0.67%, and content of MgO reduces by 1.74%, MgO decreasing ratio and reaches 76.3%.
(6), after the middle removing impurities liquid sedimentation of step (4), bottom desilting is collected into ore pulp storage tank; In supernatant liquid, add ammoniacal liquor, adjust ph 6 ~ 8, mix rear standing 40min, be then sent to pressure filter press filtration, obtain magnesium ammonium phosphate product, its purity is 93.48%.
(7) by the finished product phosphate ore pulp in step (4) for the production of in, the phosphorus ammonium two ammonium product analysis index produced is N%:17.42%, P
2o
5 is effective: 47.14%, P
2o
5 is water-soluble%:41.96%, total nutrient %:64.56%, moisture: 1.70%, water has ratio: 89.01%, reaches choicest quality figureofmerit.
Embodiment 3
Repeat embodiment 1, have following difference:
(1) get mass percentage concentration be 98% sulfuric acid and ardealite storage yard backwater in the ratio of 1:14, being mixed with compound, to remove agent stand-by.
(2) P is got
2o
5% content is 28.14%, and content of MgO is 2.42%, and granularity is 60% 1 part, the raw ore crossing 200 mesh sieves, is placed in reactor; Add the ore pulp that 1.5 parts of water make solid content 40% again.
(3) slowly add in the ore pulp of step (2) by the agent 0.8 part that removes of step (1), control temperature is 30 ~ 50 DEG C, and stir speed (S.S.) is 300r/min, and reaction 120min, de-magging completes.
(4) by the reaction slurry of step (3) through one-level swirler cyclone classification, bottom desilting is finished product phosphate ore pulp, removing impurities liquid introduce subsider.
(5) finished product phosphate ore pulp in step (4) is analyzed, P in finished product phosphate ore pulp
2o
5% content is 28.96%, and content of MgO is 0.61%, and solid content is 63.75%.Compared with raw pulp before treatment, P
2o
5% content rises 0.82%, and content of MgO reduces by 1.81%, MgO decreasing ratio and reaches 74.8%.
(6), after the middle removing impurities liquid sedimentation of step (4), bottom desilting is collected into ore pulp storage tank; In supernatant liquid, add weak ammonia, adjust ph 6 ~ 8, mix rear standing 30min, be then sent to pressure filter press filtration, obtain magnesium ammonium phosphate product, its purity is 91.98%.
(7) by the finished product phosphate ore pulp in step (4) for the production of in, the phosphorus ammonium two ammonium product analysis index produced is N%:17.48%, P
2o
5 is effective: 46.80%, P
2o
5 is water-soluble%:41.66%, total nutrient %:64.28%, moisture: 1.62%, water has ratio: 89.02%, reaches choicest quality figureofmerit.
Claims (2)
1. promote a method for diammonium phosphate product quality, comprise the following steps:
(1) obtain after the vitriol oil of 1 weight part being mixed with the ardealite storage yard backwater of 13 ~ 32 weight parts in tempering tank and remove agent;
(2) phosphorus ore raw ore is obtained fineness-200 order >=50% after fragmentation, ore grinding, classification, the phosphate ore pulp of solid content 40 ~ 50%;
(3) 1 part being removed agent slowly adds in 1 ~ 7 part of phosphate ore pulp, under 30 ~ 50 DEG C of conditions, react 1.0 ~ 2.0h, and the solid content controlling the rear slip of reaction is 25 ~ 35%;
(4) slip completing reaction obtains finished product phosphate ore pulp and the removing impurities liquid of 60 ~ 70% solid contents after cyclone classification;
(5) removing impurities liquid natural subsidence, bottom desilting introduces phosphate ore pulp storage tank, and supernatant liquid adds 1 ~ 2 part of NH
3as precipitation agent, regulate pH to be 6 ~ 8, mix rear standing 30 ~ 45min; Again through pressure filter press filtration, obtain magnesium ammonium phosphate and de-magging liquid phase;
(6) namely finished product phosphate ore pulp obtains phosphorus ammonium two ammonium premium grads through former features of DAP production device again.
2. the method for lifting diammonium phosphate product quality according to claim 1, it is characterized in that: further, de-magging liquid phase described in step (5) is introduced Wet Phosphoric Acid Plant production and application, enter ardealite storage yard with phosphogypsum slag slurry, ardealite storage yard backwater realizes recycle.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112191361A (en) * | 2020-09-27 | 2021-01-08 | 湖北祥云(集团)化工股份有限公司 | Method and production system for preparing powdered ammonium and high-quality ammonium phosphate by phosphorite classification |
| CN112374477A (en) * | 2020-11-16 | 2021-02-19 | 贵州开磷集团矿肥有限责任公司 | Production method of 68% DAP |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992284A (en) * | 2012-12-12 | 2013-03-27 | 贵州开磷（集团）有限责任公司 | High-magnesium phosphorite de-magging method with by-product magnesium ammonium phosphate |
| CN103303884A (en) * | 2013-05-27 | 2013-09-18 | 瓮福（集团）有限责任公司 | Method for treating phosphorus concentrates and recovering phosphorus by using phosphogypsum slag dump pool water |
-
2015
- 2015-05-25 CN CN201510270823.0A patent/CN104828796A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992284A (en) * | 2012-12-12 | 2013-03-27 | 贵州开磷（集团）有限责任公司 | High-magnesium phosphorite de-magging method with by-product magnesium ammonium phosphate |
| CN103303884A (en) * | 2013-05-27 | 2013-09-18 | 瓮福（集团）有限责任公司 | Method for treating phosphorus concentrates and recovering phosphorus by using phosphogypsum slag dump pool water |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112191361A (en) * | 2020-09-27 | 2021-01-08 | 湖北祥云(集团)化工股份有限公司 | Method and production system for preparing powdered ammonium and high-quality ammonium phosphate by phosphorite classification |
| CN112374477A (en) * | 2020-11-16 | 2021-02-19 | 贵州开磷集团矿肥有限责任公司 | Production method of 68% DAP |
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Application publication date: 20150812 |